Preparation method of rubber vulcanization accelerator DCBS

A rubber vulcanization and accelerator technology, applied in organic chemistry and other fields, can solve problems such as environmental hazards, high raw material costs, and unqualified product quality, and achieve the effects of low environmental pollution, low cost, and reduction of three wastes

Inactive Publication Date: 2012-12-26
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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  • Preparation method of rubber vulcanization accelerator DCBS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 100g of crude MBT obtained from the high pressure reaction (measured MBT purity is 89.0%, mass percentage) directly into a container containing 44.5g of water (the weight ratio of water to purified MBT is 0.5:1) under stirring , add dropwise the sodium hydroxide aqueous solution of mass content 20% in the container, maintain the pH value in the container at 9.5, MBT is all dissolved and made M-Na salt solution, after the sodium hydroxide aqueous solution consumes 74.5g, the pH of the reactant Keep 9.5 unchanged within 30 minutes, and transfer the supernatant to the metering tank after standing;

[0031] 1780g of isopropanol (the weight ratio of isopropanol to MBT (after conversion) is 20:1) and 96.5g of dicyclohexylamine (the molar ratio of dicyclohexylamine to MBT (after conversion) is 1 : 1) The sodium hypochlorite solution with 12% available chlorine, M-Na salt solution, and 20% sulfuric acid solution are added dropwise in the container at the same time. During t...

Embodiment 2

[0033] Add 100g of crude MBT obtained from the high pressure reaction (measured MBT purity is 89.0%, mass percentage content) directly into a container containing 89g of water (the weight ratio of water to crude MBT is 1:1) under stirring, and pour into the container Add an aqueous sodium hydroxide solution with a mass content of 20% dropwise to maintain the pH value in the container at 9.5, so that MBT is completely dissolved to make a M-Na salt solution. After the aqueous sodium hydroxide solution consumes 75.3g, the pH of the reactant is within 30min Keep 9.5 unchanged, and transfer the supernatant to the metering tank after standing;

[0034] 1780 g of isopropanol (the weight ratio of isopropanol to MBT (after conversion) is 20:1) and 96.5 g of dicyclohexylamine (the molar ratio of dicyclohexylamine to MBT (after conversion) is 1 : 1) The sodium hypochlorite solution with 12% available chlorine, M-Na salt solution, and 25% sulfuric acid solution were added dropwise in the ...

Embodiment 3

[0036] The crude MBT 100g obtained by the high pressure reaction (measured MBT purity is 89.0%, mass percentage content) is directly added to the container containing 53.4g water (the weight ratio of water and crude MBT is 0.6:1) under stirring, Add dropwise sodium hydroxide aqueous solution with a mass content of 40% in the container to maintain the pH value in the container at 9.5, so that MBT is completely dissolved to make M-Na salt solution. After 85.5 g of sodium hydroxide aqueous solution is consumed, the pH of the reactant is 30 minutes Keep 9.5 unchanged, and after standing, transfer the supernatant to the metering tank;

[0037] 1780g of isopropanol (the weight ratio of isopropanol to MBT (after conversion) is 20:1) and 96.5g of dicyclohexylamine (the molar ratio of dicyclohexylamine to MBT (after conversion) is 1 :1) Add sodium hypochlorite solution with 12% available chlorine, M-Na salt solution, and 20% sulfuric acid solution dropwise in the container at the same ...

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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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
Inventor 尹红伟
Owner KEMAI CHEM
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