Carbonate ester purification method, carbonate ester solution production method, and carbonate ester purification apparatus
US-2017355659-A1 · Dec 14, 2017 · US
US10131617B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10131617-B2 |
| Application number | US-201515308983-A |
| Country | US |
| Kind code | B2 |
| Filing date | May 4, 2015 |
| Priority date | May 9, 2014 |
| Publication date | Nov 20, 2018 |
| Grant date | Nov 20, 2018 |
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The invention concerns a method for producing diaryl carbonates from monophenols and phosgene or chloroformic acid aryl esters in the presence of at least one optionally substituted pyridine or the hydrochloride salt thereof as catalyst, and the recovery and reinjection thereof back into the method. The method is carried out at least partially in a liquid phase without the use of an additional solvent, the catalyst being separated by means of distillation and recovered.
Opening claim text (preview).
The invention claimed is: 1. A process for preparing diaryl carbonate comprising: a. reacting at least one monophenol with phosgene and/or at least one aryl chloroformate in the presence of at least one optionally substituted pyridine, in free form and/or in the form of a hydrochloride salt thereof, as catalyst, wherein the reaction is carried out in a reactor under pressures of 1-50 bar (absolute), b. transferring the reaction mixture from the reactor into a single-stage distillation apparatus or a multistage distillation apparatus, c. separating a catalyst-containing distillate off at the top of at least one distillation column, d. at least partially recirculating the catalyst-containing distillate into the reactor at step a), and e. separating diaryl carbonate off via a side stream from the distillation apparatus, wherein an aqueous solution is not used in any of the steps a) to e). 2. The process as claimed in claim 1 , wherein the at least one monophenol comprises phenol. 3. The process as claimed in claim 1 , wherein not more than 10 mol % of the optionally substituted pyridine is present in free form. 4. The process as claimed in claim 3 , wherein the catalyst comprises pyridine hydrochloride. 5. The process as claimed in claim 1 , wherein hydrogen chloride formed in step a) is not neutralized. 6. The process as claimed in claim 1 , wherein hydrogen chloride formed in step a) is separated off by distillation in a first distillation stage and the catalyst-containing distillate and the diaryl carbonate-containing side stream are separated off in a further distillation stage. 7. The process as claimed in claim 1 , further comprising: taking off as a side stream from the distillation apparatus a mixture comprising—at least part of the optionally substituted pyridine in the form of the hydrochloride and diaryl carbonate; and fractionating the side stream in a separate heteroazeotropic distillation, wherein the diaryl carbonate is separated off as a bottom product. 8. The process as claimed in claim 1 , further comprising further purifying the diaryl carbonate separated off via the side stream from the distillation apparatus. 9. The process as claimed in claim 1 , wherein not more than 1 mol % of the optionally substituted pyridine is present in free form. 10. The process as claimed in claim 1 , wherein the at least one monophenol consists essentially of phenol. 11. The process as claimed in claim 3 , wherein the catalyst consists essentially of pyridine hydrochloride.
Purification; Separation; Stabilisation · CPC title
from phosgene or haloformates · CPC title
Recycling of unreacted starting or intermediate materials · CPC title
Esters of carbonic or haloformic acids · CPC title
with nitrogen contained as ring member in aromatic compounds or moieties, e.g. pyridine · CPC title
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