Method for preparing rubber accelerator DM (2,2'-dithiobis(benzothiazole)) from 2-mercaptobenzothiazole coarse product as raw material
A technology of rubber accelerator and benzothiazole, which is applied in the production field of preparing DM (dibenzothiazole disulfide), can solve problems such as residue and unqualified product quality, and achieve the effect of reducing waste water discharge and energy consumption.
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Embodiment 1
[0014] Add 100g of crude product M and 100g of water into the reactor (the weight ratio of the crude product M is 1:1), add 24g of sodium hydroxide solid (the weight ratio of the crude product M is 100:24), and the M sodium salt liquid generated by the reaction is passed through Set aside to settle, add the supernatant to the oxidation kettle, and add 1% hydrogen peroxide and 1% dilute sulfuric acid dropwise to the oxidation kettle at a temperature of 20°C and a stirring speed of 50 rpm Mix the solution, the flow rate is controlled at 8m 3 / h, until the pH value of the solution reaches 4, stop adding the oxidant solution dropwise, the molar ratio of hydrogen peroxide to sulfuric acid is 1:1; the product is washed with 1% ethanol solution of 500g (500:100 by weight with crude M) DM material , filtered, washed with water, and dried to obtain DM. The product DM84g was obtained, with a melting point of 170.6°C.
Embodiment 2
[0016] Add 100g of crude product M and 1000g of water into the reactor (the weight ratio of the crude product M is 10:1), add 24g of sodium hydroxide solid (the weight ratio of the crude product M is 100:24), and the M sodium salt liquid generated by the reaction is passed through Set aside to settle, add the supernatant to the oxidation kettle, and add 1% hydrogen peroxide and 1% dilute sulfuric acid dropwise to the oxidation kettle at a temperature of 20°C and a stirring speed of 50 rpm Mixed solution (the molar ratio of hydrogen peroxide to sulfuric acid is 1.6:1), the flow rate is controlled at 8m 3 / h, until the pH value of the solution reaches 4, stop adding the oxidant solution dropwise, wash the DM material with 50g (50:100 by weight of the crude product M) solution of DM, filter, wash with water, and dry to obtain DM. The product DM83.1g was obtained with a melting point of 170.1°C.
Embodiment 3
[0018] Add 100g of crude product M and 2000g of water into the reactor (the weight ratio to crude product M is 20:1), add 200g of sodium hydroxide solution with a mass percentage concentration of 30% (the weight ratio of pure sodium hydroxide to crude product M is 100: 60), the M sodium salt liquid produced by the reaction was left to settle, and the supernatant was added to the oxidation kettle. Under the condition of 60°C and the stirring speed was 1000 rpm, the concentration of 27.5 % hydrogen peroxide and 30% dilute sulfuric acid mixed solution (the molar ratio of hydrogen peroxide to sulfuric acid is 1.2:1), the flow rate is controlled at 1m 3 / h, until the pH value of the solution reaches 9, stop adding the oxidant solution dropwise, wash the DM material with 50g (50:100 by weight of the crude product M) solution of DM, filter, wash with water, and dry to obtain DM. The product DM83g was obtained with a melting point of 170.2°C.
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