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Methylene bis(dialkyldithiocarboxamide) production method

A production method, the technology of methylene bis, applied in the direction of organic chemistry, etc., can solve the problems of environmental and health impact, carbon disulfide has a bad smell, and the temperature is as low as -30 ℃, and achieves the effect of improving chroma, improving color and avoiding oxidation

Inactive Publication Date: 2016-02-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing process adopts dropwise addition of carbon disulfide. Carbon disulfide is a flammable and explosive dangerous chemical with a low boiling point of only 46.5°C and a flash point as low as -30°C. The storage of carbon disulfide during the dropwise addition process cannot avoid contact with air. Vapors can form a wide range of explosive mixtures with air, increasing the risk of explosion in production operations
At the same time, carbon disulfide has a foul smell, and it is difficult to avoid its volatilization during the dropping process, which has a great impact on the environment and health

Method used

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  • Methylene bis(dialkyldithiocarboxamide) production method
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  • Methylene bis(dialkyldithiocarboxamide) production method

Examples

Experimental program
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Embodiment 1

[0020] Example 1: Turn on the ice machine to lower the temperature of the reactor, add 2419.17kg of sodium hydroxide aqueous solution (20% by mass fraction, 12.10kmol) into the reactor, start stirring and lower the temperature, and when the temperature reaches below 20°C, add 750kg (9.77kmol ) Carbon disulfide is slowly added to the reaction kettle, continue to stir and cool down, the temperature of the reaction solution is below 15°C, start to add 1212.41kg (9.30kmol) di-n-butylamine solution dropwise, control the temperature and add dropwise for 5 hours, after the drop is complete, raise the temperature to 50°C, Continue to react for 2 hours; add 479.32kg (5.58kmol) of dichloromethane dropwise to the solution, raise the temperature to 70°C after 2 hours, react for 2.5 hours, and the reaction ends. Wash with water after separation, and distill under reduced pressure at 5KPa and 80°C to obtain a light yellow transparent oily liquid with a yield of 93.4%. Its kinematic viscosit...

Embodiment 2

[0021] Example 2: Turn on the ice machine to lower the temperature of the reactor, add 2257.89kg potassium hydroxide aqueous solution (30% by mass, 12.10kmol) into the reactor, start stirring to lower the temperature, and when the temperature reaches below 20°C, add 750kg (9.77kmol ) Carbon disulfide is slowly added to the reaction kettle, continue to stir and cool down, the temperature of the reaction solution is below 15°C, start to add 1212.41kg (9.30kmol) di-n-butylamine solution dropwise, control the temperature and add dropwise for 5 hours, after the drop is complete, raise the temperature to 50°C, Continue to react for 2 hours; add 479.32kg (5.58kmol) of dichloromethane dropwise to the solution, raise the temperature to 70°C after 2 hours, react for 2.5 hours, and the reaction ends. Wash with water after separation, and distill under reduced pressure at 5KPa and 80°C to obtain a light yellow transparent oily liquid with a yield of 94.1%. Its kinematic viscosity is 15.25...

Embodiment 3

[0022] Example 3: Turn on the ice machine to cool down the reaction kettle, add 2486.84kg sodium hydroxide aqueous solution (20% by mass fraction, 12.43kmol) into the reaction kettle, start stirring to cool down, and when the temperature reaches below 20°C, add 750kg (9.77kmol ) Carbon disulfide is slowly added to the reaction kettle, continue to stir and cool down, and the temperature of the reaction solution is below 20°C, start to add 706.10kg (8.88kmol) of di-n-propylamine solution dropwise, control the temperature and add dropwise for 4 hours, after the drop is completed, raise the temperature to 50°C, continue React for 2 hours; add 495.66kg (5.77kmol) of dichloromethane dropwise to the solution, raise the temperature to 70°C after 2 hours, react for 2.5 hours, and the reaction ends. Wash with water after separation, and distill under reduced pressure at 5KPa and 75°C to obtain a light yellow transparent oily liquid with a yield of 92.1%. Its kinematic viscosity is 15.02...

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Abstract

The present invention relates to a methylene bis(dialkyldithiocarboxamide) production method, which comprises: adding secondary alkylamine to a carbon disulfide and alkali solution mixing solution in a dropwise manner, maintaining the temperature at 0-20 DEG C, increasing the temperature to 40-65 DEG C after the adding, continuously carrying out the reaction for 1-10 h, adding dichloromethane to the methylene bis(dibutyldithiocarbamate) solution in a dropwise manner at a temperature of 40-60 DEG C, increasing the temperature to 50-905 DEG C after the adding, carrying out a reaction for 2-10 h, and carrying out liquid separation, water washing and distillation to obtain the product. According to the present invention, the nitrogen protection is used, the material feeding way is not required to be changed, the high risk grade carbon disulfide is not required to be added in the dropwise manner, other solvents are not required to be added, the reaction time and the operation steps are reduced, the production is stable, the yield is significantly improved, and the product performance meets the requirement.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and relates to a preparation and production method of methylene bis(dialkyldithioformamide). Specifically, the present invention relates to a method for producing a lubricating oil additive dialkyl dithiocarbamate by reacting raw materials secondary alkylamine, alkali solution, carbon disulfide and methylene chloride in two steps. Background technique [0002] With the improvement of the level of mechanization, especially the increasing development of the automobile industry, the development of the lubricant industry has also risen. However, during the use of the oil, due to friction on the metal surface, high temperature, moisture, and light, the oxidation reaction inevitably occurs and deteriorates, which causes the acid value of the lubricating oil to increase, the viscosity increases, and sludge or precipitation is formed. The performance is greatly reduced; with the rapid development of mod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/20
Inventor 何志勇黄伟孔伟伟任磊平俊彦金刚李秀清
Owner CHINA PETROLEUM & CHEM CORP