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Preparation method for dialkyl dithiocarbamate and anti-wear and rust-proof composite agent

A technology of dialkyl dithiocarbamate and antirust agent, which is applied in additives, lubricating compositions, organic chemistry, etc., can solve the problems of storage stability and lack of compatibility, and achieve excellent storage stability, The effect of excellent compatibility

Active Publication Date: 2018-01-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The dialkyl dithiocarbamate products prepared by the above-mentioned patents and literatures still have certain deficiencies in storage stability and compatibility.

Method used

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  • Preparation method for dialkyl dithiocarbamate and anti-wear and rust-proof composite agent
  • Preparation method for dialkyl dithiocarbamate and anti-wear and rust-proof composite agent
  • Preparation method for dialkyl dithiocarbamate and anti-wear and rust-proof composite agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047]Add 16.8g sodium hydroxide and 33.6g water in the 250ml there-necked bottle that is equipped with cooling pipe, be made into sodium hydroxide aqueous solution (mass concentration 33%), then add 51.6g di-n-butylamine, 18g ethanol, 17.7g di Chloromethane, stir evenly, slowly add 31.6g of carbon disulfide dropwise, condense volatilized carbon disulfide and methylene chloride with a cooling tube, and control the reaction temperature within the range of 30°C. After adding carbon disulfide, react within this temperature range for 1h. Then, the temperature was raised to 70° C., and the reaction was continued for 5 h. After completion of the reaction, add solvent gasoline 70g, extract for 20 minutes, separate the alcoholic aqueous phase and sodium chloride solid, add 10g concentration of 15% dilute hydrochloric acid solution to the organic phase, stir for 20 minutes, and record the pH value of the mixed phase After the water phase is separated, the remaining organic phase is wa...

Embodiment 2

[0049] Add 17.1g sodium hydroxide and 68.4g water in the 250ml there-necked bottle that is equipped with cooling tube, be made into sodium hydroxide aqueous solution (mass concentration 20%). Then add 51.6g of di-n-butylamine and 20.4g of dichloromethane, stir evenly, slowly add 32.2g of carbon disulfide dropwise, condense the volatilized carbon disulfide and dichloromethane with a cooling tube, and control the reaction temperature within the range of 25°C. After adding carbon disulfide, keep the temperature within the range and react for 1 hour. Then, the temperature was raised to 70° C., and the reaction was continued for 5 h. After completion of the reaction, add solvent gasoline 70g, stir for 20 minutes, separate the alcoholic water phase and sodium chloride solid, add 20g of concentration in the organic phase and be 10% dilute hydrochloric acid solution, stir for 40 minutes, and record the mixed phase pH value as At about 4.5, separate the water phase and wash until neut...

Embodiment 3

[0051] Add 16.6g sodium hydroxide and 36.2g water in the 250ml there-necked flask that is equipped with cooling tube, be made into aqueous sodium hydroxide solution (mass concentration 33%). Then add 51.6g of di-n-butylamine and 18g of ethanol, stir evenly, slowly add 31.6g of carbon disulfide dropwise, use a cooling tube to condense the volatilized carbon disulfide, and control the reaction temperature within the range of 35°C. After adding carbon disulfide, react for 1 hour, add 17.7 g of dichloromethane dropwise, raise the temperature to 80°C, and react for another 4 hours. After completion of the reaction, add solvent gasoline 70g, add solvent gasoline 70g, stir for 20 minutes, separate the alcoholic water phase and sodium chloride solid, add 10g of concentration in the organic phase and be 15% acetic acid solution, stir for 60 minutes, record the mixed The pH value of the phase is about 5.5. After the water phase is separated, it is washed until neutral, and then distille...

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Abstract

The invention provides a preparation method for dialkyl dithiocarbamate and an anti-wear and rust-proof composite agent. The preparation method for the dialkyl dithiocarbamate comprises the followingsteps: step 1, performing a reaction on an alkali metal hydroxide, a secondary amine, dichloromethane and carbon disulfide, performing extraction on a reaction product through a solvent, and performing separation to obtain an organic phase; step 2, mixing the organic phase obtained in the step 1 and a water soluble acid solution; and step 3, washing a mixed liquid obtained in the step 2 by using water until the mixed liquid is neutral, and collecting the product. The dialkyl dithiocarbamate prepared by the method has excellent storage stability and compatibility.

Description

technical field [0001] The invention relates to a dialkyl dithiocarbamate, in particular to a preparation method of a dialkyl dithiocarbamate. Background technique [0002] Lubricating oil will inevitably contact with oxygen in the air and metal surface during use, and oxidation reaction will deteriorate, which will increase the viscosity of the oil, increase the acid value, generate sludge and precipitation, and cause corrosion and wear to metal parts . In order to extend the service life of the oil, delay its oxidation process, and slow down the friction and wear of the equipment, antioxidants and anti-wear agents can be added to the oil to effectively improve the performance of the oil. [0003] As a kind of ashless multi-effect additive with good oil solubility, dialkyl dithiocarbamate has outstanding anti-oxidation performance, good anti-wear performance and extreme pressure performance, and is widely used in steam turbine oil , hydraulic oil, gear oil, internal combu...

Claims

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Application Information

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IPC IPC(8): C07C333/20C10M135/18C10M141/08C10N30/06C10N30/12
Inventor 张辉李新华段庆华
Owner CHINA PETROLEUM & CHEM CORP