Preparation method of rubber vulcanization accelerator DCBS

Abstract

The invention relates to a preparation method of a rubber vulcanization accelerator DCBS. The preparation method comprises the following steps of: directly adding crude MBT obtained in a high-pressure reaction into a container filled with water under violent stirring, dropping a sodium hydroxide aqueous solution into the container to ensure that the MBT is completely dissolved into an M-Na saline solution, standing still, and then transferring supernatant liquor into a measuring tank; simultaneously dropping a sodium hypochlorite solution, the M-Na saline solution and a sulfuric acid solution into a container filled with isopropanol and dicyclohexylamine, and after the M-Na saline solution is finished being dropped, stopping dropping the other two solutions; standing still a reaction mixture obtained at a reaction endpoint, separating out saline water and the isopropanol, wherein the isopropanol is directly recycled; carrying out suction filtration on a material layer, washing a filter cake with water to neutrality, and distilling material washing water to recover the isopropanol; and drying the material to obtain a DCBS finished product. According to the preparation method, because the MBT crude product is used as a raw material to directly synthesize the accelerator, the preparation method has the advantages of simple operation, low cost, small environmental pollution and high yield.

Description

technical field [0001] The present invention relates to a kind of preparation technology of rubber vulcanization accelerator N, N-dicyclohexylamine benzothiazole sulfenamide (DCBS, DZ), specifically, relates to a kind of synthetic method of producing DCBS with crude MBT, belongs to Accelerator DCBS production technology field. Background technique [0002] Accelerator N, N-dicyclohexylamine benzothiazole sulfenamide (DCBS, DZ) is an excellent delayed-acting sulfenamide accelerator, which has good dispersion performance in rubber and long burning time in rubber Long, high operating safety, suitable for thick products and high-activity reinforcing materials with large dosage. The synthesis of DCBS generally uses the accelerator MBT or MBTS, and dicyclohexylamine as raw materials to synthesize the product under the action of an oxidizing agent (usually sodium hypochlorite). Its chemical reaction equation is: [0003] [0004] The literature (Fine Petrochemical Industry, 2...

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Problems solved by technology

[0005] The raw material accelerator MBT used in the above methods is a refined finished product. The MBT refining process generally adopts the acid-base method, and a large amount of waste water and waste gas are generated during the production process, which has caused serious harm to the environment, and the cost of raw materials is high.

The literature that has been consulted has not found a process for synthesizing DCBS with crude MBT as a raw material, and there are impurities such as intermediate products and tar in the crude MBT, and the mass content of MBT is about 80-90%, which will remain in the finished product when synthesizing DCBS. resulting in substandard product quality

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