Preparation method of bis-[3-(triethoxy silicon)-propyl]-disulfide

Abstract

The invention discloses a preparation method of bis-[3-(triethoxy silicon)-propyl]-disulfide, relates to the technical field of silane coupling agent synthesis, and in particular relates to a preparation method of bis-[3-(triethoxy silicon)-propyl]-disulfide. The preparation method comprises the following steps: step 1, reacting potassium hydroxide with water to prepare a potassium hydroxide solution; step 2, adding potassium carbonate and powdered sulfur into the potassium hydroxide solution, and reacting to obtain a potassium disulfide solution; step 3, adding a phase transfer catalyst into the potassium disulfide solution, then dropwise adding 3-chloropropyltriethoxysilane, and carrying out a reaction so as to obtain bis-[3-(triethoxy silicon)-propyl]-disulfide; the molar ratio of the potassium hydroxide to the potassium carbonate to the sulfur powder to the 3-chloropropyltriethoxysilane is (1.2-1.5) : (0.3-0.6) :(1.2-1.8) : 1. The method has the positive effects of avoiding the generation of hydrogen sulfide gas, being simple in post-treatment, being green and environment-friendly, and improving economic benefits.

Description

Technical field [0001] The present invention relates to the field of silane coupling agent synthesis, and more particularly to a bis-[3- (triethoxy silicon)-propyl] - disulfide preparation method. Background technique [0002] Double - [3- (triethoxy silicon) - propyl] - disulfide is a commonly used silane coupling agent, which is widely used in various rubber industries. At present, the preparation method of dual-[3- (triethoxysil silicon)-propyl] - disulfide is generally prepared with sodium sulfide, sodium carbonate, sulfur powder, and then the action of phase transfer catalyst The lower reaction with 3-chloropropyltriethoxysilane reacts double-[3- (triethoxy silicon)-propyl]-disulfide, the preparation method due to the presence of sodium hydrogen fluid, during the reaction process Hydrogen sulfide gas will result in not only pollute the atmospheric environment, but also threatened personal safety. It is necessary to absorb by a fresh film absorber, and the equipment cost and ...

AI Technical Summary

Problems solved by technology

At present, the preparation method of bis-[3-(triethoxysilyl)-propyl]-disulfide is generally to prepare sodium disulfide by reacting sodium bisulfide, sodium carbonate, and sulfur powder, and then in the effect of phase transfer catalyst Reaction with 3-chloropropyltriethoxysilane to make two-[3-(triethoxysilane)-propyl]-disulfide, this preparation method is due to the existence of sodium hydrosulfide, in the reaction process It will produce hydrogen sulfide gas, which not only pollutes the atmosphere, but also threatens personal safety

It needs to be absorbed by falling film absorber, which increases equipment cost and land occupation

At the same time, the wastewater produced is mainly sodium salt wastewater containing sodium chloride and sodium carbonate, which increases the difficulty of post-treatment and increases the production cost.