USOO5955040A

United States Patent (19) 11 Patent Number: 5,955,040

Bunger et al. (45) Date of Patent: Sep. 21, 1999
54 INTEGRATED APPARATUS AND PROCESS 56) References Cited
FOR HIGH RECOVERY OF ACETYLENE
FROM THE REACTION OF CALCUM U.S. PATENT DOCUMENTS
CARBIDE WITH WATER
5,082,644 1/1992 Bunger et al. .......................... 423/497
75 Inventors: James W. Bunger; Christopher P. 5,284,630 2/1994 Bunger et al. .......................... 422/189
Russell, both of Salt Lake City; Jerald
W. Wiser, Kaysville; Jesse C. Tsai,
Salt Lake City, all of Utah Primary Examiner Hien Tran
Attorney, Agent, Or Firm-James L. Sonntag
73 Assignee: James W. Bunger and Associates, 57 ABSTRACT
Inc., Salt Lake City, Utah
An apparatus for the manufacture of acetylene and hydrated
21 Appl. No.: 08/880,933 lime from the reaction of calcium carbide and an excess of
1-1. water is disclosed. A primary reactor for the initial reaction
22 Filed: Jun. 23, 1997 of the calcium carbide and water is disposed concentrically
51 Int. Cl." ......................................................... B01J 8/00 within a Secondary reactor. Hydrated lime and unreacted
52 U.S. Cl. .............................. 422/189: 422/188; 4.8/38; calcium carbide flow directly from the primary reactor to the
48/57; 48/216 Secondary reactor, where the carbide lime Settles from the
58 Field of Search ............................ 422/181, 188-189, Water and is removed.
422/193; 48/38, 57, 216; 209/158; 423/497,
636 16 Claims, 10 Drawing Sheets

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U.S. Patent Sep. 21, 1999 Sheet 5 of 10 5,955,040

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U.S. Patent Sep. 21, 1999 Sheet 6 of 10 5,955,040

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U.S. Patent Sep. 21, 1999 Sheet 7 of 10 5,955,040

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INTEGRATED APPARATUS AND PROCESS all, commercially practiced wet acetylene processes
FOR HIGH RECOVERY OF ACETYLENE approximate the CFSTR configuration.
FROM THE REACTION OF CALCUM In the CFSTR there is unreacted carbide that is mixed
CARBIDE WITH WATER throughout the reactor. The particle size of the unreacted
carbide varies from larger, recently introduced particles to
RELATED APPLICATIONS Smaller leSS-recently introduced particles that are nearing the
completion of reaction. In an ideal CFSTR Some of these
(Not applicable) Smaller unreacted particles will be discharged with the
hydrated lime slurry. Any acetylene generated by a particle
STATEMENT REGARDING FEDERALLY after it has been discharged from the reactor may be lost to
SPONSORED RESEARCH OR DEVELOPMENT the atmosphere. The premature discharge of unreacted par
(Not applicable) ticles is referred to as “breakthrough” and, if the reaction
kinetics are known, the extent to which breakthrough occurs
FIELD OF THE INVENTION can be estimated through calculations about an ideal
CFSTR.
15
This invention relates to an apparatus, control, and pro Practical evidence as well as theoretical calculations of
ceSS for the production of acetylene and hydrated lime by the CFSTR kinetics shows that this breakthrough can be sig
reaction of calcium carbide with water. nificant. While the actual amount of breakthrough is affected
by the particle size of the carbide feed, the hydrodynamic
BACKGROUND OF THE INVENTION behavior of a carbide particle reacting to form acetylene, the
In a typical wet proceSS for manufacture of acetylene from internal configuration of the reactor and the inherent reac
calcium carbide, particles of calcium carbide are introduced tivity of the calcium carbide, the amount of breakthrough
to an excess of water in a reactor vessel on a continuous or increases as the Space Velocity of the reactor increases.
Semi-continuous (on/off) basis. Water is added continuously Space Velocity is defined conventionally as the number of
to the reactor and acetylene and a hydrated carbide lime 25
reactor Volumes displaced in one hour.
Slurry are withdrawn from the reactor on a continuous basis. FIG. 1 is a graph showing the mathematical relationship
A System is provided for Stirring the contents of the reactor between the Space Velocity and breakthrough, assuming
to mix the calcium carbide with the water and to maintain a ideal behavior and relying on published data for CFSTR
more-or-less uniform slurry of hydrated carbide lime. kinetics. For reactors of Space Velocities equaling four or
Because the reaction of calcium carbide with water is greater (4000 liter/hr. in FIG. 1), the ideal conversion is
exothermic, the temperature must be controlled, typically by about 96% or less, which means that the breakthrough losses
the rate at which fresh water is added. A greater rate of water are greater than 4% of the acetylene that is produced from
addition results in cooler temperatures and a lesser rate of a given carbide feed. Most commercial reactors in operation
water addition results in warmer temperatures. today operate at a Space velocity greater than four, which
35
means that the breakthrough losses are even greater.
There are Several undesirable characteristics of the pro Dissolution Losses
ceSS of the prior art. These in Summary are: Another problem with traditional technologies is the
1. Some acetylene yield is lost through the premature losses of acetylene to dissolution in water. FIG. 2 shows the
discharge of unreacted calcium carbide. Solubility of acetylene in water as a function of temperature
2. Some acetylene yield is lost through the solubility of 40
for three commonly operated preSSures. It may reasonably
acetylene in the large Volume of water passing through be assumed that the water of the hydrated lime discharge
the reactor. Slurry is Saturated in acetylene, and unless this water is
3. Operational difficulties occur due to large, Solid inert recycled to the System, all of the acetylene dissolved in the
particles that enter the System and interfere with the water will eventually be lost to the atmosphere. The amount
Stirring mechanism and discharge pumpS and valves. 45
of acetylene contained in the discharge hydrated lime slurry
4. The Overall process efficiency is reduced because a low can be calculated by knowing the amount of water exiting
concentration of hydrated lime in the discharge Stream the reactor and its outlet temperature and pressure. Even if
results in low contact times in the reactor and poor use Some of the water is recycled to the reactor the open vessels
of the reactor Space. which Serve as Settling tanks to thicken the hydrated lime are
exposed to the atmosphere and a large portion of the
5. The hydrated carbide lime value is reduced due to the 50
acetylene So dissolved is lost.
presence of granular impurities and variable hydrated To illustrate, if pure calcium carbide (MW=64) is reacted
lime concentrations.
These characteristics are described further as follows: to form acetylene (MW=26) with enough water to result in
Discharge of Unreacted Carbide (breakthrough) a 5% hydrated lime (MW=74) slurry, the amount of water
In a typical reactor configuration the reaction kinetics are 55
flowing from the outlet per Kg of acetylene produced will
be:
approximated by a Constant Flow Stirred Tank Reactor
(CFSTR). According to Levenspiel, Chemical Reaction
Engineering, 2nd Edition, John Wiley and Sons, Inc. 1972, (1 - .05) 0.05:26 = 54 Kg-WaterfKg-Acetylene
Chapter 5, page 97. “one type of ideal steady-state flow
reactor is called the mixed reactor, the backmix reactor, the 60
ideal stirred tank reactor, or the CFSTR (constant flow Assuming that the outlet temperature is 50° C. and the
Stirred tank reactor) and, as the name Suggests, it is a reactor reactor pressure is 0.3 atm-gauge (a typical set of
in which the contents are well Stirred and uniform through conditions), the amount of acetylene contained in 54 Kg of
out. Thus the exit stream from this reactor has the same water is 0.09% or 0.05 Kg. Thus about 5% of the acetylene
composition as the fluid within the reactor. We refer to this 65 generated is lost to the atmosphere through the dissolution in
type of flow as mixed flow, and the corresponding reactor, water. This loSS is in addition to the acetylene lost as a result
the mixed reactor, or the mixed flow reactor.” Most, if not of breakthrough of unreacted particles.
 5,955,040
3 4
Operational Difficulties Objects of the Invention
Another problem with conventional technologies pertains An object of the present invention is to reduce the
to the operational difficulties created when non-reactive aforementioned problems of a) loss of acetylene due to
materials are introduced along with the calcium carbide. breakthrough, b) loss of acetylene due to Solubility, c)
These unreactive materials, which are present in all com operational difficulties due to inert materials, d) loss of
mercially available calcium carbide materials, usually com process efficiency due to low hydrated lime concentrations,
prise inert coke, Solid ferrosilicate and other metallic or and e) loss of hydrated lime value due to particulates and
mineral particles. These are materials introduced with the low, or variable, hydrated lime concentrations.
limestone or coke fed to the furnaces that manufacture It is also an object of the present invention to provide an
apparatus and a process for reacting calcium carbide with
calcium carbide and are carried through to the final product. water that provides a high level of recovery of the acetylene
These inert materials accumulate in the reactor and if not produced.
removed will eventually interfere with the stirring mecha It is also an object of the invention to improve the level
nism and discharge pumps or valves, causing mechanical of recovery of acetylene in the reaction of calcium carbide
breakdown. Smaller particles that do not rapidly Settle are with water by reducing or eliminating breakthrough and
carried through to the Settling tanks where they may 15
minimizing the acetylene dissolved in the water discharge
accumulate, causing difficulties with the discharge System. Stream.
