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Method for preparing silane peroxide coupling agent

A technology of silane peroxide and coupling agent, which is applied in the field of preparation of silane peroxide coupling agent, can solve the problem of low yield, achieve the effect of increasing reaction yield, reducing the probability of by-products, and reducing side reactions

Active Publication Date: 2019-01-11
山东元禾新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by this invention is to overcome the low defect of the yield existing in the preparation method of existing silane peroxide coupling agent, and then provide a kind of preparation method of silane peroxide coupling agent

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  • Method for preparing silane peroxide coupling agent

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Experimental program
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Effect test

Embodiment 1

[0026] The preparation method of the silane peroxide coupling agent provided by the present embodiment may further comprise the steps:

[0027] (1) Preparation of 1,1-diperoxy-tert-butyl-4-hydroxycyclohexane

[0028] Mix 10g of tert-butanol hydroperoxide and 4-hydroxycyclohexanone in a molar ratio of 1:2, and put it into a reaction stirring tank, control the reaction temperature at 20°C, and add concentrated sulfuric acid with a concentration of 98wt% while stirring 1 mL, after the dropwise addition, continue to stir and react at a temperature of 20°C for 4 hours, and the obtained product is washed with water, filtered, and vacuum-dried to obtain 1,1-diperoxy-tert-butyl-4-hydroxycyclohexane, which The H spectrum is as follows: 1 H NMR (600MHz, CDCl 3 ,TMS): δ3.81(t,1H,COH), 2.14(s,1H,CH), 1.81(m,4H,CHCH 2 CH 2 ), 1.67 (s,4H,CHCH 2 CH 2 ), 1.24(t,18H,CCH 3 );

[0029] (2) Preparation of peroxide silane coupling agent

[0030] Get 1mol step (1) to make 1,1-diperoxy tert...

Embodiment 2

[0038] The preparation method of the silane peroxide coupling agent provided by the present embodiment may further comprise the steps:

[0039] (1) Preparation of 1,1-diperoxy-tert-butyl-4-hydroxycyclohexane

[0040] Mix 10g of tert-butanol hydroperoxide and 4-hydroxycyclohexanone in a molar ratio of 1:10, and put it into a reaction stirred tank, control the reaction temperature to be -10°C, and add a concentration of 98wt% concentrated solution while stirring. Sulfuric acid 0.5mL, after the dropwise addition, continue to stir and react at -10°C for 10h, the product obtained is washed with water, filtered, and vacuum-dried to obtain 1,1-diperoxy-tert-butyl-4-hydroxycyclohexane alkyl;

[0041] (2) Preparation of peroxide silane coupling agent

[0042] Take 1 mol of 1,1-diperoxy-tert-butyl-4-hydroxycyclohexane, 0.2 mol of tetramethoxysilane and 0.05 mol of titanium tetrachloride, and add 100 mL of CH 2 Cl 2 and CCl 4 A mixture of which, CH 2 Cl 2 and CCl 4 The volume rat...

Embodiment 3

[0047] The preparation method of the silane peroxide coupling agent provided by the present embodiment may further comprise the steps:

[0048] (1) Preparation of 1,1-diperoxy-tert-butyl-4-hydroxycyclohexane

[0049] Mix 10g of tert-butanol hydroperoxide and 4-hydroxycyclohexanone in a molar ratio of 1:5, and put it into a reaction stirred tank, control the reaction temperature to 0°C, and add concentrated sulfuric acid with a concentration of 98wt% while stirring 0.8mL, after the dropwise addition, continue to stir and react at 0°C for 5h, and the obtained product is washed with water, filtered, and vacuum-dried to obtain 1,1-diperoxy-tert-butyl-4-hydroxycyclohexane;

[0050] (2) Preparation of peroxide silane coupling agent

[0051] Take 1 mol of 1,1-diperoxy-tert-butyl-4-hydroxycyclohexane, 2.5 mol of tetramethoxysilane and 0.02 mol of titanium tetrachloride, and add 100 mL of CH 2 Cl 2 Form a reaction system, then control the temperature of the reaction system at 3°C, a...

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Abstract

The invention provides a method for preparing a silane peroxide coupling agent. The preparation method comprises the following steps: mixing 1,1-di-tert-butyl peroxide-4-cyclohexanamide, tetramethoxysilane, titanium tetrachloride and a non-protonic solvent, adding diisopropylcarbondiimide under the temperature condition of 0-5 DEG C, and controlling the reaction temperature to be 25-50 DEG C afterdiisopropylcarbondiimide addition completion, thereby obtaining the silane peroxide coupling agent. The addition process of the diisopropylcarbondiimide is controlled at the temperature of 0-5 DEG C,so that the reaction between an intermediate in a transient state and 1,1-di-tert-butyl peroxide-4-cyclohexanamide can be promoted, the probability that the intermediate in the transient state is rearranged to produce by-products is reduced, and side reactions can be greatly reduced; and therefore, the reaction yield is improved. According to calculation, the yield in the method disclosed by theinvention is 90-96%.

Description

technical field [0001] The invention belongs to the technical field of silane coupling agent preparation, in particular to a preparation method of silane peroxide coupling agent. Background technique [0002] As a "bridge" to improve the interface between inorganic materials and organic materials, coupling agents are used more and more widely. Among them, the silane coupling agent is the one with the largest amount and the most varieties at present. Silane coupling agent is a silicone monomer with two or more different reactive groups in the molecule, which can chemically bond with organic and inorganic materials to increase the adhesion of the two materials. The general structural formula of silane coupling agent is RSiX 3 , where X represents an alkoxy group that can be hydrolyzed, such as halogen, alkoxy, acyloxy, etc., R represents an active functional group that has affinity or reactivity with polymer molecules, such as oxygen, mercapto, vinyl, epoxy group, amido gro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/04
Inventor 潘海刚刘春枝张娟刘超
Owner 山东元禾新材料科技股份有限公司