Preparation process of ultralow-viscosity dimethyl silicone oil
A technology of dimethyl silicone oil and preparation process, which is applied in the field of preparation technology of ultra-low viscosity dimethyl silicone oil, can solve the problems of long process flow, increased equipment investment and the like, achieves high purity, low ring content, and improves one-time yield. rate effect
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Embodiment 1
[0023] Treat hexamethyldisiloxane and dimethylcyclosiloxane with molecular sieves in advance, and add the treated hexamethyldisiloxane and dimethylcyclosiloxane to 1000ml of In the flask, start to heat up, and at the same time pass dry nitrogen into the flask, pull out water for half an hour, heat up to 80°C, add dry 602 resin, react at 80°C for 8h, the viscosity does not change, cool down to room temperature, filter, and The filtrate is transferred to a flask with a rectification tower for rectification, and the lower fraction at 91°C / -90KPa is cut off, which is octamethyltrisiloxane, with a yield of 8%, and its purity is 99.8% by analysis; cut off at 127°C / -90KPa lower fraction, the yield reaches 9%, and its purity is 99.1% by analysis; the lower fraction of 158°C / 90KPa is intercepted, the yield is 9%, and its purity is 98.5% by analysis; then it is rectified at 163 / -90KPa to No liquid flows out, gets still liquid, and yield is 63%, and its viscosity of analysis is 5.1mm 2...
Embodiment 2
[0025] Use a pump to transport hexamethyldisiloxane and octamethylcyclotetrasiloxane from their respective storage tanks to the molecular sieve adsorbent cartridge, pass through the adsorbent cartridge and pour into the 8000L enamel reaction kettle, hexamethyldisiloxane and The mass ratio of octamethylcyclotetrasiloxane is controlled at 35:65, and the total feeding amount is 5000L. The reaction kettle is heated by low-pressure steam, and nitrogen is introduced into the kettle through the bottom insertion tank, and the water is pulled out for 45 minutes, and the temperature rises. To 70°C, add the pre-dried catalyst, balance the reaction at 70°C for 10 hours, the viscosity will not change, transfer the material to the filter and filter, then transfer to the rectification tower kettle, turn on the vacuum system, set the rectification parameters, intercept The lower fraction at 91°C / -90KPa is octamethyltrisiloxane, with a yield of 8%, and its purity is 99.5%; the lower fraction at...
Embodiment 3
[0027] Use a pump to transport hexamethyldisiloxane and octamethylcyclotetrasiloxane from their respective storage tanks to the molecular sieve adsorbent cartridge, pass through the adsorbent cartridge and pour into the 8000L enamel reaction kettle, hexamethyldisiloxane and The mass ratio of octamethylcyclotetrasiloxane is controlled at 20:80, the total feeding amount is 5000L, the reactor is heated by low-pressure steam, and nitrogen gas is introduced into the kettle through the bottom insertion tank, and the water is pulled out for 45 minutes. Raise the temperature to 60°C, add the pre-dried catalyst, and react at 60°C for 13 hours. The viscosity will not change. Transfer the material to the filter and then transfer it to the rectification tower kettle. Turn on the vacuum system and set the rectification parameters. Cut off the lower fraction at 91°C / -90KPa, which is octamethyltrisiloxane, with a yield of 6%, and analyze its purity to 99.5%; cut off the lower fraction at 127°...
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