Loss of Process Efficiency It is also an object of the invention to provide an apparatus
Another problem of traditional Systems is that the con and a process which allows for high completion of reaction
centration of hydrated lime in the reactor is kept low, usually and low breakthrough of calcium carbide in a given reactor
below about 10 weight percent, to reduce premature Settling Space.
of hydrated lime, i.e., to keep the Slurry of the hydrated lime It is also an object of the invention to provide an apparatus
precipitate in a free-flowing State. If allowed to Settle the and process which provides low loSSes due to dissolution of
hydrated lime would result in plugging of discharge lines or acetylene.
create unmanageable accumulations of hydrated lime in the 25 It is also an object of the invention to provide an apparatus
reactor, or both. Low hydrated lime concentrations also and a proceSS which Segregates large particles from Small
result from the manner in which temperature is controlled. particles thereby improving the operability of the proceSS
In a typical process, temperature is controlled at 50 C. If the and the value of the co-produced hydrated carbide lime.
temperature begins to rise, the usual procedure is to increase It is also an object of the invention to provide an apparatus
the rate of water feed, which brings down the temperature, and a process which improves the process efficiency by
but also has the undesirable result of further diluting the improved utilization of reactor Space.
hydrated lime output Stream. In hot weather, where heat It is also an object of the invention to provide an apparatus
losses to the environment are reduced, and for very large and a proceSS which provides for control functions which
Systems, the hydrated lime concentration in the output allow for flexible acetylene output while maintaining a
Stream can fall to as little as 3 weight percent. 35 Steady-state hydrated lime concentration and constant tem
The operational requirement for low concentrations of perature.
hydrated lime requires larger reactors for a given Space rate It is also an object of the invention to provide control of
or a higher space rate for a given reactor size. Larger reactors the pressure of the apparatus while allowing variable acety
require greater capital costs. Higher space rates result in lene production and Steady-State concentration of hydrated
greater breakthrough. Low hydrated lime concentrations 40 lime and constant temperature.
also result in a greater per unit water throughput increasing It is also an object of the invention to provide a process
the losses due to solubility. The combined losses due to these control Strategy which provides for maintaining the pre
effects are typically 8 to 12%, which means that only 88 to ferred temperature and hydrated lime concentration condi
92% of the acetylene produced by a given calcium carbide tions while varying acetylene output.
is recovered. Finally, the resulting hydrated lime discharge 45 It is also an object of the invention to provide an
Stream must be sent to larger holding vessels in order to acetylene/calcium hydroxide production process in which
provide adequate residence time for the hydrated lime to the calcium hydroxide product is uniform in quality (particle
thicken for Subsequent use or disposal. These vessels occupy size, purity and concentration).
more land and require the need for additional capital invest It is also an object of the invention to provide an apparatus
ment. 50 and proceSS in which the hydrated lime product can be
Loss of Calcium Hydroxide Product Value recovered from the reactor at high Ca(OH)2 concentrations.
Particulate impurities contained in the calcium carbide are It is also an object of the invention to provide an apparatus
carried into the hydrated lime product unless they are filtered and process which minimizes the requirements for internal
out at Some expense and operational effort. These Small moving parts and as a consequence Simplifies the construc
particle impurities may adversely affect the value of the 55
tion and operation of the apparatus.
hydrated lime for downstream utilization. In general, the It is also an object of the invention to provide an apparatus
value of hydrated lime improves if the granular impurities and process which minimizes the number and size of ports,
are reduced in both size and quantity. The value of hydrated external fittings, and moving Seals through the preSSure
lime also improves with concentration and with consistency vessel, and as a consequence simplifies the construction and
in concentration. Most downstream uses require the trans 60
improves the overall Safety and operability of the apparatus
portation of the hydrated lime and the greater the and process.
concentration, the more Ca(OH) is transported per ton of Further objects of the invention will become evident in
Slurry. In commercial practice of the prior-art, little if the description below.
anything is done to Segregate Small particle impurities. In BRIEF SUMMARY OF THE INVENTION
addition, processes to increase the concentration of the 65 Overview
hydrated lime are separate from the reactor and add addi The present invention is an improvement of the apparatus
tional capital and operating costs. and process disclosed in U.S. Pat. Nos. 5,082,644 and
 5,955,040
S 6
5,284,630 to Bunger et al. (Bunger et al.), which are hereby no element of fluid overtaking or mixing with any other
incorporated by reference. The Bunger et al. System com element ahead or behind. Actually, there may be lateral
prises two Successive reaction Steps. In the first Step par mixing of fluid in a plug flow reactor; however, there must
ticulate calcium carbide is charged into an entrained or be no mixing or diffusion along the flow path. The necessary
ebulated flow primary reactor containing water. The water and Sufficient condition for plug flow is for the residence
in the primary reactor is directed upward to ebulate calcium time in the reactor to be the same for all elements of fluid.”
carbide particles. The calcium carbide particles react with The majority of the reaction occurs in the primary reactor
the water until their size becomes Small enough to become ebulated bed reaction system (essentially CFSTR), and is
entrained and carried upward in the upward flow of water. then transferred to a plug-flow reaction System in the Sec
These particles of unreacted calcium carbide and the Solid ondary reactor. The plug-flow reaction environment in the
calcium hydroxide reaction product entrained in the upward Secondary reactor allows for Substantial completion of the
water flow are conveyed through a conduit to a Separate reaction of calcium carbide with water. The advantage of
Secondary reactor to complete the reaction of the calcium any plug flow reactor is that a reaction can be completed in
carbide particles under plug flow conditions. The calcium the Smallest possible reactor Space. Further, there is no
hydroxide produced in the primary and Secondary reactors is 15 mixing of unreacted materials with that element in the
allowed to Settle in the Secondary reactor and is recovered. reaction System which has completed its reaction.
Acetylene gas generated in both reactors is drawn off above Acetylene is drawn off as it is generated in the primary
either or both reactors. and Secondary reactors. Calcium hydroxide formed by the
The Bunger et al. reaction System is continuous. The reaction is separated in the Secondary reactor by Settling and
calcium carbide feed can be metered in a controlled manner is removed from the dense Zone at the bottom of the
into the reaction System. The calcium hydroxide is typically Secondary reactor.
much purer than that produced by conventional acetylene A Suspension of unreacted calcium carbide particles and
processes, because the entrained flow in the primary reactor calcium hydroxide is transferred between the primary reac
Serves to effectively Separate out particulate impurities intro tor and the Secondary reactor over a concentric overflow
duced with the calcium carbide, Such as oversized coke and 25 Weir at the periphery of the primary reactor. Since the
mineral impurities, which are usually are not entrained and Suspension flows directly from the primary reactor into the
carried into the Secondary reactor. Thus, the calcium hydrox Secondary reactor, the need of any croSS-Over piping is
ide product has a higher market value and can be used as a eliminated. With no cross-over piping the possibility of
feedstock for the production of high-value calcium deriva plugging of a pipe and the heat loSS from the Surface of the
tives. piping is eliminated. The two-stage, Single vessel reaction
Apparatus and Process of the Present Invention System is also mechanically simpler, and thus less expensive
The present invention utilizes the same dual reaction to build and maintain. In the Secondary reactor itself no
System as the Bunger et al. System. However, in the present mechanical mechanism is required, Such as rakes. However,
invention, the entrained flow primary reactor is positioned it is contemplated to use Such rakes if desired. The internal
within the Secondary reactor, preferably in a concentric 35 placement of the primary reactor within the Secondary
manner with the axis of the two reactors coinciding. Thus, reactor permits a much Smaller footprint than Separate
the present invention has the same advantages as the Bunger placement of the two reactors.
et al. System. However, the placement of the primary reactor Another advantage is that only one pressure vessel need
within the Secondary reactor materially increases the control be built. The walls of the primary reactor are only required
over the reaction, eases construction and reduces costs, 40 to Separate it from the Secondary reactor. Since there is
augments the efficiencies of the System, and improves the Virtually no pressure differential between the reactors, the
product purity. construction of the primary reactor may be of light-weight
The apparatus of the present invention is a Single-Vessel, design. The pressurization for the entire reaction System is
two-stage reactor System for producing acetylene by reac maintained by the Outer walls of the reaction vessel, requir
tion of calcium carbide and water. In the first or primary 45 ing construction and certification of only one preSSure
reactor, calcium carbide is continuously charged into an vessel.
ebulated and entrained flow reaction environment contain The concentric internal placement of the primary and
ing an excess of water. The primary reactor is disposed Secondary reactorS allows a common header at the top of the
concentrically within Secondary reactor, Such that the Sec preSSure containment vessel to be used for gas collection for
ondary reactor Surrounds the primary reactor in an annular 50 both the primary and Secondary reactors. The result is a
fashion. The unreacted water with unreacted calcium car Significant overall reduction in gas Volume in the reaction
bide and calcium hydroxide product from the primary reac System, as compared to Separating the two reaction Systems
tor flows over an overflow (e.g., weir or ports) at the into Separate pressure vessels. This increases the Volume
perimeter of the primary reactor directly into the Secondary available for reaction, and increases Safety by decreasing the
reactor. The Secondary reactor is configured as a dense 55 Volume for potential adverse and undesirable reactions.
