CN1673233A - Carboxymethyl hydroxyethyl cellulose producing process - Google Patents
Carboxymethyl hydroxyethyl cellulose producing process Download PDFInfo
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- CN1673233A CN1673233A CN 200410012892 CN200410012892A CN1673233A CN 1673233 A CN1673233 A CN 1673233A CN 200410012892 CN200410012892 CN 200410012892 CN 200410012892 A CN200410012892 A CN 200410012892A CN 1673233 A CN1673233 A CN 1673233A
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- hydroxyethyl cellulose
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Abstract
The carboxymethyl hydroxyethyl cellulose producing process includes the steps of: crushing material, alkalization, carboxymethylation, the first separation, hydroxyethylation, neutralization, the second separation, refining and drying. The present invention has reasonable technological process and the carboxymethyl hydroxyethyl cellulose product has high quality and the main technological indexes of: viscosity of 30-60000 mpa.s, ash content not more than 5 %, pH 5-7, humidity not higher than 8 %, molar hydroxyethyl substitution degree of 0.8-2.0 and molar carboxymethyl substitution degree of 0.2-0.8.
Description
Technical field: the present invention relates to cellulose raw production art field.
Background technology: carboxymethyl hydroxyethyl cellulose is the mixed ether of a kind of ionic and non-ionic type; have higher solvability, resistance to enzymolysis, temperature tolerance, appearance salt and anti acid alkali performance; as thickening material, tackiness agent, stablizer, dispersion agent, suspending agent, colloid protective agent and alleviation material, be widely used in chemical industries such as coating, high molecular polymerization, petroleum drilling and mining, building materials, weaving, printing and dyeing, papermaking, toothpaste, makeup.The present domestic carboxymethyl hydroxyethyl cellulose production of still not having, domestic needs solves by import.
Summary of the invention: purpose of the present invention is exactly to lean on the deficiency of import solution at the demand of present domestic carboxymethyl hydroxyethyl cellulose, and provide a kind of carboxymethyl hydroxyethyl cellulose production technique, its technology is reasonable, and the carboxymethyl hydroxyethyl cellulose of producing reaches the quality of external like product fully.A kind of carboxymethyl hydroxyethyl cellulose production technique, its production craft step is:
A, raw material pulverizing: it is 40-80 purpose cotton fibre powder that purified cotton is crushed to fineness with the purified cotton pulverizer;
B, quaternization: cotton fibre powder is put into the stirring of reactor adding sodium hydroxide carried out quaternization in 0.5-2 hour, make soda cellulose;
C, carboxymethylation reaction: soda cellulose is put into reactor adding Mono Chloro Acetic Acid heat to 60-80 ℃ reaction times 0.5-3 hour while stirring;
D, separation first: above-mentioned carboxymethylation reaction thing is isolated the reaction precipitation thing that water capacity is 30-70 by whizzer;
E, ethoxyl etherification: the reaction precipitation thing after the above-mentioned separation is put into reactor add the sodium hydroxide stirring, and then adding oxyethane is heated while stirring to 50-90 ℃ reaction times 0.5-3 hour;
F, neutralization: the reactant of above-mentioned ethoxyl etherification is cooled to normal temperature in reactor, adds Glacial acetic acid and stir, transferring to pH value is 6-7;
G, separation once more: the reactant after the above-mentioned neutralization is isolated the carboxymethyl hydroxyethyl cellulose crude product that water capacity is 30-70% by whizzer;
H, refining: above-mentioned carboxymethyl hydroxyethyl cellulose crude product is put into rinse bath washed with isopropyl alcohol 1-4 time, isolate the wet product of carboxymethyl hydroxyethyl cellulose that water capacity is 20-30% by whizzer;
I, drying: with above-mentioned water capacity is that to put into the water capacity that vacuum drier is dried to carboxymethyl hydroxyethyl cellulose be 3-8% for the wet product of carboxymethyl hydroxyethyl cellulose of 20-30%.
