CN104558205B - A kind of preparation method of low-viscosity sodium carboxymethyl cellulose - Google Patents
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Abstract
The present invention relates to a kind of preparation method of low-viscosity sodium carboxymethyl cellulose, belong to technical field of polymer chemistry.Methods described is with inexpensive wood pulp cellulose as raw material, alkalization is mixed by the mixed solution with sodium hydrate aqueous solution and ethanol, it is 6.5~8.0 with chloroacetic ethanol solution etherificate, the oxidizing viscosity reduction with ethanol dilution, with acid for adjusting pH value, again with three washings of ethanol water, centrifugation, prepared low-viscosity sodium carboxymethyl cellulose is finally dried.Methods described is simple; without pretreatment of raw material process; it is easy to operate, process stabilizing, low production cost, it is easy to large-scale production; obtained sodium carboxymethylcellulose is white or micro-yellow powder; uniformity is good, and viscosity is low, is 10~60mPas; purity is high, with dissolution velocity it is fast, good dispersion, transparency are good the characteristics of.
Description
Technical field
The present invention relates to a kind of preparation method of low-viscosity sodium carboxymethyl cellulose, belong to technical field of polymer chemistry.
Background technology
Sodium carboxymethylcellulose (abbreviation CMC or Na-CMC), be native cellulose in the basic conditions with chloroacetate reaction
Obtained from a kind of water-soluble ionic-type ether, be widely used in daily chemical industry, textile industry, paper industry and oilfield exploitation
Deng field.CMC shows the performance of many brilliances in paper industry, is received by increasing enterprise.CMC is mainly used in
The coating waste water of paper and cardboard, as the rheological control agents of coating, water-loss reducer, film forming agent and auxiliary adhesive and some spies
Plant the Cypres of paper.Meanwhile, CMC is also acted as and is helped fluid flow enhancer, and cationic starch is replaced with a small amount of CMC, can be obtained
Good synergy.Due to CMC function admirables, converted starch, current China are not used in the preparation of European coating
Required CMC almost all in terms of painting processing paper production relies on import.
CMC industrialized productions mainly have water-borne method, solvent method and solwution method.Water-borne method is in alkalization and etherification procedure
With water as reaction medium, its technological process and equipment are relatively simple, mainly for the production of oil, the field such as weaving and detergent industry
Low side sodium carboxymethylcellulose.Solvent method in alkalization and etherification procedure with organic solvent as reaction medium, its production cycle
It is short, but high cost, mainly for the production of middle and high end sodium carboxymethylcellulose.Solwution method, also known as ionic liquid, because solvent is returned
Receive and economically the reason for, still in the laboratory research stage.
Using cellulose pulp or the poor-performing of wood pulp cellulose, obtained CMC in being prepared due to many productions at present
Viscosity is high, and yellowish, purity is not high.Produced under similar process conditions, it is high to there is also the purified cotton prices of raw materials,
The characteristics of efficiency is low, and post-processing technology difficulty is larger is etherified, the viscosity of obtained CMC is higher, significantly limit its popularization
Using.
The method for preparing low viscosity CMC at this stage is concentrated mainly on by oxidative degradation so as to obtain low viscosity CMC, as in
State's patent CN101548732, CN102367279, CN1490336, CN101455286 and CN101548733.In patent
In CN101548732, CN101455286 and CN101548733, viscosity reduction is to complete in neutral conditions, so to obtain relatively low
The CMC of viscosity is accomplished by extending process time；In CN102367279, by adding thinner by several times at different conditions, so
Operation difficulty is increased, while also more difficult control viscosity reduction degree, is unfavorable for obtaining the CMC of target viscosities；Patent CN1490336
In, under the conditions of slurry process, low viscosity CMC is obtained by oxidizing reduction, increased the cost of solvent recovery.Chinese patent
CN103242453 is raw material by from microcrystalline cellulose, and low viscosity CMC is obtained by alkalization, etherificate, is increased in preparation process
The preprocessing process of cellulosic material is added, so that manufacturing cost rises.
The content of the invention
For the defect that prior art is present, it is an object of the invention to provide a kind of low-viscosity sodium carboxymethyl cellulose
Preparation method, methods described as raw material, washed from inexpensive wood pulp by alkalization, etherificate, oxidizing reduction, neutralization, from
The heart, secondary washing, centrifugation, three washings, it is centrifuged and dries each operation and carry out synthesis low-viscosity sodium carboxymethyl cellulose successively.
To realize the purpose of the present invention, there is provided following technical scheme.
