Preparation method of rubber accelerator dibenzothiazyl disulfide

A technology of dibenzothiazole disulfide and rubber accelerator, which is applied in the direction of organic chemistry, etc., can solve the problems of energy waste, prolong the reaction cycle, increase production cost, etc., and achieve the improvement of product quality and purity, shorten the process cycle and environmental pollution. small effect

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

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Problems solved by technology

Regarding the production process of DM, there are also some reports at home and abroad, mainly using 2-mercaptobenzothiazole (M) as raw material, and oxidizing it with oxidants. The main oxidants used are nitrous acid, oxygen, chlorine, potassium permanganate, etc. Although the above methods have their own advantages, they produce a large number of by-products, which have a certain impact on the environment and bring great pressure to the water treatment project. The process conditions are not easy to control and the operation is complicated.
[0003] Literature (Advances in Fine Petrochemical Industry, 2006, 7(9): 35) reported the oxidation of M with hydrogen peroxide and the preparation of DM with isopropanol as a carrier. Isopropanol can be recycled. , reduce the pressure on environmental pollution, but increase the mother liquor separation process, the distillation of the mother liquor requires a lot of energy, increase the production cost, the process is complicated, and it is not easy to operate
The patent (200710016805.5, 2007-7-9) reported that after dissolving M with ammonia water or liquid ammonia, the ammonium salt soluti

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: The configuration process of the oxidant: in the container, hydrogen peroxide and sulfuric acid are mixed according to the molar ratio of hydrogen peroxide:sulfuric acid in a ratio of 0.5~0.8:1, and the hydrogen peroxide stabilizer of 2~4g / L is added to the mixture of hydrogen peroxide and sulfuric acid simultaneously. GJ-101, mix well.

[0016] Oxidation process: at room temperature, measure 500ml of M-Na salt solution, the density is 1.014~1.016g / m 3 , put it into a 1000ml four-necked bottle, the reaction temperature is controlled at 70~80℃, and 58~80ml / L oxidant is added dropwise to the reactor at the same time, and the oxidant is added dropwise while stirring to measure the end point pH=7. Add 0.1-0.2g of 30% sodium hydroxide solution, the reaction time is 2h, after the reaction is finished, suction filtration and drying to obtain the finished product DM in white powder form, the initial melting point is 173°C, and the purity is 99.5%.

Embodiment 2

[0017] Embodiment 2: hydrogen peroxide and sulfuric acid are mixed according to the molar ratio hydrogen peroxide: sulfuric acid in the ratio of 0.8~1.1:1, add the hydrogen peroxide stabilizer GJ-101 of 2~4g / L in the mixture of hydrogen peroxide and sulfuric acid simultaneously, mix Evenly.

[0018] Oxidation process: at room temperature, measure 500ml of M-Na salt solution, the density is 1.017~1.019g / m 3 , put it into a 1000ml four-necked bottle, the reaction temperature is controlled at 70~80℃, and 58~80ml / L oxidant is added dropwise to the reactor at the same time, and the oxidant is added dropwise while stirring to measure the end point pH=7. Add 0.1-0.2g of 30% sodium hydroxide solution, the reaction time is 2h, after the reaction is completed, suction filtration and drying to obtain the finished product DM in white powder form, the initial melting point is 174°C, and the purity is 99.6%.

Embodiment 3

[0019] Embodiment 3: in the container, hydrogen peroxide and sulfuric acid are mixed in a ratio of 1.1 to 1.5:1 according to the molar ratio of hydrogen peroxide: sulfuric acid, and the hydrogen peroxide stabilizer GJ-101 of 2 to 4 g / L is added to the mixture of hydrogen peroxide and sulfuric acid simultaneously, and mixed. Evenly.

[0020] Oxidation process: at room temperature, measure 500ml of M-Na salt solution, the density is 1.020~1.022g / m 3 , put it into a 1000ml four-necked bottle, the reaction temperature is controlled at 75~80℃, and 58~80ml / L of oxidant is added dropwise to the reactor at the same time, and the oxidant is added dropwise while stirring to measure the end point pH=7, after the pH is stable Add 0.1-0.2g of 30% sodium hydroxide solution, the reaction time is 2h, after the reaction is completed, suction filtration and drying to obtain the finished product DM in white powder form, the initial melting point is 176°C, and the purity is 99.8%.

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Abstract

The invention relates to a preparation method of rubber accelerator dibenzothiazyl disulfide. The preparation method comprises the following steps of: measuring 500 ml of M-Na salt solution; dropwise adding mixed oxidant into a container with the M-Na salt solution according to a proportion of 58-80 ml of mixed oxidant per every liter of M-Na salt solution under a stirring condition at 70-80 DEG C; controlling the pH (Potential of Hydrogen) to be stable in a range of 6.5 to 7.5; adding 0.1-0.2 g of 30 percent sodium hydroxide solution after the pH is stabilized; directly oxidizing the M-Na salt to obtain a DM product. The preparation method has the advantages that (1) a hydrogen peroxide stabilizer is added, so that the oxidation of the oxidant is improved, (2) no toxic gas is produced in a production process, so that the environmental pollution is less, the operation is easy and the production period is short, (3) a product has white appearance, high purity and a melting point of greater than or equal to 173 DEG C, (4) a small amount of caustic soda liquid is added, so that the product quality and the purity are improved, and (5) separation can be performed without cooling after the reaction is finished, so that the process period is shortened, the energy consumption is reduced and the cost is saved.

Description

technical field [0001] The invention relates to a preparation method for synthesizing dibenzothiazole disulfide (DM) as a rubber accelerator by utilizing hydrogen peroxide, and belongs to the technical field of rubber accelerator DM synthesis. Background technique [0002] Rubber accelerators play a very important role in the rubber vulcanization process, accelerating the reaction between rubber and vulcanizing agents and improving production efficiency. DM is an indispensable auxiliary in the rubber accelerator industry. Regarding the production process of DM, there are also some reports at home and abroad, mainly using 2-mercaptobenzothiazole (M) as the raw material, which is obtained by oxidation with an oxidant. The main oxidants used are nitrous acid, oxygen, chlorine, potassium permanganate, etc., Although the above methods have their own advantages, they produce a large number of by-products, which have a certain impact on the environment, bring a lot of pressure to t...

Claims

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Application Information

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IPC IPC(8): C07D277/78
Inventor 李霞
Owner KEMAI CHEM
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