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Preparation method of granular diisobutylthiuram disulfide

A granular technology of diisobutyl disulfide, which is applied in the direction of organic chemistry, can solve problems such as non-compliance with environmental protection, energy saving and emission reduction, easy occurrence of viscous substances, long production cycle, etc., and achieve improvement of viscous substances and other problems. The effect of small land area and shortened production cycle

Active Publication Date: 2020-05-08
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process has a long production cycle, huge equipment, and a large floor area. A large amount of dust will be generated during crushing, and sticky substances are prone to appear during the production process, resulting in agglomeration and product waste. It does not meet the relevant national policies and regulations on environmental protection, energy conservation and emission reduction.

Method used

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  • Preparation method of granular diisobutylthiuram disulfide
  • Preparation method of granular diisobutylthiuram disulfide
  • Preparation method of granular diisobutylthiuram disulfide

Examples

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preparation example Construction

[0032] According to one aspect of the present invention, a preparation method of granular diisobutylthiuram disulfide is provided in at least one embodiment, comprising:

[0033] (a) by diisobutylamine, liquid caustic soda and carbon disulfide mixed reaction, obtain diisobutyl dithiocarbamate sodium solution;

[0034] (b) mixing sodium diisobutyldithiocarbamate solution, seed crystal and surfactant, and the crystal seed comprises diisobutylthiuram disulfide powder;

[0035] (c) mixing the solution obtained in step (b) with H 2 SO 4 and H 2 O 2 The mixed reaction gave granular diisobutylthiuram disulfide.

[0036] The above-mentioned preparation method has been improved in the traditional process. After the mixed reaction of diisobutylamine, liquid caustic soda and carbon disulfide is carried out to obtain the sodium diisobutyl dithiocarbamate solution, it is mixed with crystal seed and surfactant, and finally mixed with the diisobutyl dithiocarbamate solution. The mixed r...

Embodiment 1

[0058] A kind of preparation method of granular diisobutylthiuram disulfide, such as figure 1 shown, including:

[0059] (a) 500g of pure water, 50g of liquid caustic soda and 50g of diisobutylamine were added to a 1000mL reaction flask, and after mixing and stirring, 33g of carbon disulfide liquid was added dropwise at a constant speed for 3h, and the reaction temperature was controlled to be 25°C. After the reaction, two Sodium isobutyl dithiocarbamate solution;

[0060] (b) add 1g TiBTD powder and 0.5g sorbitol fatty acid ester, stir to make diisobutyl dithiocarbamate sodium solution, TiBTD powder and sorbitol fatty acid ester fully mixed;

[0061] (c) take by weighing 150g of pure water, add 20g concentrated sulfuric acid (concentration is 98wt%) and 27g hydrogen peroxide (concentration is 27.5wt%) under stirring to obtain mixed oxidant, uniformly add oxidant dropwise, take 4h, and control the reaction temperature to be 25 ℃, after the reaction is completed, tetraisobuty...

Embodiment 2

[0063] A preparation method of granular diisobutylthiuram disulfide is different from Example 1 in that in this example, sorbitan fatty acid ester is replaced with polysorbate, and the rest are the same as in Example 1. The obtained tetraisobutylthiuram disulfide product was light yellow granules with a yield of 98.6% and an initial melting point of 67.8°C.

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Abstract

The invention relates to the field of preparation of rubber vulcanization accelerators, and particularly provides a preparation method of granular diisobutylthiuram disulfide. The preparation method comprises the following steps: (a) mixing diisobutylamine, liquid caustic soda and carbon disulfide for a reaction to obtain a sodium diisobutyldithiocarbamate solution, (b) uniformly mixing the sodiumdiisobutyldithiocarbamate solution, a seed crystal and a surfactant, wherein the seed crystal comprises diisobutylthiuram disulfide powder, and (c) mixing the solution obtained in the step (b) with H2SO4 and H2O2 to obtain the granular diisobutylthiuram disulfide. According to the method, the seed crystal and the surfactant are introduced in the technological process, the granular diisobutylthiuram disulfide can be directly obtained after a reaction, subsequent processes such as crushing and granulation are not needed, the production period is greatly shortened, the energy consumption is low,the occupied area is small, a large amount of dust cannot be generated, the environmental protection property is good, and the product yield and purity are high.

Description

technical field [0001] The invention relates to the field of preparation of rubber vulcanization accelerators, in particular to a preparation method of granular diisobutylthiuram disulfide. Background technique [0002] Rubber Vulcanization Accelerator Diisobutylthiuram disulfide (TiBTD, tetra(isobutyl)thioperoxydicarbamic acid) is a green and environmentally friendly rubber accelerator, which is a substitute for accelerators TMTD, TETD, TMTM, etc. to produce N-nitrosamines It is widely used in the vulcanization of natural rubber, isoprene rubber, styrene-butadiene rubber, butadiene rubber, EPDM rubber and nitrile rubber. [0003] Due to the poor fluidity of traditional powdered TiBTD, it is easy to generate dust during use, and the flying dust can easily cause skin allergies when it contacts the skin. Therefore, it is required to process TiBTD into granular products. The traditional production process of granular TiBTD is as follows: the crude TiBTD product is obtained fir...

Claims

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Application Information

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IPC IPC(8): C07C333/32C07C333/16C08K5/40
CPCC07C333/32C07C333/16C08K5/40
Inventor 郭德义章娟尹跃宁丁胜强李泽涛史国鑫
Owner WILLING NEW MATERIALS TECH CO LTD
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