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Dibutyltin dilaurate catalyzes the method for synthesizing methoxyxime ketone silane

A dibutyltin laurate catalyzed synthesis of methoxyxime ketone silane and methoxy ketone silane, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can Solve the problems of low cross-linking activity of cross-linking agents, potential safety hazards, and environmental pollution, and achieve low synthesis costs, ease backlogs, and low prices

Active Publication Date: 2016-09-14
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

The boiling point of the amine compound and the methoxyxime ketone silane complex is relatively close, and it is difficult to separate the amine compound from the methoxy oximone silane complex; the synthetic crosslinking agent crosslinks due to the residue of the amine compound in the reaction product. The linkage activity is low, and the reaction product of amino compound remains and it is easy to turn yellow after long-term storage
[0008] (2) The methoxyxime ketone-based silane compound uses chlorosilane and organochlorosilane as raw materials. The reaction between chlorosilane and organochlorosilane will produce hydrogen chloride gas, which will pollute the environment, and there are certain hidden dangers in safety

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] In the three-necked flask of 1000ml, add 500g tetramethoxysilane, 125g butanone oxime and 0.75g dibutyltin dilaurate, the three-necked flask is equipped with agitator, reflux condenser, gas phase extraction device and thermometer, and the three-necked flask is Raise the temperature and detect the temperature of the gas phase extraction outlet. When the temperature of the gas phase extraction outlet is 72°C, start the gas phase extraction. When the gas phase extraction outlet temperature is 76°C, start total reflux. Keep the gas phase extraction outlet temperature not higher than 76°C and continue to extract Methanol gas, keep the temperature in the three-necked flask at 121°C and stir the reaction for 2 hours to obtain the product to be distilled, and distill the product to be distilled at the temperature of 100°C and the pressure of -0.095Mp to obtain the methoxyxime ketone group Silane complex.

[0036] It has been verified that the obtained methoxyximeketosilane comple...

Embodiment 2

[0039] In the three-necked flask of 1000ml, add 500g tetramethoxysilane, 100g butanone oxime and 0.25g dibutyltin dilaurate, the three-necked flask is equipped with agitator, reflux condenser, gas phase extraction device and thermometer, and the three-necked flask is Raise the temperature and detect the temperature of the gas phase extraction outlet. When the temperature of the gas phase extraction outlet is 70°C, start the gas phase extraction. When the gas phase extraction outlet temperature is 76°C, start total reflux. Keep the gas phase extraction outlet temperature not higher than 76°C and continue to extract Methanol gas, stirred and reacted for 5 hours at a temperature of 125°C in a three-necked flask to obtain the product to be distilled, and distilled the product to be distilled at a temperature of 115°C and a pressure of -0.096Mpa to obtain methoxyxime ketone Silane complex.

[0040] It has been verified that the obtained methoxyximeketosilane complex has a mass of 2...

Embodiment 3

[0043] In the three-necked flask of 1000ml, add 200g tetramethoxysilane, 500g butanone oxime and 1g dibutyltin dilaurate, the three-necked flask is equipped with a stirrer, reflux condenser, gas phase extraction device and thermometer, and the three-necked flask is Raise the temperature and detect the temperature of the gas phase extraction outlet. When the temperature of the gas phase extraction outlet is 75°C, start the gas phase extraction. When the gas phase extraction outlet temperature is 76°C, start total reflux. Keep the gas phase extraction outlet temperature not higher than 76°C and continue to extract Methanol gas, stirred and reacted for 7 hours at a temperature of 129°C in a three-necked flask to obtain the product to be distilled, and distilled the product to be distilled at a temperature of 120°C and a pressure of -0.098Mpa to obtain methoxyxime ketone Silane complex.

[0044] It has been verified that the obtained methoxyximeketosilane complex has a mass of 260...

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Abstract

The invention discloses a method for synthesizing methoxyssilane under catalysis of dibutyltin dilaurate, and relates to the cross-linking field. The method comprises the following steps of adding 1 part of tetramethoxysilane, 0.2-2.5 parts of diacetylmonoxime and 0.0005-0.005 part of dibutyltin dilaurate in parts by weight to a reaction kettle with a gaseous-phase extraction device, stirring for reacting for 3-7 hours under the condition that the temperature in the reaction kettle is in the range from 121 DEG C to 129 DEG C and then obtaining a product to be distilled, distilling the product to be distilled under the conditions of a temperature ranging from 100 DEG C to 120 DEG C and pressure ranging from -0.095 MPa to -0.098MPa, and then obtaining a methoxyssilane compound. According to the method, the dibutyltin dilaurate can be taken as a catalyst for molding silicone rubber by vulcanizing at the room temperature, and also can be left in the reaction products after the reaction is completed, and the reaction steps are quite simple; the tetramethoxysilane is taken as the raw material of the method so that the synthesis cost of the method is quite low.

Description

technical field [0001] The invention relates to the field of crosslinking agents, in particular to a method for catalyzing the synthesis of methoxyximeketosilane by dibutyltin dilaurate. Background technique [0002] Existing room temperature vulcanized silicone rubber usually uses methyl tributylketoxime silane, tetrabutyl ketoxime silane, methyl trimethoxysilane and oxime ketone methoxy silane compound as cross-linked silicone rubber in the curing molding process. Linking agent to realize the curing and molding of room temperature vulcanized silicone rubber. [0003] When methyl tributylketoxime silane is used as a crosslinking agent, the curing speed of room temperature vulcanized silicone rubber is relatively slow; when tetrabutylketoxime silane is used as a crosslinking agent, due to the high freezing point (about 40°C), tetrabutylketoxime silane is easy to crystallize when used, which makes it difficult to control the curing and molding speed of room temperature vulca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C07F7/10C08K5/5465C08K5/57
Inventor 梁成凯王成申勇刘潘高建秋黄苏雨冯琼华肖俊平
Owner 湖北新蓝天新材料股份有限公司
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