CN1075149A - The new synthetic process of sodium starch glycolate - Google Patents
The new synthetic process of sodium starch glycolate Download PDFInfo
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- CN1075149A CN1075149A CN 93112338 CN93112338A CN1075149A CN 1075149 A CN1075149 A CN 1075149A CN 93112338 CN93112338 CN 93112338 CN 93112338 A CN93112338 A CN 93112338A CN 1075149 A CN1075149 A CN 1075149A
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Abstract
Sodium starch glycolate, form by the starch carboxymethylation, substitution value is 0.1-1 (butt calculating), viscosity is 10-1000 centipoises (butt calculates, 2% concentration, 25 ℃), at normal temperatures can be water-soluble fully, good stability, perviousness is strong, can be widely used in fields such as weaving, printing and dyeing, papermaking, food, medicine, oil recovery.Its synthetic method adds the starch pulping for liquid caustic soda is dissolved in the alcohol, after overcuring, add again with in the liquid caustic soda and after chloroacetic alcoholic solution carry out carboxymethylation reaction, product is made white fine powder shape sodium starch glycolate through neutralization, washing, dry, pulverizing.
Description
This invention is a kind of new synthetic process that is widely used in the sodium starch glycolate in fields such as textile sizing, printing and dyeing, papermaking, food, medicine, daily use chemicals, oil.
The quality of stock quality directly has influence on the efficient and the quality of textile industry.Starch be commonly employed so far in textile sizing, printing and dyeing, but starch penetration is poor as a kind of natural polymer, and stability is bad, and serous coat is hard and crisp, is difficult for destarch again, has seriously restricted the quality and the class of textiles.From the sixties, China begins to be used for starching, printing and dyeing with carboxymethyl cellulose (CMC) substituted starch.Along with the rising of cotton price, cost up, the CMC price rises always, in addition, often contain a large amount of short fiber of plant among the CMC, causes that fabric face is coarse, broken end is many, has had a strong impact on quality, efficient and the production environment of weaving.Sodium starch glycolate for the raw material carboxymethylation forms, possesses the qualitative two-fold advantage of starch price and CMC with starch, has overcome deficiency separately again effectively, more and more is subjected to user's welcome.
Sodium starch glycolate also can be widely used in industry such as papermaking, medicine, food, daily use chemicals, oil, therefore, seeks a kind of easy, economic, practical synthetic method, is a problem of extensively paying attention to always.
U.S. Pat 4716186 reports, with starch pulping in organic pure liquid, add Mono Chloro Acetic Acid and liquid caustic soda again and carry out carboxymethylation, at last with organic acid neutralization, washing, separate and make sodium starch glycolate, this method is because various raw material single stage method carboxymethylations, cause to replace inequality and side reaction increase, because of using organic acid, increased production cost again.
Chinese patent CN 1064081 report stirs evenly sodium hydroxide and yellow soda ash in alcohol, add the starch pulping, and the spirituous solution that adds Mono Chloro Acetic Acid, yellow soda ash again carries out carboxylic first classization, washing at last, dry and make sodium starch glycolate.This method is because sodium hydroxide and yellow soda ash dissolve difficulty in alcohol, consume excessive alkali, increase the growing amount of the three wastes, because of using in the yellow soda ash and Mono Chloro Acetic Acid, generated a large amount of bubbles again, cause operational difficulty, in addition, starch just carries out carboxymethylation without abundant processing during owing to reaction, causes replacement inhomogeneous, consumed excessive Mono Chloro Acetic Acid again, it is very low to react chloroacetic transformation efficiency.
The object of the invention is to seek a reaction conditions gentleness, rapid, and easy to operate, practical, reaction raw materials consumption is few, the transformation efficiency height, the three wastes generate the synthetic method of few sodium starch glycolate, and gained sodium starch glycolate solvability, stability, perviousness are all good, replace evenly.
