Green synthesizing method for thiuram rubber vulcanizing accelerant

A technology of rubber vulcanization and thiuram, which is applied in the green synthesis of rubber vulcanization accelerators and green synthesis of thiuram disulfide) rubber accelerators, can solve the problems of a large amount of waste water and sodium sulfate waste salt, and achieve The effect of reducing the amount of waste water and inorganic waste salt, rich sources of raw materials, and low cost

Inactive Publication Date: 2018-08-14
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The main problem of this method is to use a large amount of sodium hydroxide and sul

Method used

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  • Green synthesizing method for thiuram rubber vulcanizing accelerant
  • Green synthesizing method for thiuram rubber vulcanizing accelerant
  • Green synthesizing method for thiuram rubber vulcanizing accelerant

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Dissolve 10.6g Na in 100mL water with stirring 2 CO 3 , add 22.5g 40% dimethylamine aqueous solution, control the temperature to 20°C, slowly add 7.6g CS 2 After the dropwise addition, the stirring was continued for 30 min to obtain a dithiocarbamate solution. The temperature of the solution was lowered to 5 °C, and CO was slowly introduced into the 2 , and then slowly dropwise added 5.7 g of 30% H 2 o 2 The aqueous solution was kept warm for 60 minutes after the dropwise addition was completed, and the product tetramethylthiuram disulfide was obtained by filtration, and the mother liquor was retained for future use. Concentrate the obtained mother liquor by evaporation and add 0.5gNa 2 CO 3 , repeat the above experiment, the mother solution can be applied mechanically more than 3 times. In the cycle experiment, the yield of tetramethylthiuram disulfide was >97.0%, and the product purity by liquid chromatography was >98%.

Embodiment 2

[0024] Dissolve 27.6g of K in 250mL of water with stirring 2 CO 3 And 7.2g diethylamine, control temperature is 30 ℃, slowly drop 7.6g CS 2 After the dropwise addition, the stirring was continued for 30 min to obtain a dithiocarbamate solution. The temperature of the solution was stabilized at 30 °C, and CO was slowly introduced into the 2 , and then slowly dropwise added 20 g of 10% H 2 o 2 The aqueous solution was kept warm for 60 minutes after the dropwise addition was completed, and the product tetraethylthiuram disulfide was obtained by filtration, and the mother liquor was retained for future use. The obtained mother liquor was concentrated by evaporation and supplemented with 0.8g K 2 CO 3 , repeat the above experiment, the mother solution can be applied mechanically more than 3 times. In the cycle experiment, the yield of tetraethylthiuram disulfide was >96.0%, and the product purity by liquid chromatography was >98%.

Embodiment 3

[0026] Dissolve 55.2g K in 500mL water with stirring 2 CO 3 And 10.1g dipropylamine, control the temperature at 30°C, slowly add 7.6g CS 2 After the dropwise addition, the stirring was continued for 30 min to obtain a dithiocarbamate solution. Raise the temperature of the solution to 60°C, and condense the evaporated water vapor to reflux, and slowly introduce CO 2 , and then slowly introduce air to bubble for 5 hours, and filter to obtain the product tetrapropylthiuram disulfide after the bubbling is over, and keep the mother liquor for future use. Add 50 mL of water and 0.9 g of K to the obtained mother liquor 2 CO 3 , repeat the above experiment, the mother solution can be applied mechanically more than 5 times. In the cycle experiment, the yield of tetrapropylthiuram disulfide was >95.0%, and the product purity by liquid chromatography was >97%.

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Abstract

The invention belongs to the technical field of chemistry and chemical engineering and discloses a synthesizing method of a thiuram(bi(amino thiocarbonyl)disulfide) rubber vulcanizing accelerant. According to the method, parahelium, carbon disulfide and alkali carbonate water solution are utilized as reactants to obtain dithiocar-bamate; then carbon dioxide is utilized as an acidifying agent; hydrogen peroxide, oxygen or air is utilized as an oxidizing agent to oxidize the dithiocar-bamate to generate thiuram compound and the alkali carbonate water solution. The method has the advantages thatthe carbon dioxide is utilized as the acidifying agent, the raw materials has rich source, and cost is low; the carbonate is utilized for replacing traditional sodium hydroxide as an alkaline medium,the carbonate is recycled in a reaction process, and generation of wastewater and waste inorganic salt is obviously reduced.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and in particular relates to a green synthesis method of a rubber vulcanization accelerator, in particular to a green synthesis method of a thiuram (bis(aminothiocarbonyl) disulfide) type rubber accelerator. Background technique [0002] Rubber vulcanization accelerator is an industrial raw material, mainly used in the manufacture of tires, tapes, rubber shoes and other industrial rubber products. Accelerators generate free radicals during rubber vulcanization, which can shorten the vulcanization time, lower the vulcanization temperature, improve the appearance of rubber products, improve the physical and mechanical properties of rubber products and increase the service life of rubber products. There are four main categories of commonly used accelerators: thiurams, thiazoles, guanidines and sulfenylamines, among which thiurams accelerators are one of the most widely use...

Claims

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Application Information

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IPC IPC(8): C07C333/32
CPCC07C333/32
Inventor 骆广生王凯胡佳宇
Owner TSINGHUA UNIV
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