CN102391378B - Method for preparing cellulose acetate from wheat straws - Google Patents
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Abstract
The invention discloses a method for preparing cellulose acetate from wheat straws. The method comprises the following steps of: performing activating and bleaching pretreatment on the wheat straws; mechanically crushing; performing acetylation reaction; recovering the esterified liquid in a low-temperature condensation mode; separating acetylized products; and extracting the acetylized products with different components by using solvents to separate out the products such as cellulose triacetate, cellulose diacetate, acetylized hemicellulose, acetylized lignin and the like. The invention provides an economic and effective method for pretreating the wheat straws. By the method, the defect of the single catalyst in the traditional acetylation process is overcome; the cellulose acetate with high substitution degree and polymerization degree is prepared in a new catalyst system; and the wheat straws are utilized reasonably.
Description
Technical field
The present invention relates to wheat stalk renewable resources and utilize technical field, particularly a kind of method improving preparing cellulose acetate from wheat straws under catalyst system effect.
Background technology
Natural cellulosic feedstocks is renewable organic substance the abundantest on the earth.China can produce the natural cellulosic feedstocks of approximately 11.45 hundred million tons by photosynthesis every year, and only one of agricultural crop straw, cot are just up to more than 700,000,000 tons, and wherein wheat stalk accounts for 21%.In China, most of stalk is used as fuel or is directly burnt in field, has not only destroyed the eubiosis, makes soil fertility exhaustion, causes the vicious cycle in agricultural, and contaminate environment, also has disaster hidden-trouble.
Along with the attention of people to environment protection and renewable resources utilization, comprise that the utilization of the agricultural straw resource of wheat stalk more and more receives the concern of countries in the world.People, by carry out graft modification on natural cellulose molecular chain, prepare the high added value material that necessary for human is wanted in recent years, thereby have effectively utilized this renewable resources and reduced its impact on environment.
But wheat stalk is because many, the complex structure of component, present stage to its development and utilization not yet in the development of economy and making a breakthrough property of technical field.The formations such as wheat stalk cell walls three major polymers: cellulose, hemicellulose and xylogen.The structure of wheat stalk cell walls is very tight, exists different bonding forces between Mierocrystalline cellulose, hemicellulose and lignin molecule.Combination between Mierocrystalline cellulose and hemicellulose or lignin molecule mainly depends on hydrogen bond; Between hemicellulose and lignin molecule, except hydrogen bond, also exist the combination of chemical bond.Therefore; want to make full use of wheat straw resource, an important gordian technique is to carry out pre-treatment and activation to it, breaks the bonding force between Mierocrystalline cellulose, hemicellulose and lignin molecule; reduce the degree of crystallinity of stalk, thereby provide possibility for improving the accessibility of follow-up acetylization reaction.
Cellulose acetate is the second largest industrial fiber element kind that is only second to viscose fiber at present, have that snappiness is good, transparency is high, glossiness good, melt fluidity is good, thermoplasticity is strong, intensity is high and to the feature such as light is stable, nonflammable, can be widely used in manufacturing textiles, the field such as filter tip, sheet base, plastics for cigarette.Successively there is the methods such as low temperature process, pyroprocess, homogeneous phase method and gas phase esterification process in the preparation of cellulose acetate; at present domestic low temperature acetylize and the medium temperature hydrolyzation (50～70 ℃) of adopting, trends towards developing the novel procesies such as medium and high temperature acetylize and pyrohydrolysis abroad more more.
