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ChemicalBook CAS DataBase List 1,3-Diphenylguanidine

1,3-Diphenylguanidine synthesis

9synthesis methods
-

Yield:102-06-7 96.1%

Reaction Conditions:

with ammonium hydroxide;oxygen;copper diacetate in ethyl acetate;acetone at 60; under 1875.19 Torr; for 0.05 h;Reagent/catalyst;Temperature;Pressure;Solvent;

Steps:

1 A method for continuously producing a vulcanization accelerator DPG, comprising the following steps:
(1) 400 g of diphenyl thiourea, 0.5 g of catalyst copper acetate and 372 mL of concentration 24wt.% ammonia water, Then, the slurry is mixed with 3500 mL of a mixed solvent of acetone and ethyl acetate (volume ratio of acetone to ethyl acetate of 3:1) under stirring to obtain a reaction raw material mixture; (2) The reaction raw material mixture and oxygen are 2.9 mL/min according to the raw material mixture. oxygen gas flow rate of 14.3mL / min into the microchannel reactor for oxidation reaction, Reaction temperature 60 °C, The residence time is 3 min, and the reaction pressure is 0.25 MPa; The microchannel reactor is 10 pieces in series. The volume of the single piece is 1.86 mL, and the full volume is 18.6 mL; (3) The product solution obtained by the reaction is subjected to distillation under reduced pressure to recover an organic solvent, and the obtained solid material is subjected to alkali washing, washing with water, and drying to obtain a vulcanization accelerator DPG.According to the calculation, the DPG yield of this example was 96.1% (calculated as CA dosage), and the appearance was white microcrystalline powder.

References:

Kemai Chemical Co., Ltd.;Meng Qingsen;Li Xia;Hao Pengfei CN108586295, 2018, A Location in patent:Paragraph 0046-0050; 0054; 0055; 0061; 0066; 0067; 0072-0073

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