Alkoxy silane acetylenic silicon hydrogen addition inhibitor and preparation method thereof

A technology for alkoxysilylation of alkynes and hydrosilylation, which is applied in the field of multifunctional alkoxysilylation of acetylenic hydrosilylation inhibitors and their preparation, and can solve the problem of poor storage stability of glue A, etc. To solve the problem of toxicity, good reproducibility of the reaction, and the effect of reducing volatility

Active Publication Date: 2016-03-23
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the residual silicon hydrogen will lead to poor stora

Method used

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  • Alkoxy silane acetylenic silicon hydrogen addition inhibitor and preparation method thereof
  • Alkoxy silane acetylenic silicon hydrogen addition inhibitor and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0023] Embodiment two, preparation

[0024] In a 250ml three-necked round-bottom flask equipped with a magnet, a reflux condenser, a bubbler and a nitrogen device, add successively, 12.4g (0.1mol) ethynyl cyclohexanol, 30.4g (0.2mol) tetramethoxysilane , 0.1 g butyl titanate. React at a temperature of 60 degrees for 24 hours to obtain a blood red liquid. After cooling, the oil pump reduced pressure distillation to remove low boilers, and then raised the temperature to 90°C to extract the product to obtain 24.0 g of a colorless transparent liquid. 1 H-NMR (CDCl 3 ,300MHz)δ[ppm]:3.60(s,9H,OCH 3 ), 2.53(s,-C≡C-H), 1.95(br,2H), 1.69-1.59(m,5H), 1.58-1.49(m,2H), 1.26(br,1H)

Embodiment 3

[0025] Embodiment three, preparation

[0026] Add 12.6g (0.15mol) methyl butynol, 44.4g (0.3mol) vinyltrimethoxysilane successively in the 250ml three-neck round-bottomed flask equipped with magneton, reflux condenser, bubbler and nitrogen device , 0.15g stannous isooctanoate, react at 90 degrees for 6 hours. After cooling, a pale yellow liquid was obtained. The oil pump decompressed to remove the low boilers, and then heated up to 60°C to extract the product to obtain 29.5 g of a colorless transparent liquid. 1 H-NMR (CDCl 3 ,300MHz)δ[ppm]:6.16-5.88(m,3H,-CH=CH 2 ),3.58(s,6H,OCH 3 ),2.45(s,1H,-C≡C-H),1.59(s,6H,-CH 3 )

Embodiment 4

[0027] Example 4, preparation

[0028] In the 250ml three-neck round-bottomed flask that is equipped with magneton, reflux condenser, bubbler and nitrogen device, successively 14.2g ethynyl cyclohexanol (0.11mol), 33.8g (0.23mol) vinyltrimethoxysilane, 0.12g potassium carbonate, react at 20 degrees for 20 hours. After cooling, potassium carbonate was removed by centrifugal filtration. Oil pump reduced pressure distillation to remove low boilers, and then heated up to 90 degrees to extract the product to obtain 25.9 g of colorless transparent liquid. 1 H-NMR (CDCl 3 ,300MHz)δ[ppm]:6.11-5.89(m,3H,-CH=CH 2 ),3.54(s,9H,OCH 3 ),2.49(s,-C≡C-H),1.89(br,2H),1.68-1.57(m,5H),1.55-1.48(m,2H),1.26(br,1H)

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Abstract

The invention relates to an alkoxy silane acetylenic silicon hydrogen addition inhibitor and a preparation method thereof. The alkoxy silane acetylenic silicon hydrogen addition inhibitor uses alkynol and alkoxy silane as main materials, and an inhibitor which is added through alkoxy silane acetylenic silicon hydrogen is generated under the action of a catalyst. The method for preparing the alkoxy silane acetylenic silicon hydrogen addition inhibitor is simple, the alkoxy silane acetylenic silicon hydrogen addition inhibitor which is obtained through the method for preparing the alkoxy silane acetylenic silicon hydrogen addition inhibitor can overcome the defects that alkynol inhibitors and base glue are poor in compatibility, are easy to volatilize and residue has toxicity and the like. The alkoxy silane acetylenic silicon hydrogen addition inhibitor can prolong storage life in room temperature by being used in additional liquid silicone rubbers, enables the surfaces of the additional liquid silicone rubbers to be smooth after being solidified, can improve bonding with base materials through organic groups which are connected with the inhibitor, and gives better bonding force to glue.

Description

technical field [0001] The invention relates to the field of organosilicon materials, in particular to a multifunctional alkoxysilylated acetylenic hydrosilylation inhibitor and a preparation method thereof. Background technique [0002] Since the discovery of Sommer et al. (SommerLH, PietruszaEW, WhitmoreFC. Peroxide-catalyzed addition of trichlorosilaneto1-octene [J]. Journal of the American Chemical Society, 1947, 69 (1): 188-188.), the hydrosilylation reaction has become the most important in organosilicon chemistry. It is widely used in the synthesis of carbon-functional organosilicon compounds / polymers, organosilicon dendrimers, and addition-type silicone rubber vulcanization. The hydrosilylation reaction speed needs to be properly regulated according to the needs of use. For example, in addition-type silicone rubber, in order to meet the needs of pouring, coating or injection molding processes, after mixing the two components of two-component addition-type liquid sil...

Claims

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Application Information

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IPC IPC(8): C07F7/18C07F7/04
CPCC07F7/045C07F7/1804C07F7/188
Inventor 唐红定熊英刘进
Owner WUHAN UNIV
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