Preparation method of zinc dibutyldithiocarbamate

A technology of zinc dibutyldithiocarbamate and dibutylamine, applied in organic chemistry and other directions, can solve the problems of low solvent and product recovery rate, waste liquid polluting the environment, complicated steps, etc., and achieve labor saving and efficient production. , the effect of improving yield

Active Publication Date: 2018-06-12
WILLING NEW MATERIALS TECH CO LTD
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  • Abstract
  • Description
  • Claims
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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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  • Preparation method of zinc dibutyldithiocarbamate

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[0028] The invention provides a method for preparing zinc dibutyldithiocarbamate, which involves dropping carbon disulfide into a reaction solution containing zinc oxide, dibutylamine, a dispersant and a first organic solvent for reaction, and obtaining dibutyl dithiocarbamate 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 zinc dibutyldithiocarbamate is slightly soluble in the first organic solvent, the solubility of zinc dibutyldithiocarbamate in the first organic solvent is not greater than 1g / 100g.

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

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

Embodiment 1

[0055] Present embodiment is a kind of preparation method of zinc dibutyldithiocarbamate, comprises the following steps:

[0056] Step a): Add 240mL of xylene, 5.15g of zinc oxide, 0.027g of fatty alcohol polyoxyethylene ether AEO-7 and 27.2g of Dibutylamine is stirred and mixed evenly 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), and add the dropwise time for 0.6h. After the dropwise addition, Continue to stir and react for 15 minutes, then raise the temperature to 26°C for 0.4 hours to complete the reaction; the product is filtered, the filter cake is dried and pulverized to obtain zinc dibutyldithiocarbamate;

[0058] Step c): the first organic solvent is reused after liquid separation to remove the generated water.

[0059] The schematic diagram of the process flow of the p...

Embodiment 2

[0061] Present embodiment is a kind of preparation method of zinc dibutyldithiocarbamate, comprises the following steps:

[0062] Step a): At 13°C, add 805 mL of xylene, 12.02 g of zinc oxide, 3.85 g of fatty alcohol polyoxyethylene ether AEO-9 and 27.2 g of Dibutylamine is stirred and mixed evenly to obtain a reaction solution;

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

[0064] Step c): the first organic solvent is reused after liquid separation to remove the generated water.

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Abstract

The invention relates to the field of rubber vulcanizing promoter and particularly relates to a preparation method of zinc dibutyldithiocarbamate. The preparation method comprises the following stepsof: dropping carbon disulfide into reaction solution containing zinc oxide, dibutylamine, a dispersing agent and a first organic solvent to carry out reaction, and after reaction is ended, obtaining the zinc dibutyldithiocarbamate, wherein the first organic solvent is insoluble in water and the obtained zinc dibutyldithiocarbamate is insoluble or slightly soluble in the first organic solvent. Thepreparation method of the zinc dibutyldithiocarbamate has the beneficial effects that an anhydrous solvent method is adopted to prepare the zinc dibutyldithiocarbamate, so that the generation of salt-containing waste water is avoided; since the first organic solvent is insoluble in water, the first organic solvent and the water can be separated by liquid-separating operation; the first organic solvent after water removal can be repeatedly utilized, so that the solvent cost is reduced and simultaneously the yield of a product is increased; the operation is simple and convenient, the generationof the salt-containing waste water is avoided, and the method is a cleaning environment-friendly new method, and is easily applied in large-scale production practice.

Description

technical field [0001] The invention relates to the field of rubber vulcanization accelerators, in particular to a preparation method of zinc dibutyldithiocarbamate. Background technique [0002] The current synthetic method of dibutylzinc dithiocarbamate (BZ) usually has three kinds of aqueous solution method, wet alkali method and solvent method, commonly used is wet alkali method and solvent method. At present, zinc dibutyl dithiocarbamate, a vulcanization accelerator widely used in the rubber industry, is produced by wet alkali method. Usually, dibutylamine, carbon disulfide and sodium hydroxide are used to synthesize dibutyl dithiocarbamate in water. Sodium formate, and then use the synthetic sodium salt to react with zinc sulfate or hydrochloride to prepare BZ. In this method, the use of strong alkali and zinc sulfate or hydrochloride in the production process will produce a large amount (16-17t of waste water per ton of product) containing sodium sulfate or sodium ch...

Claims

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Application Information

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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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