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Method for preparing Bola ionic liquid type organosilicon surfactant

A technology of surfactants and ionic liquids, which is applied in the field of synthesis of silicone surfactants, can solve the problems affecting the activity of surfactants and unsatisfactory surface tension, and achieve easy operation, excellent thermal stability and biophase The effect of capacitive and simple process steps

Active Publication Date: 2015-04-08
JIUJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although many Bola-type surfactants have been reported at present, their ability to reduce the surface tension of water is not ideal, such as Bola-type surfactant 1,12-di The γCMC of glutamic acid-based dodecyl diamine salt is 50.5 mN / m, see Xian Shuyong, master thesis, Yangzhou University, 2010; Bola type polyurethane surfactant γ CMC is greater than 39.0 mN / m, see Zhang Jing, master thesis, North University of China, 2013; Hao Chuanming prepared Bola-type organic matter with γCMC of 24.6mN / m by hydrosilylation For silicon surfactants, see Hao Chuanming, Cui Xiao, Li Junying, Abstracts of the 29th Annual Academic Conference of the Chinese Chemical Society - Section 26: Colloids and Interfaces, 2014-8-4; but there are α and β due to hydrosilylation Addition reaction, so there are isomers in the synthesized product, which affects the activity of the surfactant

Method used

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  • Method for preparing Bola ionic liquid type organosilicon surfactant
  • Method for preparing Bola ionic liquid type organosilicon surfactant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 6.0 g of octamethylcyclotetrasiloxane, 2.9 g of 1,3-di(chloropropyl)tetramethyldisiloxane, and the addition of concentrated sulfuric acid catalyst in the reactor are 2% (mass fraction), After stirring at room temperature for 2-4 hours, wash with water until neutral, and remove from low boiling. α, ω-dichloropropylpolysiloxane was obtained with a degree of polymerization of 6.6.

[0024] In a 100ml three-neck flask equipped with a condenser tube, add 5.0 g α, ω-dichloropropyl polysiloxane, 6.0 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 precipitate again, and the dissolution-precipitation was repeated 5 times with anhydrous methanol...

Embodiment 2

[0026] 6.0 g of octamethylcyclotetrasiloxane, 2.9 g of 1,3-di(chloropropyl)tetramethyldisiloxane, and concentrated sulfuric acid catalyst were added in an amount of 2% (mass fraction) in the reactor, After stirring at room temperature for 2-4 hours, wash with water until neutral, and remove from low boiling. α, ω-dichloropropyl polysiloxane was obtained, and the polymer was 6.6.

[0027] In a 100 ml three-necked flask equipped with a condenser tube, add 5.0 g α, ω-dichloropropyl polysiloxane, 6.2 g N-methylpyrrolidine, 10 ml isopropanol, N 2 React at 80°C for 34 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 precipitate again, and the dissolution-precipitation was repeated 5 times with anhydrous methanol-...

Embodiment 3

[0029] In the reactor, 7.4 g of octamethylcyclotetrasiloxane, 2.4 g of 1,3-bis(chloromethyl)tetramethyldisiloxane, and the addition of concentrated sulfuric acid catalyst are 2% (mass fraction), Stir at room temperature for 2 to 4 hours, wash with water until neutral, and take off the low boil. α, ω-Dichloromethylpolysiloxane was obtained with a degree of polymerization of 8.9.

[0030] In a 100ml three-necked flask equipped with a condenser tube, add 5.0 g α, ω-dichloromethylpolysiloxane, 5.8 g N-methylimidazole, 20 ml isopropanol, N 2 React at 80°C for 30 hours under protection, and cool to room temperature naturally after the reaction. Pour into 40 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 precipitate again, and the dissolution-precipitation was repeated 6 times with anhydrous methanol-ethyl...

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Abstract

The invention discloses a method for preparing a Bola ionic liquid type organosilicon surfactant. The Bola ionic liquid type organosilicon surfactant has the Bola amphiphilic molecule structure characteristics, and is prepared from reaction of alpha, omega-dichloro propyl polysiloxane or alpha, omega-dichloro methyl polysiloxane and N-methylimidazole, N-methylpyrrolidine or pyridine. The method is simple in preparation step and easy to operate, and the prepared surfactant is excellent in surface activity, has certain sterilization property and can be used in fields such as medicine slow release, functional nano materials and textile processing additives.

Description

technical field [0001] The invention relates to a preparation method of a Bola ionic liquid type silicone surfactant, belonging 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 of silicone downstream products, the variety of silicone surfact...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F17/54C09K23/54
Inventor 谭景林肖梅红严平彭游
Owner JIUJIANG UNIVERSITY
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