Method for preparing mercaptoalkyl alkoxy silane
A technology of mercaptoalkylalkoxysilane and chloroalkylalkoxysilane, which is applied in the field of preparation of mercaptoalkylalkoxysilane, can solve the problems of cumbersome operation, easy mixing of products, and difficulty in removal, and achieve the goal of supply Sufficient, cheap, convenient source effect
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Embodiment 1
[0028] Weigh 54.5g of sodium methoxide with a content of 99%, put it into a 500mL autoclave with stirring, pass cooling water, cool down, and start stirring. Adjust the stirring speed to 100 rpm, slowly feed 37.4 g of hydrogen sulfide with a purity of 99%, keep the temperature in the kettle at 40°C, and the pressure at 0.4Mpa.
[0029] 200g of chloropropyltrimethoxysilane was added dropwise into the small autoclave, and the dropwise addition took 0.5 hours. During the whole dropping process, the temperature was controlled at 60°C and the pressure was 0.6Mpa. After the dropwise addition, the temperature was raised to 100° C., and the reaction was completed after 4 hours of heat preservation.
[0030] Cool down, absorb excess hydrogen sulfide with sodium methoxide, filter, and collect the filtrate for distillation. The condenser is made of low-temperature freezing liquid as cooling medium (the temperature of the freezing liquid is 0° C.), and vacuum distillation collects 191 g ...
Embodiment 2
[0032] Weigh 109g of sodium methoxide with a content of 99%, put it into a stirred 1000mL autoclave, pass cooling water, cool down, and start stirring. Adjust the stirring speed to 100 rpm, slowly feed 74.8g of hydrogen sulfide with a purity of 99%, keep the temperature in the kettle at 50°C, and the pressure at 0.6Mpa.
[0033] 367g of chloropropylmethyldimethoxysilane with a content of 99% was added dropwise into the small autoclave. The dropwise addition took 1.5 hours. The temperature during the entire dropping process was controlled at 60°C and the pressure was 0.3Mpa. After the dropwise addition, the temperature was raised to 90° C., and the reaction was completed after 6 hours of heat preservation.
[0034] Cool down, absorb excess hydrogen sulfide with sodium methoxide, filter, and collect the filtrate for distillation. The condenser uses low-temperature freezing liquid as the cooling medium (the temperature of the freezing liquid is 0°C), the filtrate is distilled un...
Embodiment 3
[0036] Claim 275Kg content and be 99% sodium ethylate, put into the 2000L autoclave with stirring, feed cooling water, cool down, start stirring, adjust stirring speed to be 300 revs / min, slowly feed into 155Kg of hydrogen sulfide with a purity of 99%, keep The temperature in the kettle is 50°C, and the pressure is 0.5Mpa. After passing the hydrogen sulfide, stir, keep warm and keep the pressure for 3 hours.
[0037]965Kg of chloropropyltriethoxysilane with a content of 99% was added dropwise into the autoclave, and the dropwise addition took 4 hours. The temperature during the entire dropping process was controlled at 60°C and the pressure was 0.8Mpa. After the dropwise addition, the temperature was raised to 85° C., and the reaction was completed after 6 hours of heat preservation.
[0038] Cool down, absorb excess hydrogen sulfide with sodium ethoxide, filter, and collect the filtrate for distillation. The condenser is used as the cooling medium by the refrigerated liquid ...
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