In the preparation process of cellulose acetate, use dispersion agent, esterifying agent and catalyzer.Dispersion agent is thinner namely, and its use is the bath raio for augmenting response, catalyst-solvent, the carrying out of impelling reaction.Conventional dispersion agent has: glacial acetic acid, trichloromethane, methylene dichloride, benzene,toluene,xylene, tetracol phenixin etc., wherein glacial acetic acid is more conventional, because it is except can be used as dispersion agent, can also play the effect of activated cellulose.In acetylation, adopt acetic anhydride as esterifying agent.Catalyzer is of a great variety, can be divided into acid catalyst, alkali catalyst and saline catalyst etc.Wherein acid catalyst has sulfuric acid, hydrochloric acid, phosphoric acid, perchloric acid, methylsulfonic acid and p-methyl benzenesulfonic acid etc.In European patent WO9403497, mention with methylsulfonic acid as catalyzer.In US Patent No. 4329446, use p-methyl benzenesulfonic acid as the catalyzer of Mierocrystalline cellulose acetylization reaction.S.D.Bhattacharya adopts perchloric acid, as catalyzer, cotton is carried out to acetylize processing, has also obtained reasonable effect.Sulfuric acid is as a kind of active catalyst, and because effect is remarkable, it is widely used in acetylizing, but it to cellulosic Degradation also clearly, and the productivity ratio that can cause like this generating cellulose acetate is lower; Alkali catalyst has sodium hydroxide, aluminium hydroxide etc., but because this type of catalyst effect is not good enough, practical application is fewer; The catalyzer of salt has carbonate, supercarbonate, hydrosulfate, organic acid salt of basic metal or alkaline-earth metal etc., as sodium carbonate, sodium-acetate, calcium acetate, lithium hydrogen sulfate, sodium pyrosulfate, p-methyl benzenesulfonic acid sodium, carbonic acid derivatives, inorganic sulfoacid compound etc.Zinc chloride also can be used as acetylizad catalyzer, industrial, has obtained certain application.European patent also has use N,N-dimethylacetamide as the record of catalyzer, yet can generate amine by product or ammonia by product and N in acetylation, N-dialkylamine, and these by products have toxicity.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of preparing cellulose acetate from wheat straws.The method adopts simply, effective wheat stalk pretreatment process, simultaneously in order to overcome the deficiency of single catalyst in traditional acetylation, carries out acetylization reaction, thereby prepare the cellulose acetate of high added value under new catalyst system.Whole technical process has higher economy and security, and the cellulose acetate making under new catalyst system has farthest kept high substitution value and the polymerization degree.
For solving the problems of the technologies described above, the present invention has adopted following technical scheme: the method comprises the steps: the first step, pre-treatment and activation and bleaching: wheat straw is carried out to high temperature poach, activation, bleaching; Second step, mechanical disintegration: the wheat straw of processing through the first step is carried out to mechanical disintegration processing; The 3rd step, acetylization reaction: by the wheat straw placing response device after pulverizing, add esterifying liquid, and add catalyzer to carry out acetylize processing; The 4th step, adopts cryogenic condensation mode to recycle esterifying liquid; The 5th step, acetylize product separation: the solution supernatant liquor in reactor is separated, discarded precipitation; In supernatant liquor, add distilled water, separate out precipitation, washed several times with water, to neutrality, through suction filtration, vacuum-drying, finally obtains acetylize product, then carries out pulverization process; The 6th step, the acetylize product different to solvent extraction component: 1. the acetylize product of handling well in the 5th step is carried out to extracting with acetone; 2. steam the most of acetone in previous step solution, then in solution, add distilled water again to isolate insolubles according to step 5, then use the mixed solution extracting of acetone and water; 3. use the solute in the mixed solution extracting previous step of second alcohol and water, by extracting the insolubles obtaining for above-mentioned three times, dry and get final product finished product.
Furthermore, in technique scheme, in described the first step pre-treatment and activation and bleaching process, by wheat stalk high temperature poach, add sodium hydroxide to activate, add clorox and mixed solution of hydrogen peroxide to bleach simultaneously, the amount that wherein adds sodium hydroxide is to add 1% of quality, and the amount that adds clorox and mixed solution of hydrogen peroxide is to add 2% of volume of water.
Furthermore, in technique scheme, in described second step mechanical disintegration process, the granularity of the wheat straw after pulverizing is 150 orders.
Furthermore, in technique scheme, in the 3rd described step acetylization reaction process, in esterifying liquid, diacetyl oxide accounts for 20%～25% of esterifying liquid volume, and glacial acetic acid accounts for 75%～80% of esterifying liquid volume; Described catalyzer is sodium pyrosulfate, hydrofluoric acid and the vitriol oil, wherein sodium pyrosulfate add-on be in reactor wheat stalk solid masses 0.5%～3%, the add-on of hydrofluoric acid is 1%～3% of esterifying liquid volume, the add-on of the vitriol oil is 0.3%～2% of esterifying liquid volume.
