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The preparation method of zinc dibutyl dithiocarbamate

A technology of zinc dibutyldithiocarbamate and xylene, which is applied in the direction of organic chemistry, can solve the problems of low solvent and product recovery, waste liquid pollution of the environment, and cumbersome steps, and achieve manpower saving, high-efficiency production, The effect of increasing the yield

Active Publication Date: 2020-06-12
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to provide a kind of preparation method of zinc dibutyldithiocarbamate, to alleviate the waste liquid pollution environment when producing zinc dibutyldithiocarbamate in the prior art, step is loaded down with trivial details, cost is higher and Technical issues such as low solvent and product recoveries

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  • The preparation method of zinc dibutyl dithiocarbamate

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[0028] The present invention provides a method for preparing zinc dibutyl dithiocarbamate, wherein carbon disulfide is added dropwise to a reaction solution containing zinc oxide, dibutylamine, a dispersant and a first organic solvent for reaction, and dibutyl is obtained after the reaction is completed. Zinc dithiocarbamate;

[0029] The first organic solvent is insoluble in water, and the obtained zinc dibutyldithiocarbamate is insoluble or slightly soluble in the first organic solvent.

[0030] It should be noted that when the zinc dibutyldithiocarbamate is slightly soluble in the first organic solvent, the solubility of the zinc dibutyldithiocarbamate in the first organic solvent is not more than 1g / 100g.

[0031] The reaction materials used in the preparation method of the present invention are as follows:

[0032] Carbon disulfide: colorless or light yellow transparent liquid, pure product has the taste of ether, volatile, insoluble in water, soluble in most organic solvents suc...

Embodiment 1

[0055] This embodiment is a method for preparing zinc dibutyl dithiocarbamate, which includes the following steps:

[0056] Step a): At 15℃, add 240mL xylene, 5.15g zinc oxide, 0.027g fatty alcohol polyoxyethylene ether AEO-7 and 27.2g into a 1000mL four-necked flask equipped with electric stirring and dropping funnel. Dibutylamine is stirred and mixed uniformly to obtain a reaction solution;

[0057] Step b): Dissolve 16.07g of carbon disulfide in 12ml of xylene, maintain the temperature at 15°C, add the mixed solution of carbon disulfide and xylene dropwise to the reaction solution obtained in step a) for 0.6h, after the addition is complete, Continue to stir and react for 15 minutes, then heat to 26°C and react for 0.4 hours to end the reaction; the product is filtered, the filter cake is dried and crushed to obtain zinc dibutyl dithiocarbamate;

[0058] Step c): The first organic solvent is separated to remove the generated water and reused again.

[0059] The process flow diagra...

Embodiment 2

[0061] This embodiment is a method for preparing zinc dibutyl dithiocarbamate, which includes the following steps:

[0062] Step a): Add 805 mL xylene, 12.02 g zinc oxide, 3.85 g fatty alcohol polyoxyethylene ether AEO-9 and 27.2 g in a 1000 mL four-neck flask equipped with electric stirring and dropping funnel at 13°C Dibutylamine is stirred and mixed uniformly to obtain a reaction solution;

[0063] Step b): Dissolve 20.89g of carbon disulfide in 112ml of xylene, maintain the temperature at 13°C, and add the mixed solution of carbon disulfide and xylene dropwise to the reaction solution obtained in step a) for 6.7 hours. After the addition is complete, Continue to stir and react for 50 minutes, then heat to 55°C and react for 2 hours to end the reaction; the product is filtered, the filter cake is dried and crushed to obtain zinc dibutyl dithiocarbamate;

[0064] Step c): The first organic solvent is separated to remove the generated water and reused again.

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Abstract

The invention relates to the field of rubber vulcanization accelerators, in particular, it provides a method for preparing zinc dibutyldithiocarbamate, which is added to a reaction solution containing zinc oxide, dibutylamine, a dispersant and a first organic solvent Carbon disulfide is added dropwise to react, and zinc dibutyldithiocarbamate is obtained after the reaction, wherein the first organic solvent is insoluble in water, and the obtained zinc dibutyldithiocarbamate is insoluble or slightly soluble in the first organic solvent . The method adopts an anhydrous solvent method to prepare zinc dibutyldithiocarbamate, which eliminates the generation of saline waste water. Since the first organic solvent is insoluble in water, the two can be separated by liquid separation. The first organic solvent The solvent can be reused after removing the water, reducing the cost of the solvent and increasing the yield of the product. The above method is easy to operate, avoids the generation of salty waste water, is a clean and environmentally friendly new method, and is easily applied to large-scale production practices.

Description

Technical field [0001] The invention relates to the field of rubber vulcanization accelerators, in particular to a method for preparing zinc dibutyl dithiocarbamate. Background technique [0002] The current synthesis methods of zinc dibutyl dithiocarbamate (BZ) usually include aqueous solution method, wet alkali method and solvent method. The commonly used methods are wet alkali method and solvent method. At present, zinc dibutyl dithiocarbamate, a vulcanization accelerator widely used in the rubber industry, is produced by the wet alkali method, usually by first synthesizing dibutyl dithioamino in water with dibutylamine, carbon disulfide and sodium hydroxide Sodium formate, then the synthetic sodium salt is reacted with zinc sulfate or hydrochloride to prepare BZ. This method uses strong alkali and zinc sulfate or hydrochloride in the production process to produce a large amount of waste water (16-17t waste water per ton of product). Waste water containing sodium sulfate or s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/16
CPCC07C333/16
Inventor 丁俊杰谭西良宋风朝陶险峰王志强郭同新李宏喜朵延魁葛同伟
Owner WILLING NEW MATERIALS TECH CO LTD
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