A kind of preparation method of low-viscosity sodium carboxymethyl cellulose, methods described step is as follows：
(1) alkalize：The mixed solution of sodium hydrate aqueous solution and ethanol is mixed with wood pulp cellulose, at 20 DEG C~35 DEG C
Alkali cellulose is generated after alkalization 30min~60min；
Wherein, wood pulp cellulose and the mass ratio of NaOH are 10:3~7；
(2) it is etherified：To chloroacetic ethanol solution is added in alkali cellulose, add and stir below 35 DEG C, so
After be warming up to 78 DEG C~80 DEG C and carry out etherification reaction 20min~60min；
Wherein, wood pulp cellulose and chloroacetic mass ratio are 10:3~8, chloroethene in the chloroacetic ethanol solution
The mass percent of acid is 58%~62%；
(3) oxidative degradation：The material that step (2) etherification reaction is obtained is cooled to less than 60 DEG C, is added and is diluted through ethanol
Oxidant, oxidative degradation 20min~50min；
Wherein, wood pulp cellulose and the mass ratio of oxidant are 10:1~3；The oxidant is hypochlorous acid, hydrogen peroxide
Or potassium permanganate；It is preferred that at the uniform velocity being added in 10min~15min；
(4) washing centrifugation is neutralized：The pH value for obtaining material with sour regulating step (3) oxidative degradation is 6.5~8.0, then is used
Ethanol water is washed, and is then centrifuged for removing ethanol；
Wherein, the percentage by volume of ethanol is 65%~75% in the ethanol water；It is described acid be preferably hydrochloric acid or
Acetic acid；
(5) secondary washing centrifugation：Material after being centrifuged to step (4) with ethanol water is washed, and is then centrifuged for
Except ethanol；
Wherein, the percentage by volume of ethanol is 70%~80% in the ethanol water；
(6) three washing centrifugations：Material after being centrifuged to step (5) with ethanol water is washed, and is then centrifuged for, and is obtained
To being precipitated as wet sodium carboxymethylcellulose；
Wherein, the percentage by volume of ethanol is 80%~90% in the ethanol water；
The percentage by volume of ethanol increases successively in step (4), (5), the ethanol water used in (6)；
(7) dry：By the wet sodium carboxymethylcellulose that step (6) is obtained dry weight/mass percentage composition to water 2% with
Under, dry sodium carboxymethyl starch is obtained, it is a kind of low-viscosity sodium carboxymethyl cellulose of the present invention.
Beneficial effect
1., the invention provides a kind of preparation method of low-viscosity sodium carboxymethyl cellulose, methods described uses inexpensive wood
Pulp cellulose is raw material, effectively reduces production cost；
2., the invention provides a kind of preparation method of low-viscosity sodium carboxymethyl cellulose, used in methods described
Oxidant is added after etherification reaction, oxidizing reduction is carried out in the basic conditions, the feed postition of oxidant uses oxidant
After being diluted through ethanol solution, it is uniformly added into 10min~15min, the sodium carboxymethylcellulose uniformity for obtaining is good, and viscosity is
10mPas~60mPas；
3. the invention provides a kind of preparation method of low-viscosity sodium carboxymethyl cellulose, washing process elder generation in methods described
Using the washing of low concentration ethanol water twice, it is used to improve the purity of resulting material, the low viscosity carboxylic for finally obtaining can be made
Purity >=98% of sodium carboxymethylcellulose pyce, then using high concentration ethanol water wash, obtain apparent condition for white or
It is the low-viscosity sodium carboxymethyl cellulose of yellow；
4., the invention provides a kind of preparation method of low-viscosity sodium carboxymethyl cellulose, methods described is simple, without raw material
Preprocessing process, easy to operate, process stabilizing, low production cost, it is easy to large-scale production；
5. the invention provides a kind of preparation method of low-viscosity sodium carboxymethyl cellulose, obtained carboxylic first in this way
Base sodium cellulosate, apparent condition is white or micro-yellow powder, and viscosity is low, and purity is high, with dissolution velocity is fast, good dispersion,
The characteristics of transparency is good.
Specific embodiment
The present invention, but not limited to this are described in detail in detail with reference to specific embodiment.
In following examples：
The wood pulp cellulose produces " silver-colored star " board wood pulp for Chile, and the degree of polymerization is 1000~1200.
The detection of the low-viscosity sodium carboxymethyl cellulose for preparing is according to GB 1904-2005《Food additives carboxymethyl
Sodium cellulosate》Described in method carry out；Viscosity is 2% aqueous solution, under the conditions of 25 DEG C, is examined with Brookfield LVT viscosimeters
Survey.