phase, laminar plug-flow reactor where calcium hydroxide Control of the Process
product is allowed to settle and is removed from the bottom Temperature
of the reactor. Most of the calcium hydroxide settles, but a The concentric construction of the primary reactor within
minor portion may remain in Suspension in the water, that is the Secondary reactor allows for an unprecedented control of
withdrawn from the secondary reactor over an overflow weir 60 the process, measurably greater than in conventional Sys
and recycled to the primary reactor. tems and the dual reactor Bunger et al. System. Since the
According to Levenspiel (1972), “the other of the two primary reactor is contained within the Secondary reactor,
ideal Steady-State flow reactorS is variously known as the there is a much lower heat loSS from the primary reactor as
plug flow, Slug flow, piston flow, ideal tubular, and unmixed compared to a separated reactor construction as disclosed in
flow reactor, ... We refer to it as the plug flow reactor and 65 the Bunger et al. patent. Most of the heat of reaction is
to this pattern of flow as plug flow. It is characterized by the generated in the primary reactor, and instead of losing heat
fact that the flow of fluid through the reactor is orderly with to the external environment, it is insulated from the external
 5,955,040
7 8
Surfaces of the reactor vessel by the Surrounding Secondary concentration of the hydrated lime is high, that dictates that
reactor. Thus, heat leaves the primary reactor mainly by the absolute amount of excess water used in the System is
Vapor generation, by reactant/product flow into the Second lower. The lower amount of water reduces the amount of
ary reactor and through the wall Separating the reactors. water that is available for dissolving acetylene. AS indicated
Thus, the Secondary reactor can be maintained at a higher above, a significant loSS of acetylene is due to acetylene
temperature to decrease acetylene Solubility. Temperature becoming dissolved in the exceSS Water that passes out of the
control of the primary reactor is eased, Since the Secondary System. Reducing the water in the System by increasing the
reactor is usually at a higher temperature than the external hydrated lime concentration materially reduces these losses.
environment and heat lost from the primary reactor out Another advantage of the reduction of water flow through
through the primary reactor walls to the Secondary reactor is the System is that the Space Velocity is reduced for the same
minimized since the Secondary reactor temperature differs Size reactor, which reduces the possibility of breakthrough,
Slightly from that of the primary reactor. i.e., calcium carbide being carried through and out with the
Basically, the present System allows for retention and water/lime output. By the practice of the invention, with its
reduction of dissolved acetylene and the Significant reduc
recovery of much of the reaction heat produced in the tion in breakthrough, theoretical calculations show that 99
primary reactor where most of the heat from the calcium 15 percent, or more, of the acetylene available from the calcium
carbide/water reaction is produced. The lower heat loSS carbide feed can be recovered.
allows for better temperature control in the primary reactor Another advantage of the reduction of water flow through
and operation at a higher reaction temperature. The Second the System is that the reactor Size can be reduced for the
ary reactor may also be operated at a higher temperature, Same Space Velocity. This reduces the size of the reactor and
because of the higher temperature of the primary reactor and as a result reduces the capital costs. The use of a plug-flow
heat added from the primary reactor. The higher reaction reactor regime results in a more effective use of the available
temperature is favorable as it lowers the solubility of acety space than for CFSTR reactors. Total internal volumes of
lene in water, reducing the reservoir of unrecoverable acety less than /3 of conventional reactor Volumes are possible
lene dissolved in the water in the reaction System and without an increase in breakthrough.
allowing it to be recovered as the desired product gas. 25 Another advantage of reducing the water input is that the
The process temperature may be conveniently controlled heat loSS from the System through the water is reduced. A
by adjusting the loSS of heat to the Surroundings. Because of Substantial amount of the heat is lost from the System
the concentric, heat conserving dual reactor design, tem through the heated excess water leaving the System. This
perature is conveniently controlled by conserving the heat limits the operating temperature of the System. By reducing
generated in the System, if a higher temperature is required, the amount of water passing through the System the oper
or dissipating heat to the environment, if cooling is desired. ating temperature can be increased, which reduces the losses
Heat conservation may be accomplished, for example, by from acetylene dissolved in water since the solubility of
heat exchanging the Slurry output with the water inlet. acetylene is reduced.
Dissipating heat to the environment or may be A high lime-concentration Slurry can be handled in the
accomplished, by cooling the water recycled between the 35 present invention because of the higher quality of the
Secondary reactor and the primary reactor. This means of hydrated lime product. In conventional practice there is no
temperature control is a significant departure from conven classification and Separation of Solid impurities. Thus, if the
tional practice which uses the water input as a means of hydrated lime product were removed in a Settled, thickened
temperature control. Making temperature control indepen state from the bottom of a conventional CFSTR reactor, it
dent of the water input flow rate allows for independent 40 would contain significant amounts of “rocks', which would
adjustment of the water input flow rate to maintain a create Severe operational problems. Accordingly, the
predetermined hydrated lime Slurry concentration. hydrated lime is removed in conventional Systems as a
Control of Hydrated Lime Product Concentration free-flowing Suspended slurry, and the rocks that Settle are
By practice of the present invention, the concentration of periodically removed from the bottom of the reactor by a
Ca(OH) in the hydrated lime slurry removed from the 45 Separate means. In contrast, in the present invention these
System can be set at essentially any convenient impurities are removed in the primary reactor entrainment
concentration, even at high concentrations wherein the System, leaving the Slurry in the Secondary reactor essen
hydrated lime is settled and in the form of a semisolid slurry. tially free thereof. Operationally, this allows slurry removal
In principle, the hydrated lime concentration can be as high through a simple metering pump, throttling valve, or other
as desired, and is limited in practice only be its flow 50 appropriate means. Thus, the rate of removal of the hydrated
characteristics. This contrasts with conventional Systems lime, and hence the hydrated lime concentration in the
which require operation in a regime of an agitated free water/lime slurry and the amount of water throughput, can
flowing and dilute liquid slurry for the removal of the slurry. easily be controlled. Basically, the only upper limitation to
In the present invention, there is a Secondary reactor in the concentration of the hydrated lime in the slurry is the
which the hydrated lime is allowed to settle into a thickened 55 Viscous effects that occur when the concentrations of the
Slurry that is free of particulate impurities that would Seri hydrated lime exceeds about 40 wt.%.
ously interfere with its easy removal from the reactor. BRIEF DESCRIPTION OF THE DRAWINGS
The hydrated lime Slurry, by the present process, can be
produced at a consistent composition, i.e., with a consistent FIG. 1 is a graph showing conversion of calcium carbide
water concentration. This consistency of composition along 60 and breakthrough in a prior-art continuous stirred tank
with the removal of impurities in the entrainment System, reaction System.
results in a purer, higher-value product. FIG. 2 is a graph showing the Solubility of acetylene in
The high concentration of hydrated lime and its corre Water.
sponding lower concentration of water allows for many FIG. 3 is a cross-section of a reactor system of the
advantages. The absolute amount of hydrated lime produced 65 invention.
is Set by the acetylene demand, because it is Stoichiometri FIG. 4 is a Schematic of an apparatus of the invention
cally related to the amount of acetylene produced. If the incorporating a reactor as in FIG. 3.
 5,955,040
9 10
FIG. 5 is a schematic showing a preferred material control convenient distribution method. The top inlet port 120 may
method of the invention. optionally include SprayerS as shown.
FIG. 6 is a Schematic showing an alternate material The primary reactor 109 is sized to be sufficiently small
control method. in diameter as to provide maximum Settling time in the upper
FIG. 7 is a Schematic showing a temperature control part of the Secondary reactor and to minimize the mass flow
method. rate of the recycle Stream needed to ebulate the reactor bed.
FIG. 8 is a graph showing the percent of acetylene Conversely, the primary reactor is sized to be Sufficiently
produced which is lost through Solubility as a function of large in diameter So that the reactor operates in a bubble
hydrated lime concentration. flow regime and not a Slug-flow regime. The height of the
FIG. 9 is a graph describing the kinetics of the reaction of primary reactor is sized So as to contain a Sufficient Volume
calcium carbide with water, showing conversion parameter for controlled reaction of the instantaneous Steady-state
V. time. inventory of calcium carbide, but not So large that Space is
FIG. 10 is a graph showing Settling Velocity of calcium inefficiently used.
hydroxide with respect to calcium hydroxide concentration The baffle 106 is sized large enough to reduce the down
in terms of weight percent.
15 ward Velocity of the liquid Overflowing the primary reactor
wall but Small enough to provide long residence time in the
DETAILED DESCRIPTION OF THE rising portion 112 of the Secondary reactor 121. The annulus
INVENTION between the weir wall 102 and the main reactor vessel wall
Apparatus is sized to be Sufficiently large to accommodate the flow of
Reference is made to FIGS. 3 and 4, which illustrate an recycle water, but not So large that it reduces the available
apparatus of the invention. The apparatus is comprised of a space needed for the baffle 106 or the primary reactor 109.
main reactor vessel 101 designed to withstand internal In the illustrated design, the only internal movable part is
operating pressures according to regulatory Standards. the Screen, and this part only moves occasionally during
Within the cylindrical portion of the reactor walls is fitted a cleaning. Thus the only moving Seal in the preSSure vessel is
cylindrical weir wall 102 which top provides a circular weir 25 that required for the Screen axis, which is not required to
103 over which water/slurry may flow. At the bottom of the operate during normal operation of the System. This con
weir wall and between the weir wall and the reactor wall is trasts with conventional CFSTR designs that have many
fitted a plate 104 at such an angle to the horizontal so that penetrations of the pressure vessel with moving Seals, Such
water/slurry will be directed to the low point of the plate as for rakes, grates, etc., which function continuously
105. through the process. In addition, the mechanical energy for
Between the weir wall 102 and a primary reactor 109 is the process of the present invention is Supplied by an
fitted a baffle 106 which top elevation 107 exceeds the top external pump 142 that drives the recycle Stream, which
elevation 110 of the primary reactor 109 and which bottom requires no drive shafts penetrating the reactor vessels. The
elevation 108 extends below the elevation of the circular reduction of moving Seals in the preSSure vessel materially
weir 103. The top elevation 110 of the primary reactor 109 35 Simplifies the mechanics and increases the reliability of the
is intermediate between the top elevation of the circular weir System.
