Production process of rubber vulcanization accelerator mbts

A production process and rubber vulcanization technology, which is applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., and can solve problems such as increasing production costs, difficult wastewater treatment, and inability to continue to apply them. , to achieve the effect of improving environmental protection and high selectivity

Active Publication Date: 2022-03-15
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is mature, but about 10-15 tons of high-salt and high-organic waste water is produced per ton of product. Currently, it can be seen that the reported wastewater treatment processes are all costly, and at the same time, waste salt NaCl of average quality is produced, which is difficult to treat.
[0006] 2) At 55-65°C, use a mixture of hydrogen peroxide and sulfuric acid as an oxidizing agent to directly oxidize 2-mercaptobenzothiazole sodium salt. When the pH is stable at 6.5-7.5, the reaction ends, and the solid-liquid separation is carried out at a controlled temperature of about 30°C. , the product DM is obtained, about 8-10 tons of saline organic wastewater is produced per ton of product, the treatment cost is high and Na2SO4 will be produced, which is difficult to handle
[0007] 3) MBT is oxidized with hydrogen peroxide, and MBTS is prepared with isopropanol as a carrier. Isopropanol can be recycled. Although this process uses an environmentally friendly oxidant, it reduces the pressure on environmental pollution, but the concentration of hydrogen peroxide is 27.5%. A large amount of organic waste water is produced, which increases the separation process of mother liquor. The distillation of mother liquor requires a lot of energy, which increases the production cost, and the process is complicated and difficult to operate.
[0008] 4) After dissolving MBT with ammonia water or liquid ammonia, the obtained ammonium salt solution is filtered, and the catalyst is added to react with oxygen or air for a certain period of time at a certain temperature and pressure to obtain the MBTS product. This process is complicated to operate, and the ammonium salt solution needs to be filtered. , the whole process needs a catalyst, and the content of ammonia nitrogen in the wastewater is high
Although this scheme uses oxygen as the oxidant, since the process yield is generally less than 90%, the by-products are mostly dissolved in ammonia water, so that the process still produces a large amount of wastewater that is difficult to treat, and the ammonia nitrogen content in the wastewater is often extremely high
Although the patent proposes that no three wastes are produced, the catalyst NO / NO2 itself is a gas pollutant, and the process makes the catalyst unable to realize recycling
In addition, the MBTS product yield of this technology is about 96%, that is, about 4% of the by-products will be dissolved in the solvent water or methanol, ethanol, isopropanol, benzene or toluene, and the by-products will reach saturation in the repeated application process At this time, the mother liquor cannot continue to be used mechanically, and then waste water or waste solvent will be produced, and this part of waste water or waste solvent and by-products belong to solid waste and waste liquid
[0010] To sum up, the currently commonly reported MBTS synthesis technology cannot effectively avoid the generation of the three wastes, and the generated "three wastes" also have the problems of difficulty in processing and high processing costs. It is necessary to develop a new MBTS synthesis process to solve or Alleviate the above problems

Method used

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  • Production process of rubber vulcanization accelerator mbts

Examples

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Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: a kind of production technology of rubber vulcanization accelerator MBTS comprises the following steps:

[0032] (1) At 35°C, mix MBT with a mass ratio of 1:5 and the solvent for 0.6h under stirring. The solvent is a mixture of ammonia, water and toluene. In the solvent, ammonia:water:toluene=1:15: 13. After the mixing is completed, it is the raw material liquid;

[0033](2) After putting the raw material liquid into the autoclave, add a macroporous anion exchange resin catalyst with a mass three times the mass of MBT. After starting the stirring, introduce air to a pressure of 0.7Mpa to start the oxidation reaction. During the process, the reaction temperature was controlled at 40°C. When the total mass of the air introduced reached 0.25 times the mass of the input MBT, the air was stopped, and the reaction was completed after continuing to stir for 2 hours.

[0034] (3) After the pressure in the kettle is released, the material is passed through a coar...

Embodiment 5

[0041] In Example 5, since there is no toluene component in the solvent, and the ammonia content in the system is relatively high due to the ratio problem, the raw material MBT is oxidized to other by-products during the oxidation process, which reduces the reaction yield. At the same time, this technology controls the overall oxygen intake in the oxidation process, and the deep oxidation of the raw material MBT consumes excess oxygen, so that not only peroxidation by-products are produced during the reaction process, but also the raw material MBT is unreacted. In addition, since there is no toluene solvent in the system, the oil-soluble impurities in MBT cannot be separated from the product, resulting in a decrease in the purity of MBTS. After detection and analysis, the yield of the product MBTS was only 89.0%, and the purity was 95.4%. At this time, the water phase is red, and the COD of the wastewater is 42600mg / L.

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Abstract

The invention belongs to the field of heterocyclic compounds, and in particular relates to a production process of a rubber vulcanization accelerator MBTS. The process includes the following steps: (1) Mix MBT and solvent under stirring conditions to obtain a raw material liquid; (2) Put the raw material liquid obtained in step (1) into an autoclave, and then add a catalyst with a tertiary amino group Porous anion exchange resin, after starting the stirring, air is introduced to a pressure of 0.7-4Mpa, and the oxidation reaction begins; during the process, the reaction temperature is controlled at 30-60°C, and the total mass of the air is 0.23-0.4 times the mass of the input MBT , stop feeding air, and continue to stir until the reaction is over; (3) After the pressure in the kettle is released, the material is first passed through a filter to recover the catalyst, and the filtrate is filtered through a medium-speed filter paper for a second time, and after washing with water, the target product can be obtained. Product MBTS.

Description

technical field [0001] The invention belongs to the field of heterocyclic compounds, and in particular relates to a production process of a rubber vulcanization accelerator MBTS. Background technique [0002] In the process of using rubber to produce various rubber products such as tires, hoses, and rubber shoes, five types of additives must be used, which are rubber vulcanization accelerators (referred to as accelerators), rubber antioxidants, rubber vulcanization and vulcanization active agents, Type rubber additives and special functional additives. The vulcanization accelerator is called accelerator for short. Substances that promote vulcanization. It can shorten the vulcanization time, lower the vulcanization temperature, reduce the amount of vulcanizing agent and improve the physical and mechanical properties of rubber. [0003] Rubber vulcanization accelerator MBTS (chemical name 2,2'-dithiodibenzothiazole, also known as DM) is a general-purpose accelerator for nat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/80B01J31/08
CPCC07D277/80B01J31/08B01J2231/70
Inventor 孟庆森赵玉军陆平回俊博孔令鑫黄汇江
Owner KEMAI CHEM
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