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Production method of rubber vulcanization accelerator DM

A technology of rubber accelerator and production method, applied in the direction of organic chemistry, etc., can solve the problems of inability to realize industrialization and inadvisability

Active Publication Date: 2015-01-07
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

Of course, in some literatures, it is mentioned that hydrogen peroxide is used to directly oxidize without waste water. It has been proved by practice that the yield of rubber vulcanization accelerator DM in the method mentioned in the literature is far lower than that of DM produced by the above two methods. Yield, therefore not desirable and not industrializable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0015] The production method of the rubber vulcanization accelerator DM, the following steps are carried out in turn: a first add 5000L of water, 500kg of rubber accelerator M, and 3kg of surfactant OP-10 in the mixing tank; ℃, stirring for 1 hour; c, put the material into the oxidation kettle through the slurry pump, add 6kg of sodium acetate at the same time, and heat the mixture in the oxidation kettle with water steam. When the mixture is heated to 60 degrees, it will start to oxidize. 65°C; d dropwise add hydrogen peroxide solution with a mass fraction of 8%, the dropping rate is 120L per hour, and the reaction time is 3.2h; e. The end point of the reaction is determined by 1% cobalt oleate. After measurement, the reaction material has no color change, indicating that the reaction has reached At the end point, after the reaction is finished, it is washed with water, spin-dried, dried, and packaged.

Embodiment 2

[0017] The production method of the rubber vulcanization accelerator DM, the following steps are carried out in sequence: a first add 5000L of water, 500kg of rubber accelerator M, and 5kg of surfactant OP-10 in the mixing tank successively; b heat up to 50 while stirring ℃, stirring for 1 hour; c, put the material into the oxidation kettle through the slurry pump, add 8kg of sodium acetate at the same time, and heat the mixture in the oxidation kettle with water steam. When the mixture is heated to 60 degrees, oxidation begins, and the oxidation temperature is controlled at 75°C; d dropwise add hydrogen peroxide solution with a mass fraction of 11%, the dropping rate is 180L per hour, and the reaction time is 3.8h; e. The end point of the reaction is determined by 1% cobalt oleate. After measurement, the reaction material has no color change, indicating that the reaction has reached At the end point, after the reaction is finished, it is washed with water, spin-dried, dried, a...

Embodiment 3

[0019] The production method of rubber vulcanization accelerator DM, carries out the following steps successively: a first successively add the water of 5000L in the mixing tank, the rubber accelerator M of 500kg, the surfactant OP-10 of 4kg; B heat up to 50 while stirring ℃, stirring for 1 hour; c, put the material into the oxidation kettle through the slurry pump, add 7kg of sodium acetate at the same time, and heat the mixture in the oxidation kettle with water steam. When the temperature of the mixture rises to 60 degrees, oxidation begins, and the oxidation temperature is controlled at 70°C; d dropwise add hydrogen peroxide solution with a mass fraction of 10%, the dropping rate is 160L per hour, and the reaction time is 3.5h; e. The end point of the reaction is determined by 1% cobalt oleate. After measurement, the reaction material has no color change, indicating that the reaction has reached At the end point, after the reaction is finished, it is washed with water, spi...

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Abstract

The invention discloses a production method of a rubber vulcanization accelerator DM, belonging to the technical field of production of rubber accelerators. The production method disclosed by the invention sequentially comprises the following steps of: a, adding 5000 L of water, 500 kg of a rubber accelerator M and 2-6 kg of a surface active agent OP-10 into a mixing tank in sequence; b, increasing the temperature to 40-55 DEG C while stirring for 1 h; c, pumping materials into an oxidization kettle through a slurry pump, simultaneously, adding 4-10 kg of sodium acetate, beginning to oxidize while the temperature in the oxidization kettle is increased to 60 DEG C, and controlling oxidization temperature at 60-80 DEG C; d, dropping hydrogen peroxide solution with the mass fraction of 7-12%, wherein the dropping speed is 100-200 L per hour, and the reaction time is 3-4 h; and e, determining reaction endpoint by using 1% cobalt oleate, if the reaction materials are not changed in colour, determining that reaction is finished, after reacting, washing by using water, whirling, drying and packaging. The production method disclosed by the invention has the advantages that little materials, the surface active agent and sodium acetate are contained in reaction water, so that the reaction water can be used repetitively; the purposes of protecting the environment and reducing consumption are achieved; the product quality achieves national primary standards; and the product yield is above 99.5%.

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] 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 . Of course, in some literat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/78
CPCC07D277/78
Inventor 苗进之刘志勇严敬磊王奎亮李胜利常淑娟
Owner 河南省开仑化工有限责任公司
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