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Preparation method of rubber vulcanization accelerator tetra(isobutyl)thioperoxydicarbamic acid (TiBTD)

A technology of diisobutyl disulfide, rubber vulcanization, applied in organic chemistry and other directions, can solve the problems of non-compliance with national environmental protection policy production requirements, difficult to clean "green" production, difficult to meet high-end requirements, etc., to achieve excellent vulcanization performance , The effect of short curing time and long scorch time

Active Publication Date: 2011-01-19
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The production technology of rubber vulcanization accelerator diisobutylthiuram disulfide (TiBTD) is generally produced by acid-base method in China. In addition to producing a large amount of inorganic salt waste water in these processes, the more serious problem is that The use of a large amount of highly corrosive raw materials such as acids and alkalis leads to high hidden dangers in production safety and high energy consumption, which brings great difficulties to environmental protection and makes it difficult to achieve "clean" and "green" production. It does not comply with national environmental protection policies and regulations Production Requirements for Energy Saving and Emission Reduction
At the same time, in some existing preparation methods, the yield of the reaction is low, and the obtained product has a low melting point, low purity, and yellow appearance, which is difficult to meet the high-end requirements of the domestic and foreign sales markets.

Method used

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  • Preparation method of rubber vulcanization accelerator tetra(isobutyl)thioperoxydicarbamic acid (TiBTD)
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Embodiment 1

[0025] In this embodiment, the raw materials used are respectively diisobutylamine, carbon disulfide, hydrogen peroxide and sodium dodecylsulfonate, and the stoichiometric molar ratio is: diisobutylamine: carbon disulfide: hydrogen peroxide: dodecyl Sodium sulfonate=1:1.26:0.49:0.015;

[0026] The process is as follows: into the 2000L enamel reaction kettle, add the specified amount of diisobutylamine, alcohols or water, and sodium dodecylsulfonate in sequence under stirring; turn on the cooling water, cool down to 42°C, and start adding dropwise Accurately metered carbon disulfide liquid, the control time is 6 hours. After the dropwise addition, the pH value of the reaction solution was measured to be 8. After the pH value was stabilized, the temperature was controlled at 58° C., and hydrogen peroxide was started to be added dropwise, and the oxidation reaction was carried out for 5 hours. After the oxidation is finished, heat the reaction for another 1 hour, carry out solid...

Embodiment 2

[0028] In this embodiment, the raw materials used are respectively diisobutylamine, carbon disulfide, hydrogen peroxide and sodium dodecylsulfonate, and the stoichiometric molar ratio is: diisobutylamine: carbon disulfide: hydrogen peroxide: dodecyl Sodium sulfonate=1:1.27:0.51:0.017;

[0029] The process is as follows: add a specified amount of diisobutylamine, alcohols or water, and sodium dodecylsulfonate to the 2000L enamel reaction kettle in a stirring state; turn on the cooling water, cool down to 44°C, and start adding dropwise Accurately metered carbon disulfide liquid, the control time is 6.5 hours. After the dropwise addition, the pH value of the reaction solution was measured to 8.5. After the pH value was stabilized, the temperature was controlled at 60° C., and hydrogen peroxide was added dropwise, and the oxidation reaction was carried out for 5.5 hours. After the oxidation is finished, heat the reaction for another 1 hour, carry out solid-liquid separation, dis...

Embodiment 3

[0031] In this embodiment, the raw materials used are respectively diisobutylamine, carbon disulfide, hydrogen peroxide and sodium dodecylsulfonate, and the stoichiometric molar ratio is: diisobutylamine: carbon disulfide: hydrogen peroxide: dodecyl Sodium sulfonate=1:1.28:0.53:0.019;

[0032] The process is as follows: add a specified amount of diisobutylamine, alcohols or water, and sodium dodecylsulfonate to the 2000L enamel reaction kettle in a stirring state; turn on the cooling water, cool down to 46°C, and start adding dropwise Accurately metered carbon disulfide liquid, the control time is 7 hours. After the dropwise addition, the pH value of the reaction solution was measured to be 9. After the pH value was stabilized, the temperature was controlled at 62° C., and hydrogen peroxide was added dropwise, and the oxidation reaction was carried out for 6 hours. After the oxidation is completed, heat the reaction for 1 hour, separate the solid and liquid, discard the liqui...

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Abstract

The invention provides a preparation method of a rubber vulcanization accelerator tetra(isobutyl)thioperoxydicarbamic acid (TiBTD). In the method, the rubber vulcanization accelerator TiBTD comprises 1 portion of diisobutylamine, 1.26-1.28 portions of carbon bisulfide, 0.49-0.53 portion of oxidant and 0.015-0.019 portion of anionic surfactant. The method comprises the following steps: orderly adding specified amounts of di-iso-butylmanice, alcohols or water, and anionic surfactant into a 2000L enamel reaction kettle while stirring; starting cooling water, cooling to 42-46 DEG C, and dropwise adding accurately metered carbon bisulfide liquid for 6-7 hours; after dropwise adding finishes, measuring the pH value of the reactant liquor to 8-9, and after the pH value becomes stable, and starting to dropwise add oxidant at 58-62 DEG C to carry out oxidation reaction for 5-6 hours; and after the oxidation finishes, keeping the temperature to react for 1 hour, carrying out solid-liquid separation, discarding the liquid, drying the solid, pulverizing, screening and packaging. The oxidant is hydrogen peroxide or sodium hypochlorite, and the anionic surfactant is sodium dodecylsulfate.

Description

technical field [0001] The invention relates to a rubber vulcanization accelerator, especially a production method of the rubber vulcanization accelerator diisobutylthiuram 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 joining the WTO, although the production of rubber accelerator products in my country has been greatly improved, compared with developed countries in the world, there is still a big gap in product intrinsic quality and "green" environmental protection technology. China's auxiliaries industry will expand the market share of green and non-toxic auxiliaries, and greatly reduce the sulfenamide accelerators containing nitrosamines and producing...

Claims

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Application Information

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IPC IPC(8): C07C333/32C08K5/40
Inventor 王志强郭同新王平生岳法亮史宗浩徐治松王飞
Owner WILLING NEW MATERIALS TECH CO LTD
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