Continuous production method for vulcanization accelerator DPG
A vulcanization accelerator and production method technology, applied in the field of rubber accelerators, can solve problems such as increased process risk, high safety risk, and large amount of ammonia water feeding, and achieve the effects of improving the intrinsic safety of the process, shortening the reaction time, and reducing the risk of explosion
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Embodiment 1
[0047] A continuous production method of vulcanization accelerator DPG, comprising the steps of:
[0048] (1) 400g diphenylthiourea, 0.5g catalyzer copper acetate and 372mL concentration are beating the ammoniacal liquor of 24wt.%, then slurry is mixed with the mixed solvent of 3500mL acetone and ethyl acetate (acetone and ethyl acetate The volume ratio of ester is 3:1) after mixing, obtain reaction raw material mixture;
[0049] (2) The reaction raw material mixture and oxygen are passed into the microchannel reactor for oxidation reaction according to the raw material mixture 2.9mL / min, and the flow velocity of oxygen 14.3mL / min. The reaction temperature is 60°C, the residence time is 3min, and the reaction pressure is 0.25MPa; Microchannel reaction The device is 10 pieces connected in series, the single piece volume is 1.86mL, and the total volume is 18.6mL;
[0050] (3) Distilling the product solution obtained from the reaction under reduced pressure to recover the organi...
Embodiment 2
[0053] A continuous production method of vulcanization accelerator DPG, comprising the steps of:
[0054] (1) beating 700g diphenylthiourea, 0.5g catalyst copper chloride and 680mL concentration of 20wt.% ammonia water, and then mixing the slurry with 8400mL ethyl acetate to obtain a reaction raw material mixture;
[0055] (2) The reaction raw material mixture and oxygen are passed into the pipeline reactor for oxidation reaction according to the flow rate of the raw material mixture 10.5mL / min and oxygen 99mL / min, the reaction temperature is 55°C, the residence time is 3min, and the reaction pressure is 0.1MPa; the volume of the pipeline reactor 150mL;
[0056] (3) Distilling the product solution obtained from the reaction under reduced pressure to recover the organic solvent, and the solid material obtained is washed with alkali, washed with water, and dried to obtain the vulcanization accelerator DPG.
[0057] After calculation, the yield of DPG in this example is 94.9% (b...
Embodiment 3
[0059] A continuous production method of vulcanization accelerator DPG, comprising the steps of:
[0060] (1) beating 700g diphenylthiourea, 0.7g catalyst copper acetate and 1000mL concentration of ammonia water of 15wt.%, then dissolving the slurry into 5600mL of acetone to obtain a reaction raw material mixture;
[0061] (2) The reaction raw material mixture and oxygen are passed into the tower reactor for oxidation reaction according to the flow rate of raw material mixture 5.6mL / min and oxygen 60mL / min, the reaction temperature is 65°C, the residence time is 3min, and the reaction pressure is 0.15MPa; the pipeline reactor The volume is 100mL;
[0062] (3) Distilling the product solution obtained from the reaction under reduced pressure to recover the organic solvent, and the solid material obtained is washed with alkali, washed with water, and dried to obtain the vulcanization accelerator DPG.
[0063] After calculation, the yield of DPG in this example is 95.5% (based on...
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