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Preparation method of heat-resisting crosslinking anionic starch adhesive

A technology of anionic starch and cross-linked starch, applied in the directions of starch-derived adhesives, adhesive types, etc., can solve problems such as inability to meet, and achieve the effects of high reaction efficiency and simple production process

Inactive Publication Date: 2012-07-04
HUNAN UNIV OF SCI & ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The cross-linked anionic starch obtained by the currently used cross-linking agents epichlorohydrin, formaldehyde, phosphorus oxychloride, trimeta or sodium tripolyphosphate, etc., has improved heat resistance, but still cannot meet the requirements of some higher temperature applications. Fields, such as the production of iron pellets and other requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Put 100g of starch and 150ml of water in a cylindrical glass bottle equipped with a stirrer, add 1.5g of p-chlorosulfonic acid benzoyl chloride, stir electrically and maintain a constant temperature water bath at 25°C. After mixing evenly, start to add sodium hydroxide solution dropwise (6g of sodium hydroxide is dissolved in 40ml of water), and the dropwise addition is completed. After reacting for 5 hours, adjust the pH to 6.0-7.0 with a sulfuric acid solution with a concentration of 3 mol / L, let it stand for a while, filter, wash, suction filter and dry to obtain the cross-linked starch.

[0011] In a cylindrical glass bottle equipped with a stirrer, add 10g of cross-linked starch and 10mL of 5% sodium hydroxide solution, stir at room temperature for 20min, then add 2g of chloroacetic acid, continue stirring for 10min at room temperature, and react at 50°C for 3h , to obtain a semi-solid crude product. The crude product is soaked and neutralized by 80% ethanol aqueo...

Embodiment 2

[0013] Add 100g of cornstarch, 2g of p-chlorosulfonic acid benzoyl chloride and 100ml of water into a cylindrical glass bottle equipped with a stirrer, add 30mL of 25% sodium hydroxide solution dropwise under stirring, and then place it in a 40°C In a constant temperature water bath, stir and react for 3h. After the reaction is completed, adjust the pH to 6.0-7.0 with a sulfuric acid solution with a concentration of 3 mol / L, let it stand for a period of time, filter, wash, suction filter, and dry to obtain the cross-linked starch.

[0014] Weigh 10g of cross-linked starch into a cylindrical glass bottle equipped with a stirrer, add 6ml of distilled water, stir at room temperature for 20min, then add 1.5g of chloroacetic acid, continue stirring at room temperature for 10min, and react at 50°C for 3h to obtain Semi-solid crude product. Neutralize with ethanol with a volume fraction of 70% containing a small amount of acetic acid to a pH of about 6.5, filter, wash with ethanol w...

Embodiment 3

[0016] Add 100g of cornstarch, 3g of p-chlorosulfonic acid benzoyl chloride and 100ml of water into a cylindrical glass bottle equipped with a stirrer, add 30mL of 25% sodium hydroxide solution dropwise under stirring, and then place it in a 50°C In a constant temperature water bath, stir and react for 3 hours. After the reaction is completed, adjust the pH to 6.0-7.0 with a sulfuric acid solution with a concentration of 3 mol / L, let it stand for a period of time, filter, wash, suction filter, and dry to obtain the cross-linked starch.

[0017] Weigh 10 g of cross-linked starch into a cylindrical glass bottle equipped with a stirrer, add 6 mL of distilled water, stir for 20 min at room temperature, then add 3 g of chloroacetic acid, continue stirring for 10 min at room temperature, and react at 50 ° C for 3 h to obtain half Guben crude products. Neutralize with 70% ethanol containing a small amount of acetic acid to a pH of 6.5, filter, wash with 70% ethanol, wash with water,...

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Abstract

The invention relates to a novel preparation method of heat-resisting crosslinking anionic starch adhesive. Under the alkaline condition, starch and parachlorine sulfonyl benzoyl chloride take reaction and then take reaction with chloroacetic acid to obtain the high-temperature-resisting crosslinking anionic starch adhesive, the synthesis process is simple, the pollution is avoided, and the cost is low. Simultaneously, through changing the dosage of the parachlorine sulfonyl benzoyl chloride and anionic etherification agents, the adhesives with different heat resistance performances and different viscosities can be obtained, the development of the starch adhesive in China is promoted, the anionic starch adhesives with different heat resistance performances and different viscosities are produced, the repeated utilization of renewable resources is realized, the product is safe and reliable and can be widely applied to the fields of living, metallurgy and the like, and good economic, environmental-friendly and social benefits are realized.

Description

technical field [0001] The invention relates to a preparation method of a heat-resistant cross-linked anionic starch adhesive, which belongs to the technical field of fine chemical production. Background technique [0002] In the present invention, the anionic starch is a carboxymethyl-containing polymer electrolyte. After the starch is carboxymethylated, the original structure of the granules is destroyed, the product has strong water solubility, and the aqueous solution has high viscosity. Anionic starch also has the characteristics of degradability, good water dispersibility, low retrogradation and good adhesiveness. Therefore, anionic starch is widely used in various fields, such as adhesives for metallurgical pellet production, thickeners, suspending agents and adhesives in the food industry, fluid loss reducers in the petroleum industry, and sizing in the textile industry Starch is also used as an additive in daily chemicals and pharmaceuticals, such as cement disper...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J103/08C08B31/14C08B31/12
Inventor 姜红宇湛雪辉李朝辉湛含辉
Owner HUNAN UNIV OF SCI & ENG
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