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Novel process for anhydrous clean production of vulcanization accelerator DM

A vulcanization accelerator and clean production technology, applied in the field of rubber vulcanization accelerator DM and dibenzothiazole disulfide

Inactive Publication Date: 2020-06-09
河南省开仑化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main production processes of rubber vulcanization accelerator DM at home and abroad are sodium nitrite method and hydrogen peroxide method. The sodium nitrite method is facing the situation of being eliminated due to the production of carcinogens in the oxidation process, while most of the hydrogen peroxide method is The raw material accelerator M (2-mercaptobenzothiazole) is first reacted with sodium hydroxide solution to generate M-Na salt, and then oxidized with the oxidant prepared by hydrogen peroxide and sulfuric acid, a large amount of waste water is generated in the whole procedure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0013] The new process of anhydrous and clean production of vulcanization accelerator DM, the following steps are carried out in sequence: a. Add 25-35L organic solvents (ethanol, ethylene glycol, isopropanol, dichloromethane, chloroform, One of acetone and ethyl acetate) to dissolve 2.5-3.5kg of accelerator M, and at the same time add 5% to 20% of catalyst (one of diphenyl tellurium, nickel chloride, 2-iodyl benzoic acid), and then Heat it with steam to 50-100°C, and slowly introduce oxygen at a rate of 100-300ml / min for oxidation. When the pressure in the kettle reaches 0.3MPa, the reaction starts. Keep the reaction pressure between 0.3-1.5MPa. When the pressure begins to increase to 1.5MPa, the reaction is over (reaction time 3-6h), stop feeding oxygen, c continue to keep warm for 1-3h, stop keeping warm; d conduct heat filtration in a closed container to obtain crude DM; e use crude DM The pure organic solvent is washed 2 to 4 times; f the washed material is dried in a clo...

Embodiment 2

[0015] The new process of anhydrous and clean production of vulcanization accelerator DM, the following steps are carried out in sequence: a. Add 28 to 32 L of organic solvents (ethanol, ethylene glycol, isopropanol, dichloromethane, chloroform, One of acetone and ethyl acetate) to dissolve 2.8-3.2kg of accelerator M, and at the same time add 9% to 16% of catalyst (one of diphenyl tellurium, nickel chloride, and 2-iodylbenzoic acid), and then Heat it with steam to 50-100°C, and slowly introduce oxygen at a rate of 100-300ml / min for oxidation. When the pressure in the kettle reaches 0.3MPa, the reaction starts. Keep the reaction pressure between 0.3-1.5MPa. When the pressure begins to increase to 1.5MPa, the reaction is over (reaction time 3-6h), stop feeding oxygen, c continue to keep warm for 1-3h, stop keeping warm; d conduct heat filtration in a closed container to obtain crude DM; e use crude DM The pure organic solvent is washed 2 to 4 times; f the washed material is drie...

Embodiment 3

[0017] The new process of anhydrous and clean production of vulcanization accelerator DM, the following steps are carried out in sequence: a. Add 29 to 31 L of organic solvents (ethanol, ethylene glycol, isopropanol, methylene chloride, chloroform, One of acetone and ethyl acetate) to dissolve 2.9-3.1kg of accelerator M, and at the same time add 11% to 14% of catalyst (one of diphenyl tellurium, nickel chloride, 2-iodyl benzoic acid), b then Heat it with steam to 50-100°C, and slowly introduce oxygen at a rate of 100-300ml / min for oxidation. When the pressure in the kettle reaches 0.3MPa, the reaction starts. Keep the reaction pressure between 0.3-1.5MPa. When the pressure begins to increase to 1.5MPa, the reaction is over (reaction time 3-6h), stop feeding oxygen, c continue to keep warm for 1-3h, stop keeping warm; d conduct heat filtration in a closed container to obtain crude DM; e use crude DM The pure organic solvent is washed 2 to 4 times; f the washed material is dried...

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PUM

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Abstract

The invention discloses a novel process for anhydrous clean production of a vulcanization accelerator DM, belonging to the technical field of rubber accelerator production. The novel process sequentially comprises the following steps: a, adding 25-35 L of one selected from a group consisting of organic solvents including ethanol, ethylene glycol, isopropanol, dichloromethane, chloroform, acetone and ethyl acetate into a reaction kettle, dissolving 2.5 to 3.5 kg of an accelerant M, and adding 5%-20% of a catalyst which is one selected from a group consisting of diphenyl tellurium, nickel chloride and 2-iodoxybenzoic acid; b, introducing steam, carrying out heating to 50-100 DEG C, slowly introducing oxygen at a speed of 100-300 ml / min, ending a reaction when the inner pressure of the kettlebegins to increase to 1.5 MPa, stopping introduction of oxygen; c, continuing to keep the temperature for 1-3 h; d, carrying out hot filtration in a closed container to obtain a crude product DM; e,carrying out washing with a pure organic solvent 2-4 times; and f, drying a washed material, and carrying out packaging to obtain a finished product. The novel process provided by the invention has the advantages that problems in treatment of the three wastes in a traditional process are thoroughly solved, sustainable development of an enterprise is facilitated, and a brand-new thought is providedfor rapid development of the industry.

Description

technical field [0001] The invention belongs to the technical field of production of rubber accelerators, in particular to a rubber vulcanization accelerator DM (the chemical name of the vulcanization accelerator DM is dibenzothiazole disulfide, and its molecular formula is C 14 h 8 N 2 S 4 ) production method. Background technique [0002] Vulcanization accelerator DM, chemical name 2,2'-dibenzothiazole disulfide, is a general-purpose accelerator for natural rubber, synthetic rubber, and reclaimed rubber, and is widely used in the manufacture of general industrial products such as tires, rubber hoses, rubber shoes, and tapes. At present, the main production processes of rubber vulcanization accelerator DM at home and abroad are sodium nitrite method and hydrogen peroxide method. The sodium nitrite method is facing the situation of being eliminated due to the production of carcinogens in the oxidation process, while most of the hydrogen peroxide method is The raw materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/78
CPCC07D277/78
Inventor 苗进之严敬磊王奎亮刘志勇李丛林
Owner 河南省开仑化工有限责任公司