102 and the top elevation 107 of the baffle 106. The baffle Process
106 is used to direct the flow of Ca(OH) and unreacted In the process of the invention calcium carbide is intro
calcium carbide in a downward direction toward the Sec duced to the primary reactor 109 by any suitable calcium
ondary reactor plug-flow reaction Zone 111 and to provide a 40 carbide feeding means 141 through the calcium carbide feed
quiescent environment Settling of Ca(OH) into a dense Zone port 117. The calcium carbide reacts with water in the
125. primary reactor 109. The water is recycled by pump 142
The primary reactor 109 may be fitted with a rotatable from the Secondary reactor 121 through a water recycle pipe
screen 113 (shown in FIG. 3 in its vertical, discharge 143, and introduced to the primary reactor from the bottom
position and in FIG. 4 in its operating horizontal position) in 45 through the Velocity control restrictor 114 to create a reac
the bottom portion or bottom elevation of the primary tion in an ebulated environment with water flowing up
reactor 109 which supports the bed of calcium carbide. This through Solid particles. Large particles Settle to the level of
screen 113 may be rotated about a horizontal axis to allow the screen 113 where they react until they become small
for discharge of any unreactive material that has been enough to become entrained by the upward Velocity of water
retained on the screen 113. 50 in the primary reactor 109 when they are carried over into
Below the primary reactor is fitted a velocity control the secondary reactor 121. Particles of impurities settle
restrictor 114 which supplies water/slurry to the primary through the Screen or are periodically discharged (by rotat
entrained flow primary reactor 109 and allows for discharge ing the screen 113) and allowed to settle through the velocity
of unreactive particles. The velocity control restrictor 114 control restrictor into a holding tank 147 fitted at the bottom.
originates in a disengagement Zone and holding tank or Zone 55 The Screen is rather coarse, e.g., about 10 mm or coarser, So
147 which allows for separation of inert particles from the that only large particles are retained on the Screen. The
Slurry recycle. holding tank 147 is periodically emptied through a discharge
The plug-flow reaction Zone 111 of the Secondary reactor port 129.
121 is configured as a simple cone 115 which angle 116 is Small particles of unreacted carbide, Ca(OH) and inert
greater than the angle of repose of Settled hydrated lime. 60 materials are carried over the top 110 of the primary reactor
Alternatively, the cone may be fitted with a slow-moving 109 after which they flow downward by the force of gravity
rake (not shown). into the annular space 122 between the primary reactor 109
The top of the reactor is fitted with a port 117 for and the baffle 106. The downward momentum of the fluid
introducing calcium carbide, a port 118 for discharge of and its entrained particles passing over the primary reactor
acetylene and appropriate over pressure relief devices 119. 65 wall 110 so that the particles drop to the elevation of the
Make-up water is introduced to the System at a top water water, (as determined by the elevation of the circular weir
inlet port 120 and is introduced to the vapor Space by any 103) assures that the particles are completely Submerged in
 5,955,040
11 12
water, thereby reducing or eliminating the accumulation of charged by means of a metering valve 205. The rate at which
dry particles on the Surface that may occur when feeding hydrated lime slurry is discharged may be a fixed ratio of the
calcium carbide of Small particle size. calcium carbide fed, thereby establishing a fixed concentra
Calcium hydroxide and any unreacted calcium carbide are tion of slurry.
allowed to travel downward between the annular space 122 An optional density/mass flow meter 209 provides infor
between the primary reactor and the baffle, where they begin mation to the controller about the actual flow rate and
to settle into the dense Zone 125 of the secondary reactor. A density of the slurry. Information regarding the density of
portion of the slurry travels under the lower elevation 108 of the slurry may be used for fine tuning of the metering valve
baffle 106 and rises in the space for the rising portion 112 of 205.
the secondary reactor 121 between the weir wall and the Fresh water is added through water inlet ports 120 to
baffle where it overflows the top of the weir wall. Water/ maintain the liquid inventory at a constant level in the
slurry overflowing this weir wall is drained to the lowest reactor system. The reactor system is fitted with a level
point 105 where it exits the reactor vessel and is recycled detection device 211 of any convenient design. An electronic
through line 143 to the bottom of the velocity control differential pressure device is one Such means and this
restrictor. 15 device monitors the level of fluid in the weir annulus 171. A
The material introduced through the recycle line 143 to Signal from the level detection device is Sent to a controller
the bottom of the primary reactor 109 through the velocity 213 which controls the flow of fresh water by means of a
control restrictor 114 Serves as the mixer in the primary throttling valve 215. If the level of fluid falls below a
reaction, creating the flow of water necessary for the ebul predetermined level, the level controller 213 farther opens
lated reaction environment, and the classification of particles the throttling valve 215 to direct water through. Conversely,
in the velocity control restrictor 114. The recycle rate also if the level of fluid rises above a predetermined level the
affects the hydrodynamic behavior in the primary reactor level controller 213 further closes the metering valve 215 to
109 and the upper portion of the secondary reactor 121 and restrict the flow of water through 120. The level of water in
provides a means for distributing heat from the primary the weir annulus 171 is thus maintained at a level preestab
reactor to the Secondary reactor. While the recycle is pri 25 lished by the desired set-point on the level detection device
marily used to recycle water, the material in the recycle loop 211.
may include in addition to water, Suspended Solids Such as In the process of the invention the rate of water addition
calcium hydroxide, and other Solids. Using any appropriate is controlled to maintain a steady inventory of fluid in the
Screening apparatus 123, the recycle loop may serve the System and is a consequence of control of other process
purposes of Screening from the System any lighter-than variables. Combined with a steady-state flow of calcium
water debris that may inadvertently be introduced to the carbide to the reactor this allows for a steady-state concen
System, Since Such debris will be retained in the loop. tration of Slurry from the reactor. By prescribing the desired
Below the lower elevation 108 of the baffle 106 and the concentration of the outlet slurry the rate of discharge can be
top 124 of the cone the hydrodynamic behavior undergoes a precisely adjusted to achieve that concentration and the
transition to a condition approximated by Plug Flow Reac 35 remainder of the flow parameters, Specifically the water
tion (PFR) kinetics, which has been defined above. For first flow, are automatically adjusted accordingly.
order chemical reactions the ideal PFR is the only reactor An alternative mass flow control Strategy is shown in FIG.
which, in theory, will allow for (very nearly) complete 6. In the alternative strategy the carbide feed rate means 303
reaction within a finite reaction Space. Thus, the apparatus of is controlled by a controller 301 sensing downstream
the invention provides a reaction environment in the lower 40 demand, as before. An optional flow measuring device 307
portion of the Secondary reactor which approximates that of is used to measure the production rate and may be used to
a PFR and as a result, in theory, allows for virtually complete fine tune the control.
reaction and as a consequence, the almost total elimination In the alternative Strategy, a predetermined flow rate of
of breakthrough. water is established based on the anticipated amount for
Settled and concentrated calcium hydroxide is discharged 45 reaction losses, humidity losses and free water desired in the
from the bottom of the cone through line 128 to a hydrated slurry. An optional flow meter 306 is used to provide
lime containment area. In the process of the invention the information to the controller 305 as to the actual flows.
reaction is performed under conditions which maximize the In the alternative strategy the inventory of fluid within the
concentration of Slurry. The Segregation of large particulates reactor is detected by a level detection device 312 and set to
in the primary reactor allows for thickening and Settling in 50 a prescribed level in the weir annulus 371. The level is
the Secondary reactor without concern for operational dif influenced by the rate of discharge of hydrated lime slurry
ficulties that occur with CFSTR reactors. This allows for controlled by a device 309 controlling the hydrated lime
convenient operation of a throttling valve in the exit Stream slurry outlet valve 311.
