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Simplified production technology of bisultap

A production process and a technology for killing insects, which can be used in biocides, plant growth regulators, animal repellents, etc., can solve the problems of difficult acid value control, unfavorable product processing, increased energy consumption and production costs, and achieve significant results. Advances and substantial features, the effect of reduced production costs, shorter reaction times

Inactive Publication Date: 2008-08-13
段儒华
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  • Application Information

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Problems solved by technology

There are following defects in the above-mentioned prior art: 1) it is difficult to ensure the anhydrous condition of the chlorination addition reaction system by adding water to increase the temperature to remove the solvent. Once a trace amount of water enters the addition system, H 2 O+Cl 2 →The reaction of HClO+HCl, and then causes the oxidation of dimethylaminopropene hydrochloride by HClO, and yield is reduced; The HCl that generates simultaneously can be brought into dimethylaminodichloropropane hydrochloride by water again, makes It is difficult to control the acid value below 1%
2) Adding alkali to neutralize at low temperature will increase its energy consumption and production cost
3) The dimehypo product finally obtained can only be an aqueous solution with a content of about 30%, which is not conducive to the processing of subsequent products, and the yield is not high

Method used

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  • Simplified production technology of bisultap
  • Simplified production technology of bisultap

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Embodiment Construction

[0017] Further illustrate the production technique of dimehypo of the present invention with preparation example below. The first step: first dissolve dimethylaminopropene hydrochloride in dichloroethane solvent, if necessary, carry out azeotropic removal of possible water, and pass dry chlorine gas at a temperature of 40°C to generate chlorine Chlorine addition reaction, when the reaction temperature begins to drop, stop the chlorine flow; then distill off 1 / 3 of the solvent in the reactant flow, and then crystallize and filter to obtain a solid with a purity of 98% and an acid value below 0.5%. Dimethylaminodichloropropane hydrochloride. The second step: directly use the high-purity, low-acid value solid dimethylaminodichloropropane hydrochloride and sodium thiosulfate prepared in the previous step to mix and dissolve in methanol solvent at a molar ratio of 1: 2.08, and select NaOH as the Catalyst, carry out sulfonation reaction at 60°C under stirring for 2-3 hours, the res...

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Abstract

A simplified process for preparing the bisultap from dimethylamino acrylate includes such steps as chloridizing addition and direct sulfonating. Its advantages are high output rate, low cost and high purity.

Description

1. Technical field [0001] The invention belongs to agricultural insecticides, in particular to a production process of carbon- and sulfur-containing thiosulfonate organic compounds. 2. Background technology [0002] Dimehypo (N, N-dimethylamino-1,3-sodium dithiosulfonate propane) is a kind of highly efficient, low-toxic biomimetic agricultural insecticide, and prior art is all based on dimethylamine Propylene hydrochloride is used as the starting material, and it is produced by a three-step process of chlorination addition, low-temperature neutralization, and then sulfonation. For example, there is a Chinese invention patent application with the publication number CN1273240A published on November 15, 2000. It dissolves dimethylaminopropene hydrochloride in an organic solvent, and then feeds dry chlorine gas under anhydrous conditions to complete the process. Chlorination addition reaction, add water and heat up to remove all solvents, obtain content between 45-55% (percenta...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C381/02A01N41/04
Inventor 段儒华
Owner 段儒华