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Improved process of aldehyde and amine accelerant DHP

A technology of accelerators and aldehydes and amines, which is applied in the field of improved technology of aldehydes and amines accelerator DHP, can solve the problems of limited practical application, complex and unpleasant smell, etc., and achieve high market application value, light appearance color, and reduce residue effects

Inactive Publication Date: 2021-07-09
河南易交联新材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Because the accelerator 808, DHP and A20 products and their by-products all have a relatively large odor, and the residual small amount of aniline and highly volatile butyraldehyde in the product make the odor of the product more complicated and unpleasant, which seriously limits this type of product practical application of

Method used

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  • Improved process of aldehyde and amine accelerant DHP
  • Improved process of aldehyde and amine accelerant DHP
  • Improved process of aldehyde and amine accelerant DHP

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 58.86g of n-heptanal and 1.40g of acetic acid into a 200ml flask, stir for 1h, cool down to 0°C, control the temperature at 0-5°C, slowly add 9.31g of aniline dropwise, and keep warm for 10h after the dropwise addition. Turn on the oil pump to keep the system under negative pressure, start to heat up, and distill off the water at 30-60°C; continue to heat up to 110-120°C to recover n-heptanal, and cool down to obtain 51.13g of the product, which is yellow and clear liquid, and the heptanal group is detected by gas chromatography DHP content is 60.52%, and heptanal and aniline residues are not detected.

Embodiment 2

[0041] Add 58.86g of n-heptanal and 1.40g of acetic acid into a 200ml flask, stir the reaction for 1h, control the temperature at 20-30°C, slowly add 9.31g of aniline dropwise, and continue to keep warm for 5h after the dropwise addition. Turn on the oil pump to keep the system under negative pressure, start to heat up, and distill off the water at 30-60°C; continue to heat up to 110-120°C to recover n-heptanal, and cool down to obtain 51.03g of the product, which is yellow and clear liquid, and the heptanal group is detected by gas chromatography The content of DHP is 63.21%, and no residues of heptanal and aniline are detected.

Embodiment 3

[0043] Add 58.86g of n-heptanal and 1.40g of acetic acid into a 200ml flask, stir the reaction for 1h, control the temperature at 30-40°C, slowly add 9.31g of aniline dropwise, and continue to keep warm for 4h after the dropwise addition. Turn on the oil pump to keep the system under negative pressure, start to heat up, and distill off the water at 30-60°C; continue to heat up to 110-120°C to recover n-heptanal, and cool down to obtain 51.06g of the product, which is yellow and clear liquid, and the heptanal group is detected by gas chromatography The content of DHP is 63.13%, and no residues of heptanal and aniline are detected.

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Abstract

The invention provides an improved process of an aldehyde and amine accelerator DHP. The process comprises the following specific synthesis steps: (1) adding heptanal and organic acid into a reactor, stirring and mixing; (2) controlling the temperature, dropwise adding aniline, and carrying out heat preservation reaction after dropwise adding; and (3) carrying out reduced pressure distillation, removing water generated in the system, and recovering heptanal to obtain a residual liquid which is a product. The product content is not lower than 50%, and the product is small in smell and light in color.

Description

technical field [0001] The invention relates to the field of rubber vulcanization accelerators, in particular to an improved process of an aldehyde-amine accelerator DHP. Background technique [0002] The vulcanization critical temperature of the aldehyde-amine vulcanization rubber accelerator is 120°C, and the optimum vulcanization temperature range is 120-160°C. It is especially suitable for the thiadiazole vulcanization system of chlorinated polyethylene rubber CM. The strength, aging resistance, and Heat, oil resistance and flame retardancy are significantly improved. In addition, aldehyde and amine accelerators can be used for the vulcanization of natural rubber, synthetic rubber and latex, and can also be used as active agents for acidic accelerators, which are widely used in the vulcanization of neoprene rubber, styrene-butadiene rosin rubber, butadiene rubber, etc. The use of aldehyde and amine accelerators as secondary accelerators together with thiuram, guanidine ...

Claims

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Application Information

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IPC IPC(8): C07D213/127C07D213/16C08K5/3432C08L7/00
CPCC07D213/127C07D213/16C08K5/3432
Inventor 付顺国宋士杰常帅军杨瑞朝张雁秦金良宋志强张旭旭闫学军王芳晓杨建轲侯万喜杨利琴王艳利王茜愉聂鹏蒋秀娜
Owner 河南易交联新材料研究院有限公司
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