Preparation method of cross-linked sodium carboxymethyl cellulose

A technology of sodium carboxymethyl cellulose and carboxymethyl cellulose is applied in the field of cross-linking preparation of nano-composite materials, and can solve the problems of no cis-diol structure, unsatisfactory cross-linking effect, and less than ideal, etc. The effect of high swelling degree, large industrial application value and high viscosity

Active Publication Date: 2012-07-25
美信佳中维药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology is still not ideal, because not only to form a polymer solution, but also to add an aluminum salt chelating agent
The effect of crosslinking with borate is also not ideal, because borate is more effective for cellulose ethers containing dihydroxyl groups, and CMC does not have a cis-diol structure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation method of croscarmellose sodium comprises the following steps:

[0023] 1. dissolving 15 grams of sodium carboxymethyl cellulose with 50 grams of aprotic polar solvent, stirring and dissolving to obtain a uniform sodium carboxymethyl cellulose solution;

[0024] ②Add an inorganic acid catalyst to the above-mentioned sodium carboxymethyl cellulose solution to make the reaction system acidic, with a pH value of 1.5, and react at room temperature for 30 minutes to obtain a carboxymethyl cellulose solution;

[0025] ③ Take 1.1 g of cross-linking agent and disperse it in 9.0 g of carboxymethyl cellulose solution, pre-polymerize in ultrasonic wave for 6 hours after deoxygenation and nitrogen flushing, and then polymerize at 90°C for 36 hours to obtain cross-linked carboxymethyl cellulose;

[0026] ④ Cool down to room temperature, add alkalized 95% ethanol-water solution dropwise to the croscarmellose solution obtained above to obtain croscarmellose sodium, fil...

Embodiment 2

[0034] The preparation method of croscarmellose sodium comprises the following steps:

[0035] 1. dissolving 16 grams of sodium carboxymethyl cellulose with 50 grams of aprotic polar solvent, stirring and dissolving to obtain a uniform sodium carboxymethyl cellulose solution;

[0036] ②Add an inorganic acid catalyst to the above-mentioned sodium carboxymethyl cellulose solution to make the reaction system acidic, with a pH value of 2.0, and react at room temperature for 30 minutes to obtain a carboxymethyl cellulose solution;

[0037] ③ Take 1.1 g of cross-linking agent and disperse it in 9.0 g of carboxymethyl cellulose solution, place it in ultrasonic wave for 6 hours after deoxygenation and nitrogen flushing, and then polymerize at 100°C for 35 hours to obtain cross-linked carboxymethyl cellulose.

[0038] ④ Cool down to room temperature, add alkalized 95% ethanol-water solution dropwise to the croscarmellose solution obtained above to obtain croscarmellose sodium, filter, ...

Embodiment 3

[0046] The preparation method of croscarmellose sodium is characterized in that it comprises the following steps:

[0047] 1. dissolving 17 gram sodium carboxymethyl cellulose with 50 gram aprotic polar solvent, stirring and dissolving to obtain homogeneous sodium carboxymethyl cellulose solution;

[0048] ②Add an inorganic acid catalyst to the above-mentioned sodium carboxymethyl cellulose solution to make the reaction system acidic, with a pH value of 2.5, and react at room temperature for 60 minutes to obtain a carboxymethyl cellulose solution;

[0049] ③ Take 1.2 grams of cross-linking agent and disperse it in 9.0 grams of carboxymethyl cellulose solution, place it in ultrasonic wave for 6 hours after deoxygenation and nitrogen flushing, and then polymerize at 90°C for 36 hours to obtain cross-linked carboxymethyl cellulose.

[0050] ④ Cool down to room temperature, add alkalized 95% ethanol-water solution dropwise to the croscarmellose solution obtained above to obtain cros...

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Abstract

The invention relates to a preparation method of cross-linked sodium carboxymethyl cellulose. The preparation method of the cross-linked sodium carboxymethyl cellulose comprises the following steps of: adding an inorganic acid catalyst into sodium carboxymethyl cellulose solution to change a reaction system to be acidic; after reaction, adding a cross-linking agent; removing oxygen and charging nitrogen; prepolymerizing and polymerizing to obtain cross-linked carboxymethyl cellulose solution; dropwise adding alkalized ethanol-water solution to obtain cross-linked sodium carboxymethyl cellulose solution; and drying to obtain the cross-linked sodium carboxymethyl cellulose powder. According to the preparation method, a silicon dioxide composite nanomaterial, silicon dioxide-hydroxyl propyl acrylate, is used as the cross-linking agent, sodium carboxymethyl cellulose is used as a raw material, and cross-linking is performed under an alkaline condition to prepare the cross-linked sodium carboxymethyl cellulose. The cross-linked sodium carboxymethyl cellulose prepare by the invention has the characteristics of high transparence, high viscosity, high swelling degree and the like, and hasextremely high industrial application value.

Description

technical field [0001] The invention relates to a preparation method for cross-linking nanocomposite materials, in particular to a preparation method for cross-linked sodium carboxymethyl cellulose. Background technique [0002] Carboxymethyl cellulose (CMC for short) is the largest type of cellulose ether produced and sold in the world, widely used in detergents, food, toothpaste, textiles, printing and dyeing, papermaking, petroleum, mining, medicine, ceramics, electronics Components, rubber, coatings, pesticides, cosmetics, leather, plastics and oil drilling, etc., known as "industrial monosodium glutamate". Products produced by traditional methods tend to form insoluble or insoluble salts with multivalent cations during the exchange process, and the products generally have insufficient substitution uniformity, transparency, solution rheology, and corrosion resistance. characteristics of poor sex. Crosslinking is one of the convenient ways to functionalize modified cell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/24C08L1/26C08K9/04C08K3/36C09C1/28C09C3/08
Inventor 费玉元费锦华
Owner 美信佳中维药业股份有限公司
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