Can after the quaternization step, carry out the ethoxyl etherification step earlier: soda cellulose is put into reactor add the sodium hydroxide stirring, and then adding oxyethane is heated while stirring to 50-90 ℃ reaction times 0.5-3 hour; Behind separating step first; Carry out carboxymethylation reaction step again: will be first from after the reaction precipitation thing put into reactor and add Mono Chloro Acetic Acid and heat to 60-80 ℃ reaction times 0.5-3 hour while stirring; Neutralize subsequently, separate once more, make with extra care, dry, step.
In the quaternization step, cotton fibre powder and sodium hydroxide weight ratio are: cotton fibre powder: sodium hydroxide=1: 0.5-1.2.
In carboxymethylation reaction step, soda cellulose and Mono Chloro Acetic Acid weight ratio are: soda cellulose: Mono Chloro Acetic Acid=1: 0.2-1.
In the ethoxyl etherification step, the reaction precipitation thing after separating first with the sodium hydroxide of adding and the weight ratio of oxyethane is: the reaction precipitation thing after separating first: sodium hydroxide: oxyethane=1: 0.3-0.5-0.5-1.5.
The invention has the advantages that its technology is reasonable, the carboxymethyl hydroxyethyl cellulose of producing reaches the quality of external like product fully.The key technical indexes: viscosity (20 ℃ of 2% aqueous solution) mpa.s is 30-60000; Ash content (Na
2SO
4Meter)≤5%; PH value 9 (2% aqueous solution) 5-7; Humidity≤8%; The hydroxyethyl molar substitution is 0.8-2.0; Degree of substitution by carboxymethyl DS is 0.2-0.8.
Embodiment:
A, raw material pulverizing: it is 40-80 purpose cotton fibre powder that purified cotton is crushed to fineness with the purified cotton pulverizer;
B, quaternization: the 100kg cotton fibre powder is put into the stirring of reactor adding 100kg sodium hydroxide carried out quaternization in 0.5-2 hour, make soda cellulose;
C, carboxymethylation reaction: the 100kg soda cellulose is put into reactor add the 80kg Mono Chloro Acetic Acid
Heat to 60-80 ℃ reaction times 0.5-3 hour while stirring;
D, separation first: above-mentioned carboxymethylation reaction thing is isolated the reaction precipitation thing that water capacity is 30-70 by whizzer;
E, ethoxyl etherification: the reaction precipitation thing 100kg after the above-mentioned separation is put into reactor add the stirring of 40kg sodium hydroxide, and then adding 100kg oxyethane is heated while stirring to 50-90 ℃ reaction times 0.5-3 hour;
F, neutralization: the reactant of above-mentioned ethoxyl etherification is cooled to normal temperature in reactor, adds Glacial acetic acid and stir, transferring to pH value is 6-7;
F, separation once more: the reactant after the above-mentioned neutralization is isolated the carboxymethyl hydroxyethyl cellulose crude product that water capacity is 30-70% by whizzer;
G, refining: above-mentioned 100kg carboxymethyl hydroxyethyl cellulose crude product is put into rinse bath 1000kg washed with isopropyl alcohol 1-4 time, isolate the wet product of carboxymethyl hydroxyethyl cellulose that water capacity is 20-30% by whizzer;
H, drying: with above-mentioned water capacity is that to put into the water capacity that vacuum drier is dried to carboxymethyl hydroxyethyl cellulose be 3-8% for the wet product of carboxymethyl hydroxyethyl cellulose of 20-30%.
Be crushed to the order number that needs with pulverizer at last, get final product after the packing.
