CN110396134A - A kind of synthetic method of cellulose triacetate - Google Patents
A kind of synthetic method of cellulose triacetate Download PDFInfo
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- CN110396134A CN110396134A CN201910729615.0A CN201910729615A CN110396134A CN 110396134 A CN110396134 A CN 110396134A CN 201910729615 A CN201910729615 A CN 201910729615A CN 110396134 A CN110396134 A CN 110396134A
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- chloroacetic chloride
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B3/00—Preparation of cellulose esters of organic acids
- C08B3/06—Cellulose acetate, e.g. mono-acetate, di-acetate or tri-acetate
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Abstract
It is that the method that acylation synthesizes Triafol T occurs with cellulose for acylating reagent that the invention discloses a kind of using chloroacetic chloride.Its specific practice is as follows :(a) lignocellulosic glacial acetic acid is sequentially added reaction kettle, stir-activating to system is in uniform pulpous state；(b) chloroacetic chloride is added in Xiang Shangshu system and catalyst, catalyst are the concentrated sulfuric acid;(c) deionized water and neutralizer are added after insulation reaction, into system, a large amount of white solids of precipitation through negative pressure leaching, deionized water washing, dry etc. handle degree of substitution be 2.8 ~ 3.0 Triafol T.This method replaces traditional acetic anhydride that esterification occurs with cellulose for raw material and synthesizes cellulose acetate using chloroacetic chloride, because chloroacetic chloride boiling point is relatively low, esterification is set to maintain the reflux for state substantially, easily controllable reaction temperature, the defect that traditional higher boiling acetic anhydride later period consumes due to hydrolysis generates a large amount of acetic acid is efficiently avoided, production cost is reduced.
Description
Technical field
The invention belongs to cellulose fields, and in particular to fine for three acetic acid of Material synthesis using a kind of chloroacetic chloride and cellulose
The method for tieing up element.
Background technique
Cellulose is a kind of natural high molecular substance, mainly passes through Isosorbide-5-Nitrae-dehydration polymerization into long-chain high score by β-glucose
Son, each glucose unit can be replaced containing there are three alcoholic extract hydroxyl group (- OH) by nucleophilic group or nucleophilic compound, generate corresponding
Cellulose esters.Cellulose acetate (cellulose acetate) is important one of the derivative of cellulose, is by German for the first time
Schuzenberger in 1865 with cellulose and acetic acid certain pressure, at a temperature of synthesize, generally according to acetyl content
Difference, cellulose acetate can be mainly divided into Triafol T (TAC) and cellulose diacetate (DAC).The wherein substitution of TAC
Degree is 2.7 ~ 3.0, and acetic acid binding capacity range is 59 ~ 62%, can be dissolved in chloroform, in methylene chloride-methanol mixed solution, mainly
For photographic film, textile fabric, liquid crystal display polarizing film and other function fiber membrane material etc.；The substitution of DAC
Degree is 2.2 ~ 2.5, and acetic acid binding capacity range is 52 ~ 56%, dissolves in acetone, tetrahydrofuran and 1:1 benzene-methanol mixed solvent, main
It is used for the raw material such as plastics, packaging material, cigarette filter and textile fabric.
Cellulose acetate is mostly the hydroxyl using natural wood pulps or Cotton Pulp as primary raw material, on cellulose molecular chain
Product after being replaced by acetoxyl group.Mostly use in existing Triafol T mass production techniques using glacial acetic acid as solvent and
Under catalyst existence condition, esterification is carried out using various native celluloses and acetic anhydride, then pass through saponification adjustment degree of substitution
Afterwards, the process route of Triafol T is prepared through processes such as filtering, molding, cleaning, dehydration, drying.It is existing disclose it is more
In the patent of a countries and regions such as: Chinese patent CN107286258B, CN100484960C, CN102153660B,
CN108948214A,CN108383915A；Japan Patent JP2016-160563A, United States Patent (USP) US4888147, British patent
GB169741A and TaiWan, China patent TW1404844B, TW201129737A etc. all refer to above-mentioned cellulose acetate preparation
Technology.In existing public technology, relative to cellulose largely excessive acylating reagent acetic anhydride mostly with later period hydrolytic process
It generates acetum and isolates acetic acid use through rectifying, is i.e. increase energy consumption consumes a large amount of acetic anhydride again, it is raw to directly affect product
Produce cost.
