Method for producing 2-dimethylamino-1, 3-dithiocyano-propane

A dithiocyano- and dimethylamino-based technology, which is applied in the field of synthesizing cartap intermediates, can solve the problems of low powder yield, low crystallization temperature, and long crystallization time of monosultap, and achieve long crystallization time and crystallization The effect of low temperature and easy crystallization

Inactive Publication Date: 2012-01-25
广东立威化工有限公司
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Problems solved by technology

At present, domestic cartap manufacturers all use monosodium dimetap (abbreviation: monosultap) to synthesize cartap, but the powder yield of monosultap produced with sul

Method used

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  • Method for producing 2-dimethylamino-1, 3-dithiocyano-propane

Examples

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[0017] Examples:

[0018] The insecticidal monoammonium salt with a mass percentage content of 98% was prepared with water to form an insecticidal monoammonium salt aqueous solution with a mass concentration of 47.5%, stirred, adjusted to pH=10.25 with sodium hydroxide, and cooled to 10°C. Sodium cyanide is formulated into a sodium cyanide aqueous solution with a mass concentration of 12.5%; in the sodium cyanide aqueous solution, add dichloroethane, stir, and cool to 4°C, drop the insecticidal monoammonium salt aqueous solution, continue to stir and add dropwise Time: 60 minutes; keep at 4°C for 1.5 hours under stirring; let stand at room temperature until the layering stops, and then separate the upper and lower layers, the lower organic layer is dichloroethane and 2-dimethylamino-1,3 -Dithiocyano-propane, the upper inorganic layer is cyanide wastewater, which is subjected to centralized disinfection treatment.

[0019] Among them, the molar ratio of the three monomer feeds of i...

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Abstract

The invention discloses a method for producing 2-dimethylamino-1, 3-dithiocyano-propane by using a monosultap ammonium salt, which is carried out according to the following steps: a, preparing the monosultap ammonium salt into a monosultap ammonium salt aqueous solution with a mass concentration of 40-55%, regulating a PH value to be equal to 6.0-8.0 by using sodium carbonate and sodium hydroxide, and cooling the aqueous solution to 15-25 DEG C; b, preparing sodium cyanide into a sodium cyanide aqueous solution with the mass concentration of 10-15%; c, adding dichloroethane in the sodium cyanide aqueous solution, and cooling to 10-15 DEG C; d, dripping the monosultap ammonium salt aqueous solution in the solution obtained in the step c; e, preserving heat for 1-5 hours at 0-10 DEG C; and f, standing the mixture at a room temperature until delamination, and separating an upper layer from a lower layer to obtain the 2-dimethylamino-1, 3-dithiocyano-propane, wherein the mol ratio of three monomers fed, namely, 98% monosultap ammonium salt, the sodium cyanide and the dichloroethane, is 1: (1-3): (0.2-0.3), and the steps a, c, d and e are all carried out in an agitation condition. The output, the content and the yield of the method are all normal and stable; the average yield reaches 98.54%; the content of the used raw material, namely the monosultap ammonium salt, can be up to 98%; the crystallization is easy; the energy consumption is low during production; and the flour extraction can reach 70%.

Description

technical field [0001] The invention relates to a production method for synthesizing cartap intermediate, in particular to a method for producing 2-dimethylamino-1,3-dithiocyano-propane by utilizing insecticidal monoammonium salt. Background technique [0002] In recent years, the recovery of the cartap market, especially the increase in the demand in the international market, has led to a sharp rise in the price of cartap, and the research on the synthesis of cartap by many research institutions at home and abroad is also gradually heating up. Thiocyanide is an intermediate in the production of synthetic cartap, therefore, more and more researches have been done on the preparation methods of thiocyanide. At present, domestic cartap manufacturers all use monosodium dimetap (abbreviation: monosultap) to synthesize cartap, but the powder yield of monosultap produced with sulfonated liquid dimetap is low (only 60-63%) , the content is low (only 95%), and the crystallization te...

Claims

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Application Information

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IPC IPC(8): C07C331/12
Inventor 董超林
Owner 广东立威化工有限公司
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