Synthesis method of bis(di-n-butylamine) disulfide

Abstract

The invention discloses a synthesis method of bis(di-n-butylamine) disulfide. The synthesis method comprises the following steps: (1) respectively introducing an organic solution of di-n-butylamine and an organic solution of sulfur monochloride into a first reactor containing a reaction channel, mixing to initiate a reaction, and carrying out a partial reaction in the reaction channel of the firstreactor to obtain a reaction mixed solution; and (2) continuously introducing the reaction mixed solution into a second reactor containing a reaction channel, introducing a sodium hydroxide solutioninto the second reactor, and fully reacting to obtain bis(di-n-butylamine) disulfide. The continuous synthesis method improves the yield of bis(di-n-butylamine) disulfide, reduces the generation of byproducts, reduces the feeding amount of sulfur monochloride and sodium hydroxide, can greatly slow down the reaction heat release speed, and has the advantages of simple process flow, high productionefficiency, low cost, high safety and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical products, and relates to a method for synthesizing an important intermediate of carbosulfan butylsulfide, in particular to a method for continuous synthesis of bis-n-butylamine disulfide. Background technique [0002] Di-n-butylamine disulfide is an important intermediate of carbosulfur-containing sulfur-containing derivative carbosulfan. At present, di-n-butylamine and sulfur monochloride are mainly used in industry to carry out the process under the action of acid binding agent sodium hydroxide. Low temperature batch preparation. However, this commonly used synthesis method has the following defects: (1) The reaction is violently exothermic, and the reaction is usually performed at a lower temperature (<10 °C) in industry, and the process safety is ensured by controlling the temperature of the cooling medium and the dropping rate; ( 2) There are many by-products. There a...

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Problems solved by technology

However, this commonly used synthesis method has the following defects: (1) The reaction is exothermic violently, and the industry usually reacts at a lower temperature (<10°C), and the process safety is ensured by controlling the temperature of the cooling medium and the rate of addition; ( 2) There are many by-products, there are organic phase and water phase in the reaction solution, sulfur monochloride will be partially decomposed when it meets water, and by-products such as sulfur, sulfur dioxide (sulfurous acid), and hydrogen sulfide will be generated; (3) Based on making dinormal In consideration of the complete conversion of butylamine, an excess of 5% to 6% of sulfur monochloride is used in industry, and an excess of 10% to 30% of acid is applied, which is very costly