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A kind of hydrolysis-resistant si-c-si type cationic silicone surfactant

A surfactant and cationic technology, which is applied in the preparation of surfactants and in the field of hydrolysis-resistant Si-C-Si cationic silicone surfactants, can solve problems that are not suitable for industrial production and affect the activity of surfactants. Achieve the effects of feasible preparation method, excellent hydrolysis resistance and easy operation

Active Publication Date: 2017-10-24
JIUJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, they are basically non-ionic silicone surfactants, and the hydrosilylation method is used to introduce hydrophilic groups such as polyether into the hydrophobic segment. Since there are α and β addition reactions in the hydrosilylation addition, the synthesized There are isomers of the product, which affects the activity of the surfactant
The applicant used trimethylsilyllithium to prepare chloropropylsilane and then prepared Si-C-Si type silicone surfactant, but in this method, relatively expensive trimethylsilyllithium reagent was used. See Tan, J. L.; Feng, S.Y., Colloid Polym. Sci., 2013,29(6):1487-1494, not suitable for industrial production

Method used

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  • A kind of hydrolysis-resistant si-c-si type cationic silicone surfactant
  • A kind of hydrolysis-resistant si-c-si type cationic silicone surfactant
  • A kind of hydrolysis-resistant si-c-si type cationic silicone surfactant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] N 2 Under protection, in a 250 ml four-neck flask, add 8.6 g of chloropropylmethyldichlorosilane to 50 ml of anhydrous tetrahydrofuran, cool to 0 °C, add 8 g of trimethylsilylmethylmagnesium chloride dropwise, and let it rise naturally to room temperature and stirring was continued for 4 hours. After the reaction is completed, the reaction is terminated with anhydrous methanol, separated by filtration, extracted and separated, and concentrated to obtain chloropropyltrisilazane.

[0026] In a 100ml three-necked flask equipped with a condenser, add 5.0 g chloropropyl trisilane, 4.0 g N-methylimidazole, 10 ml isopropanol, N 2 React at 85°C for 36 hours under protection, and cool to room temperature naturally after the reaction. Pour into 30 ml of ethyl acetate to precipitate the crude product, pour off the upper layer solution, and then add 2 ml of anhydrous methanol to dissolve the crude product. Then the dissolved product was added to 30 ml of ethyl acetate to precipi...

Embodiment 2

[0028] N 2 Under protection, in a 250 ml four-necked flask, 8.6 g of chloropropylmethyldichlorosilane was added to 50 ml of anhydrous tetrahydrofuran, cooled to 0 ° C, and 12 g of phenyldimethylsilylmagnesium chloride Grignard reagent was added dropwise, Naturally rose to room temperature and continued to stir for 5 hours. After the reaction is completed, the reaction is terminated with anhydrous methanol, separated by filtration, extracted and separated, and concentrated to obtain chloropropyltrisilazane.

[0029] In a 100ml three-necked flask equipped with a condenser, add 6.0 g of phenylchloropropyl trisilane, 4.0 g of N-methylimidazole, 10 ml of isopropanol, N 2 React at 85°C for 36 hours under protection, and cool to room temperature naturally after the reaction. Separation with n-hexane, and then remove the n-hexane to obtain a solid at 0.1 MPa, dry at 40°C for 1 day, and obtain a phenyl-containing Si-C-Si type silicone surfactant after cooling. The yield was 89%. Ke...

Embodiment 3

[0031] N 2 Under protection, in a 250 ml four-necked flask, add 9.1 g of chloropropylmethyldimethoxysilane to 50 ml of anhydrous tetrahydrofuran, add 8 g of trimethylsilylmagnesium chloride Grignard reagent dropwise, and heat up after the addition Slightly reflux and stirring was continued for 4 hours. After the reaction is completed, the reaction is terminated with anhydrous methanol, separated by filtration, extracted and separated, and concentrated to obtain chloropropyltrisilazane.

[0032] In a 100ml three-necked flask equipped with a condenser, add 5.0 g chloropropyl trisilane, 4.0 g N-methylimidazole, 10 ml isopropanol, N 2 React at 85°C for 36 hours under protection, and cool to room temperature naturally after the reaction. Pour into 30 ml of ethyl acetate to precipitate the crude product, pour off the upper layer solution, and then add 2 ml of anhydrous methanol to dissolve the crude product. Then the dissolved product was added to 30 ml of ethyl acetate to precip...

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Abstract

The present invention relates to a kind of hydrolysis-resistant Si-C-Si type cationic organosilicon surfactant, it passes chloropropyl silane and N-methylimidazole, N-methylpyrrolidine, N,N-dimethylethanolamine , Trimethylamine, triethylamine or pyridine and other reactions. The surfactant prepared by the invention has excellent surface activity and certain bactericidal properties, and can be used in the fields of pesticide auxiliaries, drug sustained release, functional nanometer materials, textile processing aids and the like.

Description

technical field [0001] The invention discloses a hydrolysis-resistant Si-C-Si type cationic silicone surfactant, and specifically relates to a preparation method of the surfactant, which belongs to the technical field of synthesis of silicone surfactants. Background technique [0002] Silicone surfactants are a new type of high-efficiency surfactants, which are composed of siloxane / carbonane as hydrophobic chain links and one or more hydrophilic groups. Not only has better surface activity and "super-spreading" properties than alkane surfactants, but also has excellent properties such as high and low temperature resistance, weather aging resistance, non-toxic and physiological inertia of silicone materials. This type of silicone surfactant is widely used in polyurethane foam, pesticides, textile auxiliaries, daily auxiliaries, oilfield chemicals and other fields due to its excellent performance. With the further development of silicone materials and the in-depth development...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/10B01F17/54C09K23/54
Inventor 谭景林肖梅红
Owner JIUJIANG UNIV
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