Water-phase synthesis method for di-[(triethoxylsilicon)propyl]-bisulfide

Abstract

The invention provides a method for the aqueous synthesis of bis-[(tirethoxy silicon)propyl]-bisulfides, relating to a method of synthesizing bis-[(tirethoxy silicon)propyl]-bisulfides. The invention resolves the problems that because the production of sodium disulphide needed for the preparation of Si-75 is conducted in a nitrogen protection and ethanol system, the operating requirement is high and manufacturing costs are increased. The steps of the method are as follows: the elemental sulfur and alkali metal hydrosulfides or alkali metal sulphides are dissolved in the aqueous phase, and the Ph value is adjusted, and after the phase transfer catalyst and the hydrolysis inhibitor are added to solution, the chloropropyl triethoxy silane is dropwise added to the solution, and the upper layer organic phase is isolated after the backflow, cooling and filtering, and the active carbons are used for the adsorption after processes of washing, separation and deposition, combination and drying of the organic phase. In the invention, the preparation of Si-75 is completed in the aqueous phase, and the ethanol used as a solvent is unnecessary and the nitrogen protection is also unnecessary, thereby the method of the invention has the advantages of simple reaction condition, easy collection of materials, low manufacturing costs and suitable mass production.

Description

technical field [0001] The invention relates to a method for synthesizing disulfides. Background technique [0002] Bis-[(triethoxysilyl)propyl]-disulfide (Si-75) is a sulfur-containing silane coupling agent with high application value and commercial value, especially in SiO 2 In vulcanized tire rubber as a reinforcing agent, Si-75 is an essential additive. There are many kinds of traditional Si-75 synthesis routes, but most of the methods include a basic reaction, that is, the reaction of sodium disulfide and chloropropyl triethoxysilane in ethanol solvent, the reaction formula is as follows: [0003] 2ClCH 2 CH 2 CH 2 Si(OCH 2 CH 3 ) 3 +NaS 2 → [0004] [(OCH 2 CH 3 ) 3 SiCH 2 CH 2 CH 2 ] 2 S 2 +2NaCl [0005] The synthetic method of the required sodium disulfide of this reaction mainly contains following four kinds: [0006] 1. Add metallic sodium to absolute ethanol to obtain sodium ethylate, then pass hydrogen sulfide gas into the sodium ethylate solu...

AI Technical Summary

Problems solved by technology

[0015] The purpose of the present invention is to solve the problem that the production of sodium disulfide required for the preparation of Si-75 is carried out in a nitrogen protection and ethanol system, resulting in high operational precision requirements and increased production costs, and provides a water-phase synthetic bis-[ (Triethoxysilyl)propyl]-disulfide method