Preparation method of organotin catalyst, organotin catalyst and application thereof

A catalyst and organotin technology, applied in the field of organic synthesis, can solve problems such as weak catalytic activity, corrosion, and easy crystallization, and achieve the effects of wide application range, simple production process, and low crystallization point

Inactive Publication Date: 2019-05-07
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

In the case of the same amount of tin added, the catalytic activity of dibutyltin dilaurate is slightly weaker, which cannot meet the requirements for the preparation of fast-curing silicone room temperature vulcanized silicone rubber
And dibutyltin diacetate has acid substance acetic acid to generate in the process of using, has the following disadvantages: (1) the use in neutral or alkaline silicone room temperature vulcanized silicone rubber is limited; (2) the product has a pungent smell; ( 3) Silicone room temperature vulcanized silicone rubber using dibutyltin diacetate has corrosion problems when bonding metal substrates; (4) The product is easy to crystallize when used in winter, which is inconvenient to use, especially in the north

Method used

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  • Preparation method of organotin catalyst, organotin catalyst and application thereof
  • Preparation method of organotin catalyst, organotin catalyst and application thereof
  • Preparation method of organotin catalyst, organotin catalyst and application thereof

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preparation example Construction

[0028] The embodiment of the present invention provides a method for preparing an organotin catalyst, comprising the following steps:

[0029] S1: Under the protection of nitrogen or inert gas, add dibutyltin diacetate and tetraalkoxysilane to the reaction kettle, the molar ratio of dibutyltin diacetate and tetraalkoxysilane is 1:1.5~2;

[0030] S2: Under stirring and heating conditions, carry out reflux reaction;

[0031] S3: Filtration, the obtained clear and transparent liquid is the organotin catalyst.

[0032] Compared with traditional organotin catalysts, the catalytic activity of the organotin catalysts prepared in the examples of the present invention is higher than that of dibutyltin dilaurate, which can meet the requirements of customers for preparing organosilicon room temperature vulcanized silicone rubbers with different curing speeds; Compared with butyl tin, it has no irritating odor, and the product has no irritating and corrosive small molecular substances du...

Embodiment 1

[0048] Reflux reaction: 175.5g of dibutyltin diacetate and 152g of tetramethoxysilane are added in a 500ml four-necked flask with reflux condenser, stirrer, thermometer and nitrogen protection, and the molar ratio is dibutyltin diacetate:tetramethoxysilane= 1:2. Then control the temperature of the heating mantle to raise the temperature of the material at 200° C., and control the stirring speed at 150 r / min. As the reaction continues, reflux is gradually generated, and the maximum material reflux temperature reaches 115°C. As the reflux rate increases, the material reflux temperature gradually decreases and finally stabilizes at 90-95°C, and the reaction is continued for 4 hours.

[0049] Distillation operation: change the reflux device to a collection device, and start to collect by-product ester small molecule substances. With the gradual separation of by-products, the temperature of the material rises gradually, and when the temperature of the material reaches 100°C, stop...

Embodiment 2

[0052] The operation steps of this embodiment are basically the same as those of Example 1, the difference is as follows: no distillation operation is carried out. Finally, 327.3 g of the light yellow, transparent liquid target product without mechanical impurities is obtained, and the tin content is 17.43%.

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Abstract

The invention discloses a preparation method of an organotin catalyst, an organotin catalyst and an application thereof. The preparation method comprises the following steps: S1,under the protection of nitrogen or an inert gas, dibutyltin diacetate and tetraalkoxysilane are added into a reaction kettle, and the molar ratio of dibutyltin diacetate to tetraalkoxysilane is 1:1.5-2; S2: reflux reaction is performed under stirring and heating conditions; S3: filtration is performed to obtain the organotin catalyst. The catalytic activity of the organotin catalyst prepared by the invention is higherthan that of dibutyltin dilaurate, and can meet the requirements of customers for preparing silicone room temperature vulcanization silicone rubber with different curing speeds.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing an organotin catalyst, the organotin catalyst and its application. Background technique [0002] The organotin catalysts often used in condensation-type silicone RTV silicone rubber are mainly dibutyltin dilaurate and dibutyltin diacetate. In the case of the same amount of tin added, the catalytic activity of dibutyltin dilaurate is slightly weaker, which cannot meet the requirements for the preparation of fast-curing silicone room temperature vulcanized silicone rubber. And dibutyltin diacetate has acidic substance acetic acid to generate in the process of using, has the following disadvantages: (1) the use in neutral or alkaline silicone room temperature vulcanized silicone rubber is limited; (2) the product has a pungent smell; ( 3) The organosilicon RTV silicone rubber using dibutyltin diacetate has corrosion problems when bonding metal subst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/12C09J183/04C09J11/04C09J11/06C09J11/08C07F7/22B01J31/12
Inventor 梁成凯李胜杰邹泓李草彭迪肖俊平
Owner 湖北新蓝天新材料股份有限公司
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