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A kind of synthetic method of 4,4'-dithiodimorpholine

A technology of dithiodimorpholine and synthesis method, applied in the direction of organic chemistry, etc., can solve the problems of sulfur monochloride decomposition side reaction, complex morpholine recovery process, difficult to meet the index requirements, etc., to achieve simple post-processing, Strong operability and waste reduction effect

Active Publication Date: 2022-06-03
SHANDONG YANGGU HUATAI CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the commonly used acid-binding agent is morpholine itself or sodium hydroxide. When morpholine is used as an acid-binding agent, there is a problem of a large amount of waste of morpholine. During the reaction of sodium hydroxide and hydrochloric acid, water will be produced, and the existence of water will cause side reactions in the decomposition of sulfur monochloride, so that the final product yield is low, the quality is poor, and it is difficult to meet the index requirements

Method used

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  • A kind of synthetic method of 4,4'-dithiodimorpholine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 45.37g of morpholine, 81.51g of anhydrous trisodium phosphate, 500g of 120# solvent oil were added to a 1L reaction kettle, the temperature was controlled at 20°C, stirring was started, and 31.97g of sulfur monochloride was slowly added dropwise to the system, after about 2h , the dropwise addition of sulfur monochloride was completed, and the temperature was maintained to continue stirring for about 2.5h, and the reaction was completed. Add 200g of water for washing, stir for 15 minutes, suction filter and then dry the filter cake to obtain 53.57g of white needle crystals, the yield is 95.85%, the melting point detected by DSC is 123-127 ° C, and the high performance liquid chromatography analyzer detected The obtained purity was 99.61%.

Embodiment 2

[0025] 58.06g of morpholine, 104.30g of anhydrous trisodium phosphate, 600g of 120# solvent oil were added to a 1L reaction kettle, the temperature was controlled to 30°C, the stirring was started, and 40.91g of sulfur monochloride was slowly added dropwise to the system for about 1.5h After that, the dropwise addition of sulfur monochloride was completed, and the temperature was maintained to continue stirring for about 2 h, and the reaction was completed. Add 300g of water for washing, stir for 15 minutes, suction filtration and then dry the filter cake to obtain 67.82g of white needle-like crystals, the yield is 94.83%, the melting point is 123-127 ° C detected by DSC, and the high performance liquid chromatographic analyzer is detected. The obtained purity was 99.55%.

Embodiment 3

[0027] Add 52.81g morpholine, 94.86g anhydrous trisodium phosphate, 550g n-heptane to the 1L reaction kettle, control the temperature to 40°C, turn on stirring, slowly drop 37.21g sulfur monochloride into the system, after about 2h , the dropwise addition of sulfur monochloride was completed, and the temperature was maintained to continue stirring for about 2.5h, and the reaction was completed. Add 200g of water for washing, stir for 15 minutes, suction filtration and then dry the filter cake to obtain 60.74g of white needle-like crystals, the yield is 93.38%, the melting point detected by DSC is 122-126 ℃, and the high performance liquid chromatography analyzer detected The obtained purity was 99.15%.

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Abstract

The invention discloses a synthesis method of 4,4'-dithiodimorpholine, which uses sulfur monochloride and morpholine as raw materials, anhydrous trisodium phosphate as an acid-binding agent, sulfur monochloride and morpholine The reaction generates 4,4'-dithiodimorpholine and hydrochloric acid, and anhydrous trisodium phosphate can react with the hydrochloric acid generated in the reaction to avoid the reaction between hydrochloric acid and morpholine, thereby making the morpholine lose its reactivity. The method of the present invention can reduce the consumption of raw material morpholine by adding the acid-binding agent anhydrous trisodium phosphate, and save the production cost. In addition, the separation of the product and impurities can be realized by washing after the reaction, the production process is simple, and the operability is strong. , the post-processing is simple, and has industrial application value. The appearance of the obtained product is white needle crystal, the yield is above 90%, and the purity is above 98%, which meets the requirements for use.

Description

technical field [0001] The invention relates to a method for synthesizing a rubber vulcanizing agent 4,4'-dithiodimorpholine (DTDM), in particular to a method for synthesizing 4,4'-dithiodimorpholine with low cost and less morpholine waste. The synthesis method belongs to the technical field of rubber auxiliary synthesis. Background technique [0002] Rubber is currently widely used in our daily life, medical industry, rail transit industry and other industries, and plays an irreplaceable role in people's lives. Natural rubber and synthetic rubber are widely used in the current society and life, and with the continuous development of the economy, the demand for rubber in all walks of life is also increasing. 4,4'-Dithiodimorpholine (DTDM) is an important rubber vulcanization accelerator, which can replace all or part of sulfur to form an effective or semi-effective vulcanization system. 4,4'-Dithiodimorpholine is an important rubber vulcanization accelerator. Its molecule ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/26
CPCC07D295/26
Inventor 王才朋王庆振马松潘琳琳孟祥克冉升亮
Owner SHANDONG YANGGU HUATAI CHEM