In recent years, since water treatment agent hydroxy ethylene diphosphonic acid serialization commercial production scale increasingly extends, work is developed
The high added value downstream product of industry connection by-product chloroacetic chloride reduces the hot spot that major product production cost is increasingly becoming the sector research.
Summary of the invention
To solve technical problem present in prior art, it using chloroacetic chloride is acylating reagent and fine that the present invention, which provides a kind of,
The method that acylation synthesis Triafol T occurs for dimension element.Excessive chloroacetic chloride is by steaming recycling in reaction outside low-temperature negative-pressure
And can be recycled, the quantum of output of later period acetic acid is reduced, energy consumption is reduced, advantageously reduces production cost.
A kind of synthetic method of cellulose triacetate, specific technical solution are as follows:
(a) it will crush and sequentially add reaction kettle in lignocellulosic, the glacial acetic acid of cotton shape, 1 ~ 2 hour is stirred at 20 ~ 30 DEG C extremely
System is in uniform pulpous state；
(b) chloroacetic chloride and catalyst is added in Xiang Shangshu system, stirs heating and insulation reaction for a period of time；
(c) after insulation reaction, system, which is cooled to 30 ~ 40 DEG C and establishes outside -0.03 ~ -0.01MPa negative pressure, steams 1 ~ 1.5 hour,
Then deionized water and neutralizer are added into system, a large amount of white solids of precipitation wash through negative pressure leaching, deionized water, is true
Sky is dried to obtain cellulose triacetate.
Wherein, the mass ratio that feeds intake of lignocellulosic and glacial acetic acid is 1:4 ~ 10 in the step (a).
Wherein, the mass ratio of chloroacetic chloride additional amount and lignocellulosic is 9 ~ 15:1 in the step (b).
Wherein, catalyst is the concentrated sulfuric acid that mass percent concentration is 80 ~ 90% in the step (b).
Wherein, it is quality % that catalyst amount, which is 5 ~ 15%, % of lignocellulosic inventory, in the step (b).
Wherein, insulation reaction temperature is 50 ~ 55 DEG C in the step (b).
Wherein, the insulation reaction time is 2 ~ 4 hours in the step (b).
Wherein, neutralizer is sodium acetate aqueous solution that mass percentage content is 10 ~ 20% in the step (c).
The present invention using chloroacetic chloride replace traditional acid anhydrides as acylating reagent, in the prior art, chloroacetic chloride compared to
For acetic anhydride: (1) reacting more violent；(2) acetic anhydride makees catalyst using Bronsted acid, chloroacetic chloride using lewis acid or
Organic base is as acid binding agent；(3) chloroacetic chloride can will form acid anhydrides with the reaction of activator glacial acetic acid, and require absolute；(4) second
Acyl chlorides price is higher.So the prior art generally comprehensively considers, the esterification of Triafol T is carried out using acid anhydrides.
In the present invention, use chloroacetic chloride as acylating reagent, difficult point therein is to control the stabilization of reaction and chloride ion
Property and exclude in time, the glacial acetic acid that the present invention uses can stablize the stability of acyl cation as protic.More
, 5-15% is added, preferably (in the prior art using in acetic anhydride, sulfuric acid is the sulfuric acid of 10-14% as catalyst amount
0.5-5%).Chloride ion forms hydrogen chloride under strongly acidic conditions, is evaporated off, and guarantees that reaction continues, rather than uses alkaline acid binding agent
Such as triethylamine, pyridine or piperidines and lewis acid because reaction be acid condition under, and generate Triafol T exist
Hydrolyzed under basic conditions.Using low temperature (50-55 DEG C) back flow reaction, at a temperature of this, hydrogen chloride is evaporated off, monoxone then flow back and
In acetic acid solvent, to control the severe degree of reaction.
