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CELLULOSE ACETATE PRODUCTION BY ACETYLATION OF CELLULOSE

DERIVED FROM DATE PALM FRONDS

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Iraqi Journal of Agricultural Sciences –2020:51(3):967-975 Jassem & et al.
CELLULOSE ACETATE PRODUCTION BY ACETYLATION OF
CELLULOSE DERIVED FROM DATE PALM FRONDS
A.S. Jassem* Sh. K. Muallah* A. H.Mohammed**
Researcher Asst.Prof. Lecturer
* Dept. Biochemical Eng. Coll. Al-Khwarizmi Eng. University. Baghdad
** Dept. Chemical Industries. Inst. Technology Baghdad. University. Middle technical
[email protected]
ABSTRUCT
Cellulose acetate (CA) is a biopolymer produced from fronds of date palm (type teperzal) which were
taken from the Iraqi groves. The steps used to produce (CA); pretreatment, bleaching, acetylation and
hydrolysis. Organosolv pretreatment method was used to remove high lignin content under mild and
severe conditions using NaOH as a catalyst at the concentration (0.03) M. The conditions of
Organosolv pretreatment were used: temperature (125 °C mild, 160 °C severe), pretreatment time 90
min, and ethanol: water ratio 40:60 wt/wt. The acetylation of cellulose with acetic acid was used to
produce cellulose tri-(CTA) and di-(CDA) acetate for two ways: with treated and untreated fronds.
The conditions of acetylation reaction were used: temperature (50-55) °C and time (1, 2 & 3) h. The
product was characterized by the solubility test, titration method and Fourier transform infrared
spectroscopy (FTIR). The results showed that the high percentage of lignin removed was (93%), the
best degree of substitution (DS) for (CTA) and (CDA) were 3.01 and 2.60. As well as the excellent
solubility percentages for (CTA) with chloroform and mixture of chloroform/methanol were 90% and
84%, respectively. While the solubility percentage for (CDA) with acetone was 95%, these result
occurred at pretreatment temperature 160°C, pretreatment time 90 min and reaction time 3 h.
Keywords: acetylation reaction, cellulose acetate, organosolv delignification, degree of substitution.

‫جاسم وآخرون‬ 975-967:)3) 51: 2020- ‫مجلة العلوم الزراعية العراقية‬

‫انتاج خالت السليلوز بواسطة استلة السليلوز المشتق من سعف نخيل التمر‬
**‫عاصم حسن محمد‬ *‫شذى كاظم معلة‬ *‫ايات سوادي جاسم‬
‫أستاذ مساعد‬ ‫أستاذ مساعد‬ ‫باحثة‬
‫جامعة بغداد‬/‫قسم الهندسة الكيميائية االحيائية‬/‫*كلية الهندسة الخوارزمي‬
‫ الجامعة التقنية الوسطى‬/‫قسم الصناعات الكيمياوية‬/‫** معهد التكنولوجيا بغداد‬
‫المستخلص‬
‫ الخطوات المستخدمة‬.‫خالت السليلوز هو بوليمر حيوي تم إنتاجه من سعف نخيل التمر (نوع تبرزل) الذي تم أخذه من بساتين العراق‬
‫( إل زالة المحتوى‬Organosolv) ‫ تم استخدام طريقة المعالجة‬.‫ االستلة والتحلل‬،)‫ التبييض(القصر‬،‫إلنتاج خالت السليلوز هي؛ المعالجة‬
.‫) مول لكل لتر‬0.03( ‫العالي من اللجن ين في ظل ظروف معتدلة وشديدة باستخدام هيدروكسيد الصوديوم كعامل مساعد عند تركيز‬
‫ ونسبة‬،‫ دقيقة‬90 ‫ وقت المعالجة‬،)‫ درجة مئوية شديدة‬160 ،‫ درجة مئوية معتدلة‬125( ‫ درجة الحرارة‬:‫ظروف المعالجة المستخدمة هي‬
‫ تم اس تخدام عملية االستلة للسليلوز مع حامض الخليك إلنتاج خالت السليلوز الثالثي والثنائي‬.‫ نسبة وزنية‬40:60 ‫ الماء‬:‫اإليثانول‬
2 ،1( ‫) درجة مئوية وقت التفاعل‬55-50( ‫ درجة الحرارة‬:‫ وكانت ظروف تفاعل االستلة‬.‫ باستخدام سعف معالج وغير معالج‬:‫بطريقتين‬
‫( وأظهرت النتائج أن نسبة عالية‬FTIR) ‫ قابلية الذوبان وطريقة التسحيح وجهاز‬:‫ وتم اختبار المنتج باستخدام عدة طرق وهي‬.‫) ساعة‬3‫و‬
‫ وكانت‬،2.60‫ و‬3.01 ‫( لخالت السليلوز الثالثي والثنائي كانت‬DS) ‫ وأفضل درجة استبدال‬،)٪93( ‫من اللجنين التي تمت إزالتها كانت‬
‫ بالتتابع بينما كانت‬%84‫ و‬٪90 ‫نسب الذوبان الممتازة لـ لخالت السليلوز الثالثي مع الكلوروفورم وخليط من الكلوروفورم والميثانول هي‬
‫ درجة‬160 ‫ تم الحصول على هذه النتائج باستخدام المعالجة بدرجة حرارة‬،٪95 ‫نسبة الذوبانية لـ خالت السليلوز الثنائي مع األسيتون‬
.‫ ساعة‬3 ‫ دقيقة و زمن تفاعل‬90 ‫مئوية وبزمن‬
.‫ درجة االستبدال‬،‫ إزالة اللكنين بالمذيبات العضوية‬،‫ خالت السليلوز‬،‫ سليلوز‬،‫ تفاعل االستلة‬:‫الكلمات المفتاحية‬

