Preparation of rubber vulcanization accelerator tetrabenzylthiuram disulfide

A technology of tetrabenzylthiuram disulfide and rubber vulcanization, which is applied in the direction of organic chemistry, can solve the problems of difficult-to-clean and “green” production, does not meet the requirements of national environmental protection policies and energy-saving production, and has low production efficiency. Less investment, superior vulcanization performance, and short production cycle

Active Publication Date: 2009-06-24
WILLING NEW MATERIALS TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For the production technology of rubber vulcanization accelerator tetrabenzylthiuram disulfide (TBzTD), solvent methods such as methanol, ethanol, and isopropanol are commonly used in China. In addition to emitting a large amount of toxic gases of organic solvents during production, these processes; What's more serious is that there are major production safety hazards in the production process, because in the existing production process, the reaction process in the reactor is carried out under pressure, and each reaction in the reaction All substances exist in the gaseous state, and they are all flammable and explosive substances, which may explode if you are not careful, causing loss of personnel and property; at the same time, the process energy consumption of the prior art is high, and the reaction produces A large amount of waste water and waste gas bring great difficulties to environmental protection, making it difficult to achieve "clean and green" production, which does not

Method used

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  • Preparation of rubber vulcanization accelerator tetrabenzylthiuram disulfide

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Experimental program
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Effect test

Embodiment 1

[0030] The raw materials used in this embodiment and their mol ratios are:

[0031] Dibenzylamine: carbon disulfide: sodium hydroxide: hydrogen peroxide: sulfuric acid = 1: 1.2: 1.1: 0.53: 0.3;

[0032] The specific process is: under normal pressure, add dibenzylamine and sodium hydroxide sequentially into the reaction kettle filled with purified water under stirring; then cool down to 24°C, start to add carbon disulfide liquid dropwise, and the dropping time is 2.5 Hours; after the dropwise addition, continue to stir for 0.5 hours; then, at 60°C, add hydrogen peroxide dropwise to the reactant for oxidation reaction, the reaction time is 3.5 hours, when the oxidation reaction is almost finished, add sulfuric acid to adjust the reaction The pH value of the liquid is 6.8, that is, the reaction is completed; after that, the reaction is kept for 1 hour, and the solid-liquid separation is carried out, and the solid is dried, crushed, sieved, and packaged to obtain the product. The...

Embodiment 2

[0034] The raw materials used in this embodiment and their mol ratios are:

[0035] Dibenzylamine: carbon disulfide: sodium hydroxide: hydrogen peroxide: sulfuric acid = 1: 1.25: 1.16: 0.56: 0.33;

[0036]The specific process is: under normal pressure, add dibenzylamine and sodium hydroxide sequentially into the reaction kettle filled with purified water under stirring; then cool down to 26 ° C, start to add carbon disulfide liquid, and the dropping time is 3 Hours; after the dropwise addition, continue to stir for 0.5 hours; then, at 62°C, add hydrogen peroxide dropwise to the reactant for oxidation reaction, the reaction time is 3.2 hours, when the oxidation reaction is about to end, add sulfuric acid to adjust the reaction The pH value of the liquid is 7.1, that is, the reaction is completed; after that, the reaction is kept for 1 hour, and the solid-liquid separation is carried out, and the solid is dried, crushed, sieved, and packaged to obtain the product. The color of ...

Embodiment 3

[0038] The raw materials used in this embodiment and their mol ratios are:

[0039] Dibenzylamine: carbon disulfide: sodium hydroxide: hydrogen peroxide: sulfuric acid = 1: 1.3: 1.2: 0.6: 0.35;

[0040] The specific process is as follows: under normal pressure, add dibenzylamine and sodium hydroxide sequentially into the reaction kettle filled with purified water under stirring; then cool down to 28°C, start to add carbon disulfide liquid dropwise, and the dropping time is 3.8 Hours; after the dropwise addition, continue to stir for 0.5 hours; then, at 63°C, add hydrogen peroxide dropwise to the reactant for oxidation reaction, the reaction time is 3.0 hours, when the oxidation reaction is about to end, add sulfuric acid to adjust the reaction The pH value of the liquid is 7.4, that is, the reaction is completed; after that, the reaction is kept for 1 hour, and the solid-liquid separation is carried out, and the solid is dried, crushed, sieved, and packaged to obtain the produ...

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Abstract

The invention relates to a method for preparing a thiofide of tetraethylthiuram disulfide. The method uses raw materials with the mol ratio as follows: the mol ratio of dibenzyl amine, carbon bisulfide, sodium hydroxide, hydrogen peroxide and sulphuric acid is 1:1-1.30:1.0-1.2:0.5-0.6:0.28-0.35mol. The method comprises the technical process as follows: under normal pressure, the dibenzyl amine and the sodium hydroxide are sequentially added into a reaction kettle which contains purified water under the state of being stirred; subsequently, the temperature is reduced to 20 DEG C to 30 DEG C, liquid carbon bisulfide is dropwise added for 2 to 3 hours; after dropwise adding, reactant continues to be stirred for 0.5 hour; then, at the temperature of 58 DEG C to 63 DEG C, the hydrogen peroxide is dropwise added into the reactant for oxidation reaction which lasts 3 to 4 hours; when the oxidation reaction is going to finish, the sulphuric acid is added to adjust the pH value of reaction solution to be within the range of 6.5-7.5, and the reaction is finished; then the reaction is taken for 1 hour again by heat preservation for solid-liquid separation, and the solid is dried, crushed, filtered and packed to obtain a product. The method can improve the quality, the yield and the performance of the product effectively, reduce the potential safety hazard during the production process greatly, save energy, reduce consumption, reduce the waste water and exhaust emission during the production process and meet the national relative policy of environmental protection.

Description

1. Technical field: [0001] The invention relates to a preparation method of a rubber vulcanization accelerator, in particular to a preparation method of a rubber vulcanization accelerator tetrabenzylthiuram disulfide. 2. Background technology: [0002] In recent years, with the rapid development of the rubber processing industry, domestic automobile industry and communication industry, the rapid growth of the rubber processing industry has been driven, which has 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, compared with foreign developed countries, 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 contai...

Claims

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Application Information

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IPC IPC(8): C07C333/32C08K5/40C08L21/00
Inventor 郭同新岳法亮王平生徐治松宋风朝屈军伟史宗浩
Owner WILLING NEW MATERIALS TECH CO LTD
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