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Method for synthesizing 4,4'-dithiodimorpholine

A technology of dithiodimorpholine and a synthesis method, which is applied in the direction of organic chemistry and the like, can solve the problems of the decomposition of sulfur monochloride, the side reaction of sulfur monochloride, the complex recovery process of morpholine, and it is difficult to meet the requirements of indicators, so as to reduce the difficulty of post-processing. , Post-processing is easy to implement, and the effect of reducing material consumption

Active Publication Date: 2019-10-15
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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  • Method for synthesizing 4,4'-dithiodimorpholine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 45.37g of morpholine, 81.51g of anhydrous trisodium phosphate, 500g of 120# solvent oil into a 1L reaction kettle, control the temperature at 20°C, start stirring, and slowly drop 31.97g of sulfur monochloride into the system, after about 2 hours , the addition of sulfur monochloride was completed, and the temperature was maintained to continue stirring for about 2.5 hours, and the reaction was completed. Add 200g of water for washing, stir for 15 minutes, filter with suction and then dry the filter cake to obtain 53.57g of white needle crystals with a yield of 95.85%. The purity obtained was 99.61%.

Embodiment 2

[0025] Add 58.06g of morpholine, 104.30g of anhydrous trisodium phosphate, 600g of 120# solvent oil into a 1L reactor, control the temperature at 30°C, start stirring, and slowly add 40.91g of sulfur monochloride into the system dropwise for about 1.5h Finally, the sulfur monochloride was added dropwise, and the temperature was maintained to continue stirring for about 2 hours, and the reaction was completed. Add 300g of water for washing, stir for 15 minutes, filter with suction and then dry the filter cake to obtain 67.82g of white needle crystals with a yield of 94.83%. The melting point detected by DSC is 123-127°C. The purity obtained was 99.55%.

Embodiment 3

[0027] Add 52.81g of morpholine, 94.86g of anhydrous trisodium phosphate, and 550g of n-heptane into a 1L reactor, control the temperature at 40°C, start stirring, and slowly drop 37.21g of sulfur monochloride into the system, after about 2 hours , the addition of sulfur monochloride was completed, and the temperature was maintained to continue stirring for about 2.5 hours, and the reaction was completed. Add 200g of water for washing, stir for 15 minutes, filter with suction and then dry the filter cake to obtain 60.74g of white needle crystals with a yield of 93.38%. The purity was 99.15%.

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Abstract

The invention discloses a method for synthesizing 4,4'-dithiodimorpholine. Sulfur monochloride and morpholine are used as raw materials, anhydrous trisodium phosphate is used as an acid binding agent,the sulfur monochloride and morpholine are reacted to produce 4,4'-dithiodimorpholine and hydrochloric acid, and the anhydrous trisodium phosphate can react with the hydrochloric acid generated in the reaction to avoid the hydrochloric acid with from reacting morpholine and the morpholine from losing the reactivity. The acid binding agent anhydrous trisodium phosphate is added in the method of the invention, so the dosage of the raw material morpholine is reduced, and the production cost is saved; and the product and impurities can be separated by washing with water after the reaction is finished, so the method has the advantages of simple production, high operability, simplicity in post-treatment and industrial application values. The appearance of the obtained product is a white needlecrystal, the yield is 90% or above, the purity is 98% or above, and use requirements are met.

Description

technical field [0001] The present invention relates to a synthetic method of rubber vulcanizing agent 4,4'-dithiodimorpholine (DTDM), in particular to the production of 4,4'-dithiodimorpholine with low cost and less waste of morpholine The synthesis method belongs to the technical field of synthesis of rubber additives. 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 growing. 4,4'-Dithiodimorpholine (DTDM) is an important rubber vulcanization accelerator, which can replace sulfur in whole or in part to form an effective or semi-effective vulcanization system. 4,4'-dithiodimorpholine is an important rubber vulcanization accelerator, which contai...

Claims

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Application Information

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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
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