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Preparation method for Si-C-Si type anionic organosilicon surfactant

A surfactant, si-c-si technology

Pending Publication Date: 2018-11-30
JIUJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the silicone surfactant with Si-O-Si as the hydrophobic group has the disadvantage of being easily hydrolyzed, which severely restricts its development in agricultural adjuvants and the like.

Method used

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  • Preparation method for Si-C-Si type anionic organosilicon surfactant

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preparation example Construction

[0023] A kind of preparation method of Si-C-Si type anionic silicone surfactant, such as figure 1 Shown, this preparation method comprises the steps:

[0024] (1) Format response: in N 2 Under protection, chloromethylsilane is first prepared into Grignard reagent; then in N 2 Under protection, add vinylalkoxysilane or vinylchlorosilane into a four-necked flask filled with anhydrous tetrahydrofuran or anhydrous ether, and drop chloromethylsilane or methyl Grignard reagent to synthesize vinylsilicane;

[0025] (2) Mercapne reaction: put the vinylsilane obtained in (1) into a three-necked flask, add mercapto compound, solvent, and catalyst, and carry out mercaptoene reaction for 0.5~4 hours; extract with water-dichloromethane , the obtained solid was dried at 0.1 MPa and 40°C for 24 hours, and after cooling, a Si-C-Si type anionic silicone surfactant was obtained.

[0026] The chloromethylsilane is chloromethyl trimethylsilane, chloromethyl ethyl dimethyl silane, chloromethyl ...

Embodiment 1

[0035] (1) in N 2 Under protection, in a 250 ml four-neck flask, add 7.0 g methylvinyldichlorosilane to 50 ml anhydrous tetrahydrofuran, cool to 0 °C, add 8.0 g trimethylsilylmethylmagnesium chloride dropwise, and naturally rise to Stirring was continued at room temperature for 4 hours. After the reaction was completed, the reaction was terminated with anhydrous methanol, separated by filtration, extracted and separated, and concentrated to obtain vinyltrisilazane.

[0036] (2) In a 100ml three-necked flask equipped with a condenser, add 4.88 g of vinyl trisilane, 2.74 g of sodium thioglycolate, 10 ml of methanol, 0.16 g of benzoin dimethyl ether, N 2 The thioene reaction was carried out under protection for 30 minutes. After the reaction was completed, it was naturally cooled to room temperature, poured into 30 ml of ethyl acetate to precipitate the crude product, poured out the upper layer solution, and then added 2 ml of water to dissolve the crude product. Then extract wi...

Embodiment 2

[0038] (1) in N 2 Under protection, in a 250 ml four-neck flask, add 6.6 g of methylvinyldimethoxysilane to 50 ml of anhydrous ether, cool to 0 °C, add dropwise 8.0 g of trimethylsilylmethylmagnesium chloride, and naturally Warm up to room temperature and continue 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 vinyltrisilane.

[0039] (2) In a 100ml three-necked flask equipped with a condenser, add 4.88 g of vinyl trisilane, 2.74 g of sodium thioglycolate, 10 ml of methanol, 0.16 g of benzoin dimethyl ether, N 2 Carry out the thioene reaction under protection for 30 minutes. After the reaction, naturally cool to room temperature, pour into 30 ml of ethyl acetate to precipitate the crude product, pour off the upper layer solution, add 2 ml of water to dissolve the crude product, and then use 8 ml of dichloro Methane extraction, repeated extrac...

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Abstract

The invention discloses a preparation method for a Si-C-Si type anionic organosilicon surfactant. The preparation method comprises the following steps: (1) performing a Grignard reaction: under the protection of N2, preparing a Grignard reagent by using chloromethylsilane; and under the protection of N2, adding vinyl alkoxysilane or vinyl chlorosilane into a four-necked flask containing anhydroustetrahydrofuran or anhydrous ether, and adding chloromethylsilane or a methyl Grignard reagent dropwise to synthesize vinyl carbosilane; and (2) performing a thiol-ene reaction: putting the product vinyl carbosilane obtained in the step (1) into a three-necked flask, adding a thiol compound, a solvent and a catalyst, performing the thiol-ene reaction for 0.5-4 h, performing extraction by using water-dichloromethane, drying the obtained solid for 24 h at pressure of 0.1 MPa and temperature of 40 DEG C, and performing cooling to obtain the Si-C-Si type anionic organosilicon surfactant. Accordingto the method disclosed by the invention, the surfactant prepared by the method has excellent surface activity and can be used in the fields of drug slow release, functional nano materials, textile processing auxiliary agents and the like.

Description

technical field [0001] The invention relates to a preparation method of Si-C-Si type anionic organic silicon surfactant. 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 of silicone downstream products, the variety of silicone surfactants will continue to increase, and the application fields will contin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F17/54C09K23/54
CPCC09K23/00
Inventor 谭景林肖梅红胡庆华严平
Owner JIUJIANG UNIVERSITY
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