Method for preparing tetraalkyl thiuram disulphide by utilizing micro-structured reactor

A microstructure reactor, a technology of tetraalkyl disulfide, applied in the field of N, can solve the problems of cumbersome, by-product tetraalkyl thiuram disulfide steps, difficult to remove heat in time, etc., and achieve continuous safe production and operation. The effect of easy control of conditions and convenient operation

Inactive Publication Date: 2010-06-02
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to aim at the strong exothermic reaction of the prior art, the heat is difficult to remove in time, resulting in local hot spots in the reaction mixture, which is easy to cause the thermodynamically unstable product N,N-dialkyldithiocarbamate Due to the problem of by-products generated by decomposition and the cumbersome steps of conventional batch operation to produce tetraalkylthiuram disulfide, a method for preparing tetraalkylthiuram disulfide using a microstructure reactor was proposed.

Method used

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  • Method for preparing tetraalkyl thiuram disulphide by utilizing micro-structured reactor
  • Method for preparing tetraalkyl thiuram disulphide by utilizing micro-structured reactor
  • Method for preparing tetraalkyl thiuram disulphide by utilizing micro-structured reactor

Examples

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Embodiment 1

[0024]Inject 33% dimethylamine aqueous solution and carbon disulfide into the microstructure reactor D1 with a temperature controlled at 20°C through a high-pressure pump at a molar ratio of carbon disulfide to dimethylamine of 0.5:1, in which the micromixer is a crossover Toe-shaped micro-mixer (HPIMM, IMM, Germany), the channel size (μm) is 25 × 21 × 37, the micro-channel reactor C1 is a stainless steel capillary with an inner diameter of 0.6mm, and the reaction residence time is 1.884min. Use a high-pressure pump to inject 35% hydrogen peroxide into another microstructure reactor D2 with a molar ratio of dimethylamine and hydrogen peroxide of 0.5: 1 to react with N,N-dimethyldithiocarbamate solution, The micro-mixer wherein was V2 (IMM, Germany), the temperature was controlled at -5°C, the microchannel reactor C2 was a stainless steel tube with a length of 2000mm and an inner diameter of 1mm, the temperature was controlled at 20°C, and the residence time was 30s in total. T...

Embodiment 2

[0026] Embodiment 2 is experimented with the method identical with example 1, and the aqueous solution of diethylamine and ethanol solution are respectively with carbon disulfide by the molar ratio of carbon disulfide and diethylamine as 1.1: 1 and inject into temperature control by high-efficiency liquid chromatography pump. In the microstructure reactor D1 at 25°C, the micromixer is a cross-toed micromixer (HPIMM, IMM, Germany), the channel size (μm) is 25×21×37, and the microchannel reactor C1 is the inner diameter 0.6mm stainless steel capillary. The residence time is 1.413min. Then use a high-pressure pump to pump 20% hydrogen peroxide into another microstructure reactor D2 with a molar ratio of diethylamine and hydrogen peroxide of 1.8 to react with N,N-diethyldithiocarbamic acid solution, The micromixer was V2 (IMM, Germany), and the temperature was controlled at 0°C. Microchannel reactor C2 is a stainless steel tube with a length of 2000 mm and an inner diameter of 2...

Embodiment 6

[0027] Embodiment 6 is experimented with the same method as example 2, with 33% diethylamine aqueous solution and carbon disulfide, according to the molar ratio of carbon disulfide and diethylamine is 5: 1 and injects into temperature control at 35 ℃ by high-pressure pump respectively. In the microstructure reactor D1 at ℃, the micromixer is a cross-toed micromixer (HPIMM, IMM, Germany), the channel size (μm) is 25×21×37, and the microchannel reactor C1 has an inner diameter of 0.6mm Stainless steel capillary tube, the residence time of the mixed solution in the microstructure reactor D1 is 2.885min in total. Then with a high-pressure pump, 25% hydrogen peroxide is pumped into another microstructure reactor D2 with a mol ratio of diethylamine and hydrogen peroxide at 1.6 to react with N, N-diethyldithiocarbamic acid solution, wherein The micromixer was V2 (IMM, Germany) and the temperature was controlled at 5°C. The microchannel reactor C2 is a polytetrafluoro tube with a len...

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Abstract

The invention relates to a method for preparing tetraalkyl thiuram disulphide by utilizing a micro-structured reactor, which comprises the following steps: simultaneously injecting solution of raw material secondary amine and carbon disulfide into the micro-structured reactor through pumps for condensation reaction; injecting the obtained solution of N,N-dialkyl dithiocarbamate and oxyful into another micro-structured reactor for oxidation reaction; and re-crystallizing, filtering, washing and drying the reaction product to obtain the product of tetraalkyl thiuram disulphide. In the method, the operating conditions are easy to control; blockage cannot occur in the process; the operation is convenient; the product has good selectivity; and continuous safety production is realized under theconditions of no acid or alkali and no catalyst.

Description

technical field [0001] The invention relates to a preparation method of N, N-dialkyldithiocarbamic acid and tetraalkylthiuram disulfide. In particular, it relates to a method for preparing tetraalkylthiuram disulfide using a microstructure reactor. Background technique [0002] N, N-dialkyldithiocarbamic acid is an intermediate in the synthesis of pesticides and medicines, and is widely used in mineral processing, environmental protection, medicine, agriculture and other industries. Using carbon disulfide and secondary amines as raw materials is a better way to synthesize the product. N, N-dialkyl dithiocarbamic acid reacts with hydrogen peroxide to generate alkyl thiuram rubber vulcanization accelerator. It vulcanizes the rubber under the condition of low sulfur or no sulfur, the vulcanization flatness is very wide, and it can be vulcanized at a higher temperature. With the development of the rubber industry, the demand for thiuram vulcanization accelerators has increase...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/32
Inventor 张利雄姚型军王重庆
Owner NANJING UNIV OF TECH
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