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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

Inactive Publication Date: 2015-11-04
徐州诺特化工有限公司
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

[0005] Many reports believe that the reaction between allyl chloride and sodium thiocyanate heterogeneous system, the reaction time is long, the yield is low, and the end point of the reaction is difficult to judge, the reason is mainly due to the result of the heterogeneous system of this reaction.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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

A purpose of the present invention is to provide a synthesis method of ally isothiocyanate. According to the method, novel compound catalysts such as sodium lauryl sulfate and tributyl phosphate are used to catalyze, water is adopted as a solvent, sodium sulfocyanate and allyl chloride are adopted as raw materials, a molar ratio of the sodium sulfocyanate to the allyl chloride is 1.02:1-1.04:1, the allyl chloride is pumped into a nitrogen protected stainless steel reaction kettle by using a metering pump to carry out a heterogeneous reaction, washing is performed 3 time with 10% edible salt water, the organic phase is dried with anhydrous sodium sulfate, suction filtration is performed, the filtrate is subjected to pressure reducing distillation, and the product is collected, wherein the obtained ally isothiocyanate is the colorless and transparent liquid, the product yield (calculated as the allyl chloride) achieves more than or equal to 97%, the product achieves more than or equal to 99.5%, and the moisture content is less than 0.1%.

Description

technical field [0001] The invention belongs to the technical field of biology and new medicine, and relates to a synthesis method of allyl isothiocyanate. Background technique [0002] Allyl isothiocyanate has a very important position in China and even the world because of its medical efficacy, anticancer effect, antiseptic, antibacterial and soil disinfection effects. Allyl isothiocyanate is usually obtained from mustard oil or horseradish by natural extraction, but this method consumes a lot of energy, has low yield and high cost, and is difficult to form a large-scale production. In recent years, the artificial synthesis process of allyl isothiocyanate has been developed in China, that is, the liquid-solid heterogeneous reaction of thiocyanate and allyl halide is used to directly synthesize the target product through atmospheric distillation purification; this method The raw materials are easy to obtain and the process is simple, but the reaction time is long, the yiel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C331/22
Inventor 师静静张龙王玉成杨凯王友志梁涛戚进修戴安琪崔磊
Owner 徐州诺特化工有限公司
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