Furthermore, in technique scheme, in the 6th described step, use for the second time in the mixed solution extractive process of acetone and water, the amount of water is liquor capacity 9%～11%, and the amount of acetone is liquor capacity 89%～91%.
Furthermore, in technique scheme, in the 6th described step, while using for the third time the solute in the mixed solution extracting previous step of second alcohol and water, the amount of water is liquor capacity 24%～26%, and the amount of ethanol is liquor capacity 74%～76%.
Furthermore, in technique scheme, in described acetylization reaction process, in reactor, solid volume is 16%～18%, and liquid volume is 82%～84%; This reaction is carried out 2 hours under the condition of 60～80 ℃, obtains auburn solution.
Furthermore, in technique scheme, in the 4th described step, condensation at low temperature reclaims in glacial acetic acid process, employing is heated reactor, reclaim glacial acetic acid, be wherein 0.5 hour middle heat-up time simultaneously, and reactor naturally cools to room temperature and stops reclaiming glacial acetic acid.
Furthermore, in technique scheme, in the 6th described step, institute's extracting product is respectively: extracting for the first time solute is Cellulose diacetate, acetylated hemicellulose and acetylize xylogen, and insolubles is cellulosetri-acetate; The solute extracting is for the second time acetylated hemicellulose and acetylize xylogen, and insolubles is Cellulose diacetate; The solute extracting is for the third time acetylize xylogen, and insolubles is acetylated hemicellulose.
The present invention adopts technique scheme tool to have the following advantages:
(1) high temperature poach method for pretreating makes wheat stalk under High Temperature High Pressure; the ethanoyl of hemicellulose etc. generate organic acid; then participate in not damaging again the catalytic process of hemicellulose and lignin depolymerization, make hemicellulose partial hydrolysis become soluble polysaccharide, xylogen is softening.Wheat stalk cell wall structure after poach is destroyed, and cellulosic porosity increases, and raw material is bulk is pipe tobacco shape, has greatly improved follow-up acetylizad accessibility; NaOH activation method can make wheat stalk swollen, the primary formation of stalk is destroyed, delignification successful, in the stalk after processing, Mierocrystalline cellulose has lower degree of crystallinity, less crystal size and larger spacing, thereby has improved acetylizad accessibility; Wheat stalk after mechanical crushing method is processed; material size obviously reduces; degree of crystallinity reduces; mean polymerisation degree diminishes; the solvability of material strengthens; thereby the straw substrate concentration that makes to be dissolved in esterifying liquid increases, thereby improve the concentration of saccharified liquid, also improved acetylizad accessibility and reaction efficiency.
(2) in the situation that of adding NaOH in preprocessing process, use clorox and mixed solution of hydrogen peroxide to bleach wheat stalk, can give full play to the bleaching effect of hydrogen peroxide, effectively improved the whiteness of raw material, also at utmost reduce cellulosic damage, made the cellulose acetate of preparation there is better physicochemical property.
(3) in acetylation, use sodium pyrosulfate, hydrofluoric acid and the vitriol oil as new catalyst system.Wherein sodium pyrosulfate can be urged into Mierocrystalline cellulose and esterifying liquid after activation and better mixed and be in contact with one another; Hydrofluoric acid and the vitriol oil, as strong protonic acid, not only play katalysis, to cellulosic activation also successful in reaction.New catalyst system has not only improved reaction efficiency; but also farthest reduced in traditional acetylation when the vitriol oil is as single catalyst cellulosic Degradation; make Mierocrystalline cellulose polymerization degree when acetylize be unlikely decline too violent; thereby guarantee the molecular weight of the finished product, make the cellulose acetate of preparation there is higher substitution value and the polymerization degree.
(4) use condensation at low temperature can farthest reclaim glacial acetic acid, and can reuse, reduced the wasting of resources.In expendable waste liquid, contain glacial acetic acid, sulfuric acid, diacetyl oxide etc. and also can be used in the preprocessing process of wheat stalk, meet the new trend of green economy.
(5) can from the acetylize product of wheat stalk, isolate the high value added products such as cellulosetri-acetate, Cellulose diacetate, acetylated hemicellulose, acetylize xylogen, thereby effectively utilize this renewable resources of wheat stalk, turn waste into wealth.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but embodiment of the present invention are not limited to this.