that can operate at any convenient pressure. Temperature Control
Control 55 Temperature is controlled by adjusting the heat losses to
Mass Flow Control the environment. If it is required to recover heat, as would
The preferred mass flow control strategy is shown in FIG. occur for lower concentrations of hydrated lime, colder feed
5. The downstream demand for acetylene dictates all other water or a colder environment, heat can be recovered at
process flows. The downstream demand is Sensed by the either of two convenient points. These are the hot acetylene
process control 201 which controls a calcium carbide feed 60 gas and the slurry outlet Stream. Heat recovered from either
ing means 203. An optional flow measurements device 207 of these Streams can be reintroduced into the fresh water
is used to measure acetylene production rate and may feed by a feed/effluent heat exchanger 151 or 153 shown in
provide information to Supplement the downstream demand phantom in FIG. 4 (or in FIG. 7 showing recovery from the
information. slurry effluent). Water heated from the hydrated lime slurry
The same information used to control the carbide feed rate 65 effluent in 153 may be introduced directly into the reactors
is sent to the hydrated lime slurry valve controller 204 which as in FIG. 4, or as in FIG. 7, mixed with unheated water
controls the rate at which the hydrated lime slurry is dis through a mixing valve 181, which is controlled by a
 5,955,040
13 14
controller 183 that monitors the temperature of the primary preSSure have a significant influence on the concentration of
reactor by temperature sensor 185. acetylene dissolved in the outlet water. The solubility of
For highly concentrated calcium hydroxide outlet Streams acetylene in water as a function of temperature and pressure
with a correspondingly lower water throughput or for is given in FIG. 2, which shows the solubility at various
warmer feed water temperatures or warmer environments, pressures gauge (1 atm ambient pressure). The graph shows
the operating temperature may rise above regulatory limits that the lowest Solubility occurs at high temperatures and
if a means of cooling is not provided. Under these low pressures. In the preferred mode of operation, the
reaction between calcium carbide and water is carried out at
circumstances, the temperature is maintained below regula the highest temperatures allowed by regulation and the
tory limits by a controlled release of heat to the environment. lowest pressure acceptable as an inlet preSSure for the
This can be accomplished by lowering or eliminating the downstream apparatus. Following this principal, it would be
heat recovery at exchangers 151 and 153. Heat may also be desirable, from a thermodynamic point of view, to operate
released to the environment by cooling the recycle Stream by the System at pressures below atmospheric (vacuum) and
a suitable heat exchanger 155. (See FIGS. 4 and 7.) such operation is within the spirit of the invention. Practical
The preferred temperature control Strategy is shown in problems with potential ingreSS of air and regulatory Stan
FIG. 7. The desired temperature is sensed 185 in the primary 15 dards may limit the actual pressure conditions of the process
reactor and a Set point is Selected, not to exceed regulatory to Something greater than atmospheric pressure, preferably
limits. The controller 183 controls the proportion of fresh 0.02 bar or greater.
process water 154 which passes through a feed/effluent heat In the process of the invention the loss of acetylene due
eXchanger 153 and that which does not pass through the heat to Solubility in the discharge water is due to two factors, the
eXchanger. This temperature control loop is operational amount of acetylene dissolved in a unit of water (or other
whenever the desired temperature is higher than the oper wise retained in the slurry output) and the number of units
ating temperature. of water discharged per unit of acetylene produced.
When the operating temperature is higher than the desired Simple mass balance calculations show that the number of
temperature, the System may be cooled by withdrawing heat units of water discharged per unit of acetylene generated is
from the recycle loop or water reycle pipe 143 by means of 25 directly reflected in the concentration of hydrated lime in the
a heat exchanger 155 cooled by cooling water 156. A outlet. FIG. 8 illustrates the percent of the acetylene manu
controller 184 controls the rate at which cooling water 156 factured which is lost through solubility as a function of
passes through the heat eXchanger 155 by means of a hydrated lime concentration operating at three typical pres
throttling valve 157. Sures and at thermally adiabatic conditions and for a calcium
In effect, temperature is controlled by conserving or carbide feed that is 80% CaC and 20% CaO (a typical
dissipating heat between the reactor and its Surroundings. composition). AS Seen from the graph, as the hydrated lime
The strategy allows for control of temperature without concentration increases, the lost acetylene decreases.
Accordingly, preferred operating conditions are at higher
having to influence any of the process flow rates. hydrated lime concentrations, at lower pressures, and higher
Specifically, maintaining a constant System temperature temperatures. Using mathematical modeling, an acetylene
does not require adjustments in any of the process flow rates, 35
recovery of 97.2% can be achieved at secondary reactor
even when the carbide feed rate varies or when there are temperature of 70° C., a pressure of 1.3 bar, and 14 wt.%
uncontrolled temperature effects (changes in fresh water hydrated lime concentration. This recovery can be increased
temperature, changes in the temperature of ambient to 99.8% by a secondary reactor temperature of 90° C., and
Surroundings, etc.). Thus, the process of the invention pro a pressure of 0.05 bar, and a hydrated lime concentration of
vides for unusually Steady-State operation in all major pro 40 40 wt.%. In Summary, to achieve an acetylene recovery
ceSS Variables. Most importantly, a steady-State of calcium greater than 97%, the process of the invention is operated at
hydroxide outlet concentration can be achieved and a a Secondary reactor temperature above 70° C., a pressure
Steady-state operating temperature is maintained even when between 0.02 and 1.3 bar gauge, and a hydrated lime
the rate of acetylene and calcium hydroxide production is concentration between 14 and 40 wt.%.
varied. 45 Rate and Thermal Effects
This uncoupling of the temperature control and mass flow Details of the invention are further understood in view of
rate control is a significant departure from the prior art in the rate and thermal effects.
which temperature and mass flow rates are highly coupled. Rate Effects
By uncoupling the two requirements, both temperature and Reaction Kinetics-Reaction kinetics refer to the rate of
mass flow rates can be independently controlled for opti 50
reaction of calcium carbide with water. This rate depends on
mum performance without the need to compromise one or the Starting Size of calcium carbide particles, pH of water,
the other. but not much on temperature or pressure. Rates may also
Safety Control vary in unknown ways with carbide Sources from differing
Appropriate Safety devices are designed to shut down the calcium carbide manufacturing processes.
System in the event of over- or under-filling, for over 55 FIG. 9 illustrates the kinetics of calcium carbide reaction
temperature, for over-pressure, or for loss of fresh water or with water. Here the conversion parameter (S) is defined as;
recycle flow. Additionally precautions are taken against
under-pressure that may occur when a low pressure opera C2H2
tion is shut down and cooled. All customary engineering
precautions are taken to ensure Safe operation in the event of 60
1-1 (CaC2)
partial or total failure of electrical or mechanical compo
nentS. where CH is the amount of acetylene evolved at time (t)
Preferred Process Conditions and (CH) is the total amount of acetylene that can be
In the process of the of the invention, calcium carbide is evolved. Defining a conversion parameter is this fashion is
fed to the primary reactor and the reaction is allowed to 65 a way of linearizing the rate of evolution of acetylene from
proceed under temperature and pressure conditions which a three-dimensional shrinking calcium carbide particle as it
maximize the recovery of acetylene. Both temperature and reacts with water.
 5,955,040
15 16
As shown from the graph of FIG.9, which is derived from 3. The size of particle allowed to settle in the velocity
actual data, the reaction is initially quite rapid as shown by control restrictor increases.
the Steep slope of the line. This is following by a regime 4. The rise rate of water between the baffle and the weir
exhibiting much slower reaction kinetics. The present inven wall increases reducing the Settling of Ca(OH) and
tion utilizes the two reactor design to exploit this kinetic thereby increases the concentration of slurry in the
behavior. In the primary reactor, the initial rapid reaction recycle loop.
Stage takes place, along with a rapid generation of heat. The
reacting of the particle in the slower regime does not occur 5. The size of unreacted particles that might Settle in the
until after the particle has been Substantially reduced in size Velocity control restrictor is increased.
and has been carried into the Secondary reactor. The Sec 6. Consumption of electrical energy is increased.
ondary reactor has a long residence time. Because most of Conversely, a lower recycle rate has the following effects:
the reactor Space is used to perform this Secondary reaction 1. The ebullation effect in the primary reactor is decreased
and because a plug flow reaction regime is maintained, the and the size of the particle entrained is decreased.
calcium carbide particles can become fully reacted, in Spite
of the fact that their reaction rate is slow when they are in 2. The temperature rise in the primary reactor increases,
the Second reaction regime. 15 placing an upper temperature limit on how hot the
Settling Velocity-This rate effect addresses settling recycle Stream can be.
Velocity of carbide particles, calcium hydroxide particles 3. The Segregation of particles between the Secondary
and inert impurities in the original carbide. The Settling reactor and the primary reactor results in a cleaner
Velocity depends on particle size, density of the particles, hydrated lime product.
density of the fluid, and viscosity of the fluid. In the case of 4. The rise rate between the baffle and the weir wall is
calcium hydroxide, the Settling rate also depends on the decreased leading to Settling and lower concentrations
Settling effects in a slurry, which are highly complex and not of hydrated lime in the recycle Streams.
easily described mathematically. The larger the particle, the
more important are the bulk Slurry properties, the Smaller the 5. The downward velocity between the primary reactor
particle, the more important are the Surrounding fluid prop 25 and the baffle is decreased, resulting in decreased
erties. Particle size may be influenced by the carbide manu mixing in the Secondary reactor plug-flow regime.
facturing process. Particulates of alumina have significant 6. Consumption of electrical energy is decreased.
effects of Settling Velocities because they create hydrates The optimum recycle rate will be one which properly
which interfere with Settling at the microscopic and molecu classifies particles between the primary reactor and Second
lar level. FIG. 10 is an illustration of the settling velocity of ary reactor, which allows for consistent temperature control
Ca(OH) versus the weight fraction in the slurry. As shown with an acceptable, higher Slurry outlet temperatures, and
from the graph, the Settling Velocity decreases as the weight which allows for an acceptable rate of settling of Ca(OH)
fraction increases, which indicates the difficulty of achieving particles in Secondary reactor. In general, the recycle rate
high concentrations of hydrated lime by gravity Settling should be the lowest that will allow for acceptable tempera
from dilute hydrated lime Suspensions of the prior-art. 35 ture control.
