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A kind of preparation method of improved allyl thiocarbamate
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A technology of allyl thiocarbamate and allyl ester, which is applied in the field of preparation of allyl thiocarbamate, can solve the problems of complex post-processing, low product purity, and high energy consumption, and achieve Improve product purity, reduce by-products, and improve the effect of purity
Active Publication Date: 2017-03-29
SHENYANG RES INST OF NONFERROUS METALS
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[0010] The purpose of the present invention is to solve the problems of low purity of the product prepared in the prior art, the need for decompression purification, high energy consumption, complex post-processing, and many impurities. After repeated research and a large number of test screenings, a kind of Halopropene and thiocyanate are used as raw materials, water is used as solvent, no phase transfer catalyst is used to prepare allyl isothiocyanate intermediate, and allyl isothiocyanate with high purity is directly prepared by reacting with fatty alcohol in a certain proportion Thiocarbamate product, the product does not need to be purified by vacuum distillation
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Embodiment 1
[0030] Add 40 grams of sodium thiocyanate to the reactor, add 55 ml of water, mix and stir for 20 minutes, add hydrochloric acid to adjust the pH value of the system to 4, then add 41 grams of allyl chloride, stir and gradually increase the temperature, and react at 90 to 100 ° C for 2 hours. After the reaction was finished, static separation was performed to remove the water phase, and the organic phase was distilled to remove residual chloropropene to obtain 45 grams of intermediates. Then add 40 grams of isobutanol to the intermediate, add 0.2 grams of tetrabutyl titanate, react for 3 hours at a temperature between 90 and 100 ° C, and cool to directly obtain N-allyl-O isobutylthioamino Formate product 85 grams, gas chromatography analysis purity reaches 96.3%.
Embodiment 2
[0032] Add 40 grams of ammonium thiocyanate to the reactor, add 55 ml of water, mix and stir for 20 minutes, add sulfuric acid to adjust the pH value of the system to 6, then add 42 grams of allyl chloride, stir and gradually increase the temperature, and react at 90 to 100 ° C for 2 hours. After the reaction is finished, separate statically, remove the water phase, and distill the organic phase under reduced pressure to remove residual chloropropene to obtain 45 grams of intermediate, add 40 grams of isopropanol, add 0.2 grams of tetrabutyl titanate, React for 3 hours, cool, and directly obtain 85 grams of N-allyl-O-isobutylthiocarbamate product, and the gas chromatograph analysis purity reaches 96%.
Embodiment 3
[0034] Add 48 grams of potassium thiocyanate to the reactor, add 68 ml of water, mix and stir for 20 minutes, add nitric acid to adjust the pH value of the system to 5, then add 42 grams of allyl chloride, stir and gradually increase the temperature, and react at 90 to 100 ° C for 3 hours. After the reaction was finished, static separation was performed to remove the water phase, and the organic phase was distilled to remove residual chloropropene to obtain 45.2 grams of intermediates. Add 33 grams of isopropanol and 0.3 grams of tetrabutyl titanate, react at a temperature between 90 and 100°C for 3 hours, cool down, and directly obtain N-allyl-O-isopropylthiocarbamate product 78 grams, the gas chromatograph analysis purity reached 94%.
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Abstract
The invention relates to an improved preparation method of allyl thiocarbamate, which is characterized in that halopropenes and thiocyanate are used for synthesizing an allyl isothiocyanate intermediate without a phase-transfer catalyst, the intermediate is prepared by the method that a pH state of a thiocyanate aqueous solution is changed, the preparation method comprises the following steps: a)adjusting pH state of a thiocyanate aqueous solution, adding halopropenes for a reaction, preparing the allyl isothiocyanate intermediate; and b)reacting the allyl isothiocyanate intermediate and fatty alcohol, adding tetrabutyl titanate to prepare the allyl thiocarbamate products. During the preparation of the allyl isothiocyanate intermediate, the phase-transfer catalyst is not employed, no pollution is generated in the whole reaction, the final product has the advantages of high product yield and little impurity, and steps of underpressure distillation, and alcohol removal and extraction are not required, and the allyl thiocarbamate with high purity can be obtained, production cost is low, energy consumption is low, and the method has strong market competitiveness.
Description
technical field [0001] The invention relates to a preparation method of allyl thiocarbamate as a sulfide ore collector, in particular to an improved preparation method of allyl thiocarbamate. The present invention is an improvement to the preparation method of allyl thiocarbamate prepared from allyl isothiocyanate intermediate synthesized by allyl halide and thiocyanate, and can be prepared in aqueous solution without using phase transfer catalyst Allyl isothiocyanate reacts with fatty alcohol to obtain allyl thiocarbamate product with higher purity, and the product does not need decompression purification treatment, which belongs to the technical field of mineral dressing agents. Background technique [0002] Allyl thiocarbamate is a polar nonionic chelating collector. It has the advantage of strong collection force under high selectivity. [0003] Allyl thiocarbamate is mainly used in the flotation of polymetallic sulfide ores. It has strong collection ability for copper...
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