Embodiment 1: the wheat stalk powder 34g that pre-treatment is good is placed in reactor, adds 150ml esterifying liquid; Add the vitriol oil of the sodium pyrosulfate of 0.5% quality, the hydrofluoric acid of 1% volume and 2% volume as catalyzer, the vitriol oil adds and frontly with distilled water, dilutes at 1: 1; Reaction is stirred 2 hours under the condition of 60 ℃, obtains auburn solution; The discharge port of reactor is connected on condenser, continues reflux 0.5 hour, collect glacial acetic acid simultaneously.Question response device stops collecting after naturally cooling to room temperature.
Solution supernatant liquor in reactor is separated, discarded precipitation.In supernatant liquor, add distilled water, separate out precipitation, washed several times with water, to neutrality, through suction filtration, vacuum-drying, finally obtains acetylize product.
The acetylize product of solvent extraction different components: 1. by the acetone extracting of acetylize product, insolubles is cellulosetri-acetate; 2. steam most of acetone in previous step solution, in solution, add distilled water again to isolate insolubles, the acetone that is then 9: 1 by volume ratio and water carry out extracting, and insolubles is Cellulose diacetate; 3. the solute in the second alcohol and water extracting previous step that is 3: 1 by volume ratio again, the solute extracting is acetylize xylogen, insolubles is acetylated hemicellulose etc.Then insoluble cellulosetri-acetate, Cellulose diacetate, acetylated hemicellulose etc. are dried.
Obtain experimental data as follows:
Cellulosetri-acetate productive rate: 28.7%
Substitution value (DS): 2.85
The polymerization degree (DP): 162
Cellulose diacetate productive rate: 12.5%
Acetylated hemicellulose productive rate: 14.6%
Embodiment 2: the wheat stalk powder 34g that pre-treatment is good is placed in reactor, adds 150ml esterifying liquid; Add the vitriol oil of the sodium pyrosulfate of 2% quality, the hydrofluoric acid of 2% volume and 0.3% volume as catalyzer, the vitriol oil adds and frontly with distilled water, dilutes at 1: 1; Reaction is stirred 2 hours under the condition of 70 ℃, obtains auburn solution; The discharge port of reactor is connected on condenser, continues reflux 0.5 hour, collect glacial acetic acid simultaneously.Question response device stops collecting after naturally cooling to room temperature.
Solution supernatant liquor in reactor is separated, discarded precipitation.In supernatant liquor, add distilled water, separate out precipitation, washed several times with water, to neutrality, through suction filtration, vacuum-drying, finally obtains acetylize product.
The acetylize product of solvent extraction different components: 1. by the acetone extracting of acetylize product, insolubles is cellulosetri-acetate; 2. steam most of acetone in previous step solution, in solution, add distilled water again to isolate insolubles, the acetone that is then 9: 1 by volume ratio and water carry out extracting, and insolubles is Cellulose diacetate; 3. the solute in the second alcohol and water extracting previous step that is 3: 1 by volume ratio again, the solute extracting is acetylize xylogen, insolubles is acetylated hemicellulose etc.Then insoluble cellulosetri-acetate, Cellulose diacetate, acetylated hemicellulose etc. are dried.
Obtain experimental data as follows:
Cellulosetri-acetate productive rate: 37.6%
Substitution value (DS): 2.89
The polymerization degree (DP): 179
Cellulose diacetate productive rate: 10.7%
Acetylated hemicellulose productive rate: 13.5%
Embodiment 3: the wheat stalk powder 34g that pre-treatment is good is placed in reactor, adds 150ml esterifying liquid; Add the vitriol oil of the sodium pyrosulfate of 3% quality, the hydrofluoric acid of 3% volume and 0.5% volume as catalyzer, the vitriol oil adds and frontly with distilled water, dilutes at 1: 1; Reaction is stirred 2 hours under the condition of 80 ℃, obtains auburn solution; The discharge port of reactor is connected on condenser, continues reflux 0.5 hour, collect glacial acetic acid simultaneously.Question response device stops collecting after naturally cooling to room temperature.
Solution supernatant liquor in reactor is separated, discarded precipitation.In supernatant liquor, add distilled water, separate out precipitation, washed several times with water, to neutrality, through suction filtration, vacuum-drying, finally obtains acetylize product.
