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Polymeric acid cross-linking agent, preparation method and sealant with cross-linking agent

A cross-linking agent and sealant technology, applied in the direction of adhesive additives, polymer adhesive additives, non-polymer adhesive additives, etc., can solve the problems of increasing cross-linking density, crystallization, bubbles, etc., and achieve reaction The effect of mild conditions and easy separation

Active Publication Date: 2017-06-13
湖北新蓝天新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Triacetoxysilane is mainly used as a crosslinking agent for deacetate-type room temperature vulcanizing silicone sealant (RTV-1). Now the commonly used acetoxysilane crosslinking agent is mainly methyltriacetoxysilane, and methyl The crystallization point of triacetoxysilane is 40°C. When the temperature is lower than 40°C, methyltriacetoxysilane will crystallize, which is difficult to use normally, and will lead to the use of methyltriacetoxysilane RTV produced as a crosslinking agent also crystallizes at low temperatures, which affects the use of RTV
[0005] a. Adding tetramethoxysilane and curing agent dibutyltin dilaurate to methyltriacetoxysilane, although this method can reduce the crystallization point of methyltriacetoxysilane, but due to the introduction of tetrafunctional Links will increase the cross-linking density, which will greatly reduce the elongation and adhesion of the produced RTV-1
[0006] b. Add the mixture of methyltriacetoxysilane and alkyltriacetoxysilane to RTV. This method can make RTV not crystallize when the temperature is higher than -10°C. However, when the temperature is lower than -10°C crystallization still occurs
[0007] c. Replacing methyltriacetoxysilane with methylalkoxyacetoxysilane, although it can lower the crystallization point, it will introduce alcohols, which will release alcohols during use. If they cannot be removed in time, it will cause glue The phenomenon of air bubbles in the interior affects the sealing performance

Method used

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  • Polymeric acid cross-linking agent, preparation method and sealant with cross-linking agent
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  • Polymeric acid cross-linking agent, preparation method and sealant with cross-linking agent

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preparation example Construction

[0026] The embodiment of the present invention provides a kind of preparation method of polyacidic crosslinking agent, comprises the following steps:

[0027] In parts by mass, add 100 parts of alkyl triacetoxy and 1 to 5 parts of aluminum acetate into the reaction kettle and mix evenly, heat up to 70-90°C and react for 8-10 hours. The acetic anhydride generated by the reaction is removed under the conditions of a pressure of -0.098MPA and a temperature of 90°C to obtain a polymerized alkyltriacetoxysilane.

[0028] The alkyltriacetoxysilane in the embodiment of the present invention is methyltriacetoxysilane, ethyltriacetoxysilane, propyltriacetoxysilane or vinyltriacetoxysilane.

[0029] Due to the high hydrolysis activity of alkyltriacetoxysilane, direct water hydrolysis is easy to cause local polycondensation into high polymers, so it is necessary to add a large amount of acetic acid to dilute. The boiling point of alkyltriacetoxysilane is close to that of alkyl triacetox...

Embodiment 1

[0039] Add 440 grams of methyltriacetoxysilane and 4.4 grams of aluminum acetate into a three-necked flask with a capacity of 1 L, mix well and react at a temperature of 90°C for 8 hours, filter out the aluminum acetate, and use negative pressure to remove acetic anhydride to obtain Polymerized alkyltriacetoxysilane (hereinafter referred to as product 1).

[0040] After chromatographic analysis, the contents of each component in Product 1 are: 0.5% acetic acid, 1.5% acetic anhydride, 15.9% methyltriacetoxysilane, 60.4% methyltriacetoxysilane dimer, methyltriacetoxysilane Silane trimer 19.3%.

Embodiment 2

[0042] Add 440 grams of ethyltriacetoxysilane and 22 grams of aluminum acetate into a three-necked flask with a capacity of 1 L, mix well and react at a temperature of 70°C for 10 hours, then filter to remove aluminum acetate, and use negative pressure to remove acetic acid anhydride to obtain polymerized alkyltriacetoxysilane (hereinafter referred to as product 2).

[0043] After chromatographic analysis, it can be known that the content of each component in product 2 is: 0.6% of acetic acid, 1.8% of acetic anhydride, 14.3% of ethyl triacetoxysilane, 61.4% of ethyl triacetoxysilane dimer, ethyl triacetyl Oxysilane trimer 18.6%.

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Abstract

The invention discloses a polymeric acid cross-linking agent, a preparation method and a sealant with the cross-linking agent, and relates to the field of cross-linking agents. The preparation method comprises the following steps: uniformly mixing 100 parts of an alkyl triacetyl oxo group and 1-5 parts of aluminum acetate in a reaction kettle, heating to 70-90 DEG C to react for 8-10 hours, filtering off the aluminum acetate, and removing acetic anhydride generated in the reaction from filtrate, thereby obtaining polymeric alkyl triorganoacetoxysilane, wherein the polymeric acid cross-linking agent comprises the following components in percentage by mass: 14-17.3% of an alkyl triorganoacetoxysilane monomer, 60-61.5% of alkyl triorganoacetoxysilane dimer, 16.3-19.3% of alkyl triorganoacetoxysilane trimer and the balance of impurities. A cross-linking agent of which the RTV (Room Temperature Vulcanized Silicone Rubber) crystallization point is remarkably reduced can be prepared, and in addition, the cross-linking agent is relatively gentle when being used and can form complete RTV.

Description

technical field [0001] The invention relates to the field of crosslinking agents, in particular to a polyacidic crosslinking agent, a preparation method and a sealant with the crosslinking agent. Background technique [0002] Triacetoxysilane is mainly used as a crosslinking agent for deacetate-type room temperature vulcanizing silicone sealant (RTV-1). Now the commonly used acetoxysilane crosslinking agent is mainly methyltriacetoxysilane, and methyl The crystallization point of triacetoxysilane is 40°C. When the temperature is lower than 40°C, methyltriacetoxysilane will crystallize, which is difficult to use normally, and will lead to the use of methyltriacetoxysilane The RTV produced as a cross-linking agent also crystallizes when the temperature is low, which affects the use of RTV. [0003] Since the use environment of RTV is normal temperature or lower temperature, when the crosslinking agent crystallizes, the sealing performance of RTV is poor, and the sealing effec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/14C08G77/06C08G77/08C09J183/06C09J183/04C09J11/04C09J11/06C09J11/08
CPCC08G77/06C08G77/08C08G77/14C08L2205/02C08L2205/025C08L2205/03C09J11/04C09J11/06C09J11/08C09J183/04C09J183/06C08L83/04C08L83/06C08K3/36C08K5/57
Inventor 高建秋梁成凯肖俊平邹泓
Owner 湖北新蓝天新材料股份有限公司
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