However, in the present invention, where concentrations of Thermal Effects
hydrated lime are maintained at high values at all times, long Heats of Reaction-This thermal effect considers the heat
Settling times are not needed to obtain a product of high released by reaction of calcium carbide with water and by
concentration. reaction of calcium oxide with water, coupled with the rates
Preferably the hydrated lime concentration in the process 40 of these reactions. The first effect from heat released by
of the invention is 14 wt.% or higher. The withdrawal rate reaction of calcium carbide with water is discussed above.
for withdrawing the slurry is preferably at a ratio of the rate The second effect from hydration from calcium oxide is
to the mass flow rate of the calcium carbide feed less than taken to be instantaneous and all the heat generated is
8, more preferably less than 5. considered liberated in the primary reactor, although in
Mass Flow Rates-This rate effect considers the rate at 45 practice a Small amount may be carried to the Secondary
which water and carbide (CaC, CaO, impurities) enter the reactor before hydrating.
reactor, the rate at which acetylene and calcium hydroxide In adiabatic Steady-state operation of the process of the
are produced by the reactions and the rate at which calcium invention the energy balance equation can be written as:
hydroxide and water are discharged from the reactor. The
input and output rates are dictated by Stoichiometric rela 50
accumulation=in-out+generation
tionships and desired slurry concentration. The overall mass where, at Steady-state,
balance for varying operating conditions are discussed in accumulation=0
further detail below.
The mass flow rate also includes the rate of recycle even in=sensible heat of carbide feed and water
though this rate does not affect the Overall mass balance. 55 out-sensible heat of slurry and enthalpy of the humid
Unless heat is deliberately removed from the recycle stream, acetylene Stream
the recycle rate also has little influence on the overall energy generation=heat of reactions
balance. However, the rate of recycle is highly important to Combining the energy and mass balances allows for math
Several operational parameters. AS recycle rate is increased, ematical modeling for the process performance at differing
the following occur: 60 Steady-state conditions. The interrelationship of proceSS
1. The ebulation effect in the primary reactor is increased variables is demonstrated in Tables I to VI, for 25 mi/hour
and the size of particles entrained in the vertical flows acetylene at a primary reactor temperature of 90° C., feeding
increases. an 80% purity CaC. The tables provide data for water inlet
2. The temperature rise from the bottom to the top or the temperatures of 20° C. and 40 C. and system pressures of
primary reactor decreases, allowing the temperature in 65 0.05, 0.3 and 1.3 bar gauge. The data in these tables
Secondary reactor to be higher without exceeding regul quantitatively illustrate the relationship of process variables
latory temperatures in the primary reactor. for an adiabatic System in which no heat is consumed or
 5,955,040
17 18
dissipated. AS Stated elsewhere, for lower concentrations of bility of acetylene falls to Zero as the water reaches its
hydrated lime it is desirable to conserve heat to reduce the boiling point at the prevailing pressure and dissolved Solids
acetylene losses. For concentrations higher than those conditions. In any case, the temperature does not exceed the
shown in Tables I to VI, cooling will be required. For such regulatory limits Set by Safety regulations.
cases and for a constant Secondary reaction temperature the In general, the temperature of the System is increased by
lost acetylene is directly proportional to the amount of free lowering heat losses from the reactor and is decreased by
water discharged with the hydrated lime slurry. increasing heat losses from the reactor. LOSSes from the
Heat Transfer-This thermal effect considers free con reactor occur from three principal Sources 1) the enthalpy of
vective heat transfer, forced convective heat transfer and the hydrated lime slurry outlet stream, 2) the enthalpy of the
conductive heat transfer through Solid barriers. All these humid acetylene outlet Stream, and 3) conductive and con
combine in appropriate ways to provide energy flows from vective heat losses to the ambient Surroundings. Theoretical
the primary reactor to the Secondary reactor, from the calculations Show that for typical conditions the greatest
Secondary reactor to the Surroundings and from the recycle heat losses occur with item 1) and the least with item3), with
loop to the Surroundings. item 2) being intermediate to 1) and 3).
Temperature is most directly increased by decreasing the
Equilibrium-This thermal effect considerS phase equi 15 flow of the hydrated lime slurry outlet Stream (by increasing
libria of three species in the System that depend on tem the hydrated lime concentration). Once the desired mass
peratures: the Solubility of calcium hydroxide in water, the flow rates and Slurry concentration have been Set, a desirable
Vapor pressure of water above the liquid in the reactor and means of temperature control is to regulate the amount of
the solubility of acetylene in the liquid in the reactor. All of heat losses, and to do So without interfering with the desired
these depend on temperature and the latter one depends on mass flows. This can be accomplished by varying the
System preSSure as well. amount of heat transferred from the outlet streams to the
Process Controls of the Invention inlet Streams. A convenient way to do this would be, for
Mass flow rate, liquid level, preSSure, and temperatures example, to preheat the inlet water using the Sensible heat of
are monitored and appropriate actions are taken regarding the hydrated lime slurry outflow. Alternately, the sensible
carbide input, water input, recycle rate, hydrated lime out 25 heat of the acetylene Stream can be used to preheat the inlet
flow and Splitting ratioS to heat transfer units. This is guided water. If cooling is required, heat may be lost to the
by Safety, production and economic considerations. environment by cooling the recycle Stream.
Flow Rates- There are two input flows, two output flows, Overall Control Strategy
and one internal flow stream. The choice of the internal flow The control System described above is particularly advan
rates depends on hydrodynamic factors that are described tageous where the acetylene demand is variable. In most
above. The input flow of calcium carbide is dictated by the acetylene production Systems, the downstream demand for
output demand for acetylene. The input flow of water is acetylene can vary widely. The acetylene production is
dictated by the desired output Ca(OH) slurry concentration. increased or decreased by Varying the input of calcium
Therefore, the two output Streams, acetylene and hydrated carbide. The desired Ca(OH) concentration can be main
lime slurry, dictate the control over the two inlet Streams, 35 tained at a constant level by increasing or decreasing the
calcium carbide and water, respectively. Table VII shows the slurry out flow to correspond with the calcium carbide
relationship of these Streams for differing acetylene outputs in-flow. Make-up water for reactions, and losses to humidity
in an adiabatic System. and Slurry outflow is accurately adjusted by maintaining a
Liquid Level The total liquid inventory in the reactor is constant liquid inventory. Temperature is controlled by
conveniently and accurately controlled by monitoring the 40 varying the heat conserved from or dissipated to the envi
liquid level in the annulus between the weir wall 102 and the rOnment.
outer wall 101 and by using this information to control the In an adiabatic System, dissipation to the environment is
flow of water entering the system (see FIG. 5, the preferred usually needed for slurry concentrations above about 20% to
method). Alternatively, this same information could be used maintain the preferred temperature condition. However, for
to control the slurry outflow from the Secondary reactor (See 45 a non-adiabatic System, the isothermal condition, where no
FIG. 6, the alternative method). heat conservation or dissipation is required, will be a little
Pressure-System pressure may be controlled by any higher because of uncontrolled heat losses. For practical
convenient means. Establishing the gas delivery pressure Systems where there are variable heat losses to the environ
establishes the other System pressure requirements Such as ment (Summer VS. winter temperature difference) or where
Slurry outlet, carbide feed, and minimum water feed pres 50 the recycle rate is fixed and where there are uncontrolled
Sure. Generally, a lower pressure is preferred, as the Solu convective and conductive heat losses to the environment,
bility of acetylene in water is lower at lower pressures than the energy and mass balance equations Suggest that the
at higher pressures. The lowest practical limit is about 0.02 natural isothermal conditions occur at about 20-24%. Solids
bar gauge. If the delivery System requires a higher pressure, in the hydrated time slurry and for reactor pressure of 0.05
the operating temperature may by increased, within regula 55 bar gauge, and feed water temperatures of about 20 C. To
tory limits, to partly compensate for the higher Solubility of achieve preferred temperature conditions for hydrated lime
acetylene in water at higher pressures. LOSSes due to higher Slurries below this concentration, heat may need to be
Solubility may also be reduced by increasing the hydrated conserved. For concentrations higher than this level, heat
lime concentration in the lime slurry outlet. Higher pressures may need to be dissipated.
are often desired in captive acetylene Systems to avoid 60 The temperature control strategy is illustrated in FIG. 7,
downstream compressors, e.g., where the acetylene is which is more fully describe elsewhere and which shows
required at higher pressures for direct use or as a feedstock how the System can be operated with constant temperature
for another process. conditions and constant hydrated lime slurry composition
Temperature-Preferably, the temperature is as high as under varying acetylene demand.
allowed by regulatory Standards, which typically limit the 65 Illustrations of Controlled Conditions
maximum temperature to between 80 C. and 90° C. Fun Tables VIII and IX show for a differing acetylene output
damental thermodynamic considerations Show that the Solu Stream were the recycle Stream is kept constant and the
 5,955,040
19 20
temperature in controlling by controlling heat transfer to the The process of the invention maintains high recovery of
environment. Heat transfer to the environment is controlled acetylene by operating at high temperatures and high slurry
either 1) by conserving heat by heating the water in Stream concentrations even when demand for acetylene production
with the exit hydrated lime stream, which is shown in the is varied.
table by a water-in temperature greater than 20°C., or 2) by
cooling the recycle Stream as shown by a positive value for
recycle heat loSS. While this invention has been described with reference to
Table VII is for a calcium hydroxide concentration of 17 certain Specific embodiments and examples, it will be rec
wt.% with a variable recycle Stream but constant Secondary ognized by those skilled in the art that many variations are
reactor temperature. Table IX is for a calcium hydroxide
concentration of 35 wt.%. In the latter, heat losses to the possible without departing from the Scope and Spirit of this
environment through the exit hydrated lime Stream are invention, and that the invention, as described by the claims,
insufficient to maintain the temperature low enough, So is intended to cover all changes and modifications of the
cooling is required for the recycle Stream at all of the invention which do not depart from the spirit of the inven
acetylene demands shown. In Table VII, at the lower acety 15 tion. It will be recognized that the proceSS conditions dis
lene demands, heat must be conserved to keep the tempera closed herein may not comply with local regulatory
ture from falling below 90° C.
