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4,4'-methylene bis(dialkyl dithioformamide) preparation method

A technology of dialkyldithiocarboxamide and methylenebis, which is used in lubricating compositions, petroleum industry, additives, etc., can solve problems such as hidden dangers of environment and health, increase of production cost and operation steps, and poor color and luster. , to achieve the effect of improving yield, saving reaction time and operation steps, and excellent product performance

Active Publication Date: 2015-03-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some also need to add other organic solvents, which increases the production cost and operation steps
Especially in the process of dropping carbon disulfide, because carbon disulfide is a flammable and explosive dangerous chemical with a low boiling point and a foul smell, it is difficult to avoid its volatilization during the dropping process, so it has great hidden dangers to the environment and health
In addition, the performance of products prepared by many methods needs to be improved, such as low purity, poor color, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: Add 242g (3.15mol) of carbon disulfide and 636g of aqueous sodium hydroxide solution (20% by mass) into a four-neck flask, stir evenly and start adding 394g (3mol) of di-n-butylamine dropwise, controlling the temperature at 10 After 2 hours, the di-n-butylamine is dropped, and the temperature is raised to 50°C, and the reaction is continued for 2 hours; then 140g (1.65mol) of dichloromethane is added dropwise to the solution, and the temperature is raised to 70°C after 2 hours. After 2.5 hours of reaction, the reaction was completed. After liquid separation, wash with water, and distill under reduced pressure at 5KPa and 70°C to obtain a light yellow transparent oily liquid with a yield of 94.3%. Its kinematic viscosity is 15.16cSt, nitrogen content is 6.81, and chromaticity is 0.5.

Embodiment 2

[0019] Example 2: Add 251g (3.3mol) of carbon disulfide and 636g of aqueous sodium hydroxide solution (20% by mass) into a four-neck flask, stir evenly and start adding 394g (3mol) of di-n-butylamine dropwise, and react under ice bath , and keep the temperature at about 10°C, di-n-butylamine drops after 2 hours, raise the temperature to 50°C, and continue the reaction for 2 hours; then add 140g (1.65mol) dichloromethane dropwise to the solution, drop it in 2 hours Afterwards, the temperature was raised to 75° C., and the reaction was completed for 2.5 hours. Wash with water after separation, and distill under reduced pressure at 5KPa and 70°C to obtain a light yellow transparent oily liquid with a yield of 95.1%. Its kinematic viscosity is 15.29cSt, nitrogen content is 6.78, and chromaticity is 1.0.

Embodiment 3

[0020] Example 3: Add 242g (3.15mol) of carbon disulfide and 848g of aqueous sodium hydroxide solution (15% in mass fraction) into a four-neck flask, stir evenly and start adding 394g (3mol) of di-n-butylamine dropwise, and keep in an ice bath The temperature is around 15°C. After 1.8 hours, the di-n-butylamine is dripped, and the temperature is raised to 50°C, and the reaction is continued for 2 hours; then 187g (1.8mol) of dichloromethane is added dropwise to the solution, and the temperature is raised to 75°C, react for 2.5 hours, and the reaction ends. After liquid separation, wash with water, and distill under reduced pressure at 3KPa and 75°C to obtain a light yellow transparent oily liquid with a yield of 95.8%. Its kinematic viscosity is 15.56cSt, nitrogen content is 6.78, and chromaticity is 0.5.

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Abstract

The present invention relates to a 4,4'-methylene bis(dialkyl dithioformamide) preparation method, which comprises: (1) adding di-n-butylamine to a mixed solution of carbon disulfide and sodium hydroxide in a dropwise manner, maintaining the temperature between 0-30 DEG C, heating to a temperature of 40-60 DEG C after completing the adding of the di-n-butylamine, and continuously reacting for 1-6 h; and (2) adding methylene chloride to the obtained solution in a dropwise manner, heating to a temperature of 50-90 DEG C after completing the adding of the methylene chloride, reacting for 0.5-8 h, and carrying out separation purification to obtain the product. With the method of the present invention, the feeding way of the material is changed, the high risk level 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 saved, the yield is significantly improved, and the product performance is excellent.

Description

technical field [0001] The invention belongs to the field of organic chemistry and relates to a preparation method of 4,4'-methylenebis(dialkyldithioformamide). Specifically, the present invention relates to a method for preparing a lubricating oil additive dialkyldithiocarbamate by reacting raw materials secondary alkylamine, sodium hydroxide aqueous 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 o...

Claims

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Application Information

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IPC IPC(8): C07C333/20C10M135/18
Inventor 孔伟伟黄伟何志勇肖宏葵平俊彦
Owner CHINA PETROLEUM & CHEM CORP
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