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Method for preparing 2-mercaptobenzothiazole

A technology of mercaptobenzothiazole and aniline, which is applied in the field of rubber vulcanization accelerator production, can solve the problem of low yield and achieve the effect of reducing the generation of asphalt-like waste

Active Publication Date: 2012-07-25
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above two patents use the method of crystallization or extraction to purify the crude MBT obtained from the reaction to obtain the product MBT, which eliminates operations such as alkali dissolution, oxidation, and acidification, and does not generate waste water and waste gas. The yield is low, and the amount of bitumen-like waste generated accordingly has not been reduced, and the problems existing in the existing process have not been completely solved

Method used

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  • Method for preparing 2-mercaptobenzothiazole
  • Method for preparing 2-mercaptobenzothiazole
  • Method for preparing 2-mercaptobenzothiazole

Examples

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Embodiment 1

[0031](1) in the reactor of 1.2L, add 400g aniline, 344g sulfur and 360g carbon disulfide are totally 1106g, (reactant proportioning is aniline: sulfur: carbon disulfide is 1: 2.5: 1.1) at 250~260 ℃, react 90min, this When the reaction is 9.1MPa, the reaction is terminated to obtain a crude product melt. Using the self-pressure generated by the reaction, the crude MBT melt is pressed into a 3L crystallizer equipped with 1200g of carbon disulfide at 140°C. The maximum temperature of the mixed solution after mixing is 165 °C. ℃, lower the temperature at a cooling rate of 0.5℃ / min, start to discharge hydrogen sulfide when the temperature in the crystallizer is 90℃, control the discharge time of hydrogen sulfide to 30min, the temperature of the mixture drops to 18℃, filter to obtain MBT filter cake and carbon disulfide mother liquor, use 600g The filter cake was washed twice with carbon disulfide, and dried under vacuum at room temperature to obtain 542 g of MBT product with a puri...

Embodiment 2

[0039] (1) in the reactor of 0.6L, add 212g aniline, 117g sulfur and 260g carbon disulfide total 589g, (reactant proportioning is aniline: sulfur: carbon disulfide is 1: 1.6: 1.5) react 120min at 240~250 ℃, stop reaction, and the reaction pressure was 6.9 MPa at this time. Using the self pressure generated by the reaction, the crude MBT melt was pressed into a 2L crystallizer containing 1000g of carbon disulfide at 130°C. The maximum temperature of the mixed liquid after mixing was 153.5°C, and the temperature was lowered at a cooling rate of 0.5°C to 1°C / min. When the temperature of the mixture in the crystallizer dropped to 70°C, hydrogen sulfide began to be discharged, the time for discharging hydrogen sulfide was controlled at 30 minutes, the temperature of the mixture was lowered to 20°C, and the MBT filter cake and carbon disulfide mother liquor were obtained by filtration, and the filter cake was washed twice with 500 g of carbon disulfide. It was dried under vacuum to ...

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Abstract

The invention discloses a method for preparing 2-mercaptobenzothiazole, which comprises the steps of: adding carbon disulfide, aniline and sulfur into a reaction kettle; and heating the mixture, finishing a reaction under the reaction pressure of 6.8 to 9.5MPa to obtain a crude product, namely a melt, pressing the melt into a crystallizer loaded with carbon disulfide, controlling the initial temperature of the crystallization, reducing the temperature, beginning to discharge hydrogen sulfide when the material temperature in the crystallizer is reduced to be between 70 and 100 DEG C, controlling the discharge time of hydrogen sulfide to be between 20 and 60min, cooling the obtained product to be between 15 and 20 DEG C, filtering the obtained product to obtain a filter cake and carbon disulfide mother liquor, washing the filter cake for 2 to 5 times by using carbon disulfide in an amount which is 1 to 3 times mass of the filter cake, and drying the scrubbed filter cake to obtain the 2-mercaptobenzothiazole at the mass percentage concentration of over 98 percent. By the method, no 'waste water' and 'waste gas' are discharged, and asphalt-like wastes are greatly reduced. The circulation of crystallization mother liquor realizes the recycling of intermediate products, and the total yield of the process is improved to be over 94 percent.

Description

technical field [0001] The invention belongs to the technical field of rubber vulcanization accelerator production, and in particular relates to a preparation method of a rubber vulcanization accelerator 2-mercaptobenzothiazole. Background technique [0002] Rubber vulcanization accelerator 2-mercaptobenzothiazole (MBT) is a widely used rubber vulcanization accelerator precursor. In industry, the Kelly process is generally used to produce MBT. In this method, aniline, carbon disulfide and sulfur are reacted under high temperature and high pressure, and then the product MBT is obtained by alkali dissolution, oxidation and acidification. The advantage of this method is that it is simple and easy to operate, but the disadvantage is that the process requires a lot of acid and alkali solutions, and about 30 to 60 tons of waste water is produced per ton of product. , only 80% to 85%, and it is difficult to handle 100 to 200kg of asphalt-like waste per ton of product; the oxidatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/72
Inventor 陈松李国兵王树华安静韩毅范江洋
Owner TIANJIN UNIV
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