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Preparation method of ABA type organosilicone glucoheptonic acid amide surface active agent

The technology of silicon glucoheptonic acid amide and glucoheptonic acid amide siloxane is applied in the field of preparation of ABA type organosilicon glucoheptonic acid amide surfactant, which can solve the problem that the grafting rate of sugar groups is low and the application scope is affected. , poor water solubility of the product, etc., to achieve the effects of high grafting rate, good water solubility, and short use time

Active Publication Date: 2019-11-12
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is non-toxic and low-cost, but due to the low grafting rate of sugar groups, the water solubility of the product is poor, which affects its application range

Method used

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  • Preparation method of ABA type organosilicone glucoheptonic acid amide surface active agent
  • Preparation method of ABA type organosilicone glucoheptonic acid amide surface active agent
  • Preparation method of ABA type organosilicone glucoheptonic acid amide surface active agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 20.8g glucoheptonolactone and 39.8g bisaminoethylaminopropyl tetramethoxydisiloxane to the flask, add 100mL methanol as solvent, react at 80°C for 2h, distill methanol off to obtain glucoheptin Sugar acid amide tetramethoxydisiloxane. Add 60.6 g of glucoheptonic acid amide tetramethoxydisiloxane and 3.7 g of eicosyldecaciloxane into the flask, add 0.037 g of tetramethylammonium hydroxide as a catalyst, and react at 90° C. for 4 hours. After the reaction, heat to 134°C to deactivate the catalyst to obtain the silicone glucoheptonic acid amide surfactant. The primary ammonia value was measured by non-aqueous potentiometric titration, and the calculated grafting rate was 95%; the minimum surface tension of the product obtained was 24.3mN / m, the critical micelle concentration was 52mg / L, and the solubility was 75g / 100g water.

[0039] The obtained product has been detected by infrared spectrum, indicating that the method has prepared an ABA type silicone glucoheptonic ...

Embodiment 2

[0041] Add 20.8g glucoheptonolactone and 39.8g bisaminoethylaminopropyl tetramethoxydisiloxane to the flask, add 140mL ethanol as solvent, react at 90°C for 3h, distill off ethanol to obtain glucoheptin Sugar acid amide tetramethoxydisiloxane. Add 60.6g of glucoheptonic acid amide tetramethoxydisiloxane and 55.5g of hexamethyltrisiloxane into the flask, and add potassium trimethylsiliconate with a mass fraction of 1.5% as catalyst 0.83g, at 85°C Under the reaction 3h. After the reaction, heat to 134°C to deactivate the catalyst to obtain the silicone glucoheptonic acid amide surfactant. The primary ammonia value was measured by non-aqueous potentiometric titration, and the calculated grafting rate was 98%; the minimum surface tension of the product obtained was 22.4mN / m, the critical micelle concentration was 390mg / L, and the solubility was 59g / 100g water.

Embodiment 3

[0043] Add 20.8g glucoheptonolactone and 31.2g bisaminopropyltetramethoxydisiloxane into the flask, add 200mL isopropanol as solvent, react at 95°C for 1.5h, distill and remove isopropanol to obtain Glucoheptonamide Tetramethoxydisiloxane. Add 37.1g of glucoheptonic acid amide tetramethoxydisiloxane and 3.7g of eicosylcyclodecasiloxane into the flask, add 0.037g of potassium trimethylsiliconate as a catalyst, and react at 110°C for 4h . After the reaction is over, add acetic acid to deactivate the catalyst, and filter to obtain the organic silicon glucoheptonic acid amide surfactant. The primary ammonia value was measured by non-aqueous potentiometric titration, and the grafting rate was calculated to be 97.5%; the minimum surface tension of the product obtained was 26.4mN / m, the critical micelle concentration was 740mg / L, and the solubility was 68g / 100g water.

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Abstract

The invention discloses a preparation method of an ABA type organosilicone glucoheptonic acid amide surface active agent. The preparation method of the ABA type organosilicone glucoheptonic acid amidesurface active agent comprises the steps that glucoheptonic acid lactone and amino-terminated double-terminated siloxane are used as raw materials, higher alcohol is used as a solvent, the reaction is carried out for 1-4 hours under the condition of 60-80 DEG C, the higher alcohol solvent is evaporated after the reaction, and glucoheptonic acid amide siloxane is obtained; and under the action ofa catalyst, the glucoheptonic acid amide siloxane and cyclosiloxane are used as raw materials, the reaction is carried out for 2-5 hours under the condition of 90-150 DEG C, after the reaction, the catalyst is deactivated, and the ABA type organosilicone glucoheptonic acid amide surface active agent is obtained. The preparation method of the ABA type organosilicone glucoheptonic acid amide surfaceactive agent has the advantages that the cost is low, preparation is simple, the preparation method is suitable for large-scale industrial production, and the water solubility of products is good.

Description

technical field [0001] The invention relates to a preparation method of an ABA type organic silicon glucoheptonate amide surfactant used in shampoos and cosmetics, and belongs to the technical field of surfactant preparation. Background technique [0002] The sugar amide is grafted on the middle or end of the siloxane to form a sugar amide modified silicone surfactant, which is a new type of high-efficiency and green surfactant. The preparation methods of organosilicon sugar amides generally include hydrosilylation and bulk polymerization-grafting. [0003] In the preparation of organosilicon sugar amides, there are relatively many reports on the hydrosilylation method. For example, Feng Shengyu et al. (Carbohydrate Polymer, 2006, 65, 321) reported a method for the preparation of organosilicon sugar amides, first reacting gluconolactone with allylamine to generate N-allyl glucamide, and then reacting with hydrogen-containing siloxane Alkanes undergo hydrosilylation reactio...

Claims

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Application Information

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IPC IPC(8): C07F7/18C08G77/26C08G77/16C08G77/06
CPCC07F7/1804C07F7/188C08G77/045Y02P20/584
Inventor 王国永郭凌霄白艳云台秀梅王天壮
Owner CHINA RES INST OF DAILY CHEM IND
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