Claims (5)
1, a kind of carboxymethyl hydroxyethyl cellulose production technique is characterized in that its production craft step is:
A, raw material pulverizing: it is 40-80 purpose cotton fibre powder that purified cotton is crushed to fineness with the purified cotton pulverizer;
B, quaternization: cotton fibre powder is put into reactor add sodium hydroxide stirring 0.5-2 hour, carry out quaternization, make soda cellulose;
C, carboxymethylation reaction: soda cellulose is put into reactor adding Mono Chloro Acetic Acid heat to 60-80 ℃ reaction times 0.5-3 hour while stirring;
D, separation first: above-mentioned carboxymethylation reaction thing is isolated the reaction precipitation thing that water capacity is 30-70 by whizzer;
E, ethoxyl etherification: the reaction precipitation thing after the above-mentioned separation is put into reactor add the sodium hydroxide stirring, and then adding oxyethane is heated while stirring to 50-90 ℃ reaction times 0.5-3 hour;
F, neutralization: the reactant of above-mentioned ethoxyl etherification is cooled to normal temperature in reactor, adds Glacial acetic acid and stir, transferring to pH value is 6-7;
G, separation once more: the reactant after the above-mentioned neutralization is isolated the carboxymethyl hydroxyethyl cellulose crude product that water capacity is 30-70% by whizzer;
H, refining: above-mentioned carboxymethyl hydroxyethyl cellulose crude product is put into rinse bath washed with isopropyl alcohol 1-4 time, isolate the wet product of carboxymethyl hydroxyethyl cellulose that water capacity is 20-30% by whizzer;
I, drying: with above-mentioned water capacity is that to put into the water capacity that vacuum drier is dried to carboxymethyl hydroxyethyl cellulose be 3-8% for the wet product of carboxymethyl hydroxyethyl cellulose of 20-30%.
2, carboxymethyl hydroxyethyl cellulose production technique according to claim 1, it is characterized in that can be after the quaternization step, carry out the ethoxyl etherification step earlier: soda cellulose is put into reactor add the sodium hydroxide stirring, and then adding oxyethane is heated while stirring to 50-90 ℃ reaction times 0.5-3 hour; Behind separating step first; Carry out carboxymethylation reaction step again: will be first from after the reaction precipitation thing put into reactor and add Mono Chloro Acetic Acid and heat to 60-80 ℃ reaction times 0.5-3 hour while stirring; Neutralize subsequently, separate once more, make with extra care, dry, step.
3, according to claim 1 and 2 described carboxymethyl hydroxyethyl cellulose production technique, it is characterized in that in the quaternization step that cotton fibre powder and sodium hydroxide weight ratio are: cotton fibre powder: sodium hydroxide=1: 0.5-1.2.
4, carboxymethyl hydroxyethyl cellulose production technique according to claim 1 is characterized in that in the carboxymethylation reaction step, and soda cellulose and Mono Chloro Acetic Acid weight ratio are: soda cellulose: Mono Chloro Acetic Acid=1: 0.2-1.
5, carboxymethyl hydroxyethyl cellulose production technique according to claim 1, it is characterized in that in the ethoxyl etherification step reaction precipitation thing after separating first with the sodium hydroxide of adding and the weight ratio of oxyethane is: the reaction precipitation thing after separating first: sodium hydroxide: oxyethane=1: 0.3-0.5-0.5-1.5.