The acetylize product of solvent extraction different components: 1. by the acetone extracting of acetylize product, insolubles is cellulosetri-acetate; 2. steam most of acetone in previous step solution, in solution, add distilled water again to isolate insolubles, the acetone that is then 9: 1 by volume ratio and water carry out extracting, and insolubles is Cellulose diacetate; 3. the solute in the second alcohol and water extracting previous step that is 3: 1 by volume ratio again, the solute extracting is acetylize xylogen, insolubles is acetylated hemicellulose etc.Then insoluble cellulosetri-acetate, Cellulose diacetate, acetylated hemicellulose etc. are dried.
Obtain experimental data as follows:
Cellulosetri-acetate productive rate: 31.5%
Substitution value (DS): 2.87
The polymerization degree (DP): 173
Cellulose diacetate productive rate: 15.3%
Acetylated hemicellulose productive rate: 12.8%
Embodiment 4: the wheat stalk powder 34g that pre-treatment is good is placed in reactor, adds 150ml esterifying liquid; Add the vitriol oil of the sodium pyrosulfate of 1% quality, the hydrofluoric acid of 2% volume and 1% volume as catalyzer, the vitriol oil adds and frontly with distilled water, dilutes at 1: 1; Reaction is stirred 2 hours under the condition of 70 ℃, obtains auburn solution; The discharge port of reactor is connected on condenser, continues reflux 0.5 hour, collect glacial acetic acid simultaneously.Question response device stops collecting after naturally cooling to room temperature.
Solution supernatant liquor in reactor is separated, discarded precipitation.In supernatant liquor, add distilled water, separate out precipitation, washed several times with water, to neutrality, through suction filtration, vacuum-drying, finally obtains acetylize product.
The acetylize product of solvent extraction different components: 1. by the acetone extracting of acetylize product, insolubles is cellulosetri-acetate; 2. steam most of acetone in previous step solution, in solution, add distilled water again to isolate insolubles, the acetone that is then 9: 1 by volume ratio and water carry out extracting, and insolubles is Cellulose diacetate; 3. the solute in the second alcohol and water extracting previous step that is 3: 1 by volume ratio again, the solute extracting is acetylize xylogen, insolubles is acetylated hemicellulose etc.Then insoluble cellulosetri-acetate, Cellulose diacetate, acetylated hemicellulose etc. are dried.
Obtain experimental data as follows:
Cellulosetri-acetate productive rate: 33.2%;
Substitution value (DS): 2.88;
The polymerization degree (DP): 175;
Cellulose diacetate productive rate: 14.3%;
Acetylated hemicellulose productive rate: 13.2%.
Claims (7)
1. a method for preparing cellulose acetate from wheat straws, is characterized in that: the method comprises the steps:
The first step, pre-treatment and activation and bleaching: wheat straw is carried out to high temperature poach, activation, bleaching;
Second step, mechanical disintegration: the wheat straw of processing through the first step is carried out to mechanical disintegration processing;
The 3rd step, acetylization reaction: by the wheat straw placing response device after pulverizing, add esterifying liquid, and add catalyzer to carry out acetylize processing;
The 4th step, adopts cryogenic condensation mode to recycle esterifying liquid;
The 5th step, acetylize product separation: the solution supernatant liquor in reactor is separated, discarded precipitation; In supernatant liquor, add distilled water, separate out precipitation, washed several times with water, to neutrality, through suction filtration, vacuum-drying, finally obtains acetylize product, then carries out pulverization process;
The 6th step, the acetylize product different to solvent extraction component: 1. the acetylize product of handling well in the 5th step is carried out to extracting with acetone; 2. steam the most of acetone in previous step solution, then in solution, add distilled water again to isolate insolubles according to step 5, then use the mixed solution extracting of acetone and water; 3. use the solute in the mixed solution extracting previous step of second alcohol and water, by extracting the insolubles obtaining for above-mentioned three times, dry and get final product finished product;
In above-mentioned the first step pre-treatment and activation and bleaching process, by wheat stalk high temperature poach, add sodium hydroxide to activate, add clorox and mixed solution of hydrogen peroxide to bleach simultaneously, the amount that wherein adds sodium hydroxide is to add 1% of quality, and the amount that adds clorox and mixed solution of hydrogen peroxide is to add 2% of volume of water;
In the 3rd described step acetylization reaction process, in esterifying liquid, diacetyl oxide accounts for 20%～25% of esterifying liquid volume, and glacial acetic acid accounts for 75%～80% of esterifying liquid volume; Described catalyzer is sodium pyrosulfate, hydrofluoric acid and the vitriol oil, wherein sodium pyrosulfate add-on be in reactor wheat stalk solid masses 0.5%～3%, the add-on of hydrofluoric acid is 1%～3% of esterifying liquid volume, the add-on of the vitriol oil is 0.3%～2% of esterifying liquid volume.