*Received:24/7/2019, Accepted:31/10/2019

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Iraqi Journal of Agricultural Sciences –2020:51(3):967-975 Jassem & et al.
INTRODUCTION Fronds of the date palm as a suitable candidate
Cellulose acetate (CA) [C6H7O2 (OH) 3-m for production of cellulose derivative for two
(OOCCH3) m], m = 0~3, is the essential reasons: The abundance of date palm trees and
organic ester of cellulose due to it’s a broad the fronds contain high cellulose percent
commercial and industrial importance. There nearly 42%, which is essential for the
are several applications of (CA): Textile and production of (CA). Fronds of the date palm
plastic industries (10,25), camera accessories, are lignocellulosic materials consist of
thermoplastic moulding, magnetic tapes, hemicellulose, cellulose and lignin, which an
photographic films, combs, electrical parts and abundant, nonfood and inexpensive biomass
telephone (14). Figure 1, shows that the most that represents a renewable and appropriate
common types of cellulose acetate include source of cellulosic fibers suitable for the
cellulose diacetate, their degree of substitution synthesis of biopolymer (15). Additionally,
(DS) ranging from 2-2.5 (6), and cellulose hemicellulose and lignin should be removed
triacetate having the DS above 2.8 (11). The from biomass because these two components
crystallinity and biodegradation in (CA) have a negative effect on acetylation
decrease according to the following order: efficiency, as well as on the properties of the
cellulose triacetate, cellulose diacetate, and product (19). Acetylation reaction used in
cellulose monoacetate (7). The acetyl content produced (CA), which are classified as
and DS heavily affect the quality of (CA) heterogeneous and homogeneous acetylation.
because it can affect the product and its (CA) obtained from heterogeneous acetylation
solubility in the solvent. Currently, different is more crystalline than from the homogeneous
types of cellulose derivatives, for instance, process. The hydrophilic hydroxyl groups of
methyl cellulose, ethyl cellulose, carboxyl cellulose in the cell walls of the wood and the
methyl cellulose, and cellulose acetate have intercellular regions convert to a hydrophobic
been produced to change the chemical and group in acetylation reaction (20).
physical properties of cellulose (10). Commercially, cellulose is acetylated by
Nowadays, acetylated wood is a commercial adding acetic anhydride, glacial acetic acid,
product in Europe (4). Generally, (CA) is and various catalysts Such as pyridine,
prepared from raw cellulose, wood pulp, or dimethyl amino pyridine, potassium acetate,
agricultural waste materials. These materials and sulphuric acid to increase the rate of
include cotton by-products, sugar cane acetylation reaction. Production of (CA) needs
baggage, banana byproducts, wheat, and rice a different time of acetylation based on
straw, and other materials have high cellulose cellulose sources to obtain suitable acetyl
content. Preparation of cellulose derivatives content. As time increase, (DS) and solubility
from these materials is an environmentally of (CA) produced increase. Several types of
friendly and economically profitable approach research carried out about the production of
(8). (CA) such as microbial cellulose takes 5-10
hr., bacterial cellulose from pineapple waste
for 2 hr., straw for 2-3 hr. (3). The main
objective of the research is to produce
cellulose acetates from date palm fronds and
determining the exact time required for
cellulose acetylation.
MATERIALS AND METHODS
Fronds of date palm type (teperzal) were used
and collected from Baghdad garden in Iraq.
Impurities should be removed by washing the
fronds then dried in sunlight. The dried
materials were cut using electric cutter,
crushed with humor and sieved with a particle
size of (90-270) µm were selected for
Figure 1. The structure of cellulose Tri- and Di- production a biopolymer (21). The chemicals
acetate (6).
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Iraqi Journal of Agricultural Sciences –2020:51(3):967-975 Jassem & et al.
used in the experimental work are: Ethanol, placed in a hot water bath at 90°C for 60 min
