Patented June 11, 1940 2,204,113

UNITED STATES PATENT OFFICE

2,204,113
CALCUM SILICATE AND METHOD OF
PREPARNG THE SAME
Raymond P. Allen, Akron, Ohio, assignor to The
B. F. Goodrich Company, New York, N. Y., a
corporation of New York
No Drawing. Application September 30, 1937,
serial No. 166,698
Claims. (C. 23-0)
This invention relates to a method of making some of the product may exist as Ca(OH)2.3SiO2.
hydrous calcium silicate, and has as its object to 2H2O.
provide a finely divided, easily friable, pure In the practice of my invention, the reactants
product. are preferably added to the reaction mixture
In the preparation of calcium silicate from a slowly and simultaneously. One very satisfactory
water-Soluble silicate and a water-soluble calcium method is to introduce one reactant at the top
Salt, many difficulties have been encountered. and the other reactant near the bottom of the
When sodium silicate and calcium chloride, for reaction vessel. The rate of addition may be
instance, are reacted in water solution in such a varied over wide limits, different rates being
manner that the concentration of reactants varies preferable for best results with different concen O
appreciably throughout the solution, there is a trations of reactants. Since it is necessary to
tendency to precipitate large amounts of Sodium minimize high local concentrations of either re
chloride with the calcium silicate thereby form actant, the stirring must be very thorough.
ing a grainy impure product. Furthermore, it is Propeller-type blades have a tendency merely to
very difficult to obtain pure calcium silicate from cut through the slurry without stirring it, so I 15
this impure product because the Sodium chloride prefer to use a paddle-type stirrer comprising a
is precipitated with the calcium silicate in such central shaft having a series of radially extending
a way that Ordinary washing methods are in blades, the plane of each blade being coaxial with
sufficient to remove the salt. A pure, smooth, the shaft. The reaction vessel may be heated if
20 finely-divided precipitate may be obtained by desired, but it is an advantage of my invention 20
that it is unnecessary to heat the reaction mix
using less concentrated reactants, but when the . ture
product is filtered, the cake dries to a hard, diff to obtain satisfactory products.
cultly friable mass. Largely because of these may The soluble silicate employed in the reaction
be either a commercial or technical grade of
25 difficulties, calcium silicate, although it imparts sodium or potassium silicate in concentrated or 25
desirable properties to rubber when compounded dilute aqueous solution. When I employ sodium
therewith, has never found wide commercial use silicate, which is cheaper and more readily avail
as a pigment in the rubber industry or otherwise.
I have discovered that by reacting a soluble able, I prefer to use a product in which the molal
ratio of SiO2 to NazO is at least 3:1. The calcium
silicate and a calcium halide in an aqueous salt is always Supplied to the reaction mixture in 30
medium in which high local concentrations of the form of a Water Solution.
either of the reactants are prevented, I am able In the preferred method of practicing my in
to precipitate pure, finely-divided calcium silicate vention, use a reaction vessel fitted with a
which may be filtered and dried to produce an suitable stirring device and containing openings
easily friable, chalky cake. To maintain as uni at the top and bottom for the admission of water 35
form a concentration as possible of reactants glass and calcium chloride solution respectively.