Subsequent processing does not need to hydrolyze, and excessive chloroacetic chloride can be evaporated off by low pressure, and reaction terminates.Reaction is whole anhydrous, dense
Water impurity in sulfuric acid generates acetic acid (solvent) and hydrogen chloride (being evaporated off) by excessive excess acetyl chloride, does not influence to react.In adding
After agent, white solid Triafol T is precipitated, in reaction process, without having to worry about the formation of sulphonic acid ester, compared to sulphonic acid ester
Reaction constant, what chloroacetic chloride esterification constant will be big is more.Due to having used suitable sulfuric acid, without the shape for worrying acid anhydrides
At on the one hand the highly acid of sulfuric acid provides hydrogen ion formation hydrogen chloride and is evaporated off, on the one hand also suppressed acetic acid ionization, acetate amount
It reduces, chloroacetic chloride is more and cellulose alcoholic extract hydroxyl group reacts, even if forming acid anhydrides on a small quantity, finally also reacts with cellulose alcoholic extract hydroxyl group
At ester.
Beneficial effect of the invention: replacing traditional acetic anhydride using chloroacetic chloride is that esterification occurs for raw material and cellulose
Synthesize cellulose acetate makes esterification maintain the reflux for state, easily controllable reaction substantially because chloroacetic chloride boiling point is relatively low
Temperature；A large amount of excessive acylating reagents can obtain high-purity acetyl chlorine through steaming recycling outside low-temperature negative-pressure and recycle, and be effectively prevented from
The defect that traditional higher boiling acetic anhydride later period consumes due to hydrolysis generates a large amount of acetic acid, reduces production cost.
Specific embodiment
For further description meaning of the present invention, content according to the present invention is carried out below with reference to embodiment
It illustrates, but its content is not defined.
Embodiment 1
The 60g lignocellulosic for being in cotton shape will be crushed and 400g glacial acetic acid sequentially adds reaction kettle, stir-activating at 20 ~ 30 DEG C
After 1.5 hours, system is in uniform pulpous state；The concentrated sulfuric acid that 600g chloroacetic chloride and 6g mass percent concentration are 82% is added to
It states pulpous state system, under stirring condition, is to slowly warm up to 50 ~ 55 DEG C of insulation reactions 4 hours, system is in micro- muddy thick, reaction life
At hydrogen chloride enter device for absorbing tail gas；System is cooled to 35 DEG C and establishes outside -0.02MPa negative pressure that steam 1 small after reaction
When obtain gas chromatographic purity be 99.54% chloroacetic chloride 145.38g；300g deionized water stirring hydrolysis 30min is added into system
Be added the aqueous sodium acetate solution neutralizer that 28g mass percent concentration is 15% afterwards, the white solid of precipitation through negative pressure leaching,
200g deionized water washs in four times, 30 ~ 40 DEG C vacuum drying 12 hours degree of substitution is 2.91, acetic acid binding capacity is 61.21%
Triafol T, chloride ion content is (with Cl in product-Meter) 0.0163%, acetic acid radical content 0.0034%.
Embodiment 2
The 60g lignocellulosic for being in cotton shape will be crushed and 380g glacial acetic acid sequentially adds reaction kettle, stir-activating at 20 ~ 30 DEG C
After 2 hours, system is in uniform pulpous state；The concentrated sulfuric acid that 720g chloroacetic chloride and 10g mass percent concentration are 85% is added to above-mentioned
Pulpous state system under stirring condition, is to slowly warm up to 50 ~ 55 DEG C of insulation reactions 3 hours, and in micro- muddy thick, reaction generates system
Hydrogen chloride enter device for absorbing tail gas；System is cooled to 35 DEG C and establishes outside -0.03MPa negative pressure that steam 1.5 small after reaction
When obtain gas chromatographic purity be 99.62% chloroacetic chloride 239.41g；After 200g deionized water stirring hydrolysis 30min is added into system
The aqueous sodium acetate solution neutralizer that 120 mass percent concentrations are 10% is added, the white solid of precipitation is through negative pressure leaching, 200g
Deionized water washs in four times, 30 ~ 40 DEG C vacuum drying 12 hours degree of substitution is 2.95, acetic acid binding capacity is the three of 61.34%
Cellulose acetate.
