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Preparation and application of a multifunctional poss type silicone curing agent

A multifunctional, organosilicon technology, applied in the fields of chemical industry and organic polymer materials, which can solve the problems of unsatisfactory POSS dispersion and so on

Active Publication Date: 2021-04-02
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the existing deficiencies, one of the purposes of the present invention is to provide a multifunctional POSS type silicone curing agent, which can be added to the silicone material as a crosslinking agent, so as to change the unsatisfactory dispersion after POSS is added in the past.

Method used

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  • Preparation and application of a multifunctional poss type silicone curing agent
  • Preparation and application of a multifunctional poss type silicone curing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 41ml of tetramethylammonium hydroxide, 50.96ml of methanol, and 15ml of water into a 500ml round bottom flask, stir in an ice bath, then add 22ml of tetraethoxysilane (0.1mol), and stir at room temperature for 24h. Afterwards, the mixture was added dropwise into another 1L three-necked flask (300ml of n-hexane and 42.9ml of 0.1mol dimethylchlorosilane had been added to the flask) under ice-bath conditions. The mixture was stirred at room temperature for 3 h. Finally, use a pear-shaped funnel to separate the liquid, take the upper layer liquid, spin evaporate, filter it with suction, wash it with methanol for 3 times, and get a white powder solid, dry it, and then get the raw material Si 8 o 12 (OSi(CH 3 ) 2 h) 8 .

[0039] Take 2g of the above-mentioned raw material POSS and put it into a 100ml three-necked flask, then add 30ml of toluene, add 0.04g of Pt catalyst dropwise, and stir at room temperature for 30min with nitrogen gas, then add 0.76g of absolute ethan...

Embodiment 2

[0042] Prepare Si according to the method in embodiment 1 8 o 12 (OSi(CH 3 ) 2 h) 8 Raw materials, take 2g of raw materials and put them into a 100ml three-necked flask, then add 30ml of toluene, add 0.04g of Pt catalyst dropwise, and stir at room temperature for 30min with nitrogen gas, then add 1.52g of absolute ethanol, react at 40°C for 24h, add activated carbon, and after ultrasonication for 1h, Suction filtration, rotary evaporation can obtain Si 8 o 12 (OSi(CH 3 ) 2 OCH 2 CH 3 ) 8 .

[0043] Prepare condensation type RTV silicone rubber according to the method of Example 1, except that the polyfunctional group POSS type silicone curing agent is prepared in this example, other formulations are the same as Example 1, and the properties of the gained silicone rubber are shown in Table 1 and figure 1 .

Embodiment 3

[0045] Prepare Si according to the method in embodiment 1 8 o 12 (OSi(CH 3 ) 2 h) 8 Raw material, take 2g of raw material and put it into a 100ml three-necked flask, then add 30ml of ether, add 0.02g of Pt catalyst dropwise, and stir at room temperature for 30min with nitrogen gas, then add 0.40g of anhydrous methanol, react at 40°C for 12h, add activated carbon, and ultrasonicate for 1h, Suction filtration, rotary evaporation can obtain Si 8 o 12 (OSi(CH 3 ) 2 h) 5 (OSi(CH 3 ) 2 OCH 3 ) 3 . The NMR characterization results of the product are:

[0046] Prepare condensation type RTV silicone rubber according to the method of Example 1, except that the polyfunctional group POSS type silicone curing agent is prepared in this example, other formulations are the same as Example 1, and the properties of the gained silicone rubber are shown in Table 1 and figure 1 .

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Abstract

The invention relates to a preparation method of a multifunctional POSS (polyhedral oligomeric silsesquioxanes) type organosilicon curing agent and application of the curing agent in organosilicon materials. The method includes the steps of: (1) carrying out silicon hydrogen condensation reaction to prepare a multifunctional POSS type organosilicon curing agent; (2) adding the multifunctional POSStype organosilicon curing agent obtained in step (1) as a cross-linking agent into a polysiloxane system with a molecular chain end or side chain in connection with Si-OH, Si-OR, and C=C, and then carrying out cross-linking curing reaction to prepare a high temperature resistant organosilicon material. The multifunctional POSS type organosilicon curing agent prepared according to the invention can realize high compatibility with a polysiloxane system, and can maintain high light transmittance of the cured organosilicon material.

Description

technical field [0001] The invention relates to the preparation and application of a polyfunctional POSS type organic silicon curing agent, belonging to the fields of chemical industry and organic polymer materials. Background technique [0002] Polyhedral oligomeric silsesquioxanes (Polyhedral oligomeric silsesquioxanes, referred to as POSS) is a class of cage-type oligosiloxanes with a three-dimensional structure. The general molecular formula is: (RSiO 1.5 ) n , wherein n=4, 6, 7, 8, 10, 12, etc., R may be a hydrogen atom, a chlorine atom, an alkyl group, an aryl group, an alkenyl group or the like. In the mid-1990s, in order to meet the needs of the Air Force for a new generation of ultra-light and high-performance polymer materials, the Propulsion Technology Committee of the Air Force Research Lab (AFRL) developed POSS, a polyhedral oligomeric double-half Siloxane Nanostructured Hybrid System. In 2003, the American Hybrid Plastics Company began commercial production ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08L83/04C08L83/06
CPCC08G77/045C08L83/04C08L83/06
Inventor 周政宋国民李齐方
Owner BEIJING UNIV OF CHEM TECH
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