Design for Optimum Efficiency Standards, and that in practice of the invention compliance
Dimensions-Diameters and wall thickness of vessels are with all regulatory Standards in effect must be made.
Specified as well as diameters and wall thicknesses for
piping. Also heights of vessels and lengths of piping are TABLE I
Specified, along with any accessory Structures Such as
gratings, weirs, etc. These decisions are guided by mass and FOR A PRESSURE OF O.OS BAR GAUGE
energy flows and restraints regarding temperatures and 25 mi/hr. ACETYLENE PRODUCTION AND
AT REACTOR TEMPERATURE OF 90° C.
preSSures. The intents and purposes of the dimensions are
discussed above. FIG. 3 is approximately to Scale for System 25
Carbide Ca(OH),
of a capacity of about 25 to 50 cubic meters acetylene per Fresh Water Re- Recycle Temper- Lime In C.H. In
hour and shows a pressure vessel 1.2 meters in diameter. (t = 20° C. cycle Rate ature Out Outlet Outlet
Breakthrough-From previous considerations of reaction in Kg/hr) Ratio (Kg/hr) Out ( C.) (Kg/Hr) (%) (Kg/hr)
rates and Settling Velocities, the amount of unreacted cal
cium carbide leaving the Secondary reactor with the 350 18.OO 63OO 86.5 383.OO 26.50 O.O79
hydrated lime slurry is calculated. Ideally the Secondary 400
450
11.25
7.55
4400
3398
84.4
82.O
437.50
491.50
23.19
2O.O2
O.106
O.136
reactor is sized So as to eliminate breakthrough. A larger 514 4.97 2555 78.7 562.78 18.00 O.183
Secondary reactor decreases or eliminates breakthrough but 540 4.41 2381 77.2 587.59 17.24 O.2O1
adds to the cost of construction and the Space required. In 550 4.19 2305 76.7 598.11 16.94 O.209
general, as long as the primary reactor is large enough to be 35 560 3.98 2229 76.1 608.77 16.64 0.217
operated in the bubble-flow regime, breakthrough will be 570 3.8O 2166 75.5 619.20 16.36 0.225
negligible for any practical Secondary reactor that can be 6OO 3.30 1980 73.9 650.68 15.57 O.250
constructed around the primary reactor. 650 2.69 1749 71.1 702.8O 14.41 O.292
Dissolved Acetvlene-From previous considerations of 700
8OO
2.25
1.67
1576
1334
68.5
63.7
754.54
857.26
13.43
11.82
O.336
O.425
acetylene Solubility and mass balance, the amount of dis 40
900 1.31 1177 59.6 959.31 10.56 0.517
Solved acetylene leaving the Secondary reactor with the 1OOO 1.07 1070 56.1 106096 9.55 O.609
hydrated lime Slurry is determined by the process 11OO O.9 990 53.1 1162.37 8.71 O.701
conditions, namely temperatures, pressure and hydrated
lime slurry concentration. Process conditions are optimized
according to these considerations. 45
Space Utilization-This design issue assesses how much TABLE II
the acetylene production rate can be enhanced without FOR A PRESSURE OF O.OS BAR GAUGE
increasing the Volume of the reactor. Differing reactor con 25 mi/hr. ACETYLENE PRODUCTION AND
figurations and process conditions will lead to differing AT REACTOR TEMPERATURE OF 90° C.
utilization of available reactor Space. In general, if more than 50
95% of the reaction is carried out in the primary reactor, then Carbide Ca(OH),
a high Space utilization will be achieved. Fresh Water Re- Recycle Temper- Lime In C.H. In
(t = 40 C. cycle Rate ature Out Outlet Outlet
Summary in Kg/hr) Ratio (Kg/hr) Out ( C.) (Kg/Hr) (%) (Kg/hr)
In Summary, the apparatus of the invention allows for a
526 13.49 7098 86.7 562.85 18.00 O.122
high level of control over mass flow and temperature and 55
610 6.84 4174 83.8 651.07 15.56 O.176
preSSure in a dual reactor System, reducing the reactor Space 650 5.50 3577 82.5 692.92 14.62 O.2O2
required to achieve a prescribed level of conversion, easing 670 S.OO 3353 81.8 713.81 1419 O.215
the fabrication requirements, providing a high level of 690 4.58 3162 81.2 734.68 13.79 O.228
recovery of acetylene produced and producing a more 730
750
3.90
3.65
2847
2738
79.9
79.3
776.29
797.12
13.05
12.71
O.256
O.269
consistent and easily managed hydrated lime slurry. 60
8OO 3.10 248O 77.9 849.03 11.93 O303
The control of the invention independently maintains 850 2.68 2278 76.5 900.73 11.25 O.338
constant Slurry concentrations and reactor temperature, even 900 2.35 2115 75.1 952.24 10.64 O.374
950 2.08 1976 73.8 10O3.6O 10.09 O.410
when acetylene demand is varied or when ambient 1OOO 1.87 1870 72.6 1054.83 9.60 O448
temperatures, feed water temperatures or other temperature 1OSO 1.69 1772 71.4 1105.95 9.16 O.485
effects are varied. The control of the invention allows for 65 11OO 1.54 1692 70.3 1156.98 8.76 O.523
operation at preferred temperature and slurry concentrations
even when the pressure is varied.
 5,955,040
21 22
TABLE III TABLE VI
FOR A PRESSURE OF 13 BAR GAUGE
FOR A PRESSURE OF O.3 BAR GAUGE
25 mi/hr. ACETYLENE PRODUCTION AND
25 mi/hr. ACETYLENE PRODUCTION ON AND AT REACTOR TEMPERATURE OF 90° C.
AT REACTOR TEMPERATURE OF 90° C.
Carbide Ca(OH),
Fresh Water Re- Recycle Temper- Lime In C.H. In
Carbide Ca(OH), (t = 40 C. cycle Rate ature Out Outlet Outlet
Fresh Water Re- Recycle Temper- Lime In C.H. In in Kg/hr) Ratio (Kg/hr) Out ( C.) (Kg/Hr) (%) (Kg/hr)
(t = 20° C. cycle Rate ature Out Outlet Outlet 700 32.OO 224OO 88.5 748.15 13.54 O.67
in Kg/hr) Ratio (Kg/hr) Out ( C.) (Kg/Hr) (%) (Kg/hr) 750 11.5O 86.25 86.0 798.90 12.68 O.76
8OO 6.90 552O 83.7 849.83 11.92 O.84
450 13.50 6075 85.3 494.2O 20.51 O.18 15 850 4.90 4165 81.6 900.44 11.25 O.93
510 7.36 3754 81.7 553.55 18.3 O.23 900 3.78 34O2 79.6 951.17 10.65 1.01
950 3.08. 2926 77.7 1OO1.98 10.11 1.10
550 5.4O 2970 79.2 595.53 17.01 0.27 1OOO 2.58 258O 76.1 1051.92 9.63 1.19
570 4.74 27O2 77.9 616.18 16.44 O.29 1OSO 2.23 2342 745 1102.29 9.19 1.27
6OO 3.97 2.382 76.O 647.28 15.65 O.33 11OO 1.96 2156 73.1 1152.45 8.79 1.36
650 3.09 2009 72.9 698.62 14.50 O.38
700 2.5O 1750 7O.O 749.81 13.51 O.43
8OO 1.78 1424 64.8 851.26 11.90 0.55 TABLE VII
900 1.38 1239 60.4 952.07 10.64 O.66 25 ADIABATIC OPERATION FOR A PRESSURE OF O.3 BAR GAUGE
PRIMARY REACTOR TEMPERATURE 90° C.
SECONDARY REACTOR TEMPERATURE 79.2 °C.
INPUT WATER 20° C.
TABLE IV TOTAL REACTOR VOLUME 1.3 m
EXIT LIME STREAM CONCENTRATION 17 WT.9%
FOR A PRESSURE OF O.3 BAR GAUGE
25 mi/hr. ACETYLENE PRODUCTION AND Acetylene Calcium Water Lime Lost
AT REACTOR TEMPERATURE OF 90° C. Demand Carbide. In In Recycle Out Acetylene
(m/hr) (Kg/hr) (Kg/hr) (Kg/hr) (Kg/hr) (Kg/hr)
Carbide Ca(OH), 50 178.4 1100 5940 1192. O.54
Fresh Water Re- Recycle Temper- Lime In C.H. In 45 160.56 990 5346 1072.8 O.486
(t = 40 C. cycle Rate ature Out Outlet Outlet 35
40 142.72 88O 4752 953.6 O.432
in Kg/hr) Ratio (Kg/hr) Out ( C.) (Kg/Hr) (%) (Kg/hr) 35 124.88 770 4158 834.4 O.39
3O 107.04 660 3564 715.2 O.32
6OO 14.5O 87OO 86.8 642.2O 15.75 O.24
25 89.2 550 2970 596 0.27
650 8.98 5837 85.1 695.74 14.56 0.27
2O 71.36 440 2376 476.8 O.22
700 6.36 4452 83.3 748.15 13.54 O.32
15 53.52 330 1782 357.6 O16
750 4.84 3630 81.5 80016 1266 O.36 40 1O 35.68 22O 11.88 238.4 O.11
8OO 3.88 3104 79.8 851.98 11.89 O.40
850 3.2O 272O 78.2 902.85 1122 O.45
900 2.73 2457 76.6 954.76 10.61 O.SO
950 2.35 2233 75.1 7005.96 1O.O7 O.54
1OOO 2.07 2070 73.7 1056.31 9.59 0.59 TABLE VIII
1OSO 1.84 1932 72.4 1108.32 9.14 O.64 45 ADABATC OPERATION EXCEPT HEATING OF INPUT
11OO 1.66 1826 71.2 1158.77 8.74 O.69
STREAMS BY EXIT LIME STREAM OR COOLING OF
RECYCLE STREAMBY COOLING WATER
RECYCLE STREAM 4000 Kg/hr
TOTAL REACTOR VOLUME 1.3 m
TABLE V PRIMARY REACTOR TEMPERATURE 90° C.
