The synthetic method of two 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) passing the organic solution of di-n-butylamine and the organic solution of sulfur monochloride into the reaction channel respectively The reaction is mixed and initiated in the first reactor, and a reaction mixture is obtained after a partial reaction occurs through the reaction channel of the first reactor; (2) The reaction mixture is continuously passed into the second reactor containing the reaction channel, and Sodium hydroxide solution is passed into the second reactor, and bis-di-n-butylamine disulfide is obtained after sufficient reaction. The continuous synthesis method of the present invention improves the yield of bis-di-n-butylamine disulfide, reduces the generation of by-products, reduces the feeding amount of sulfur monochloride and sodium hydroxide, and can greatly slow down the exothermic speed of reaction. It has the advantages of simple process, high production efficiency, low cost and high safety.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical products, and relates to a synthesis method of an important intermediate of carbosulfan, in particular to a continuous synthesis method of bis-di-n-butylamine disulfide. Background technique [0002] Bis-di-n-butylamine disulfide is an important intermediate of carbofuran’s sulfur-containing derivative carbosulfan. At present, the industry mainly uses di-n-butylamine and sulfur monochloride 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 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 mo...

AI Technical Summary

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