Method for preparation of carbonates by continuous process
A technology of diaryl carbonate and carbon atoms, which is applied in the field of direct oxidative carbonylation to prepare diaryl carbonate and lead oxide in phenol, which can solve the problems of production decline and other problems
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Embodiment 1
[0033] The phenol solution (feed stream A) was composed of 2.50 g of Pd(acac) 2 (8.20 mmol), 112.80 g of PbO (505.8 mmol; 61.7 equivalents of lead per equivalent of palladium) were prepared in 16.0 liters of phenol. A second phenolic solution (feed stream B) was prepared from 1767 grams of hexaethylguanidinium bromide (5775 mils) in 14.2 liters of phenol. Each feed stream was stored at 65°C and pumped at a rate of 0.6 liters per hour into a stirred 1 gallon continuous reactor system maintained at 65°C and 40 psig pressure. After the reactor was filled, a gas mixture of 6% oxygen in carbon monoxide was started at a rate of 1200 SLPH (standard liters per hour) to achieve a pressure of 1200 psig, and the reactor temperature was then raised to 100°C. These conditions (100° C., 1200 psig, 1200 SLPH gas flow of 6% oxygen in carbon monoxide, stirring) were maintained for about 20 hours, and the weight percent of diphenyl carbonate was determined by high pressure liquid chromatograph...
Embodiment 2
[0034] Embodiment 2 (comparison)
[0035] The phenol solution (feed stream A) consists of 1.7849 g of Pd(acac) 2 (5.86mmol), 20.14 grams of PbO (90.2mmol; 15.4 equivalents of lead per equivalent of palladium) and 11.4 liters of phenol. A second phenolic solution (feed stream B) was prepared from 1261 g of hexaethylguanidinium bromide (4112 mmol) in 3.2 liters of phenol. Each feed stream was stored at 65°C and pumped at a rate of 1.5 liters / hour into a stirred 1 gallon continuous reactor system maintained at 65°C and 40 psig pressure. After the reactor was filled, a gas mixture of 6% oxygen in carbon monoxide was started at 1200 SLPH to achieve a pressure of 1200 psig, and the reactor temperature was then raised to 100°C. These conditions (100° C., 1200 psig, 1200 SLPH, 6% oxygen in carbon monoxide, stirring) were maintained for about 7 hours, and the weight percent of diphenyl carbonate was determined by high pressure liquid chromatography throughout the reaction. After 7 h...
Embodiment 3
[0036] Embodiment 3 (comparison)
[0037] The phenolic solution (feed stream A) consists of 1.2500 g of Pd(acac) 2 (4.104mmol), 14.10 grams of PbO (63.17mmol; 15.4 equivalents of lead per equivalent of palladium) and 8.0 liters of phenol were obtained. A second phenol solution (feed stream B) was prepared from 884.0 grams of hexaethylguanidinium bromide (2889 mmol) in 7.2 liters of phenol. Each feed stream was stored at 65°C and pumped at a rate of 0.4 liters / hour into a stirred 1 gallon continuous reactor system maintained at 65°C and 40 psig pressure. The flow meter was used to measure the flow rate of the catalyst solution after mixing feed streams A and B due to the reaction failure of the flow meter blocked by white precipitate.
[0038] Contrary to Examples 2 and 3, the phenol solutions of HEGBr / phenol and lead oxide were added to the reactor separately, resulting in 14% by weight of diphenyl carbonate produced after six hours ( figure 2 ).
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