Process for preparing gamma-mercaptopropyl-trimethyloxysilane
A technology of mercaptopropyltrimethoxysilane and chloropropyltrimethoxysilane, which is applied in the field of synthesis of fine chemicals, can solve the problems of low yield and complicated operation, and achieve high yield, good purity and low product cost. low effect
Inactive Publication Date: 2003-03-12
湖北武大有机硅新材料股份有限公司
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Problems solved by technology
If adopting the preparation method of analogue γ-mercaptopropyltriethoxysilane to synthesize γ-mercaptopropyltrimethoxysilane, its yield is low, only about 55%, content>90%, complex operation, and preparation process It needs to be filtered three times and washed with a large amount of methanol
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Embodiment
[0011] Example: Dry thiourea and potassium iodide at 100-105°C for 4 hours, add 60g of γ-chloropropyltrimethoxysilane, 28g of dried thiourea, 32g of methanol, and 0.7 g, heat and stir, reflux at 69-73°C for 24 hours, cool down to 60°C, add 10g of ethylene glycol dropwise, stir at 70-73°C for 0.5 hours, change to a distillation device, distill off the solvent methanol, and then depressurize to 4132~4266Pa (31~32mmHg), the product collected at 140~150°C is γ-mercaptopropyltrimethoxysilane, the yield is 78%, and the product content is ≥98%.
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A process for preapring gamma-mercaptopropyl trimethoxysilane includes reflux reaction of the raw material (gamma-chloropropyl trimethoxysilane and thiourea), solvent (absolute alcohol) and promoter (potassium iodide) and alkalifying by ethanediamine. Its advantages are simple process, high yield (78%), high purity (more than 98%), low cost and no pollution.
Description
technical field [0001] The invention relates to a preparation method of γ-mercaptopropyltrimethoxysilane, which belongs to the synthesis of fine chemicals. Background technique [0002] γ-mercaptopropyltrimethoxysilane is an important silane coupling agent, which is widely used in epoxy resin, polyurethane, polyester, styrene-butadiene rubber and natural rubber to improve the performance of these composite materials; it can also be used in Prepare mercapto-based modified silicone oil, improve the cohesiveness of vulcanized rubber at room temperature, and can also be used as a perm agent, fabric finishing agent and prepare metal surface protective agent. [0003] The synthesis method of γ-mercaptopropyltrimethoxysilane has not been reported. If adopting the preparation method of analogue γ-mercaptopropyltriethoxysilane to synthesize γ-mercaptopropyltrimethoxysilane, its yield is low, only about 55%, content>90%, complex operation, and preparation process The medium needs...
Claims
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Inventor 张治民廖俊陈圣云朱文喜张彦谦
Owner 湖北武大有机硅新材料股份有限公司