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Aqueous high-temperature-resistant thermosetting methylphenyl silicone resin and preparation method thereof

A methyl phenyl silicon, high-resistant technology, applied in the field of polymer compound synthesis, can solve the problems of changing the performance of silicone resin, not meeting environmental protection requirements, not high temperature resistance, etc., to improve heat resistance and realize self-emulsification , Good effect of high temperature resistance

Inactive Publication Date: 2020-01-14
WUHAN INSTITUTE OF TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, most of the existing methylphenyl silicone resins are oily, do not meet the requirements of environmental protection, and are not resistant to high temperature, have poor thermosetting properties, or the properties of the original silicone resin will be changed when modified.

Method used

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  • Aqueous high-temperature-resistant thermosetting methylphenyl silicone resin and preparation method thereof
  • Aqueous high-temperature-resistant thermosetting methylphenyl silicone resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 6.8g of polydimethylsiloxane, 2.8g of polyethylene glycol (PEG800) and 1.3g of Lewis acid catalyst (zinc chloride used in this example) and 48ml of ethanol into a 500mL three-necked flask, and stir at room temperature for 10h to obtain the prepared Obtain hydrophilic sol-gel silicone. Then in a 500 mL three-necked flask, add 10 g of methyltrichlorosilane, 9 g of dimethyldichlorosilane, 25 g of phenyltrichlorosilane, and 13 g of diphenyldichlorosilane into 150 mL of xylene in sequence, and stir at 60 ° C. A mixture of acetone and excess water was added dropwise, and stirring was continued for 2 h to obtain a silicone resin. Then add the hydrophilic sol-gel silicone prepared above into the silicone resin, stir in a 1000mL three-necked flask at 100°C under normal pressure for 6h, add water to the product and stir for 3h to complete the preparation of the hydrophilic hybrid silicone resin. Self-emulsifying. The resulting hydrophilic silicone resin has good hydrophilic...

Embodiment 2

[0025] Add 4.4g of methyldiethoxysilane, 3.0g of γ-aminopropyltriethoxysilane, 1.2g of Lewis acid catalyst (such as titanium tetrachloride TiCl4) and 36ml of ethanol into a 500mL enamel reaction kettle, and stir at room temperature for 10h to obtain Prepared hydrophilic sol-gel silicone. Then add 53.4ml xylene, 4.24g methyltrichlorosilane, 3.83g dimethyldichlorosilane, 9.95g phenyltrichlorosilane, 5.15g diphenyldichlorosilane in the 500 L enamel reaction kettle successively. Under stirring at 60°C, a mixture of acetone and excess water was added dropwise, and the stirring was continued for 100 min to obtain a silicone resin. Then add the hydrophilic sol-gel silicone prepared above into the silicone resin, stir in a 2000L enamel reactor at 100°C for 6 hours under normal pressure, add water to the product and stir for 5 hours to form a water-based high temperature resistant thermosetting methyl phenyl Silicone.

Embodiment 3

[0027] The water-based high-temperature-resistant thermosetting methylphenyl silicone resin in the above-mentioned example 2 and the methylphenyl silicone resin that has not been graft-modified are tested for related performance. °C / min) thermal weight loss l -m 0 ) / m 0 ×100%, where m 0 and m 1 Respectively, the mass of the film before and after immersion, the water-based high-temperature resistant thermosetting methylphenyl silicone resin has a water absorption rate of 23%, and there is no change after immersion in water at room temperature for 48 hours. The viscosity refers to GB / T 2794-1995, and is measured with a NDJ-7 rotary viscometer at a constant temperature of 25°C. The viscosity of the water-based high-temperature-resistant thermosetting methylphenyl silicone resin is 340mpa s, and the stickiness is 2.78min. Longer, able to meet market requirements. The impact strength of the resin is increased from 35 kg·cm to 50kg·cm, and the hardness reaches the 4H standard. ...

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Abstract

The invention discloses aqueous high-temperature-resistant thermosetting methylphenyl silicone resin and a preparation method thereof. The aqueous high-temperature-resistant thermosetting methylphenylsilicone resin is characterized in that the structural formula of the aqueous high-temperature-resistant thermosetting methylphenyl silicone resin is shown in a formula (I). (Please see the specification for the formula I). The preparation method comprises the following steps that (1) a sol-gel method is adopted to obtain a hydrophilic silane prepolymer; and (2) the hydrophilic silane prepolymeris grafted onto organic silicone resin to obtain the aqueous high-temperature-resistant thermosetting methylphenyl silicone resin, a reaction formula is shown in a formula (II): (Please see the specification for the formula II). The aqueous high-temperature-resistant thermosetting methylphenyl silicone resin and the preparation method have the beneficial effects that a controllable hydrophilic group can be given to the silicone resin without changing the properties of the silicone resin, the self-emulsifying of the silicone resin is achieved, and the prepared methylphenyl silicone resin is hydrophilic, resistant to high temperature and good in thermosetting performance.

Description

technical field [0001] The invention relates to a method for synthesizing a polymer compound, in particular to a water-based high-temperature-resistant thermosetting methylphenyl silicone resin. Background technique [0002] Silicone polymers are polymers containing elemental silicon in the molecular structure and organic groups attached to the silicon atoms. The polysiloxane with repeated Si-O bonds as the main chain and the organic group connected to the silicon atom is the main structural form of the silicone polymer. Usually, the silicon atom in the molecule contains three or more hydrolyzable functional groups. Polymer materials are called silicone resins, and silicone resins are a type of thermosetting polysiloxane system with a highly cross-linked structure. [0003] At present, there are many varieties of silicone resins, mainly including methyl silicone resin, phenyl silicone resin, methylphenyl silicone resin, MQ silicone resin, emulsion silicone resin, powder sil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/44C08G77/26C08G77/06
CPCC08G77/06C08G77/26C08G77/44
Inventor 周康帝程伊前郭嘉王萍吴华东
Owner WUHAN INSTITUTE OF TECHNOLOGY
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