Comparative example 1
The 60g lignocellulosic for being in cotton shape will be crushed and 400g glacial acetic acid sequentially adds reaction kettle, stir-activating at 20 ~ 30 DEG C
After 1.5 hours, system is in uniform pulpous state；The concentrated sulfuric acid that 600g chloroacetic chloride and 2g mass percent concentration are 82% is added to
It states pulpous state system, under stirring condition, is to slowly warm up to 50 ~ 55 DEG C of insulation reactions 4 hours, system is in micro- muddy thick, reaction life
At hydrogen chloride enter device for absorbing tail gas；System is cooled to 35 DEG C and establishes outside -0.02MPa negative pressure that steam 1 small after reaction
When obtain gas chromatographic purity be 99.54% chloroacetic chloride 145.38g；300g deionized water stirring hydrolysis 30min is added into system
Be added the aqueous sodium acetate solution neutralizer that 28g mass percent concentration is 15% afterwards, the white solid of precipitation through negative pressure leaching,
200g deionized water washs in four times, 30 ~ 40 DEG C vacuum drying 12 hours degree of substitution is 2.91, acetic acid binding capacity is 61.21%
Triafol T, chloride ion content is (with Cl in product-Meter) 0.05%, acetic acid radical content 0.0034%.
Comparative example 2
The 60g lignocellulosic for being in cotton shape will be crushed and 380g glacial acetic acid sequentially adds reaction kettle, stir-activating at 20 ~ 30 DEG C
After 2 hours, system is in uniform pulpous state；The concentrated sulfuric acid that 720g chloroacetic chloride and 12g mass percent concentration are 85% is added to above-mentioned
Pulpous state system under stirring condition, is to slowly warm up to 50 ~ 55 DEG C of insulation reactions 3 hours, and in micro- muddy thick, reaction generates system
Hydrogen chloride enter device for absorbing tail gas；System is cooled to 35 DEG C and establishes outside -0.03MPa negative pressure that steam 1.5 small after reaction
When obtain gas chromatographic purity be 99.62% chloroacetic chloride 239.41g；After 200g deionized water stirring hydrolysis 30min is added into system
The aqueous sodium acetate solution neutralizer that 120 mass percent concentrations are 10% is added, the white solid of precipitation is through negative pressure leaching, 200g
Deionized water washs in four times, 30 ~ 40 DEG C vacuum drying 12 hours degree of substitution is 2.95, acetic acid binding capacity is the three of 61.34%
Cellulose acetate, but application is used as the not high of cellulose triacetate film transparency
Comparative example 3
The 60g lignocellulosic for being in cotton shape will be crushed and 400g methylene chloride sequentially adds reaction kettle, stirred and live at 20 ~ 30 DEG C
After changing 1.5 hours, system is in uniform pulpous state；600g chloroacetic chloride and 780g triethylamine are added to above-mentioned pulpous state system, stirring bar
Under part, be to slowly warm up to 50 ~ 55 DEG C of insulation reactions 4 hours, system in micro- muddy thick,；System is cooled to 35 after reaction
℃；Into system be added 300g deionized water be precipitated white solid washed in four times through negative pressure leaching, 200g deionized water, 30
~ 40 DEG C vacuum drying 12 hours degree of substitution is 2.01, the Triafol T that acetic acid binding capacity is 61.21%, in product chlorine from
Sub- content is (with Cl-Meter) 0.0163%, acetic acid radical content 0.0034%.