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| CN 200410012892 CN1673233A (en) | 2004-03-23 | 2004-03-23 | Carboxymethyl hydroxyethyl cellulose producing process |
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| CN 200410012892 CN1673233A (en) | 2004-03-23 | 2004-03-23 | Carboxymethyl hydroxyethyl cellulose producing process |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101864607A (en) * | 2010-06-23 | 2010-10-20 | 东华大学 | Method for preparing hydroxyethyl cellulose |
| CN102180978A (en) * | 2011-03-23 | 2011-09-14 | 刘传荣 | Technology for producing substitution-degree hydroxyethyl cellulose |
| CN101955546B (en) * | 2009-07-15 | 2012-07-04 | 山东赫达股份有限公司 | Process for producing cellulose ether by directly separating and recovering diluent |
| CN103509196A (en) * | 2012-06-19 | 2014-01-15 | 株式会社吴羽 | Preparation method of cellulose-type water solvent |
| CN104119453A (en) * | 2014-07-06 | 2014-10-29 | 福建农林大学 | Method for preparing hydroxyethyl cellulose by utilizing bamboo pulp |
| CN105136696A (en) * | 2015-08-17 | 2015-12-09 | 德州学院 | Method for testing hydroxypropylmethyl cellulose methyl substitution degree |
| CN107405420A (en) * | 2014-10-31 | 2017-11-28 | 核心科学创新有限公司 | Improved carboxymethyl cellulose and preparation method thereof |
| CN110156899A (en) * | 2019-05-14 | 2019-08-23 | 吉林省荣普达石油技术有限公司 | A kind of hydroxyethyl cellulose modified object of bisexual ion purification and preparation method thereof |
| CN111349180A (en) * | 2020-03-17 | 2020-06-30 | 重庆理工大学 | Synthesis method of carboxymethyl-hydroxyethyl cellulose salt |
| CN112409498A (en) * | 2020-11-25 | 2021-02-26 | 泸州北方纤维素有限公司 | Preparation method of high-stability carboxymethyl hydroxyethyl cellulose |
| CN114920853A (en) * | 2022-06-29 | 2022-08-19 | 重庆力宏精细化工有限公司 | Flexible carboxymethyl cellulose ether and preparation method and application thereof |
-
2004
- 2004-03-23 CN CN 200410012892 patent/CN1673233A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955546B (en) * | 2009-07-15 | 2012-07-04 | 山东赫达股份有限公司 | Process for producing cellulose ether by directly separating and recovering diluent |
| CN101864607A (en) * | 2010-06-23 | 2010-10-20 | 东华大学 | Method for preparing hydroxyethyl cellulose |
| CN102180978A (en) * | 2011-03-23 | 2011-09-14 | 刘传荣 | Technology for producing substitution-degree hydroxyethyl cellulose |
| CN102532327A (en) * | 2011-03-23 | 2012-07-04 | 刘传荣 | Process for producing hydroxyethyl cellulose with high degree of substitution |
| CN103509196A (en) * | 2012-06-19 | 2014-01-15 | 株式会社吴羽 | Preparation method of cellulose-type water solvent |
| CN103509196B (en) * | 2012-06-19 | 2016-02-17 | 株式会社吴羽 | The manufacture method of the cellulose family aqueous solution |
| CN104119453A (en) * | 2014-07-06 | 2014-10-29 | 福建农林大学 | Method for preparing hydroxyethyl cellulose by utilizing bamboo pulp |
| US11155642B2 (en) | 2014-10-31 | 2021-10-26 | Core Scientific Creations Ltd. | Carboxymethyl cellulose and method of preparation |
| CN107405420A (en) * | 2014-10-31 | 2017-11-28 | 核心科学创新有限公司 | Improved carboxymethyl cellulose and preparation method thereof |
| CN105136696A (en) * | 2015-08-17 | 2015-12-09 | 德州学院 | Method for testing hydroxypropylmethyl cellulose methyl substitution degree |
| CN105136696B (en) * | 2015-08-17 | 2018-08-31 | 德州学院 | A kind of test method of hydroxypropyl methyl cellulose methyl substitution |
| CN110156899A (en) * | 2019-05-14 | 2019-08-23 | 吉林省荣普达石油技术有限公司 | A kind of hydroxyethyl cellulose modified object of bisexual ion purification and preparation method thereof |
| CN111349180A (en) * | 2020-03-17 | 2020-06-30 | 重庆理工大学 | Synthesis method of carboxymethyl-hydroxyethyl cellulose salt |
| CN112409498A (en) * | 2020-11-25 | 2021-02-26 | 泸州北方纤维素有限公司 | Preparation method of high-stability carboxymethyl hydroxyethyl cellulose |
| CN114920853A (en) * | 2022-06-29 | 2022-08-19 | 重庆力宏精细化工有限公司 | Flexible carboxymethyl cellulose ether and preparation method and application thereof |
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