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Preparation method of dialkyldithiocarbamate

A technology of dialkyl dithiocarbamate and di-n-butylamine, which is applied in the field of dialkyl dithiocarbamate preparation and can solve the problem of waste water, dialkyl dithiocarbamate Problems such as low rate and low purity

Active Publication Date: 2017-07-21
XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of dialkyl dithiocarbamate prepared by the existing process is low, the purity is low, and a large amount of waste water is produced in the washing process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] The invention provides a kind of preparation method of dialkyl dithiocarbamate, comprises the following steps:

[0023] Sodium hydroxide, water, di-n-butylamine, ethanol, methylene chloride and carbon disulfide are mixed and reacted to obtain a reaction product;

[0024] The reaction product is extracted with solvent oil and separated to obtain an oil phase;

[0025] Mixing the oil phase and the carrier, filtering to obtain the mother liquor;

[0026] The mother liquor is subjected to vacuum distillation to obtain the mother liquor after distillation;

[0027] The mother liquor after the distillation is extracted with solvent oil, and then subjected to vacuum distillation to obtain dialkyl dithiocarbamate.

[0028] The method provided by the invention is a one-step method for preparing dialkyldithiocarbamate, through two solvent oil extractions, two vacuum distillations and one vacuum distillation before adopting carrier treatment, so as to achieve the purpose of not ...

Embodiment 1

[0043]Add 48.82g of sodium hydroxide solid in the quick-opening stirred reactor, then add 67.42g of water to dissolve, after cooling to room temperature, add 129.24g of di-n-butylamine, 50.32g of ethanol, and 49.89g of dichloromethane successively, and then Add 78.42g of carbon disulfide dropwise at ℃. After the dropwise addition, directly raise the temperature to 90℃ and react for 5 hours to ensure that the internal pressure of the system is 0.1MPa during the reaction. After the reaction, ethanol is distilled out under reduced pressure. #Solvent oil was extracted at 50°C for half an hour, and the upper oil phase was separated with a separatory funnel. The separated inorganic water phase was recycled as the raw material for the next batch of synthesis. 20g of polymer porous microspheres GDX was added to the oil phase at 55 Heat stirring treatment at ℃ for 20 minutes, filter and separate the oil phase, distill gasoline and volatile organic compounds under reduced pressure at 100...

Embodiment 2

[0045] Add 26.32g of sodium hydroxide solid into the quick-opening stirred reaction kettle, then add 70.16g of the inorganic water phase in Example 1 to dissolve, after cooling to room temperature, add 96.15g of di-n-butylamine in turn, distilled out in Example 1 37.44g of ethanol, 37.12g of dichloromethane, and then drop 58.34g of carbon disulfide at 25°C. After the dropwise addition, the temperature was raised to 98°C for 4 hours to ensure that the internal pressure of the reaction system was 0.1MPa, and then the ethanol was distilled off under reduced pressure. , after the ethanol is evaporated, first add 37g of 120# solvent oil and extract at 70°C for half an hour, use a separatory funnel to separate the upper oil phase, and the separated inorganic water phase is recycled as the next batch of synthetic raw materials, and add 30g to the oil phase Polymer porous microsphere GDX was heat-stirred at 60°C for 30 minutes, the oil phase was filtered and separated, gasoline and vol...

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Abstract

The invention provides a preparation method of dialkyldithiocarbamate. The preparation method includes following steps: mixing sodium hydroxide, water, di-n-butylamine, alcohol, dichloromethane and carbon disulfide for reaction to obtain a reaction product; adopting solvent oil to extract the reaction product, and separating to obtain an oil phase; mixing the oil phase with a supporter, and filtering to obtain mother liquid; performing depressurizing distillation on the mother liquid to obtain distilled mother liquid; adopting the solvent oil to extract the distilled mother liquid, and performing depressurizing distillation to obtain dialkyldithiocarbamate. The preparation method prepares dialkyldithiocarbamate through a one-step process, the objective of no washing with water is achieved through two times of extraction through the solvent oil, two times of depressurizing distillation and treatment by adopting the supporter before a time of depressurizing distillation, so that generation of wastewater is reduced, and high product yield and product purity are realized. Experiment results show that yield of dialkyldithiocarbamate is higher than 99%, and purity is higher than 98%.

Description

technical field [0001] The invention relates to the technical field of dialkyl dithiocarbamate preparation, in particular to a preparation method of dialkyl dithiocarbamate. Background technique [0002] Dialkyl dithiocarbamate compounds are an important class of organic compounds, widely used in rubber, petroleum, agriculture, mining, medicine, environmental protection, analytical chemistry and other fields. Dialkyl dithiocarbamates are generally prepared by reacting carbon disulfide with sodium hydroxide, secondary amines and methylene chloride. [0003] There are two-step method and one-step method for preparing dialkyldithiocarbamate in the prior art: as US5,015, the example 1 of 368 discloses the method that adopts two-step method to prepare dialkyldithiocarbamate, the first In the first step, carbon disulfide was added to the mixture containing di-n-butylamine, sodium hydroxide and water at about 63°C; in the second step, the temperature was raised to 88°C, and dichlo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/20
CPCC07C333/20
Inventor 郭春萱常鹏范金凤徐坤王世俊
Owner XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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