methanol, sodium hydroxide, hydrochloric (10). After bleaching completed, a large
acid, glacial acetic acid, acetic anhydride, amount of water is required for washing the
sulphuric acid, acetone, hydrogen peroxide & residual hydrogen peroxide and the residual
chloroform, all chemicals were obtained from alkali then dried (13).
LTD, India. The steps used in this research Third: Cellulose acetylation
are: Production of cellulose triacetate (CTA)
First: Compositional analysis of date palm The acetylation of cellulose for the production
fronds of cellulose Triacetate includes three steps:
The composition of fronds or other resources The activation of cellulose was done by
of lignocellulosic materials is changed mixing 60 mL of acetic acid glacial, 0.4 mL of
according to; the part of the plant from which sulphuric acid (95% concentration) and 4 g of
the sample is taken, the place and growing the bleached stalk. The system was put in a
season (1,18). The percentage of extractives, water bath at (50-55) °C for 1 h., with frequent
moisture, ash, lignin, cellulose, Holocellulose, stirring.
and hemicellulose content were investigated a- The acetylating mixture consisting of 20 mL
according to Ramsden and Blake (20) and acetic anhydride, 10 mL acetic acid glacial,
A.Sluiter et al.,(21). and 0.6 mL of H₂SO₄ added to the above
Second: Pretreatment (delignification mixture, which is placed in a water bath for 1,
process) 2 and 3 h., with stirring till a clear solution
The purpose of pretreatment to increase the obtained
accessibility of the reagent, acetic anhydride to b- The solution divided into two equal parts.
all the hydroxyl groups of cellulose, and to The first portion was used for cellulose
eliminate the non-cellulosic components such triacetate production by carefully pouring into
as hemicellulose and lignin (19). a large volume of water. Finally, Cellulose
Organosolv method: Different techniques of triacetate formed as a precipitate. The
pretreatment of lignocellulosic materials were precipitate was filtered and washed to
used, including pyrolysis, biological treatment, neutrality and dried. The second portion was
and alkaline hydrolysis, etc. (12). In this study, used for production of cellulose diacetate (2).
organic solvent (Organosolv) pretreatment was Production of cellulose diacetate
used to remove the high content of lignin from (CDA)
fronds. In this process, the lignocellulosic =The hydrolysis process of (CTA) produced
material is treated with ethanol or other (CDA). The reaction involves the use of water
solvents at rising temperature using water as a as the main reactant and acids as catalyst (10).
co-solvent in stainless steel reactor (digester) Hydrolysis is the opposite of the acetylation
with a catalyst NaOH. A mixture of biomass process where the sometimes unavoidable
(fronds)-water-ethanol was made (200 ml excess of the OH group by the acetyl group
solvent per 10 g biomass) to hydrolyze gives a high degree of substitution, which can
cellulose and hemicellulose. However, the be repaired. Hydrolysis helps in decreasing DS
main goals include the removal of lignin from of cellulose acetate from three acetyl groups
the fronds and disruption of the crystalline per cellulose to two acetyl groups in the range
structure of cellulose (16). This mixture was of (2.4-2.5).
heated in the range (125 -160°c) and stirred for This process includes:
90 min. After filtration of the slurry, the a- Mixture of 24 mL of acetic acid glacial and
remaining part was washed and then dried. 7 mL of water added to the second portion of
Bleaching process the mixture obtained from acetylation reaction,
The bleaching process is a chemical process with strong stirring to avoid precipitation, and
used in several kinds of wood pulp to change it was allowed to stand for 1 h at (50-55) °c.
the color of the pulp from brown to white and b- The mixture poured into a large volume of
to remove the remaining lignin (8). In this water, and the cellulose diacetate formed as a
process, the dried material was suspended in a precipitate. The product was filtered and
NaOH solution with 30% H₂O₂ at pH 12.0 and washed to neutrality and dried (2).