The synthetic method of sodium starch glycolate of the present invention is aqueous sodium hydroxide solution (containing alkali 30-60%) 60-400 part (weight) to be added in 300-1000 part (weight) alcoholic solution (containing pure 80-100%) stir evenly, add 300 parts of (weight) pulpings of starch, in 20-25 ℃ of slaking 0.5-2 hour, in addition 20-200 part (weight) Mono Chloro Acetic Acid is dissolved in 50-500 part (weight) alcoholic solution (containing pure 80-100%), with in aqueous sodium hydroxide solution (containing alkali 30-60%) 10-300 part (weight) and salify, gained sodium chloroacetate alcoholic solution adds in the good starch-sodium hydroxide alcoholic solution of slaking, carry out carboxymethylation reaction in 30-90 ℃, reaction times is 0.5-10 hour, the gained mix products is neutralized to pH 6.5-8.5 with concentrated hydrochloric acid (content 25-35%), centrifugation, solid washs with alcohol (containing pure 70-95%), centrifugation again, solid drying, pulverize, get white sodium starch glycolate.The alcohol that reaction is used is methyl alcohol, ethanol, propyl alcohol, the Virahol that dissolves each other with water; Starch source is in wheat, corn, cassava, potato etc.
The sodium starch glycolate that the present invention is made, substitution value calculates for the 0.1-1(butt), viscosity is 10-1000 centipoise (butt calculates, 2% concentration, 25 ℃), sodium chloride content≤6%.Its normal temperature down can be water-soluble, good stability, has good compatibility with many hydrophilic high molecular polymers such as PVA etc., serous coat is stable, mobile, perviousness all is better than modified starch and carboxymethyl cellulose, desizing agent specially, and be widely used in fields such as printing and dyeing, papermaking, food, medicine, daily use chemicals, oil.
Raw material of the present invention is easy to get, and technology is simple, and is easy to operate, and raw material consumption is low, and production cost is low, and steady quality is applicable to suitability for industrialized production.
Following example is as supplementary notes of the present invention.
Example 1
In reactor, add 1000 parts of (weight) 90% methyl alcohol, add 160 parts of (weight) 50% liquid caustic soda again, stirred 10 minutes, add 300 parts of (weight) starch, stir pulping, in 40 ℃ of stirring reactions 30 minutes, other got 80 parts of (weight) Mono Chloro Acetic Acids and is dissolved in 150 parts of (weight) 90% methyl alcohol, with 90 parts of (weight) 50% liquid caustic soda neutralizations, the gained chloracetate is added in the good starch of slaking-sodium hydroxide alcohol liquid, under 60 ℃, carry out carboxymethylation reaction, 2 hours reaction times, after reaction finishes, be chilled to 30 ℃, transferring pH with concentrated hydrochloric acid is 6.5-8.5, the centrifugal mother liquor of removing, the gained solid washs with 500 parts of (weight) 90% alcoholic solutions, mother liquor is removed in centrifugation again, solid drying, pulverize, get 368 parts of white fine powder shape sodium starch glycolatees (weight).
Embodiment 2
In reactor, add 1000 parts of (weight) 95% ethanol, add 400 parts of (weight) 45% liquid caustic soda again, stirred 10 minutes, add 300 parts of (weight) starch, stir pulping, in 40 ℃ of stirring reactions 45 minutes, other got 100 parts of (weight) Mono Chloro Acetic Acids and is dissolved in 200 parts of (weight) 95% ethanol, with 120 parts of (weight) 45% liquid caustic soda neutralizations, carry out carboxymethylation reaction, 60 ℃ of temperature of reaction, 2 hours time in the starch that gained chloracetate adding slaking is good-sodium hydroxide alcohol liquid, after reaction finishes, be cooled to 30 ℃, transferring pH with concentrated hydrochloric acid is 6.5-8.5, the centrifugal mother liquor of removing, solid washs with 500 parts of (weight) 80% alcoholic solutions, centrifugation again, the gained solid drying, pulverize, get 384 parts of white fine powder shape sodium starch glycolatees (weight).
Example 3
In reactor, add 480 parts of (weight) 95% propyl alcohol, add 80 parts of (weight) 40% liquid caustic soda again, stirred 20 minutes, add 300 parts of (weight) starch, stir pulping, in 35 ℃ of stirring reactions 60 minutes, other got 36 parts of (weight) Mono Chloro Acetic Acids and is dissolved in 100 parts of (weight) 95% propyl alcohol, with 40 parts of (weight) 40% liquid caustic soda neutralizations, carry out carboxymethylation reaction, 70 ℃ of temperature of reaction, 4 hours time in the starch that gained chloracetate adding slaking is good-sodium hydroxide alcohol liquid, after reaction finishes, be chilled to 30 ℃, transferring pH with concentrated hydrochloric acid is 6.5-8.5, the centrifugal mother liquor of removing, solid washs with 500 parts of (weight) 70% alcoholic solutions, mother liquor is removed in centrifugation again, solid drying, pulverize, get 330 parts of white fine powder shape sodium starch glycolatees (weight).
