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Hydrolysis resistant Si-C-Si type cation organosilicon surfactant

A surfactant, si-c-si technology, is used in the preparation of surfactants, and in the field of hydrolysis-resistant Si-C-Si cationic silicone surfactants, which can solve the problem of affecting the activity of surfactants and is not suitable for industrialization. production and other problems, to achieve the effects of excellent hydrolysis resistance, feasible preparation method and high surface activity

Active Publication Date: 2015-07-22
JIUJIANG UNIVERSITY
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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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  • Hydrolysis resistant Si-C-Si type cation organosilicon 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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PUM

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Abstract

The invention discloses a hydrolysis resistant Si-C-Si type cation organosilicon surfactant. The hydrolysis resistant Si-C-Si type cation organosilicon surfactant is prepared by performing reaction on the chloropropy carbosilane, N-methylimidazole, N-methylpyrrolidine, N, N-dimethylethanolamine, trimethylamine, triethylamine or pyridine. The prepared surfactant has good surface activity and a certain germicidal activity and can be used in the fields such as pesticide adjuvants, drug sustained release, functional nano-materials and textile processing aids.

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 developme...

Claims

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Application Information

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IPC IPC(8): C07F7/10B01F17/54C09K23/54
Inventor 谭景林肖梅红
Owner JIUJIANG UNIVERSITY
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