Process for producing rubber vulcanization accelerant penta-methylene thiuram tetrasulfide

A technology of double-penta-tetrasulfide and rubber vulcanization, used in organic chemistry and other directions, can solve problems such as non-compliance with national environmental protection policies and energy-saving production requirements, products that are difficult to meet high-end requirements, and difficult to clean and green" production, and achieve excellent vulcanization performance. , The effect of reducing the pollution of the three wastes and shortening the vulcanization time

Active Publication Date: 2009-05-13
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] The production technology of rubber vulcanization accelerator bispentamethylenethiuram tetrasulfide (DPTT) is generally produced by oxygen method or disulfide dichloride as raw material in China. These processes remove a large amount of organic pollutants during production. Excluding the toxic gas of the solvent; more seriously, because the reaction is carried out under pressure, the reactant in the reactor is a gaseous substance, which is very easy to explode during the reaction process, so there is a great safety hazard in the production process At

Method used

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  • Process for producing rubber vulcanization accelerant penta-methylene thiuram tetrasulfide

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Effect test

Embodiment 1

[0029] The raw materials used in the preparation method of the rubber vulcanization accelerator of the present embodiment dipentamethylene thiuram tetrasulfide (DPTT) and their mol ratio are:

[0030] Hexahydropyridine: carbon disulfide: sulfur: hydrogen peroxide = 1: 1.1: 2.0: 0.5;

[0031] The specific process is: under normal pressure, add hexahydropyridine and sulfur to the reaction kettle filled with water in a stirring state, after the addition is completed, control the temperature to 23 ° C, then add carbon disulfide liquid dropwise, and control the dropwise addition After 2 hours, measure the pH value of the reaction solution after the dropwise addition. After the pH value of the reaction solution is stabilized to 6.8, control the temperature of the reaction solution to 30°C, and start to add hydrogen peroxide to carry out the oxidation reaction. The oxidation reaction time is 3 hours ; After the oxidation reaction is finished, heat the reaction for 1 hour, then separa...

Embodiment 2

[0033] The raw materials used in the preparation method of the rubber vulcanization accelerator of the present embodiment dipentamethylene thiuram tetrasulfide (DPTT) and their mol ratio are:

[0034] Hexahydropyridine: carbon disulfide: sulfur: hydrogen peroxide = 1: 1.2: 2.3: 0.6;

[0035] The specific process is as follows: under normal pressure, add hexahydropyridine and sulfur into the reaction kettle filled with water in a stirring state, control the temperature at 25°C after the addition, and then add carbon disulfide liquid dropwise, and control the dropwise addition The time is 2.6 hours. After the dropwise addition, measure the pH value of the reaction solution. After the pH value of the reaction solution is stabilized to 7.0, control the temperature of the reaction solution to 35°C, and start to add hydrogen peroxide to carry out the oxidation reaction. The oxidation reaction time is 3.5 hours ; After the oxidation reaction is finished, heat the reaction for 1 hour,...

Embodiment 3

[0037] The raw materials used in the preparation method of the rubber vulcanization accelerator of the present embodiment dipentamethylene thiuram tetrasulfide (DPTT) and their mol ratio are:

[0038] Hexahydropyridine: carbon disulfide: sulfur: hydrogen peroxide = 1: 1.3: 2.5: 0.6;

[0039]The specific process is: under normal pressure, add hexahydropyridine and sulfur to the reaction kettle filled with water in a stirring state, after the addition is completed, control the temperature at 28°C, then add carbon disulfide liquid dropwise, and control the dropwise addition The time is 2.8 hours. After the dropwise addition, measure the pH value of the reaction solution. After the pH value of the reaction solution is stabilized to 7.3, control the temperature of the reaction solution to 40°C, and start to add hydrogen peroxide to carry out the oxidation reaction. The oxidation reaction time is 4 hours. ; After the oxidation reaction is finished, heat the reaction for 1 hour, then...

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Abstract

The invention relates to a method for preparing a rubber vulcanization accelerator, namely dipentamethylenethiuram tetrasulfide, wherein the method takes water as a solvent; raw materials together with the molar ratio thereof used in the method are: the molar ratio of piperidine to carbon disulfide to sulfur to hydrogen peroxide is 1:1-1.3:1.8-2.5:0.4-0.7; the method comprises the following concrete technological processes: under normal pressure, the piperidine and the sulfur are sequentially added to a reaction kettle holding water in a stirring state; after adding is over, temperature is controlled in a range between 20 and 30 DEG C; then carbon disulfide liquid is dripped, and the dripping time is controlled to be 2 to 3 hours; after dripping is over, the pH value of a reaction solution is measured; after the pH value of the reaction solution is steady in the range between 6.5 and 7.5, the temperature of the reaction solution is controlled between 30 and 40 DEG C; hydrogen peroxide is dipped so as to perform oxidation reaction for 3 to 4 hours; after the oxidation reaction is over, the reaction solution is thermally insulated and reacts for 1 hour; then solid-liquid separation is performed; and an obtained solid is dried, ground, sieved and packaged so as to obtain a product. The method has the advantages that the method is short in production period, high in safety factor, nearly free from exhaust emission, high in product melting point, good in product appearance, high in yield, obviously superior to other preparation methods, low in comprehensive cost and capable of improving product quality, saving energy, reducing consumption and reducing three-waste pollution.

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 bispentamethylenethiuram tetrasulfide. 2. Background technology: [0002] In recent years, with the rapid development of domestic automobile industry and communication industry, etc., it has driven the rapid growth of rubber processing industry and provided unprecedented good opportunities for the development of rubber additives industry. Rubber vulcanization accelerator Dipentamethylenethiuram tetrasulfide (DPTT) is used as an accelerator for natural rubber, synthetic rubber and latex. Because it can decompose free sulfur when heated, it can also be used as a vulcanizing agent. When used as a vulcanizing agent, it is relatively safe at operating temperature, and the vulcanized rubber has excellent heat resistance and aging resistance. This product can be used as the main accelerator in ch...

Claims

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Application Information

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IPC IPC(8): C07C333/32C08K5/40C08L21/00
Inventor 岳法亮徐治松宋风朝屈军伟史宗浩段春菊赵鹏展
Owner WILLING NEW MATERIALS TECH CO LTD
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