969
Iraqi Journal of Agricultural Sciences –2020:51(3):967-975 Jassem & et al.
Forth: Characterization of the cellulose was calculated according to equation [3]
acetates 𝑴𝟏−𝑴𝟐
𝒔𝒐𝒍𝒖𝒃𝒊𝒍𝒊𝒕𝒚% = 𝑴𝟏 …. [3]
CTA and CDA can be characterize by:
Where:
Degree of substitution (DS)
M1= total mass of cellulose acetate
The degree of substitution is an essential
M2= mass of insoluble cellulose acetate
parameter for the transformation of cellulose
Fourier Transform Infrared (FTIR)
into cellulose acetate, and it was controlled by
The functional groups of cellulose, cellulose
time of acetylation reaction. The most
tri- and di- acetate studied by using (FTIR)
common method for determined (DS) is a
apparatus. The disc was prepared by mixing
titration method. This method based on the
and compressing the sample with Potassium
hydrolysis of ester bonds in the alkali solution
bromide at a ratio 1:1. The wavelength range
(22). (DS) can be calculated as follow: 0.5 g of
from 450 to 4000 cm-1 (3).
cellulose acetate and 20 mL of (75%
RESULTS AND DISCUSSION
concentration) ethanol heated to 55 °C for 1 h
The results are divided into four parts. The
for better swelling of the sample. 20 mL of 0.5
first part deals with the results of the
mole/L NaOH solutions added to each sample,
compositional analysis of the fronds. The
and the mixture also heated at 55°C for 1 h.
second part is relates to the results of
These procedures also applied for cellulose
Organosolv method. The third part concerned
(control). The mixture stayed at a laboratory
with the results of acetylation reaction of
temperature for 72 h. The excess sodium
cellulose by two ways; using treated and
hydroxide in the samples and control titrated
untreated fronds. While the last part deals with
with 0.5 mole/L HCl using phenolphthalein as
the study of the results of cellulose acetate
an indicator. 0.5 mL of acid was added and the
characterization.
NaOH was permitted to diffuse for 24 h. after
Compositional analysis of date palm fronds
that, small amount of acid was then also
The compositions of date palm fronds were
titrated with 0.5 mole/L NaOH until the
determined as show in (Table 1).
solution had acquired a faint pink color
Table 1. The compositions of date palm
(23,17). The acetyl content (A%) was
fronds based on dry weigh
calculated according to equation [1]: Weigh%, based on (dry basis)
𝟒.𝟑𝟎𝟓
𝑨% = [(𝑫 − 𝑪)𝑵𝒂 + (𝑨 − 𝑩)𝑵𝒃] ∗ ( ) … [1] Cellulose 42
𝑾
Where: Hemicellulose 18
A&B= the volumes (mL) of NaOH required Lignin 25
for the titration of the sample and blank Extractive 8
respectively Ash 7
C&D= the volumes (mL) of HCl required for From Table 1, there is a relatively high
the titration of the sample and blank percentage of cellulose in date palm fronds;
respectively this enhances the possibility of producing
Na&Nb= the normality of HCl and NaOH cellulose acetate.
respectively Pretreatment (delignification process)
W= the mass of the CA sample used. The ( % In this research, Organosolv and bleaching
A) obtained from equation [1] was used to methods used for the delignification of fronds.
calculate the DS according to equation [2] (9). These processes aim to remove lignin content
𝟏𝟔𝟐∗𝑨%
𝑫𝑺 = 𝟒𝟑𝟎𝟓−𝟒𝟑∗𝑨% ….. [2] and hemicellulose in the range of temperature
(125-160) °C in stainless steel reactor of
Solubility test
pretreatment time 90 min with a catalyst (0.03
One of the means of biopolymer identification
M) NaOH. Composition of fronds determined