Comparative example 4
The 60g lignocellulosic for being in cotton shape will be crushed and 500g glacial acetic acid sequentially adds reaction kettle, stir-activating at 20 ~ 30 DEG C
After 1.5 hours, system is in uniform pulpous state；The concentrated sulfuric acid that 600g acetic anhydride and 13g mass percent concentration are 85% is added to
It states pulpous state system, under stirring condition, is to slowly warm up to 50 ~ 55 DEG C of insulation reactions 6 hours；It is added after reaction into system
The aqueous sodium acetate solution neutralizer that 28g mass percent concentration is 15%, body is added after 300g deionized water stirring hydrolysis 30min
Unreacted acetic anhydride is hydrolyzed to acetic acid in system, and filtrate, which is warming up to outside 90 DEG C of negative pressure, after negative pressure leaching steams recovery of acetic acid；Filtering
Afterwards gained white solid wash in four times through 200g deionized water, 30 ~ 40 DEG C vacuum drying 12 hours degree of substitution be 2.85, vinegar
The Triafol T that sour binding capacity is 59.73%.
It is attached: the detection method of product acetic acid binding capacity (degree of substitution)
Weigh 1.5g(and be accurate to 0.001g) cellulose acetate sample, it is placed in and fills 50mL dimethyl sulfoxide (analyzing pure grade)
Flask is put into 80 ± 2 DEG C of water bath with thermostatic control and shake to sample is completely dissolved by 250mL in the flask of ground glass stopper,
Flask is taken out to be cooled to room temperature.Under ceaselessly stirring state, being slowly added to 23.50mL concentration into flask with buret is
The standard solution of sodium hydroxide of 1.0mol/L continues to stir 3h, and carefully by the material wash bottle on flask neck and grinding port plug
It washes in flask, the sulfuric acid standard solution that 25mL concentration is 1.0mol/L is then added, be further continued for stirring digestion 0.5 hour；With
Phenolphthalein is indicator, and with the sulfuric acid of standard solution of sodium hydroxide overtitration, titration process to be sufficiently stirred so that acetate fiber
Element is in suspended state；Prepare only to fill the flask of 50mL dimethyl sulfoxide while doing blank test.Acetic acid binding capacity presses following public affairs
Formula calculates:
Claims (8)
1. a kind of synthetic method of cellulose triacetate, which is characterized in that specifically comprise the following steps:
Reaction kettle is sequentially added in lignocellulosic, the glacial acetic acid of cotton shape by crushing, 1 ~ 2 hour is stirred at 20 ~ 30 DEG C to body
System is in uniform pulpous state；
Chloroacetic chloride and catalyst is added to above-mentioned system, stirs heating and insulation reaction for a period of time；
After insulation reaction, system is cooled to 30 ~ 40 DEG C and establishes steaming 1 ~ 1.5 hour outside -0.03 ~ -0.01MPa negative pressure, so
Deionized water and neutralizer are added in backward system, a large amount of white solids of precipitation are through negative pressure leaching, deionized water washing, vacuum
It is dried to obtain cellulose triacetate.
2. the method according to claim 1, wherein in the step (a) lignocellulosic and glacial acetic acid throwing
Material mass ratio is 1:4 ~ 10.
3. the method according to claim 1, wherein chloroacetic chloride additional amount and wood fibre in the step (b)
The mass ratio of element is 9 ~ 15:1.
4. the method according to claim 1, wherein catalyst is mass percent concentration in the step (b)
For 80 ~ 90% concentrated sulfuric acid.
5. according to the method described in claim 4, it is characterized in that, catalyst amount is lignocellulosic in the step (b)
5 ~ 15%, % of inventory is quality %.
6. the method according to claim 1, wherein insulation reaction temperature is 50 ~ 55 DEG C in the step (b).
7. the method according to claim 1, wherein the insulation reaction time is 2 ~ 4 hours in the step (b).
8. the method according to claim 1, wherein neutralizer is mass percentage content in the step (c)
For 10 ~ 20% sodium acetate aqueous solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113582756A (en) * | 2021-08-03 | 2021-11-02 | 中诚国联（河南）生物科技有限公司 | Pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off and application thereof |
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Application publication date: 20191101 |