Preparation method of rubber vulcanization accelerator-dimethyl-diphenyl thiuram disulfide

A dimethyldiphenyl disulfide thiuram and rubber vulcanization technology is applied in the field of rubber auxiliaries to achieve the effects of low production cost, simple process operation and low equipment investment

Active Publication Date: 2012-04-11
鹤壁联昊新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) Put 1,071.5g of N-methylaniline and 1,246.7g of 15% ammonia water into the condensation kettle respectively. After mixing evenly, add 0.54g of catalyst copper acetate, stir and mix for 25 minutes at a speed of 120 rpm, and slowly drop them in a closed state 875.6g of carbon disulfide, the temperature is maintained between 30-35 ° C, after 2.5 hours of reaction, continue to stir for 25 minutes.

[0014] (2) Slowly add an oxidizing agent dropwise at a temperature of 35-38° C., and the dropping amount is 1.15 times the molar amount of N-methylaniline; the oxidizing agent is a mixture of 170 g of hydrogen peroxide and 490 g of sulfuric acid. Keep the temperature between 38-40°C and continue the reaction for 2.5 hours, then separate and dry to obtain the finished rubber vulcanization accelerator dimethyl diphenyl thiuram disulfide.

[0015] The product is a light yellow powder with an initial melting point of 180.3°C, a heating loss of ≤0.10%, a product purity of 97%, an...

Embodiment 2

[0017] (1) Put 1071.5g of N-methylaniline and 1190g of 15% ammonia water into the condensation kettle respectively, after mixing evenly, add 0.32g of catalyst copper acetate, stir and mix for 20 minutes at a speed of 120 rpm, slowly add 837.5 g carbon disulfide, the temperature is kept between 25-30°C, and after 3 hours of reaction, continue to stir for 30 minutes.

[0018] (2) Slowly add an oxidizing agent dropwise at a temperature of 38-40° C., the amount of which is 1.15 times the molar amount of N-methylaniline; the oxidizing agent is a mixture of 170 g of hydrogen peroxide and 539 g of sulfuric acid. Keep the temperature between 30-35°C and continue to react for 2 hours, then separate and dry to obtain the finished rubber vulcanization accelerator dimethyl diphenyl thiuram disulfide.

[0019] The product is a light yellow powder with an initial melting point of 181.4°C, a heating loss of ≤0.10%, a product purity of 98%, and a product yield of 97.8%.

Embodiment 3

[0021] (1) Put 1,071.5g of N-methylaniline and 1,473.3g of 15% ammonia water into the condensation kettle respectively. After mixing evenly, add 0.86g of catalyst copper acetate, stir and mix for 30 minutes at a speed of 120 rpm, and slowly drop them in a closed state 1142.1g of carbon disulfide, the temperature is maintained between 35-40 ° C, after 2 hours of reaction, continue to stir for 20 minutes.

[0022] (2) Slowly add an oxidizing agent dropwise at a temperature of 30-35° C., and the dropping amount is 1.15 times the molar amount of N-methylaniline; the oxidizing agent is a mixture of 170 g of hydrogen peroxide and 735 g of sulfuric acid. Keeping the temperature at 35-38° C. to continue the reaction for 2 hours, then separate and dry to obtain the finished rubber vulcanization accelerator dimethyl diphenyl thiuram disulfide.

[0023] The product is a light yellow powder with an initial melting point of 182.3°C, a heating loss of ≤0.10%, a product purity of 97.5%, and ...

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Abstract

The invention provides a preparation method of a rubber vulcanization accelerator-dimethyl-diphenyl thiuram disulfide. In the preparation method, N-methylaniline, ammonia water with the concentration of 10-18% and carbon disulfide are taken as reactants for reacting in the presence of a catalyst-copper acetate so as to generate the dimethyl-diphenyl thiuram disulfide under the action of an oxidant, wherein, the mole ratio of the N-methylaniline to the ammonia water with the concentration of 15% to the carbon disulfide is 1: (1.05-1.3): (1.1-1.5), the catalyst accounts for 0.03-0.08% of the total mass of the N-methylaniline, and the oxidant is a mixed solution of hydrogen peroxide and sulfuric acid. The preparation method provided by the invention has the advantages that the hydrogen peroxide is taken as the oxidant, and less waste water is generated so that the preparation process is more environmentally-friendly, and in addition, a reaction can be performed at normal pressure so as to save energy; the ammonia water is taken as a solvent so as to prevent generation of waste mirabilite; the copper acetate is taken as the catalyst so as to shorten condensation reaction time; and the process flow is short, the production cost is low, and the product competitiveness can be enhanced.

Description

technical field [0001] The invention belongs to the technical field of rubber additives, and in particular relates to a preparation method of a rubber vulcanization accelerator dimethyl diphenyl thiuram disulfide. Background technique [0002] In recent years, with the rapid development of the rubber processing industry, the rapid development of the domestic automobile industry and communication industry has driven the rapid growth of the rubber processing industry and provided unprecedented good opportunities for the development of the rubber additives industry. Since my country's accession to the WTO, although the production of rubber accelerator products in China has been greatly improved, there is still a lot of room for development in terms of product intrinsic quality and "green" environmental protection technology. [0003] Thiuram is a kind of highly active accelerator, and its disulfide and polysulfide are also vulcanizing agents for sulfur-free vulcanization system...

Claims

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Application Information

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IPC IPC(8): C07C333/32
Inventor 陈建军张智亮
Owner 鹤壁联昊新材料有限公司
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