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Method for continuous purification of rubber vulcanization accelerator m by applying solvent

A vulcanization accelerator and rubber purification technology, which is applied in the field of purification of rubber vulcanization accelerator 2-mercaptobenzothiazole (accelerator M or MBT), can solve the problems of not reducing M loss, accelerator M loss, etc. Reach the effect of reducing energy consumption, reducing the total amount, and reducing the amount of distillation

Active Publication Date: 2017-04-05
山东戴瑞克新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent uses toluene to purify the accelerator M. In addition to the good solubility of the by-products of M, toluene also has a certain solubility to M, and the solubility is 0.8g / 100mL~1.3g / 100mL. When the accelerator M is purified, a part of the accelerator M enters the toluene, resulting in the loss of the accelerator M
Nowadays, no one recovers this part of M dissolved in toluene, and there is no effective method to reduce the loss of M. If the loss of accelerator M in the process of toluene purification can be avoided, the yield of accelerator M will be greatly improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 800L of the last batch of toluene washing liquid from the washing liquid collection tank and put it into the extraction kettle, take 700kg of the accelerator M crude product into the extraction kettle, filter after stirring for 1h, and the filtered filtrate enters the toluene mother liquor tank, and the filtrate is first cooled to 20- Stand at 25°C to precipitate the dissolved accelerator M, and then recover the accelerator M by filtration. The toluene filtrate is distilled to obtain fresh recovered toluene, which is used for washing the next batch of accelerator M, and for the crude M filter cake. The fresh toluene recovered from the previous batch is washed, and the temperature of the washed toluene washing liquid is controlled at 20-30°C. The filtrate enters the washing liquid collection tank and is used for the purification and removal of impurities of the next batch of accelerator M crude product. The final filter cake was directly dried to obtain 605.5 kg of a...

Embodiment 2

[0030] Take 2500L of the last batch of toluene washing liquid from the washing liquid collection tank and put it into the extraction kettle, take 700kg of accelerator M crude product into the extraction kettle, filter after stirring for 3h, and enter the toluene mother liquor tank after filtering, and the filtrate is first cooled to 10- Accelerator M is recovered by crystallization at 15°C, and the remaining filtrate is distilled to obtain freshly recovered toluene, which is used for washing of the next batch of accelerator M. The crude product filter cake of M is washed with fresh toluene recovered from the previous batch. The temperature of the final toluene washing liquid is controlled at 10-15 °C, and the filtrate enters the washing liquid collection tank for the purification and removal of impurities in the next batch of accelerator M crude product. The washed filter cake is directly dried to obtain the pure accelerator M product. 607.6kg, the purity of accelerator M detec...

Embodiment 3

[0032] Take 3300L of the last batch of toluene washing liquid from the washing liquid collection tank and put it into the extraction kettle, take 700kg of accelerator M crude product into the extraction kettle, filter after stirring for 6h, and enter the toluene mother liquor tank after filtering, and the filtrate is first cooled to 0- Accelerator M was recovered by crystallization at 5°C, and the remaining filtrate was distilled to obtain fresh recovered toluene, which was used for washing the next batch of accelerator M. The filter cake was washed with fresh toluene recovered from the previous batch, and the washed toluene The temperature of the toluene washing liquid is controlled at 0-5°C, and the filtrate enters the washing liquid collection tank for the purification and removal of impurities of the next batch of accelerator M crude product. The washed filter cake is directly dried to obtain 612.5 kg of pure accelerator M. The purity of accelerator M detected by HPLC was 9...

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PUM

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Abstract

The invention discloses a method for continuously purifying a rubber vulcanization accelerator M by using a solvent, which comprises the following steps: adding a vulcanization accelerator M crude product into a toluene washing solution for perform purification, filtering, sending the filtrate into a toluene mother solution tank to cool and recover the accelerator M, distilling the residual mother solution to recover the toluene, washing the filter cake with the recovered toluene, and drying to obtain the rubber vulcanization accelerator M pure product, wherein the toluene washing solution cooled filtrate formed by washing the filter cake enters a washing solution collecting tank for extracting and purifying the vulcanization accelerator M crude product. The method is simple in process, and the toluene is recoverable, thereby reducing the total amount of the toluene mother solution, lowering the energy consumption and enhancing the yield. The method has the advantages of low cost and small environmental pollution, provides technical supports for continuous production of the accelerator M, has favorable economic and environmental benefits, and conforms to the requirements for national clean production.

Description

technical field [0001] The invention relates to a purification method of a rubber vulcanization accelerator 2-mercaptobenzothiazole (accelerator M or MBT), and belongs to the technical field of rubber vulcanization accelerator M preparation. [0002] technical background [0003] Rubber vulcanization accelerator M (chemical name 2-mercaptobenzothiazole) is an ultra-speed accelerator for natural rubber, which also has the effect of a plasticizer. Its vulcanization critical temperature is low, and it is easy to cause early vulcanization of the rubber. It can be used alone Or used in combination with other accelerators, suitable for tires, rubber shoes, and industrial rubber products. [0004] Nowadays, acid-base method and solvent method are commonly used in the production of accelerator M. The production of accelerator M by acid-base method will produce high-salt organic wastewater, which is difficult and costly to treat, and is gradually replaced by solvent method. Patent CN...

Claims

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Application Information

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IPC IPC(8): C07D277/72
CPCC07D277/72
Inventor 许思俊董瑞国王兴军李世梅郑崇纳马亚敏李宪索刘红
Owner 山东戴瑞克新材料有限公司
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