is solubility test. The solubility will give an
after delignification process, as shows in the
indication for the type of cellulose acetate. In
Table 2 and found that the minimum lignin
this test, cellulose tri and diacetate are put in
percent was 10.31% and 6% which obtained at
solvents: acetone, chloroform and mixture of
temperature 125°C and 160°C respectively,
chloroform/methanol in ratio (9:1 v/v) for a
thus the best removal of lignin content at a
certain time with stirring at laboratory
temperature 160°C.
temperature (10). The solubility percentage
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Iraqi Journal of Agricultural Sciences –2020:51(3):967-975 Jassem & et al.
Table 2. The compositions of date palm fronds after delignification processes
Weight %, based on (dry basis )
Sample cellulose hemicellulose lignin extractive ash
At 125°c 65 9.9 10.31 3.89 10.9
At 160°c 78 4 6 ------- 11
Production of cellulose tri- and di-acetate when the sample was treated at high
Production of cellulose acetate includes temperature of 160 °C, very high DS was
several stages; activation, acetylation, obtained since a maximum decrease in the
hydrolysis, precipitation, and drying, amount of lignin obtained, as a result
respectively. Glacial acetic acid used as an completely acetylation of cellulose was
activator and sulphuric acid as a catalyst in an occurred to form CTA and CDA. The high
activation process to increase cellulose surface value Of DS shows a high hydroxyl
area and decrease the intermolecular hydrogen substitution in the cellulose molecule by the
bonds. For the facilitating acetylation process, acetyl group
acetic anhydride used as a reagent. Cellulose
tri- and di-acetate produced in two ways:
treated and untreated fronds. Acetylation of
Cellulose caused by oxidative changes of
cellulose molecules and change the color from
white to brown. After the reaction was
completed, cellulose triacetate formed but
cellulose diacetate produced after hydrolysis
process of cellulose triacetate with acetic acid.
Cellulose acetate produced from treated fronds
was white powder, while the shape of cellulose
acetate produced from untreated fronds was a
brown powder because of the presence of
lignin which effect on the reaction efficiency
and on the characteristic of cellulose acetate
produced.
Characterization of the cellulose tri- and di-
acetate
Degree of substitution (DS): The DS for
cellulose tri- and di-acetate was determined by
the titration method with an aqueous solution
of NaOH. The amount of obtaining acetyl
content for cellulose tri- and di-acetate is
dependent on the duration of acetylation
reaction and the lignin percent. Figure (2A)
shows that the DS value for CTA and CDA
increased With time of acetylation reaction but
the value of DS is very low due to the presence
of a high percentage of lignin in the sample
that binds the cellulose molecule and prevents
the breakdown of hydrogen bonds. Thus,
accessibility of acetic anhydride to hydroxyl
group is too weak and consequently a partial
transformation of cellulose-to-cellulose acetate
Figure 2. Effect of acetylation time and
occur. In figure (2B), the value of the DS is
pretreatment on the DS of CTA and CDA
slightly higher than in figure (2A) due to use
for (A) untreated sample, (B) sample
of NaOH catalyst in the pretreatment of
treated at 125°C, and (C) sample treated at
sample at 125°C that remove high percent of
160°C.
lignin. While in figure (2C) it was found that

