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Purification method of rubber vulcanization accelerator MBT (2-mercaptobenzthiazole)

A purification method and rubber vulcanization technology, applied in the direction of organic chemistry, etc., can solve the problems of unavoidable salty waste water, high energy consumption of solvent recovery, and high environmental protection pressure, and achieve low recovery energy consumption, short melting range and simple process Effect

Inactive Publication Date: 2012-12-19
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method adopts the solvent extraction method for refining, it still cannot avoid the generation of saline wastewater, and the pressure on environmental protection is great.
Patent CN 1300123C uses toluene as the extractant to directly extract the crude MBT, no waste water is generated in the process, but the solvent recovery consumes a lot of energy, and the operation process is harmful to the human body and pollutes the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Weigh 500g of crude product MBT, with a content of 90%, put it into a 1L sealed kettle after crushing. After vacuuming, flush into nitrogen protection. Put 1000g of carbon disulfide into the sealed kettle with a peristaltic pump. After the sealing is completed, start stirring, raise the temperature to 120°C and maintain it for 120min. Slowly lower the temperature to room temperature at a rate of 1 °C / / min through jacket cooling. After filtering, washing, and drying, 440 g of the product was obtained. The mass content of the 2-mercaptobenzothiazole accelerator was 98.5%, and the melting point was 171.3° C. After distillation of the mother liquor, 960 g of carbon disulfide was obtained.

Embodiment 2

[0013] Weigh 500g of crude product MBT, with a content of 85%, put it into a 1L sealed kettle after crushing. After vacuuming, flush into nitrogen protection. Put 1500g of carbon disulfide into the sealed kettle with a peristaltic pump. After the sealing was completed, the stirring was started, and the temperature was raised to 140° C. and maintained for 60 minutes. Slowly lower the temperature to room temperature at a rate of 2°C / / min through jacket cooling. After filtering, washing and drying, 421g of the product was obtained, the mass content of the 2-mercaptobenzothiazole accelerator was 99.1%, and the melting point was 173.1°C. After distillation of the mother liquor, 1447g of carbon disulfide was obtained.

Embodiment 3

[0015] Weigh 500g of crude product MBT, with a content of 80%, put it into a 1L sealed kettle after crushing. After vacuuming, flush into nitrogen protection. Put 2500g of carbon disulfide into the sealed kettle with a peristaltic pump. After the sealing is completed, start stirring, raise the temperature to 180°C and maintain it for 30min. Slowly lower the temperature to room temperature at a rate of 3°C / / min through jacket cooling. After filtering, washing, and drying, 402 g of the product was obtained. The mass content of the 2-mercaptobenzothiazole accelerator was 99.5%, and the melting point was 177.1° C. Distillation of the mother liquor yielded 2425g of carbon disulfide.

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Abstract

The invention provides a purification method of a rubber vulcanization accelerator MBT (2-mercaptobenzthiazole), which comprises the following steps: pulverizing a crude product MBT synthesized under high pressure, and putting the pulverized MBT in a high-pressure kettle, wherein the mass percent of MBT in the crude product MBT is 80-90%; sealing the high-pressure kettle, vacuumizing, and charging a nitrogen protective atmosphere; pressing carbon bisulfide which is 2-5 times by weight of the crude product MBT into the reaction kettle; after sealing, starting stirring, heating to 120-180 DEG C, and keeping the temperature for 0.5-2 hours; cooling the reaction kettle to room temperature at the rate of 0.5-3 DEG C / min in a jacket cooling mode, filtering, washing, and drying to obtain the vulcanization accelerator MBT of which the content is higher than 98%; and distilling to recover the filtered mother liquor which can be circularly used in the reaction stage, wherein the recovery rate is up to higher than 96%. The method has the advantage of simple process, and the purity of the prepared high-content MBT is up to higher than 98%; no waste water is generated in the refinement process; and the extractant carbon bisulfide used as the reaction raw material has the advantage of low energy consumption for recovery, and can be returned to the reaction stage for circular use.

Description

technical field [0001] The invention relates to a new method for purifying rubber vulcanization accelerator 2-mercaptobenzothiazole (MBT), which belongs to the technical field of rubber vulcanization accelerator MBT purification. Background technique [0002] MBT (2-Mercaptobenzothiazole) is an essential accelerator in the rubber industry at present. At present, the domestic production process is the aniline method of accelerator MBT. The yield of the product obtained by this process is low, only about 85%, and the qualified product can only be obtained after refining. At present, the refining processes mainly include acid-base method and solvent extraction method. The acid-base method is simple and easy to operate, but it generates a lot of waste water and pollutes the environment. Literature (Northwest University for Nationalities Journal, 21,4, P8-11) reported the method of refining MBT. The synthetic crude product M is alkali-dissolved at a certain pH value, and afte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/72
Inventor 安静
Owner KEMAI CHEM
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