Claims (4)
1, the synthesis technique of sodium starch glycolate, it is characterized in that and to stir evenly in (containing pure 80-100%) in aqueous sodium hydroxide solution (containing alkali 30-60%) 60-400 part (weight) adding 300-1000 part (weight) alcoholic solution, add 300 parts of (weight) pulpings of starch, in 20-50 ℃ of slaking 0.5-2 hour, in addition 20-200 part (weight) Mono Chloro Acetic Acid is dissolved in 50-500 part (weight) alcoholic solution (containing pure 80-100%), with in aqueous sodium hydroxide solution (containing alkali 30-60%) 10-300 part (weight) and salify, gained sodium chloroacetate alcoholic solution adds in the good starch-sodium hydroxide alcoholic solution of slaking, carry out carboxymethylation reaction in 30-90 ℃, reaction times is 0.5-10 hour, the gained mix products is neutralized to pH6.5-8.5 with concentrated hydrochloric acid (content 25-35%), centrifugally remove pure liquid, solid washs with alcoholic solution (containing pure 70-95%), centrifugation again, the solid product drying, pulverize, get white sodium starch glycolate fine powder, pure liquid distillation is reclaimed.
2, feature of the present invention is in the synthesis technique of sodium starch glycolate, the slaking of starch and carboxymethylation was divided into for two steps carries out in a reactor.
3, feature of the present invention is behind Mono Chloro Acetic Acid and the liquid caustic soda reaction generation sodium salt, again as carboxymethylated raw material.
4, feature of the present invention is that used starch source can be wheat, corn, cassava, potato etc., and alcohol is methyl alcohol, ethanol, propyl alcohol, the Virahol that dissolves each other with water.
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CN 93112338 CN1075149A (en) | 1993-02-09 | 1993-02-09 | The new synthetic process of sodium starch glycolate |
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CN 93112338 CN1075149A (en) | 1993-02-09 | 1993-02-09 | The new synthetic process of sodium starch glycolate |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1037105C (en) * | 1994-08-04 | 1998-01-21 | 安徽省生物研究所 | Phase transfer synthetic process for high substitution value sodium carboxymethyl amyloether |
CN100365209C (en) * | 2005-12-30 | 2008-01-30 | 湖北达雅化工技术发展有限公司 | Water-retaining agent for coating of coated paper and preparation method thereof |
CN102153664A (en) * | 2011-01-17 | 2011-08-17 | 温州大学 | Method for preparing nanometer lamellar sodium carboxymethyl starch |
CN102731664A (en) * | 2012-07-17 | 2012-10-17 | 郑桂富 | Preparation method of pharmaceutical adjuvant sodium carboxymethyl starch |
CN102746409A (en) * | 2012-06-18 | 2012-10-24 | 新疆光大山河化工科技有限公司 | Preparation method of super sodium carboxymethyl starch |
-
1993
- 1993-02-09 CN CN 93112338 patent/CN1075149A/en active Pending
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1037105C (en) * | 1994-08-04 | 1998-01-21 | 安徽省生物研究所 | Phase transfer synthetic process for high substitution value sodium carboxymethyl amyloether |
CN100365209C (en) * | 2005-12-30 | 2008-01-30 | 湖北达雅化工技术发展有限公司 | Water-retaining agent for coating of coated paper and preparation method thereof |
CN102153664A (en) * | 2011-01-17 | 2011-08-17 | 温州大学 | Method for preparing nanometer lamellar sodium carboxymethyl starch |
CN102153664B (en) * | 2011-01-17 | 2013-11-06 | 温州大学 | Method for preparing nanometer lamellar sodium carboxymethyl starch |
CN102746409A (en) * | 2012-06-18 | 2012-10-24 | 新疆光大山河化工科技有限公司 | Preparation method of super sodium carboxymethyl starch |
CN102731664A (en) * | 2012-07-17 | 2012-10-17 | 郑桂富 | Preparation method of pharmaceutical adjuvant sodium carboxymethyl starch |
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