50 PRESSURE O.3 BAR GAUGE
FOR A PRESSURE OF 13 BAR GAUGE EXIT LIME STREAM CONCENTION 17 WT.9%
25 mi/hr. ACETYLENE PRODUCTION AND
AT REACTOR TEMPERATURE OF 90° C. Cal
cium Re
Carbide Ca(OH), Car cycle Temp
Fresh Water Re- Recycle Temper- Lime In C.H. In 55 Acety- bide Heat Lost erature
(t = 20° C. cycle Rate ature Out Outlet Outlet lene in Water Water Loss Lime Acety Sec.
in Kg/hr) Ratio (Kg/hr) Out ( C.) (Kg/Hr) (%) (Kg/hr) Demand (Kg? In In (Kcal/ Out lene Reactor
(m/hr) hr) (Kg/hr) ( C.) hr) (Kg/hr) (Kg/hr) ( C.)
540 11.10 5994 84.3 593.79 17.04 0.55
550 10.2O 561O 83.8 599.76 1689 O.56 50 178.4 11OO 2O.OO 20960 1192. O.54 79.20
560 8.8O 4928 82.9 610.24 16.60 O.58 45 160.5 990 2O.OO 1452O 1072.8 O.486 79.20
60
570 7.70 4389 82.1 62O.33 16.33 O.60 40 1427 88O 2O.OO 812O 953.6 O.432 79.20
585 6.56 3838 80.8 635.91 15.93 O.63 35 1249 770 2O.OO 1720 834.4 O.378 79.20
6OO 5.65 3390 79.6 651.03 15.56 O.66 3O 107.0 660 23.OO O 715.2 O.316 80.62
650 3.88 2522 75.7 703:47 14.40 0.75 25 89.2 550 26.40 596 O.249 82.48
700 2.94 2058 72.3 752.60 13.46 O.85 2O 71.4 440 29.86 476.8 O.185 84.27
8OO 1.96 1568 66.3 853.41 11.87 1.04 15 53.5 330 33.50 357.6 O.125 86.04
900 1.47 132O 61.5 955.66 10.60 1.24 65 1O 35.7 22O 37.31 238.4 O.069 87.78
 5,955,040
23 24
4. An apparatus as in claim 1 wherein the makeup water
TABLE IX inlet is constructed to introduce fresh makeup water directly
ADIABATC OPERATION EXCEPT COOLING OF
into the primary reactor not through the Velocity control flow
RECYCLE STREAMBY COOLING WATER
restrictor.
RECYCLE STREAM 4000 Kg/hr 5. An apparatus as in claim 1 additionally comprising a
TOTAL REACTOR VOLUME 1.3 m Screen disposed above the Velocity control flow restrictor
PRIMARY REACTOR TEMPERATURE 90° C. sized to prevent large particles from prematurely descending
PRESSURE O.3 BAR GAUGE
EXIT LIME STREAM CONCENTRATION 35 WT.9%
through the Velocity restrictor.
6. An apparatus as in claim 1 wherein the overflow
Cal comprises a weir over which water with entrained hydrated
cium
Car-
Re
cycle Temp
lime and calcium carbide particles flow from the primary
Acety- bide Heat Lost erature reactor to the Secondary reactor.
lene in Water Water Loss Lime Acety- Sec. 7. The apparatus of claim 1 wherein the secondary water
Demand (Kg? In In (Kcal/ Out lene Reactor output comprises a weir over which water leaving the
(m/hr) hr) (Kg/hr) ( C.) hr) (Kg/hr) (Kg/hr) (C.) 15 Secondary reactor flows and which maintains a predeter
50 178.4 477.O 2O.OO 423OO 582.5 O.236 73.06 mined liquid level in the Secondary reactor.
45 160.5 431.0 2O.OO 367OO 524.3 O.204 75.05 8. The apparatus of claim 7 wherein the primary and the
40 142.7 384.O 2O.OO 31OOO 465.4 O.174 76.90 Secondary reactor are enclosed within a common preSSure
35
3O
124.9
107.O
338.0
291.O
2O.OO
2O.OO
255OO
204OO
4O7.6
349.1
O.146
O.119
78.81
80.63
vessel capable of being pressurized.
25 89.2 244.O 2O.OO 157OO 291.O O.O94 82.40 9. The apparatus of claim 8 wherein an annulus is formed
2O 71.4 197.O 2O.OO 114OO 233.3 O.O72 84.17 between the Secondary reactor and the preSSure vessel and
15 53.5 148.5 2O.OO 77OO 1746 O.O51 85.72 water flowing over the weir flows into the annulus.
1O 35.7 10O.O 2O.OO 447O 116.6 O.O32 87.33 10. The apparatus of claim 9 additionally comprising a
controller for maintaining the water level in the annulus at
What is claimed is: 25 or above a predetermined level.
1. An apparatus for the production of acetylene and 11. An apparatus for the production of acetylene and
hydrated lime by the reaction of water with calcium carbide hydrated lime by the reaction of calcium carbide particles
particles comprising; with an exceSS of water comprising,
a primary reactor constructed for upward flow of water a primary reactor for initial reaction of the calcium
and with an upward water velocity control flow restric carbide particles with water,
tor disposed to direct the upward flow of water in the
primary reactor, the restrictor constructed and sized to a Secondary reactor sized and configured for reaction of
allow impurities denser than hydrated lime produced by essentially all of the calcium carbide particles that is
reaction of water and calcium carbide particles in the not reacted in the primary reactor and such that the
primary reactor to Settle into a holding Zone, and to hydrated lime produced in the primary and Secondary
entrain and carry upwards calcium carbide particles of 35 reactorS Settles into a dense Zone in bottom of the
less than a predetermined size and hydrated lime up and Secondary reactor,
over an overflow at a periphery of the primary reactor, the primary reactor concentrically disposed within the
water inlet for introducing water into the primary reactor Secondary reactor Such that water with entrained cal
for upward flow through the velocity control restrictor, cium carbide particles and hydrated lime from the
makeup water inlet for introducing makeup water into the 40 primary reactor flows directly into the Secondary reac
primary reactor, tor via an overflow at a periphery of the primary
feeder for introducing calcium carbide into the top of the reactor,
primary reactor, a hydrated lime output for withdrawing hydrated lime
Secondary reactor concentrically disposed around the pri from the dense Zone.
mary reactor Such that water with calcium carbide 45 12. An apparatus as in claim 11 wherein the primary
particles and hydrated lime from primary reactor flow reactor is constructed and configured to provide a reaction
ing over the overflow flow directly into the secondary environment where unreactive particles are allowed to Settle,
reactor, the Secondary reactor constructed and dimen and unreacted calcium carbide particles and hydrated lime
Sioned to provide essentially plug-flow reaction of produced by the reaction of water and calcium carbide
water with calcium carbide particles and to allow the 50 particles are entrained and carried to the Secondary reactor.
hydrated lime produced in the primary and Secondary 13. An apparatus as in claim 11 wherein the primary and
reactors to Settle into a dense Zone at the bottom of the
Secondary reactor, the Secondary reactor are enclosed within a common pres
acetylene output for withdrawing acetylene produced in the Sure vessel capable of being preSSurized.
14. An apparatus as in claim 11 additionally comprising a
primary and Secondary reactors, hydrated lime output for water recycle conduit for directing water form the Secondary
55
withdrawing hydrated lime that has settled in the dense Zone reactor to the primary reactor.
from the dense Zone of the Secondary reactor, 15. An apparatus as in claim 12 wherein the overflow of
Secondary water output for withdrawing water from the the primary reactor comprises a weir over which the water
Secondary reactor from a region in the Secondary with entrained calcium carbide particles and hydrated lime
reactor not in the dense Zone, from the primary reactor flows directly in the Secondary
60 reactOr.
recycle conduit directing from the Secondary water output
to the water inlet of primary reactor. 16. An apparatus as in claim 12 wherein the reaction
2. An apparatus as in claim 1 wherein the primary reactor environment is provided by an entrained flow water System
and the Secondary reactor are enclosed within a common with a water flow restrictor constructed to direct a flow of
vessel capable of being pressurized. water up through the primary reactor to create the entrained
3. An apparatus as in claim 1 wherein the makeup water 65 flow.
inlet is constructed to introduce fresh makeup water into the
upward velocity control flow restrictor.