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 Iraqi Journal of Agricultural Sciences –2020:51(3):967-975 Jassem & et al.
Solubility test mixture of chloroform/methanol (9:1, v/v) but
The solubility of cellulose acetate depends on insoluble in acetone and vice versa for the
the average degree of substitution (DS) and cellulose diacetate. Table 3shows the solubility
lignin content. The solubility test for the percentages for cellulose triacetate and
resultant product indicated that cellulose cellulose diacetate at different conditions.
triacetate was soluble in chloroform and
Table 3. The solubility test of cellulose tri- and di-acetate for acetylation time 3 h
Sample without treatment Acetone % Chloroform % Chloroform/methanol (9:1) %
cellulose triacetate insoluble 49% 44%
cellulose diacetate 53% insoluble insoluble

Sample with treatment at 160 °c Acetone % Chloroform % Chloroform/methanol (9:1) %

cellulose triacetate insoluble 90% 84%
cellulose diacetate 95% insoluble insoluble

Sample with treatment at 125 °c Acetone % Chloroform % Chloroform/methanol (9:1) %

cellulose triacetate insoluble 80% 72%
cellulose diacetate 82% insoluble insoluble
Results in Table 3 reveal that the solubility the result of FTIR analysis of the cellulose
percentage of cellulose acetate manufactured triacetate showed that the intensity in the band
from treated fronds at severe condition (160°c) of the O-H group decreased significantly,
is very high, but the solubility percentage of meaning that fully acetylated was occurred
cellulose acetate produced from untreated that all O-H group was substituted by the
fronds is low due to high lignin content and acetyl group. Other groups such as the C-H
low DS value in the sample, which Means that group was showed at 2962.66 cm-1and the
the solubility decreases by decreasing the DS carbonyl group C=O was observed at 1750
and by increasing the lignin. cm-1. While in Figure (C), the result for
Fourier Transform Infrared (FTIR) cellulose diacetate showed that the intensity of
Cellulose, cellulose tri and diacetate produced O-H groups at 3568.31 cm-1 decreased
were analyzed using Fourier transform slightly. A strong band of carbonyl group C=O
infrared ray spectroscopy (FTIR) as show in was observed at 1769.51 cm-1. This indicates
Figure 3that aims to analyze functional groups that some of the O-H groups in the cellulose
changes before and after acetylation reaction have been substituted by the acetyl group and
with regard to the formation spectrum. In the incompletely acetylated has occurred to form
Figure (A), the results of functional groups cellulose diacetate. On the other hand, the
analysis on cellulose uses FTIR showed that ether groups C-O were also showed at 1224
the O-H groups at 3348.42 cm-1 and C-O cm-1 and C-H groups at 2962.66 cm-1. The
groups at 1043.49 cm-1. The groups were a carbonyl groups C=O make up the cellulose
type of alcohol compound that was the tri- and di-acetate. The FTIR spectra were
forming cellulose group. There were also C-H established that the acetylation process of
functional groups at 2914.44 cm-1, which cellulose into cellulose tri- and di-acetates had
were hydrocarbon compounds. In figure (B), been successfully carried out.

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Iraqi Journal of Agricultural Sciences –2020:51(3):967-975 Jassem & et al.

Figure 3. FTIR Analysis of (A) cellulose, (B) cellulose triacetate, and (C) cellulose diacetate
CONCLUSION of substitution. It can be concluded that the
In this research, compositional analysis of lignin content has negative effect on the
fronds, pretreatment and preparation of pulp following: first, it consumes more acetic
from fronds, cellulose acetylation and anhydride because all component will be
cellulose acetates production has been acetylated. Second, lignin is considered a
achieved. However, this study has shown that barrier to prevent the acetylation process of a
they can be used an agricultural raw material hydroxyl group. Third, acetylated lignin effect
(date palm fronds) for the production of pulp, on the DS and the dissolution of cellulose tri-
and cellulose biopolymers (cellulose tri- and and di-acetate. Therefore, fronds of date palm
di-acetate). The reaction conditions required can be delignified by using modified
for converting the fronds powder to cellulose Organosolv method in which the lignin is
acetate was established. The production of damaged by solvent and high temperature. The
cellulose acetate from untreated fronds is not prepared cellulose acetates are characterized
preferred method because of its low solubility by FTIR spectroscopy, solubility test, and
and low degree of substitution. It was found titration method.
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