Research and development of ally isothiocyanate
A technology of isothiocyanate and allyl ester, applied in the direction of organic chemistry, can solve problems such as low yield, difficult judgment of reaction end point, and long reaction time
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Embodiment 1
[0012] Add 200g of sodium thiocyanate, 12g of composite catalyst sodium lauryl sulfate and tributyl phosphate and 400g of water into a 1L nitrogen-filled stainless steel reactor equipped with a thermometer and stirring device, stir and heat at 600r / min When the temperature reaches 80-90°C, the reaction pressure is controlled at 0.2-0.4 MPa, and 187 g of allyl chloride is injected into the stainless steel reaction kettle within 2 hours using a metering pump with a flow rate of 90 ml / h. Keep the temperature of the reaction solution at 80-90° C., control the reaction pressure at 0.2-0.4 MPa, and continue the reaction for 0.5 hours. Take a sample to detect that the residue of allyl chloride is less than 0.2%, and cool down. The lower aqueous layer was discarded, leaving the upper organic phase. The upper organic phase was washed with 200 ml×3 brine, and then dried over anhydrous sodium sulfate to remove water. Finally, the organic phase is rectified under reduced pressure, and t...
Embodiment 2
[0014] In a 1L nitrogen-filled stainless steel reactor equipped with a thermometer and stirring device, add 230g of sodium thiocyanate, 14g of composite catalyst sodium lauryl sulfate and tributyl phosphate and 460g of water, stir and heat at 600r / min When the temperature reaches 80-90°C, the reaction pressure is controlled at 0.2-0.4 MPa, and 215 g of allyl chloride is injected into the stainless steel reaction kettle within 2 hours using a metering pump with a flow rate of 90 ml / h. Keep the temperature of the reaction solution at 80-90° C., control the reaction pressure at 0.2-0.4 MPa, and continue the reaction for 0.5 hours. Take a sample to detect that the residue of allyl chloride is less than 0.2%, and cool down. The lower aqueous layer was discarded, leaving the upper organic phase. The upper organic phase was washed with 200 ml×3 brine, and then dried over anhydrous sodium sulfate to remove water. Finally, the organic phase is distilled under reduced pressure, and th...
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Abstract
Description
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Application Information
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