The preparation method of diphenyl carbonate compound
A technology of diphenyl carbonate and phenol compounds, which is applied in the field of preparation of diphenyl carbonate compounds, can solve the problems of non-environmental protection, low utilization rate of raw materials, low selectivity, etc., and achieve no corrosion of equipment, good economic benefits and Social benefits, effects of stable chemical properties
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[0015] The present invention provides a kind of preparation method of the diphenyl carbonate compound shown in formula (I), wherein, the preparation method comprises: in the presence of catalyst, the phenol compound shown in formula (II) and formula (III ) the carbonic acid diester compound shown in carries out transesterification reaction;
[0016]
[0017] Among them, R is hydrogen or C 1 -C 4 the alkyl group, R 1 and R 2 Each is independently methyl or ethyl; the catalyst contains n-butyl imidazole quaternary ammonium salt.
[0018] In the present invention, preferably, R is hydrogen, methyl or ethyl, more preferably hydrogen or methyl, even more preferably hydrogen.
[0019] In the present invention, preferably, in formula (II), R is located at the para-position of the phenolic hydroxyl group.
[0020] Specific examples of the phenolic compound represented by the formula (II) include chlorophenol, fluorophenol, and the like; p-chlorophenol and p-fluorophenol are pr...
Embodiment approach
[0043] According to a preferred embodiment of the present invention, the preparation method comprises: first mixing the phenol compound represented by formula (II) with the catalyst, heating the obtained mixture to the temperature required for the transesterification reaction, and then A diester carbonate compound represented by formula (III) is then mixed with the mixture.
[0044] According to another preferred embodiment of the present invention, the preparation method comprises: mixing the catalyst, the phenolic compound represented by formula (II) and the carbonic acid diester compound represented by formula (III), and the obtained mixture Heating to the temperature required for the transesterification reaction, and after reacting for 3.5-5 hours, adding an entrainer to the reaction liquid.
[0045] In the present invention, in order to improve the conversion rate of reactants and product selectivity, preferably, the entrainer is added to the reaction solution in 3-7 time...
Embodiment 1
[0069] Under nitrogen protection, 7.05g phenol, 0.26g 1-n-butyl-3-methylimidazole chloride, 2.07g potassium carbonate, 27g dimethyl carbonate (phenol, 1-n-butyl-3-methyl chloride The molar ratio of imidazole, potassium carbonate, and dimethyl carbonate is 1:0.02:0.2:4) mixed in a three-necked round-bottomed flask equipped with a liquid separator, and the oil bath in contact with the round-bottomed flask was heated to 95°C, The reaction was carried out under normal pressure (0.1MPa). While reacting, the azeotrope was steamed to the liquid separator by simple distillation method and removed. After reacting for 3.5 hours, after cooling for about 6 minutes, add dicarbonate to the round bottom flask. Methyl ester was added 3 times in total, the time interval between two adjacent additions was 1.5 hours, each time 10mL was added, each addition of dimethyl carbonate was added to react for 1.4 hours and methanol and azeotrope were simultaneously Distill out the round-bottomed flask, a...
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