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Method of obtaining 2-mercaptobenzothiazole

A technology for mercaptobenzothiazole and aniline, which is applied in the field of obtaining 2-mercaptobenzothiazole and can solve the problems of no description, no effect, etc.

Inactive Publication Date: 2007-01-17
DUSLO A S
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method should be sufficient to remove a calculable amount of used filtrate to maintain the purification capacity of the system, but in practice, it does not
The description also includes a discussion of the possibility of recirculating the distillation bottoms through the reactor (obtained from the amount of filtrate removed), but this possibility is not described in more detail in the examples

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (The aniline filtrate is not recycled)

[0037] 93.13 grams of aniline, 31.42 grams of sulfur and 80.67 grams of carbon disulfide were charged into a 300 ml pressure reactor. Under the conditions customary for this synthesis (220 to 300° C. / 6 to 11.1 MPa), a melt of the crude 2-mercaptobenzothiazole is prepared. After the reaction, the reactor was cooled to 180°C to 200°C, and the contents of the reactor were purged with a nitrogen flow at 200°C to remove volatile components.

[0038] 155 g of purged melt (containing 92.3% of 2-mercaptobenzothiazole, 1.72% of benzothiazole, 2.14% of sulfur and 3.84% of bitumen) and 8.9 g of volatile fraction (aniline and benzothiazole mixture)

[0039] The melt was hot-dissolved in 250 g of aniline, 2-mercaptobenzothiazole was crystallized by cooling, and after filtration and drying, 114.6 g of product were obtained (i.e., a theoretical yield of 68.5 g relative to the aniline charged to the reactor %, the yield relative to the conten...

Embodiment 2

[0040] Embodiment 2 (after reaching steady state repeatedly by part aniline filtrate circulation)

[0041] 100 g of the aniline filtrate from the crystallization step (containing 78% aniline, 9.5% 2-mercaptobenzothiazole) was mixed with 27 g of sulfur, 67 g of carbon disulfide and 9 g of the volatile fraction from the previous melt purge step ( Containing 30% aniline and 65% benzothiazole) were fed together into a 300 ml pressure reactor. Under the conditions customary for this synthesis (220 to 300° C. / 6 to 11.1 MPa), a melt of the crude product is obtained. After the reaction, the reactor was cooled to 180 to 200° C., and the contents of the reactor were purged with nitrogen flow at 200° C. to remove volatile parts.

[0042] Obtained 162.3 g of purged melt containing 91.0% of 2-mercaptobenzothiazole, 2.0% of benzothiazole, 1.5% of sulfur, 0.9% of anilinobenzothiazole, 0.1% of Phenylthiourea, 0.07% of 2-methylbenzothiazole and 4.43% of bitumen, the melt was dissolved in 222...

Embodiment 4

[0049] 20 g of aniline, 80 g of aniline filtrate from the crystallization step and of the same composition as in Example 1 (78% of aniline, 9.5% of 2-mercaptobenzothiazole) were mixed with 28 g of sulfur, 71 g of carbon disulfide and 9 g of The benzothiazole (volatile part) from the washing step was added to the reactor together. Heat the reactor to the working temperature. After the reaction, cool the reactor to 180°C to 200°C, release the accumulated hydrogen sulfide through the pressure control valve, and discharge the material in the reactor at 200°C. Volatile components in the melt were removed by distillation under a reduced pressure of 20 Torr and a temperature of 200°C.

[0050] 161 g of purged melt were obtained, containing 92.2% 2-mercaptobenzothiazole, 1.8% benzothiazole, 1.3% sulfur, 0.7% anilinobenzothiazole, 0.1% symmetric diphenylsulfide Urea, 0.05% of 2-methylbenzothiazole and 3.85% of unidentified substances. This melt was dissolved in a mixture of 222 g of ...

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PUM

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Abstract

2-Mercaptobenzothiazole is obtained from a melt of the raw product prepared by the reaction of aniline, carbon disulphide and sulphur by pressure synthesis in a reactor, where the melt contains 2-mercaptobenzothiazole, unreacted raw materials, intermediate products and pitches, so that after reaching a stationary state of the reaction medium it includes the following steps: a) crystallization of the 2-mercaptobenzothiazole raw product from an aniline solution, b) dividing the liquid phase (FK) from crystallization from step a) in three parts, c) removing one part of the liquid phase (FK1) from crystallization from step a) out of the process, d) returning the second part of the liquid phase (FK2) from crystallization from step a) into the reactor for preparation of the raw product and supplementing it with sulphur and carbon disulphide with respect to aniline, e) final purification of the crystallized 2-mercaptobenzothiazole from step a) in the aniline liquid phase and separation of pure 2-mercaptobenzothiazole, f) using the third part of the liquid phase (FK3) from crystallization from step a), supplemented with the liquid phase (FR) from final purification from step e) and possibly with aniline for crystallization of a further batch of the 2-mercaptobenzothiazole raw product, g) using the liquid phase (FR) from final purification from step f), together with a part of the liquid phase (FK3) from step e), possibly with aniline, for crystallization of the 2-mercaptobenzothiazole raw product, wherein the steps a) to g) are repeated.

Description

technical field [0001] The present invention relates to a method for obtaining 2-mercaptobenzothiazole from a crude product melt, wherein the melt contains 2-mercaptobenzothiazole, unreacted raw materials, intermediate products and asphalt. Background technique [0002] 2-Mercaptobenzothiazole (hereinafter referred to as 2-MBT) is a basic member of the benzothiazole accelerator used in the vulcanization process of unsaturated rubber, while 2-mercaptobenzothiazole is more important for industrial production The decisive basic raw materials of benzothiazole accelerators, these more important benzothiazole accelerators such as N-cyclohexylbenzothiazole sulfenamide (sulphene amide), N-tert-butylbenzothiazole sulfenamide, N, N-dicyclohexylbenzothiazole sulfenamide, N-oxydiethylene-benzothiazole sulfenamide, etc. [0003] On an industrial scale, 2-mercaptobenzothiazole is prepared directly from aniline, carbon disulfide and sulfur by high-pressure synthesis at high temperature. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/72
CPCC07D277/72
Inventor K·克里扎诺威克L·蒙塔高瓦
Owner DUSLO A S
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