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Preparation method of carboxyl silicone oil

A carboxyl silicone oil and solvent technology, which is applied in the field of carboxyl silicone oil preparation, can solve the problems of cumbersome and complicated carboxyl silicone oil processes, and achieve the effects of facilitating popularization and application, simplifying the preparation process, and simplifying the synthesis process

Inactive Publication Date: 2012-10-17
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the cumbersome and complex process of preparing carboxyl silicone oil in the prior art, the object of the present invention is to provide a method for preparing carboxyl silicone oil with easy-to-obtain raw materials and simplified synthesis process

Method used

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  • Preparation method of carboxyl silicone oil
  • Preparation method of carboxyl silicone oil
  • Preparation method of carboxyl silicone oil

Examples

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Embodiment 1

[0027] 1, Preparation of 11-carboxyundecylmethyldichlorosilane

[0028] (1) Hydrosilylation: Add 100g of undecylenic acid and 200g of toluene to a three-necked flask equipped with a magnetic stirrer, a thermometer, a reflux condenser and a nitrogen protection device, raise the temperature to 100~102°C, and add 0.15g of city For a platinum / carbon catalyst with a platinum content of 5%, start to add 63.5 g of methyldichlorohydrosilane dropwise, and finish adding within 1 hour. After dripping, keep warm for 3 hours. After the catalyst was removed by filtration, the filtrate was rotary evaporated to remove toluene to obtain light yellow and transparent 11-carboxyundecylmethyldichlorosilane. In this step, 11-carboxyundecylmethyldichlorosilane is synthesized by the direct hydrosilylation reaction of undecylenic acid and methylhydrogen dichlorosilane, and its reaction formula is as follows:

[0029]

[0030] See attached figure 1 , it is the infrared spectrogram of the 11-carbo...

Embodiment 2

[0047] The present embodiment provides a kind of preparation method of carboxyl silicone oil, and its step comprises:

[0048] (1) Hydrosilylation: In a three-necked flask equipped with a magnetic stirrer, thermometer, reflux condenser and nitrogen protection device, add 80 g of undecylenic acid and 150 g of benzotrifluoride, raise the temperature to 103~105 ° C, add 0.1 g of a commercially available platinum / carbon catalyst with a platinum content of 5%, start to add 58.0 g of methyldichlorohydrosilane dropwise, and finish adding within 1 h. After dripping, keep warm for 4 hours. After removing the catalyst by filtration, the filtrate was rotary evaporated to remove benzotrifluoride to obtain transparent 11-carboxyundecylmethyldichlorosilane.

[0049] (2) Co-hydrolysis: Add 60g of distilled water into the three-necked flask, stir at room temperature and start to drop the monomer mixture formed by 45g of 11-carboxyundecylmethyldichlorosilane and 40g of dimethyldichlorosilane,...

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Abstract

The invention discloses a preparation method of carboxyl silicone oil. Undecylenic acid and methyl hydrogen dichlorosilane are taken as raw materials to be subjected to direct hydrosilylation in the presence of a platinum / carbon catalyst to obtain 11-carboxyl undecyl methyl dichlorosilane; and the carboxyl silane monomer 11-carboxyl undecyl methyl dichlorosilane and dimethyldichlorosilane are subjected to co-hydrolysis and equilibrium polycondensation to obtain 11-carboxyl undecyl methyl silicone oil. The preparation method has the following advantages: the preparation process of carboxyl silicone oil is simplified by adopting the method for preparing the carboxyl silane monomer by one step through the direct addition reaction; the raw materials adopted for synthesis are industrial raw materials and are suitable for industrial large-scale production; and after being prepared into emulsion and compounded with amino silicone oil emulsion, the prepared carboxyl silicone oil can provide very good softness and full hand feel when being applied to textile finishing.

Description

technical field [0001] The invention relates to a preparation method of carboxyl silicone oil, which belongs to the technical field of organosilicon material synthesis. Background technique [0002] Carboxyl silicone oil is a modified silicone oil whose side chain is substituted (or partially substituted) with carboxyalkyl groups for methyl groups. It can be prepared in the following ways: (1) Reaction of aminohydrocarbyl silane with organic acid anhydride. The process provided by this method can directly use aminosilane to prepare carboxysilane monomer, but the obtained carboxyl substituent is bonded to the silicon atom through a urethane bridge group, and the urethane group has strong polarity and reactivity which may affect carboxyl silicone oil. Physical properties and application performance. (2) Condensation of chloroalkyl siloxane with carboxylate. This method has not been widely used because chlorohydrocarbyl silane and chlorohydrocarbyl siloxane are not easy to pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/14D06M15/643
Inventor 李战雄关晋平姜佳美沈玲
Owner SUZHOU UNIV
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