Embodiment 1
(1) at 35 DEG C, to adding loose wood pulp cellulose 2Kg in kneader, while add by 3000mL ethanol with
1.6Kg mass percents are the mixture of 50% sodium hydrate aqueous solution composition, raw after quaternization 60min under stirring condition
Into alkali cellulose；
(2) in alkali cellulose add 1.55Kg mass percents be 58% chloroacetic ethanol solution, 35 DEG C with
Lower addition simultaneously stirs 15min, and then heating to 78 DEG C carries out etherification reaction 20min；
(3) material that step (2) etherification reaction is obtained is cooled to 60 DEG C, at the uniform velocity added in 10min 150mL hydrogen peroxide with
The mixed solution of 1500mL ethanol, oxidative degradation 25min；
(4) the pH value ≈ 7.0 of material is obtained with hydrochloric acid regulating step (3) oxidative degradation, then is 70% with percentage by volume
Ethanol water washed, be then centrifuged for remove ethanol；
(5) material after being centrifuged to step (4) with the ethanol water that percentage by volume is 75% is washed, Ran Houli
The heart removes ethanol；
(6) material after being centrifuged to step (5) with the ethanol water that percentage by volume is 80% is washed, Ran Houli
The heart, it is wet sodium carboxymethylcellulose to be precipitated；
(7) the wet sodium carboxymethylcellulose that step (6) is obtained is dried into the weight/mass percentage composition to water 2% at 80 DEG C
Hereinafter, dry sodium carboxymethylcellulose is obtained, is a kind of low-viscosity sodium carboxymethyl cellulose of the present invention.
The low-viscosity sodium carboxymethyl cellulose that the present embodiment is prepared is detected, it is as a result as follows：
Substitution value is 0.73, and purity is 98%, and viscosity is 55mPas.
Embodiment 2
(1) at 30 DEG C, to adding loose wood pulp cellulose 2Kg in kneader, while add by 3200mL ethanol with
1.8Kg mass percents are the mixture of 50% sodium hydrate aqueous solution composition, raw after quaternization 60min under stirring condition
Into alkali cellulose；
(2) in alkali cellulose add 1.68Kg mass percents be 60% chloroacetic ethanol solution, 35 DEG C with
Lower addition simultaneously stirs 15min, and then heating to 78 DEG C carries out etherification reaction 20min；
(3) material that step (2) etherification reaction is obtained is cooled to 60 DEG C, at the uniform velocity added in 10min 200mL hydrogen peroxide with
The mixed solution of 1500mL ethanol, oxidative degradation 25min；
(4) the pH value ≈ 7.0 of material is obtained with hydrochloric acid regulating step (3) oxidative degradation, then is 70% with percentage by volume
Ethanol water washed, be then centrifuged for remove ethanol；
(5) material after being centrifuged to step (4) with the ethanol water that percentage by volume is 75% is washed, Ran Houli
The heart removes ethanol；
(6) material after being centrifuged to step (5) with the ethanol water that percentage by volume is 80% is washed, Ran Houli
The heart, it is wet sodium carboxymethylcellulose to be precipitated；
(7) the wet sodium carboxymethylcellulose that step (6) is obtained is dried into the weight/mass percentage composition to water 2% at 80 DEG C
Hereinafter, dry sodium carboxymethylcellulose is obtained, is a kind of low-viscosity sodium carboxymethyl cellulose of the present invention.
The low-viscosity sodium carboxymethyl cellulose that the present embodiment is prepared is detected, it is as a result as follows：
Substitution value is 0.75, and purity is 98%, and viscosity is 30mPas.
Embodiment 3
(1) at 30 DEG C, to adding loose wood pulp cellulose 2Kg in kneader, while add by 3300mL ethanol with
2.2Kg mass percents are the mixture of 50% sodium hydrate aqueous solution composition, raw after quaternization 60min under stirring condition
Into alkali cellulose；
(2) to the chloroacetic ethanol solution that 2.0Kg mass percents are 62% is added in alkali cellulose, below 35 DEG C
15min is added and stirs, then heating to 78 DEG C carries out etherification reaction 20min；
(3) material that step (2) etherification reaction is obtained is cooled to 60 DEG C, at the uniform velocity added in 10min 180mL hydrogen peroxide with
The mixed solution of 1500mL ethanol, oxidative degradation 20min；
(4) the pH value ≈ 7.0 of material is obtained with hydrochloric acid regulating step (3) oxidative degradation, then is 68% with percentage by volume
Ethanol water washed, be then centrifuged for remove ethanol；
(5) material after being centrifuged to step (4) with the ethanol water that percentage by volume is 80% is washed, Ran Houli
The heart removes ethanol；
(6) material after being centrifuged to step (5) with the ethanol water that percentage by volume is 85% is washed, Ran Houli
The heart, it is wet sodium carboxymethylcellulose to be precipitated；
(7) the wet sodium carboxymethylcellulose that step (6) is obtained is dried into the weight/mass percentage composition to water 2% at 80 DEG C
Hereinafter, dry sodium carboxymethylcellulose is obtained, is a kind of low-viscosity sodium carboxymethyl cellulose of the present invention.