2. the method for a kind of preparing cellulose acetate from wheat straws according to claim 1, is characterized in that: in described second step mechanical disintegration process, the granularity of the wheat straw after pulverizing is 150 orders.
3. the method for a kind of preparing cellulose acetate from wheat straws according to claim 1, it is characterized in that: in the 6th described step, use for the second time in the mixed solution extractive process of acetone and water, the amount of water is liquor capacity 9%～11%, and the amount of acetone is liquor capacity 89%～91%.
4. the method for a kind of preparing cellulose acetate from wheat straws according to claim 1, it is characterized in that: in the 6th described step, while using for the third time the solute in the mixed solution extracting previous step of second alcohol and water, the amount of water is 24%～26% of liquor capacity, and the amount of ethanol is liquor capacity 74%～76%.
5. the method for a kind of preparing cellulose acetate from wheat straws according to claim 1, is characterized in that: in described acetylization reaction process, in reactor, solid volume is 16%～18%, and liquid volume is 82%～84%; This reaction is carried out 2 hours under the condition of 60～80 ℃, obtains auburn solution.
6. the method for a kind of preparing cellulose acetate from wheat straws according to claim 1, it is characterized in that: in the 4th described step, condensation at low temperature reclaims in glacial acetic acid process, employing is heated reactor, reclaim glacial acetic acid simultaneously, wherein be 0.5 hour heat-up time, and reactor naturally cools to room temperature and stops reclaiming glacial acetic acid.
7. the method for a kind of preparing cellulose acetate from wheat straws according to claim 1, is characterized in that: in the 6th described step, institute's extracting product is respectively:
Extracting for the first time solute is Cellulose diacetate, acetylated hemicellulose and acetylize xylogen, and insolubles is cellulosetri-acetate;
The solute extracting is for the second time acetylated hemicellulose and acetylize xylogen, and insolubles is Cellulose diacetate;
The solute extracting is for the third time acetylize xylogen, and insolubles is acetylated hemicellulose.
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| CN105111461B (en) * | 2015-09-23 | 2018-04-06 | 广西大学 | A kind of method that mechanical activation solid phase reaction prepares lignin ester |
| CN105924336A (en) * | 2016-05-10 | 2016-09-07 | 复旦大学 | Method for preparation of aromatic aldehyde by means of waste biomass pretreated with dilute acid and through acetylation |
| CN111171337A (en) * | 2020-02-20 | 2020-05-19 | 广州楹鼎生物科技有限公司 | Preparation method of acetylated lignocellulose |
| CN112430910A (en) * | 2020-10-29 | 2021-03-02 | 武汉轻工大学 | Method for preparing cellulose acetate and P25 porous flexible fibrous membrane by electrospinning, porous flexible fibrous membrane obtained by same and application thereof |
| CN112898438A (en) * | 2021-02-20 | 2021-06-04 | 天津信诚康达药业有限公司 | Preparation method of cellulose acetate particles |
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| CN101139400A (en) * | 2006-09-08 | 2008-03-12 | 中国科学院过程工程研究所 | method for separating straw acetylized component and preparing straw cellulose acetate |
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| CN101139400A (en) * | 2006-09-08 | 2008-03-12 | 中国科学院过程工程研究所 | method for separating straw acetylized component and preparing straw cellulose acetate |
Non-Patent Citations (2)
| Title |
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| 叶生梅.稻草秸秆预处理实验研究.《安徽工程科技学院学报》.2008,第23卷(第4期),24-26. |
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