Preparation method of vulcanizer 1,1'-dithiodicaprolactam

A technology of dithiobiscaprolactam and caprolactam, applied in the direction of organic chemistry and the like, can solve the problems of large environmental pollution, cracking and high cost of raw materials, and achieve the effect of protecting the environment and reducing costs

Active Publication Date: 2018-10-16
杭州布朗生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Rubber is widely used in today's civilized society. Synthetic rubber must be used in automobiles, airplanes, battery cars, bicycle tires, pipes and joints in various chemical industries, and various household appliances in daily life. According to different requirements and characteristics , to make rubber products of various specifications to meet the needs of industrial and agricultural production and daily necessities, but synthetic or natural rubber will age and oxidize over time, and will expand and crack in hot and cold weather. Occurrence will cause great danger to the safety field and cause serious loss of life and property
[0003] Chinese patent application (CN103044328A) discloses the synthesis of a new type of rubber vulcanizing agent 1,1'-dithiobiscaprolactam. The acid-binding agent is caprolactam, which has high raw material cost and great environmental pollution.

Method used

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  • Preparation method of vulcanizer 1,1'-dithiodicaprolactam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 100g of caprolactam, 730g of n-heptane and 95g of triethylamine into a 1L reaction kettle, stir mechanically, cool down in an ice bath to below 5-10°C, then add 65g of disulfide dichloride dropwise, finish adding in 30 minutes, and the dropwise addition is complete Afterwards, the temperature was raised to 12-15°C, and the reaction was kept for 7 hours, and the reaction was completed. (Add 200 grams of water, stir for 15 minutes, stir well, stand to separate layers, wash the organic layer with water, wash with brine, and concentrate under reduced pressure n-heptane (0.095MPa) to obtain 111.5 grams of off-white solid, yield 87.5%. Melting point 130-137 ° C. The water layer was adjusted to PH = 13 with 32% aqueous sodium hydroxide solution, and triethylamine was collected by atmospheric distillation at 90 ° C, dried with solid sodium hydroxide and used mechanically.

Embodiment 2

[0021] Add 200g of dichloroethane, 100g of caprolactam, and 121g of N,N-dimethylaniline into a 1L reaction flask in sequence, turn on mechanical stirring, cool down to 0-5°C in an ice bath, and then dropwise add 62.7g of disulfur dichloride, The addition was completed in 1 hour, and after the dropwise addition, the temperature was raised to 15-20°C, and the reaction was kept for 6 hours, and the reaction ended.

[0022] Add 200 g of water, stir for 15 minutes, stop stirring, let stand to separate layers, wash with water, wash with brine, and concentrate dichloroethane under pressure at 0.095 MPa to obtain 71.7 g of off-white solid with a yield of 56.3%. The melting point is 128-135°C. For the water layer, use 32% sodium hydroxide aqueous solution to adjust the pH to 13, let it stand and separate layers, and the upper organic layer is N,N-dimethylaniline, dry it with a small amount of sodium hydroxide, and use it mechanically.

Embodiment 3

[0024] Add 4000g of benzene, 100g of caprolactam, and 105.9g of pyridine to a 1L reaction flask in sequence, stir mechanically, cool down to 0-5°C in an ice bath, and then add 117.4g of disulfide dichloride dropwise for 1 hour. After the addition is complete Raise the temperature to 40-45°C, keep the temperature for 5 hours, and the reaction ends.

[0025] Cool to room temperature, add 200 g of water, stir for 15 minutes, stop stirring, stand to separate layers, wash with water, wash with brine, and concentrate benzene under pressure at 0.095 MPa to obtain 91.4 g of off-white solid with a yield of 73%. Melting point 130-135°C. For the water layer, use 32% sodium hydroxide aqueous solution to adjust the pH to 13, let it stand and separate layers, the upper organic layer is pyridine, dry with a small amount of sodium hydroxide, and use it mechanically.

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Abstract

The invention belongs to the technical field of rubber synthesis, relates to additives, used to increase the wear resistance and corrosion resistance of rubber, for rubber synthesis, and particularlyto a preparation method of vulcanizer 1,1'-dithiodicaprolactam. The preparation method uses organic amine to replace caprolactam to serve as the acid-binding agent, the organic amine can be recycled,and the defects that the caprolactam cannot be recycled, and great waste is caused are overcome. Compared with the prior art, the preparation method has the advantages that the organic amine used as the acid-binding agent can be recycled after the reaction, cost is lowered, and environments are protected.

Description

technical field [0001] The invention belongs to the technical field of rubber synthesis and mainly prepares additives for synthetic rubber to increase the properties of rubber such as anti-wear, anti-corrosion and corrosion resistance. Specifically, it is the synthesis of a new type of rubber vulcanizing agent 1,1'-dithiobiscaprolactam. Background technique [0002] Rubber is widely used in today's civilized society. Synthetic rubber must be used in automobiles, airplanes, battery cars, bicycle tires, pipes and joints in various chemical industries, and various household appliances in daily life. According to different requirements and characteristics , to make rubber products of various specifications to meet the needs of industrial and agricultural production and daily necessities, but synthetic or natural rubber will age and oxidize over time, and will expand and crack in hot and cold weather. Occurrence will bring great danger to the safety field and cause serious loss ...

Claims

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Application Information

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IPC IPC(8): C07D223/10
CPCC07D223/10
Inventor 黄国祥
Owner 杭州布朗生物医药科技有限公司
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