The low-viscosity sodium carboxymethyl cellulose that the present embodiment is prepared is detected, it is as a result as follows：
Substitution value is 0.81, and purity is 99%, and viscosity is 45mPas.
Embodiment 4
(1) at 25 DEG C, to adding loose wood pulp cellulose 2Kg in kneader, while add by 3000mL ethanol with
2.2Kg mass percents are the mixture of 50% sodium hydrate aqueous solution composition, raw after quaternization 60min under stirring condition
Into alkali cellulose；
(2) to the chloroacetic ethanol solution that 2.1Kg mass percents are 62% is added in alkali cellulose, below 35 DEG C
15min is added and stirs, then heating to 78 DEG C carries out etherification reaction 20min；
(3) material that step (2) etherification reaction is obtained is cooled to 60 DEG C, at the uniform velocity added in 15min 300mL hydrogen peroxide with
The mixed solution of 1500mL ethanol, oxidative degradation 30min；
(4) the pH value ≈ 7.0 of material is obtained with hydrochloric acid regulating step (3) oxidative degradation, then is 70% with percentage by volume
Ethanol water washed, be then centrifuged for remove ethanol；
(5) material after being centrifuged to step (4) with the ethanol water that percentage by volume is 80% is washed, Ran Houli
The heart removes ethanol；
(6) material after being centrifuged to step (5) with the ethanol water that percentage by volume is 85% is washed, Ran Houli
The heart, it is wet sodium carboxymethylcellulose to be precipitated；
(7) the wet sodium carboxymethylcellulose that step (6) is obtained is dried into the weight/mass percentage composition to water 2% at 80 DEG C
Hereinafter, dry sodium carboxymethylcellulose is obtained, is a kind of low-viscosity sodium carboxymethyl cellulose of the present invention.
The low-viscosity sodium carboxymethyl cellulose that the present embodiment is prepared is detected, it is as a result as follows：
Substitution value is 0.83, and purity is 99.5%, and viscosity is 15mPas.
Embodiment 5
(1) at 25 DEG C, to adding loose wood pulp cellulose 2Kg in kneader, while add by 3500mL ethanol with
2.5Kg mass percents are the mixture of 50% sodium hydrate aqueous solution composition, raw after quaternization 60min under stirring condition
Into alkali cellulose；
(2) in alkali cellulose add 2.25Kg mass percents be 62% chloroacetic ethanol solution, 35 DEG C with
Lower addition simultaneously stirs 20min, and then heating to 78 DEG C carries out etherification reaction 20min；
(3) material that step (2) etherification reaction is obtained is cooled to 60 DEG C, at the uniform velocity added in 15min 300mL hydrogen peroxide with
The mixed solution of 1500mL ethanol, oxidative degradation 30min；
(4) the pH value ≈ 7.0 of material is obtained with hydrochloric acid regulating step (3) oxidative degradation, then is 73% with percentage by volume
Ethanol water washed, be then centrifuged for remove ethanol；
(5) material after being centrifuged to step (4) with the ethanol water that percentage by volume is 80% is washed, Ran Houli
The heart removes ethanol；
(6) material after being centrifuged to step (5) with the ethanol water that percentage by volume is 90% is washed, Ran Houli
The heart, it is wet sodium carboxymethylcellulose to be precipitated；
(7) the wet sodium carboxymethylcellulose that step (6) is obtained is dried into the weight/mass percentage composition to water 2% at 80 DEG C
Hereinafter, dry sodium carboxymethylcellulose is obtained, is a kind of low-viscosity sodium carboxymethyl cellulose of the present invention.
The low-viscosity sodium carboxymethyl cellulose that the present embodiment is prepared is detected, it is as a result as follows：
Substitution value is 0.91, and purity is 98.5, and viscosity is 13mPas.
The present invention include but is not limited to above example, it is every carried out under the principle of spirit of the present invention it is any equivalent
Replace or local improvement, all will be regarded as within protection scope of the present invention.
