Green synthesis method of dibenzothiazole disulfide as rubber vulcanization accelerator

A technology of dibenzothiazole disulfide and rubber vulcanization, applied in reagents, organic chemistry, educts, etc., can solve the problems of poisonous and harmful reaction process, endanger human health, pollute air, etc., avoid peroxidation by-products, reduce Treatment costs and the effect of reducing the generation of saline wastewater

Active Publication Date: 2019-12-20
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem with this method is that the reaction produces a large amount of saline wastewater, which is difficult to handle; nitrogen oxide tail gas is produced, which seriously pollutes the air; in addition, sodium nitrite is a strong carcinogen, which is harmful to human health
[0009] There are many problems in the previous methods, such as toxic and harmful reaction process, low product yield and purity, and high cost of environmental protection treatment. Therefore, it is necessary to develop a clean, green, and recyclable mother liquor synthesis process for the product dibenzothiazole disulfide.

Method used

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  • Green synthesis method of dibenzothiazole disulfide as rubber vulcanization accelerator
  • Green synthesis method of dibenzothiazole disulfide as rubber vulcanization accelerator
  • Green synthesis method of dibenzothiazole disulfide as rubber vulcanization accelerator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Take 50 g of an aqueous sodium carbonate solution with a mass fraction of 15%, add 5.6 g of 2-mercaptobenzothiazole, and stir magnetically at a water bath temperature of 70° C. to completely dissolve the solid raw material to obtain a solution A containing 2-mercaptobenzothiazole sodium .

[0034] (2) Cool the solution A obtained in step (1) to 50°C, slowly add 37.07g of 1.37% H 2 o 2 Aqueous solution, and pass CO2 into the solution at a flow rate of 22.8mL / min 2 , after the reaction was carried out for 40min, it was cooled to room temperature to obtain a sodium bicarbonate solution B containing dibenzothiazole disulfide solid;

[0035] (3) The solution B obtained in the step (2) was suction filtered, and the obtained solid was washed with water and dried to obtain a solid product of dibenzothiazole disulfide, with a yield of 96.8% and a purity of 99.4% as detected by liquid chromatography.

Embodiment 2

[0037] (1) Take 50 g of an aqueous sodium carbonate solution with a mass fraction of 20%, add 5 g of 2-mercaptobenzothiazole, and stir magnetically at a water bath temperature of 80° C. to completely dissolve the solid material to obtain a solution A containing 2-mercaptobenzothiazole sodium;

[0038] (2) Cool the solution A obtained in step (1) to 40°C, and slowly add 33.89g of 1.5% H 2 o 2 Aqueous solution, and pass CO2 into the solution at a flow rate of 17.8mL / min 2 , after the reaction was carried out for 30min, it was cooled to room temperature to obtain a sodium bicarbonate solution B containing dibenzothiazole disulfide solid;

[0039] (3) The solution B obtained in step (2) was suction filtered, and the obtained solid was washed with water and dried to obtain a solid product of dibenzothiazole disulfide, with a yield of 97.8% and a purity of 99.1% as detected by liquid chromatography.

Embodiment 3

[0041] (1) Get the obtained filtrate of embodiment 2 step (3) i.e. sodium bicarbonate solution, obtain sodium carbonate solution after heating at 50°C, add 2-mercaptobenzothiazole 3g in the gained sodium carbonate solution, and magnetically Stir to completely dissolve the solid material to obtain a solution A containing 2-mercaptobenzothiazole sodium;

[0042] (2) Slowly add 22.37g of 1.50% H in solution A obtained in step (1) 2 o 2 Aqueous solution, and pass CO2 into the solution at a flow rate of 10.8mL / min 2 , the reaction was carried out after 60min and cooled to room temperature to obtain a sodium bicarbonate solution B containing dibenzothiazole disulfide solid;

[0043] (3) The solution B obtained in step (2) was suction filtered, and the obtained solid was washed with water and dried to obtain a solid product of dibenzothiazole disulfide with a yield of 97.2%.

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Abstract

The invention discloses a green synthesis method of dibenzothiazole disulfide as a rubber vulcanization accelerator, and belongs to the technical field of chemical engineering. The green synthesis method specifically comprises the following steps: completely dissolving 2-mercaptobenzothiazole in a sodium carbonate aqueous solution, then dropwise adding hydrogen peroxide, feeding carbon dioxide toadjust the pH of a system, and carrying out oxidation to generate dibenzothiazole disulfide and sodium bicarbonate. A sodium carbonate solution formed by heating the obtained sodium bicarbonate solution can be used for dissolving the raw material 2-mercaptobenzothiazole so as to realize circulation of the raw materials. The purity of the product prepared by the method can reach 99% or above. Compared with a traditional mixed acid oxidation method, the green synthesis method has the advantages that a large amount of salt-containing wastewater is reduced, and the process is environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and in particular relates to a green synthesis method of a rubber vulcanization accelerator dibenzothiazole disulfide. Background technique [0002] Dibenzothiazole disulfide is a general-purpose rubber vulcanization accelerator. The vulcanization curve is flat during the vulcanization process, and the vulcanization critical temperature is relatively high. The benzothiazolyl group contained in the structure belongs to the accelerator group, and the disulfide bond belongs to the anti-scorch group, which has good aging resistance and is usually used together with other accelerators to further improve the activity. Because of its bitter taste, it is mainly used in the manufacture of some non-food rubber products such as tires and rubber shoes. Dibenzothiazole disulfide is mostly prepared from 2-mercaptobenzothiazole by oxidation with different oxidants. [0003] The mos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/78
CPCC07D277/78Y02P20/141
Inventor 骆广生田佳鑫王凯
Owner TSINGHUA UNIV
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