Method for preparing tetraethylthiuram disulfide through combined catalysis of metal catalyst and solid alkali

The preparation of tetraethylthiuram disulfide in a continuous flow fixed-bed reactor by co-catalysis of metal catalyst and solid base solves the problems of equipment corrosion and by-product generation in traditional methods, realizes an efficient, simplified, and green synthesis process, and improves product purity and production efficiency.

CN121895205APending Publication Date: 2026-04-21NANJING UNIV
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Patent Information

Application Number
CN202411470043.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-21
Publication Date
2026-04-21

AI Technical Summary

Technical Problem

Traditional methods for producing tetraethylthiuram disulfide suffer from problems such as equipment corrosion, byproduct generation, complex operation, high energy consumption, and difficulty in product purification. Existing green synthesis methods also have difficulties in effectively removing catalysts, leading to complex purification processes and increased costs.

Method used

Tetraethylthiuram disulfide was prepared by a combination of a metal catalyst and a solid base using a continuous flow fixed-bed reactor. The reaction conditions were controlled by a composite catalyst composed of molybdenum disulfide and calcium hydroxide, which avoided the formation of byproducts and simplified the post-processing.

Benefits of technology

It achieves rapid and efficient synthesis without byproduct generation, with high product purity, simplifies purification steps, improves production capacity and product quality, and reduces equipment footprint and operational complexity.

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Abstract

The invention discloses a method for preparing tetraethylthiuram disulfide through combined catalysis of a metal catalyst and solid alkali, and belongs to the technical field of organic synthesis. The method comprises the following steps: filling a continuous flow fixed bed with molybdenum disulfide and calcium hydroxide to form a composite multi-catalyst, preparing a reaction raw material solution from carbon disulfide and diethylamine as raw materials, controlling the flow of the reaction raw material solution and the flow of gas entering a reactor, and carrying out a temperature-controlled and pressure-controlled reaction to obtain a reaction solution; and carrying out post-treatment on the reaction liquid to obtain tetraethylthiuram disulfide. Molybdenum disulfide and calcium hydroxide are adopted to form a composite multi-term catalyst, a heterogeneous catalysis reaction is accurately controlled, the tetraethylthiuram disulfide crystal is obtained only through crystallization, filtration and drying of a prepared crude product, the purity and yield of the obtained tetraethylthiuram disulfide are high, and the method is environmentally friendly, high in atom economy and suitable for industrial production. Conditions are mild, the catalyst can be recycled, and products are easy to separate.
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