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Method for preparing tetraalkyl thiuram disulfide through photocatalytic oxidation

A technology of photocatalytic oxidation and tetrahydrocarbyl thiuram, applied in the directions of organic chemistry methods, chemical instruments and methods, physical/chemical process catalysts, etc. The effect of stable quality, avoiding dissolution loss and fast reaction speed

Active Publication Date: 2021-02-12
HEBI YUANHAO CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that inorganic salt by-products are produced, and the product needs a large amount of water to wash and desalt, and the water consumption is high; the mother liquor still needs further treatment, and the energy consumption is high
The disadvantages of this solution are: ①Under this condition, when the medium and air coexist, it is very easy to cause an explosion, which has a large safety risk, and once an explosion occurs, its danger is difficult to control; ②The residue of toluene in the product limits its use in high-end rubber ③This method requires the use of transition metal salts as catalysts, and such metal salts may react with the intermediate dialkyldithiocarbamic acid to form metal complexes and contaminate the product
Disadvantages: ① Due to the large amount of water contained in the hydrogen peroxide, the medium needs to be dewatered and refined after the reaction, and the energy consumption is high
②Hydrogen peroxide is strong, so the oxidation temperature needs to be strictly controlled during oxidation, and peroxidation by-products are easily produced

Method used

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  • Method for preparing tetraalkyl thiuram disulfide through photocatalytic oxidation
  • Method for preparing tetraalkyl thiuram disulfide through photocatalytic oxidation
  • Method for preparing tetraalkyl thiuram disulfide through photocatalytic oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add 7.39g of diethylamine, 90mL of absolute ethanol, and 0.052g of hematoxylin into a 250ml beaker with a cover. Turn on the stirring, control the temperature at 20-30°C, slowly add 7.81g of carbon disulfide, complete the addition in about 1 minute, and stir for 5 minutes to react. Turn on the 12W LED blue light source, the light source is located in the center of the liquid surface, 5cm above the liquid surface, turn on the Sensen ct-201 air pump (with bubble disc) to feed air into the reaction solution, light reaction for 2min, stop the aeration and the reaction is over. Ethanol was distilled off under reduced pressure and dried to obtain 14.68 g of white tetraethylthiuram disulfide crystals, with a yield of 98.99% and a purity of 99.95% as detected by liquid chromatography.

Embodiment 2

[0049]Add 36.95g of diethylamine, 0.259g of hematoxylin, and 250ml of absolute ethanol into a 500mL beaker with a cover. Turn on the stirring, control the temperature at 20-30°C, slowly add 39.05g of carbon disulfide, complete the addition in about 30 minutes, and stir for 10 minutes to react. Turn on the 12w LED blue light source, the light source is located in the center of the liquid surface, 5cm above the liquid surface, turn on the Sensen ct-201 air pump (with bubble disc) to pass air into the reaction solution for 10 minutes, stop the aeration and the reaction is over. Filter and collect the mother liquor, and dry to obtain 63.80 g of white tetraethylthiuram disulfide crystals. The yield was 86.04%, and the purity detected by liquid chromatography was 99.99%.

Embodiment 3

[0051] 36.95g of diethylamine and the mother liquor collected in Example 2 were added to a 500mL beaker with a cover. Turn on the stirring, at 20-30°C, slowly add 39.05g of carbon disulfide, complete the addition in about 30 minutes, and stir for 10 minutes to react. Turn on the 12w LED blue light source, the light source is located in the center of the liquid surface, 5cm higher than the liquid surface, turn on the Sensen ct-201 air pump (with bubble disc) to pass air into the reaction solution for 10 minutes, and stop the ventilation to complete the reaction. The mother liquor was collected by filtration and dried to obtain 74.21 g of white tetraethylthiuram disulfide crystals. The yield was 100.07%, and the purity detected by liquid chromatography was 99.98%.

[0052] After rectifying the mother liquor to recover ethanol, 10.26 g of white crystal tetraethylthiuram disulfide was obtained, and the purity detected by liquid chromatography was 99.95%. Combining the product qu...

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Abstract

The invention relates to a method for preparing tetraalkyl thiuram disulfide by photocatalytic oxidation. The method comprises the following steps: carrying out mixed reaction on secondary amine, carbon disulfide and a catalyst in a medium to generate an intermediate product; and carrying out catalytic oxidation reaction on the intermediate product under illumination to obtain tetraalkyl thiuram disulfide. According to the invention, the method is high in reaction speed and mild in condition, and energy conservation and efficiency improvement are achieved; the used medium and catalyst can be recycled, so that the resource utilization rate is improved; and the method does not produce inorganic salt by-products, and the product has high yield and high purity.

Description

technical field [0001] The invention relates to the synthesis field of rubber vulcanization accelerators, in particular to a synthesis technology of tetrahydrocarbyl thiuram disulfide. Background technique [0002] Thiuram-type vulcanization accelerators, the production technologies in the industry currently mainly include two-step alkali method, air oxidation method, and hydrogen peroxide oxidation method. [0003] (1) Patents CN101462993A, CN1299814A, etc. all adopt a technical synthesis route using carbon disulfide, alkali, hydrogen peroxide, and secondary amine as raw materials. This route has fast response and good product quality, and is currently a widely used process in the industry. The disadvantage is that inorganic salt by-products are produced, and the product needs a large amount of water to wash and desalt, and the water consumption is high; the mother liquor still needs further treatment, and the energy consumption is high. [0004] (2) Patent CN201310719619...

Claims

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Application Information

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IPC IPC(8): C07C333/32B01J31/02
CPCC07C333/32B01J31/0202B01J31/0209B01J31/0271C07B2200/13B01J35/39Y02P20/584
Inventor 王晓付顺国张旭旭许皓星王芳晓杨瑞朝袁亚楠
Owner HEBI YUANHAO CHEM CO LTD
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