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Method for producing rubber vulcanization agent 4,4'-disulfuration dimorpholine

A dimorpholine disulfide and production method technology, applied in the chemical industry, can solve problems such as low melting point, low yield, and poor quality, and achieve the effects of reducing waste water discharge, improving product quality, and increasing yield

Inactive Publication Date: 2009-04-08
SANMENXIA XIAWEI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing 4,4'-dimorpholine disulfide production method is to react morpholine and sulfur monochloride in a mixed solvent of toluene and benzene under the condition of liquid caustic soda, and produce a large amount of industrial waste water and A large amount of washing waste water has caused environmental governance difficulties, and the existence of water in the liquid caustic soda has increased the side reaction of water and sulfur monochloride, thereby making the yield of the product low and poor in quality, and the melting point of the product is low, only reaching 118- 120℃, ash content 0.5%-0.8%

Method used

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Examples

Experimental program
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Effect test

Embodiment Construction

[0007] Example 1. Add 900kg of xylene into a 2000-liter reactor, start stirring, add 111kg of sodium hydroxide fine powder in batches, and add 155kg of sulfur monochloride dropwise at a temperature of 20-40°C in 3.5 hours. Open the jacket cooling water in the middle, after the dropwise addition, continue to stir for half an hour, let it stand for stratification, drain the sodium chloride precipitated in the lower layer, continue stirring, add 100kg of water to wash the materials in the kettle once, drain the lower layer of water, and suction filter The solvent was recovered, centrifuged and dried to obtain a white crystalline product, and dried at 80° C. to obtain a 255 kg product. After testing, the melting point of the product is 123.5°C, and the ash content is 0.20%.

[0008] Example 2. Add 900kg of 120# solvent oil into a 2000-liter reactor, start stirring, add 112kg of sodium hydroxide fine powder in batches, and add 153kg of sulfur monochloride dropwise at a temperature ...

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Abstract

The invention discloses a method for producing rubber vulcanizing agent 4, 4'-dimorpholinyl disulfide, which belongs to the chemical technical field. The method comprises the following steps: prime city naphtha is added in a reaction kettle; sodium hydroxide fine powder is added to the solvent gradually under stirring condition; drewamine is added to the solvent; sulfur chloride is dripped within three to four hours at a temperature between 20 and 60 DEG C; after the mixture reacts for half an hour, the stirring is stopped; the mixture is kept stand for delamination; the sodium chloride deposited in the lower layer is discharged out; materials in the kettle are added with small amount of water to wash the materials, and are filtered to reclaim the solvent; the solvent is subjected to centrifuge-dripping to obtain a white crystal product; and the product is dried to obtain rubber vulcanizing agent 4, 4'-dimorpholinyl disulfide. The method can improve the yield and quality of the product, and reduce waste water discharge. The product has a melting point higher than 122 DEG C and ash content less than 0.5 percent.

Description

technical field [0001] The invention relates to a production method of a rubber vulcanizing agent, in particular to a production method of a rubber vulcanizing agent 4,4'-dimorpholine disulfide, which belongs to the technical field of chemical industry. Background technique [0002] 4,4'-dimorpholine disulfide is a rubber vulcanization accelerator, which can be used as a vulcanizing agent for natural rubber, various synthetic rubbers and their combined rubbers. It is suitable for various dynamic products, and is often used in radial tires, engineering tires, Manufacture of high-quality rubber products such as bias rubber tires, butyl inner tubes and rubber seals. The existing 4,4'-dimorpholine disulfide production method is to react morpholine and sulfur monochloride in a mixed solvent of toluene and benzene under the condition of liquid caustic soda, and produce a large amount of industrial waste water and A large amount of washing waste water has caused environmental gove...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/26C08C19/20C08K5/47
Inventor 薛建启赵峰张小峡
Owner SANMENXIA XIAWEI CHEM
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