Preparation method of rubber vulcanizing accelerator TBBS

A technology of rubber vulcanization and accelerator, applied in the field of preparation of rubber additives, can solve the problems of not being able to fundamentally solve the problem of waste water, increasing cost, not mentioning the recovery of decoking agent, etc., so as to reduce process safety risks and environmental problems. The effect of low pollution and low cost

Inactive Publication Date: 2015-05-13
内蒙古科迈化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method also uses sodium hypochlorite as an oxidant, which cannot fundamentally solve the problem of wastewater in the TBBS production process
At the same time, a large amount of decoking agent is introduced, and the recovery of the decoking agent is not mentioned, resulting in an increase in cost

Method used

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  • Preparation method of rubber vulcanizing accelerator TBBS
  • Preparation method of rubber vulcanizing accelerator TBBS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Crude product of synthetic accelerator MBT: 400 kg of aniline, 137.6 kg of molten sulfur obtained from the Claus process, and 326.9 kg of carbon disulfide were respectively put into an autoclave. The reaction temperature is 250°C, the final pressure is 9.05MPa, and the crude product of rubber accelerator MBT is synthesized after reaction for 5 hours. The crude MBT content is more than 90%.

[0020] (2) utilize crude product MBT to prepare accelerator TBBS:

[0021] A. Dispersion: Put 3.6t of water into the oxidation kettle and start stirring. The crude product M was transported to the oxidation kettle, stirred for 0.5 h, and the temperature was lowered to obtain the crude product MBT with a smaller particle size. Water was vented from the reaction kettle.

[0022] B. Oxidation: Add 5231kg ​​of 30% tert-butylamine into the oxidation kettle. After mixing evenly, add hydrogen peroxide oxidant dropwise, the concentration of hydrogen peroxide is 5%. The oxidation te...

Embodiment 2

[0025] (1) Crude product of synthetic accelerator MBT: 400 kg of aniline, 165.2 kg of molten sulfur obtained from the Claus process, and 490 kg of carbon disulfide were respectively put into an autoclave. The reaction temperature is 260°C, the final pressure is 11MPa, and the crude product of rubber accelerator MBT is synthesized after reaction for 3 hours. The crude MBT content is more than 90%.

[0026] (2) utilize crude product MBT to prepare accelerator TBBS:

[0027] A. Dispersion: Put 7.2t of water into the oxidation kettle and start stirring. The crude product M was transported to the oxidation kettle, stirred for 1 hour, and the temperature was lowered to obtain the crude product MBT with a smaller particle size. Water was vented from the reaction kettle.

[0028] B. Oxidation: Add 6277kg of 50% tert-butylamine into the oxidation kettle. After mixing evenly, add hydrogen peroxide oxidant dropwise, the concentration of hydrogen peroxide is 10%. The oxidation temper...

Embodiment 3

[0031] (1) Crude product of synthetic accelerator MBT: 400 kg of aniline, 151.4 kg of molten sulfur obtained from the Claus process, and 393 kg of carbon disulfide were respectively put into an autoclave. The reaction temperature is 280°C, the final pressure is 9.8MPa, and the crude product of rubber accelerator MBT is synthesized after reaction for 4 hours. The crude MBT content is more than 90%.

[0032] (2) utilize crude product MBT to prepare accelerator TBBS:

[0033] A. Dispersion: Put 5t of water into the oxidation kettle and start stirring. The crude product M was transported to the oxidation kettle, stirred for 2 hours, and the temperature was lowered to obtain the crude product MBT with a smaller particle size. Water was vented from the reaction kettle.

[0034] B. Oxidation: Add 5492kg of 40% tert-butylamine into the oxidation kettle. After mixing evenly, add hydrogen peroxide oxidant dropwise, the concentration of hydrogen peroxide is 7%. The oxidation tempera...

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Abstract

The invention relates to a preparation method of a rubber vulcanizing accelerator TBBS. The preparation method comprises the following steps: (1), synthesizing a crude product MBT, to be specific, directly adding molten sulfur as raw material sulfur, and eliminating the procedure of dissolving sulfur by carbon disulfide so as to reduce the potential risks of production; (2), synthesizing the accelerant TBBS by the crude product MBT, to be specific, adding the molten crude MBT in an oxidization kettle which contains water and starts stirring, after stirring the molten crude MBT and the water, cooling, and draining; adding a tert-butylamine water solution into the oxidization kettle, after uniformly stirring, adding hydrogen peroxide so as to perform oxidation synthesis, dripping sodium hypochlorite in the later period, and determining the end by using ammonium sulfate and a potassium iodide solution; performing suction filtration after reaction, washing filter cakes by the tert-butylamine water solution, washing the washed filter cakes with water till being neutral, and drying the filter cakes so as to obtain the qualified vulcanizing accelerator TBBS. According to the preparation method disclosed by the invention, the crude MBT is used as raw materials to directly synthesize the accelerant TBBS, the environment-friendly hydrogen peroxide is used as an oxidizing agent, the refining process of MBT is eliminated, waste water containing salt is generated, and little pollution to the environment is caused.

Description

technical field [0001] The invention belongs to the preparation method of rubber additives, in particular to a method for producing rubber vulcanization accelerator TBBS from crude MBT. Background technique [0002] Accelerator N-tert-butylbenzothiazole sulfenamide (TBBS or NS) is a sulfenamide aftereffect rubber vulcanization accelerator with excellent comprehensive performance. It is the main product used in developed countries and regions such as the United States and Western Europe. Auxiliary varieties, its consumption is about 60% of the total consumption of sulfenamide accelerators, with slight discoloration and pollution, and has multiple functions such as anti-scorch, acceleration, and activation. Since NS has a primary amine structure, it will not produce carcinogens such as nitrosamines, and is known as a standard accelerator. Excellent scorch resistance, safe processing and short vulcanization time, it is an essential accelerator in the rubber industry at present...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 田少华李全成鞠光蔡全会张云成魏伟涛李霞安静
Owner 内蒙古科迈化工有限公司
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