throughout the reaction medium, Isimultaneously When using a 110 gallon tank, I put 39 gals. of
introduce aqueous solutions of silicates and cal water therein. I use as reactants calcium chlo
cium halides into a reaction vessel, and I provide ride which contains on the average 21.2% of
the reaction vessel with a stirring means which water and Water glass which has a specific gravity 40
will rapidly mix the reactants. By this method of about 1.40 gms./c. c., a molal ratio of SiO2 to
of maintaining a uniform concentration of re Na2O of about 3.25:1, and contains on the average
actants, I am able to produce calcium silicate of 61.3% of water. I dissolve 36 lbs. Of the calcium
uniformly Small particle size. While ordinary chloride in water to make 15 gals. and dilute 11
46 methods of precipitation produce calcium silicate gals, of water glass with water to make 40 gals. 45
whose particle size may be as great as 30 microns, Islowly and continuously add the solutions to the
the diameter of most of the particles produced reaction vessel, the time consumed in the addition
by the method of my invention is about 0.3 being about 25 minutes. The aqueous slurry,
micron. which has been thoroughly stirred while the re
50 The product which I obtain is one which, to actants were being added, is then diluted with SO
nly knowledge, has never before been prepared. twice its volume of water and filtered on an Oliver
A typical analysis shows SiO2 62.0%, CaO 19.5%. filter running at about A. R. P. M. The cake is
and H2O 18.5%. The product, therefore, has a washed on the filter with a slow trickle of water,
molal ratio of 1 mol of CaO to 3 mols of SiO2. removed from the filter, and dried. The product
SS Its formula is probably CaO.3SiO2.3H2O, though is an easily friable, chalky cake which is easily SS
 2 2,204,113
ground fine enough to pass a 100 mesh screen. taneously instilling, with stirring, separate aque
Its specific gravity is 2.1. Ous solutions of calcium chloride and of Sodium
The calcium silicate prepared by the method of silicate having a molal ratio of silicon dioxide to
my invention is an extremely useful pigment, sodium oxide of at least three to one into different
5 finding application in the rubber, plastics, cement, locations in a reaction vessel.
paint, and petroleum industries. It is easily in 3. In a process of producing finely-divided,
corporated in rubber compositions wherein it easily friable calcium silicate, the steps of simul
produces a marked improvement in the tear re taneously instilling, with stirring, separate aque
sistant properties. Rubber stocks containing Ous Solutions of calcium chloride and of Sodium
O calcium silicate cure in a markedly shorter time silicate into different locations in a reaction vessel, O
than corresponding stocks containing no calcium separating the precipitate from the aqueous
silicate. It is also a good activator when used medium, washing said precipitate, and removing
in a rubber composition containing a basic ac the free moisture from the precipitate.
celerator. Its extremely small particle size makes 4. In a process of producing finely divided,
5 it useful for the decolorization of numerous easily friable calcium silicate, the step of simul
liquids, such as animal, vegetable, and mineral taneously introducing, with stirring, an aqueous.
oils. It may also be employed as a selective ab Calcium halide and a soluble silicate into different
sorbent for the treatment of gas mixtures. The locations in a reaction vessel initially containing
inexpensive, simple method of preparation and an aqueous precipitation medium.
the uniformity of the products make it acceptable 5. Easily friable precipitated calcium silicate,
in many other industrial applications. most of the particles of which have an ultimate
Although I have herein disclosed a specific em size of about 0.3 micron.
bodiment of my invention, I do not intend to 6. The process of precipitating finely divided
limit myself wholly thereto, for it will be obvious calcium silicate which comprises introducing
25 to those skilled in the art that numerous modifi Solutions of , calcium chloride and of sodium 2 5
cations such as variations in the amount, type, or silicate into a unitary body of aqueous liquid in
character of the reactants, variations in the Con Such a manner as to distribute each reagent
centration of the reactants, and variation in the through a large volume of the unitary body of
rate at which the reactants are introduced into aqueous liquid before it is brought into reacting
30 the reacting vessel are within the Spirit and Scope contact with the other reagent. 30
of the appended claims. 7. The process of precipitating finely divided
I claim: calcium silicate which comprises introducing
1. In a process of producing finely-divided, dilute solutions of calcium chloride and of sodium
easily friable calcium silicate, the step of simul silicate into different portions of a unitary agi
35 taneously instilling, with stirring, separate aque tated body of aqueous reaction liquid, whereby
ous solutions of a calcium halide and of a soluble each reagent is distributed through a large
silicate into different locations in a reaction volume of the liquid before it is brought into
vessel. reacting contact with the other reagent.
2. In a process of producing finely-divided,
40 easily friable calcium silicate, the step of simul RAYMOND PAL LEN. 40