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Mercapto nano-silica and polyether dual modified organosilicon surfactant and preparation method

A nano-silica, surfactant technology, applied in chemical instruments and methods, transportation and packaging, chemical/physical processes, etc., can solve the problem of uneven dispersion of nano-modified materials, poor compatibility, and single polysiloxane. and other problems, to achieve good hydrophilic and lipophilic and compatible properties, strong chemical stability, and broaden the application prospects.

Inactive Publication Date: 2017-05-10
JIANGSU MAYSTA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problem of uneven dispersion and poor compatibility of nano-modified materials in the above-mentioned prior art and the problem of the singleness of polyether modified polysiloxane, and propose a new type of organic silicon surfactant. Silicone surfactant grafted nano-silica particles and polyether segments on polysiloxane main chain simultaneously through click chemistry and hydrosilylation reaction

Method used

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  • Mercapto nano-silica and polyether dual modified organosilicon surfactant and preparation method
  • Mercapto nano-silica and polyether dual modified organosilicon surfactant and preparation method
  • Mercapto nano-silica and polyether dual modified organosilicon surfactant and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Preparation of mercapto nano-silica

[0045] Weigh 30.63g of nano-silica and ultrasonically disperse it in anhydrous ethanol solution at 40°C, and add 6.12g of 3-mercaptopropyltrimethoxysilane dropwise to the above-mentioned silica solution, using ammonia as a catalyst to adjust the reaction Environment to pH=8.9, react at 80° C. for 8 hours, wash with absolute ethanol, and dry to obtain mercapto-functionalized nano-silica.

[0046] (2) Preparation of vinyl polymethylhydrogen siloxane

[0047] Weigh 41.53g of octamethylcyclotetrasiloxane, 12.63g of 1,3,5,7-tetramethylcyclotetrasiloxane, 6.02g of tetravinyltetramethylcyclotetraoxane and 2.27g of hexamethylbis Add 0.94 g of concentrated sulfuric acid as a reaction catalyst to the siloxane in the reactor, and keep the reaction at 45° C. for 6 hours to obtain vinyl-containing polymethylhydrogen siloxane.

[0048] (3) Preparation of polymethylhydrogensiloxane modified by mercapto nano-silica

[0049] Take by weighing ...

Embodiment 2

[0053] (1) Preparation of mercapto nano-silica

[0054] Weigh 136.55g of nano-silica and ultrasonically disperse it in anhydrous methanol solution at 30°C, and add 32.3g of 3-mercaptopropyltriethoxysilane dropwise to the above-mentioned silica solution, using ammonia as a catalyst, adjust The reaction environment was adjusted to pH=9.2, reacted at 80° C. for 6 h, washed with absolute ethanol, and dried to obtain mercapto-functionalized nano-silica.

[0055] (2) Preparation of vinyl polymethylhydrogen siloxane

[0056] Weigh 206.45g octamethylcyclotetrasiloxane, 15.69g1,3,5,7-tetramethylcyclotetrasiloxane and 16.22g tetramethyldivinyldisiloxane in the reactor, add 11.92 g concentrated sulfuric acid was used as the reaction catalyst, and the reaction was carried out at 55° C. for 3 hours to obtain vinyl-containing polymethylhydrogen siloxane.

[0057] (3) Preparation of polymethylhydrogensiloxane modified by mercapto nano-silica

[0058] Take by weighing 103.69g step (1) merc...

Embodiment 3

[0062] (1) Preparation of mercapto nano-silica

[0063] Weigh 75.39g of nano silicon dioxide and ultrasonically disperse it in anhydrous ethanol solution at 20°C, and add 18.1g of 3-mercaptopropyltriethoxysilane dropwise to the above silicon dioxide solution, using ammonia water as a catalyst, adjust The reaction environment was adjusted to pH=8.5, reacted at 70° C. for 10 h, washed with absolute ethanol, and dried to obtain mercapto-functionalized nano-silica.

[0064] (2) Preparation of vinyl polymethylhydrogen siloxane

[0065] Weigh 206.45g of octamethylcyclotetrasiloxane, 15.69g of 1,3,5,7-tetramethylcyclotetrasiloxane, 24.82g of tetravinyltetramethylcyclotetraoxane and 17.89g of tetramethylbis Add 8.34 g of trifluoromethanesulfonic acid to the reactor with vinyl disiloxane as a reaction catalyst, and keep the reaction at 80° C. for 4.5 hours to obtain vinyl-containing polymethylhydrogen siloxane.

[0066] (3) Preparation of polymethylhydrogensiloxane modified by mercap...

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Abstract

The invention belongs to the technical field of organosilicon surfactants, and particularly relates to a mercapto nano-silica and polyether dual modified organosilicon surfactant and a preparation method. The invention discloses a method for preparing the organosilicon surfactant by combining a mercapto-ene-click chemical method and a hydrosilylation method for dual modification. The mercapto nano-silica and polyether dual modified organosilicon surfactant is successfully synthesized from vinyl-containing polymethylhydrosiloxane as a structural main body, and the product has both good oleophilic and Hydrophilically properties and compatibility due to the introduction of double functional groups. Besides, the application prospect of the organosilicon surfactant is broadened by introducing the mercapto functional group with high chemical stability.

Description

technical field [0001] The invention belongs to the technical field of organosilicon surfactant preparation, and in particular relates to an organosilicon surfactant double-modified by mercapto nano silicon dioxide and polyether and a preparation method. Background technique [0002] Organosilicon surfactants are a type of organic-inorganic hybrid polymers with repeating chains of Si-O-Si as the main chain and organic functional groups directly connected to silicon atoms, also known as polysiloxanes. Sex, flexibility, low surface tension, chemical and biological compatibility and excellent thermal stability and many other properties. In order to expand the types and application fields of organosilicon polymer products, it has been a research hotspot in the past two decades to introduce one or more special functional groups into traditional siloxane to obtain better performance organosilicon materials, such as Polyether-modified polysiloxane, long-chain alkane-modified polys...

Claims

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Application Information

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IPC IPC(8): C08G77/46C08G77/392C08G77/20B01F17/54C09K23/54
CPCC08G77/20C08G77/392C08G77/46C09K23/00
Inventor 马宏明吴培培唐雄峰孙宇
Owner JIANGSU MAYSTA CHEM
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