3-Mercaptopropylmethyldimethoxysilane synthesis

Yield:31001-77-1 94.8%

Reaction Conditions:

with sodium sulfide;tetrabutyl-ammonium chloride;N-benzyl-N,N,N-triethylammonium chloride;water;Aliquat 336 in Petroleum ether at 75 - 80; for 4 h;Large scale;

Steps:

3 Example 3
This embodiment includes the following steps:To a 1000 ml three-necked flask equipped with heating, stirring, cooling reflux and temperature measuring devices, add 130 g of water and 91.2 g of 70% sodium sulfide (0.84 mol), and start stirring. After all the solids are dissolved, add 2.5 g in turn. g composite catalyst consisting of benzyltriethylammonium chloride and 2.5g of trioctylmethylammonium chloride and tetrabutylammonium chloride, 380g of petroleum ether, 27.8g (0.7mol) of chloropropylmethyldimethoxy Silane, heated to 75 80 , and kept warm for 4 hours,Stop the stirring after the reaction and let it stand for 2 minutes. The organic layer was sampled and tracked by gas chromatography. The residual amount of chloropropylmethyldimethoxysilane was 0.45%. The aqueous phase was separated. The organic layer was evaporated under normal pressure to remove toluene. Distillation was performed under reduced pressure, and a fraction of 95-98 ° C. (absolute pressure 4 kPa) was collected to obtain 1119.9 g of a product. In this example, the content of the prepared mercaptosilane coupling agent was 99.1%, and the yield was 94.8%.

References:

Hunan Zhengliang Engineering Co., Ltd.;Yue Yanjun;Tang Youming;Hua Wei;Zhao Wairong;Long Danwanzi;Zhou Deguo;Hu Qingliang CN110483566, 2019, A Location in patent:Paragraph 0028-0030

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