Method for continuously preparing 4, 4 '-dithiodimorpholine

By using a dynamic tubular reactor for continuous DTDM production, the problems of long reaction time, low safety, and high cost in DTDM preparation have been solved, achieving efficient and safe DTDM preparation and meeting the needs of green chemical industry.

CN122103064APending Publication Date: 2026-05-29FUJIAN LISHAN HEGUANG ENGINEERING TECHNOLOGY RESEARCH CO LTD
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Patent Information

Application Number
CN202610240334.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-02-28
Publication Date
2026-05-29

AI Technical Summary

Technical Problem

Existing DTDM preparation processes suffer from problems such as large online liquid hold-up, long reaction cycles, high operational risks, serious waste of raw material costs, and poor controllability of product quality, making it difficult to meet the needs of modern green chemical industry and high-quality production.

Method used

Continuous production is carried out using a dynamic tubular reactor. DTDM is generated by reacting a mixture of sulfur monochloride, morpholine, and an acid-binding agent in the dynamic tubular reactor. The product is obtained by settling, washing, filtration, and drying. The reaction conditions are optimized to improve efficiency and safety.

Benefits of technology

It reduces reaction time from several hours to 10 minutes, achieves a product yield of up to 99%, maintains good quality consistency, significantly improves production efficiency and safety, reduces production costs, and is suitable for widespread promotion.

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Abstract

The invention belongs to the technical field of synthesis of rubber additives, and particularly relates to a method for continuously preparing 4, 4 '-dithiodimorpholine. The method comprises the following steps: taking sulfur monochloride, morpholine, 32wt% liquid caustic soda (sodium hydroxide solution) and 120 # solvent oil as raw materials, reacting in a dynamic tubular reactor to generate 4, 4 '-dithiodimorpholine, after the reaction is finished, collecting a material flowing out of the dynamic tubular reactor, and carrying out standing layering, washing, filtering and drying to obtain the 4, 4'-dithiodimorpholine. The dynamic tubular reactor is adopted for reaction, the mass transfer and heat transfer efficiency is extremely high, materials are instantly and uniformly mixed, morpholine and sulfur monochloride are subjected to rapid contact reaction, reaction heat can be instantly removed, the optimal reaction temperature can be accurately maintained, continuous production can be achieved, the production capacity is greatly improved, and the production cost is reduced. And the reaction time of a traditional tank reactor is shortened from 2-7h to 10min, the raw material conversion rate is up to 99% or above, and finally the goals of cost reduction, efficiency improvement, greenness and safety are achieved.
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