Claims (2)
1. a kind of preparation method of low-viscosity sodium carboxymethyl cellulose, it is characterised in that：Methods described step is as follows：
(1) mixed solution of sodium hydrate aqueous solution and ethanol is mixed with wood pulp cellulose, alkalize 30min at 20 DEG C~35 DEG C
Alkali cellulose is generated after~60min；
Wood pulp cellulose is 10 with the mass ratio of NaOH:3~7；
(2) to chloroacetic ethanol solution is added in alkali cellulose, add and stir below 35 DEG C, then heat to 78
DEG C~80 DEG C carry out etherification reaction 20min~60min；
Wood pulp cellulose is 10 with chloroacetic mass ratio:3~8, chloroacetic quality percentage in chloroacetic ethanol solution
Number is 58%~62%；
(3) oxidative degradation：The material that etherification reaction is obtained is cooled to less than 60 DEG C, the oxidant diluted through ethanol, oxygen is added
Change degraded 20min~50min；
Wood pulp cellulose is 10 with the mass ratio of oxidant:1~3；The oxidant is hypochlorous acid, hydrogen peroxide or permanganic acid
Potassium；
The oxidant diluted through ethanol is at the uniform velocity added in 10min~15min；
(4) washing centrifugation is neutralized：The pH value that material is obtained with acid regulation oxidative degradation is 6.5~8.0, then is entered with ethanol water
Row washing, is then centrifuged for removing ethanol；
The percentage by volume of ethanol is 65%~75% in ethanol water；
(5) secondary washing centrifugation：Material after being centrifuged to step (4) with ethanol water is washed, and is then centrifuged for removing second
Alcohol；
The percentage by volume of ethanol is 70%~80% in ethanol water；
(6) three washing centrifugations：Material after being centrifuged to step (5) with ethanol water is washed, and is then centrifuged for, and is sunk
It is wet sodium carboxymethylcellulose to form sediment；
The percentage by volume of ethanol is 80%~90% in ethanol water；
The percentage by volume of ethanol increases successively in step (4), (5), the ethanol water used in (6)；
(7) dry：Wet sodium carboxymethylcellulose is dried into the weight/mass percentage composition to water below 2%, a kind of low viscosity is obtained
Sodium carboxymethylcellulose.
2. the preparation method of a kind of low-viscosity sodium carboxymethyl cellulose according to claim 1, it is characterised in that：Step
(4) acid described in is hydrochloric acid or acetic acid.
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| CN106749685A (en) * | 2016-12-21 | 2017-05-31 | 天津润圣纤维素科技有限公司 | A kind of production technology of low-viscosity sodium carboxymethyl cellulose |
| CN109336983B (en) * | 2018-11-15 | 2020-12-29 | 泸州北方纤维素有限公司 | Preparation method for ultra-low viscosity hydroxyethyl cellulose |
| CN112125978A (en) * | 2020-09-16 | 2020-12-25 | 陕西国防工业职业技术学院 | Preparation method of high-viscosity water-soluble cellulose ether |
| CN116655810A (en) * | 2023-06-28 | 2023-08-29 | 重庆力宏精细化工有限公司 | High-permeability ultralow-viscosity sodium carboxymethyl cellulose product and preparation method and application thereof |
| CN118108863B (en) * | 2024-04-29 | 2024-07-16 | 山东光大赛路新材料科技有限公司 | Low-viscosity hydroxypropyl methyl cellulose and preparation method thereof |
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| CN1490336A (en) * | 2002-10-14 | 2004-04-21 | 中国科学院成都有机化学研究所 | Ultra low viscosity carboxymethyl cellulose and preparing method thereof |
| CN101548732A (en) * | 2008-04-03 | 2009-10-07 | 上海长光企业发展有限公司 | Preparation method for low-viscosity sodium carboxymethyl cellulose for foodstuff |
| CN101455286B (en) * | 2008-04-03 | 2011-07-06 | 上海长光企业发展有限公司 | Preparation method of sodium carboxymethyl cellulose for food |
| CN102367279B (en) * | 2011-10-18 | 2013-04-17 | 杭州弘博新材料有限公司 | Preparation method of ultralow-viscosity sodium carboxymethyl cellulose |
| CN103242453A (en) * | 2012-08-14 | 2013-08-14 | 常熟威怡科技有限公司 | Method for preparing low-viscosity sodium carboxymethylcellulose |
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| Title |
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| 纤维素提取分离技术研究进展;高璇，等;《德州学院学报》;20120430;第28卷(第2期);第69-72页 * |
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