TH76346A - Industrial processes for the manufacture of diarylls High purity carbonate - Google Patents

Abstract

DC60 (14/11/48), it is the purpose of this invention to provide A specific process that makes high-purity diaryl carbonate that can be used as a raw material of High-quality, high-performance polycarbonate that will be produced stably for a long time. On an industrial scale At not less than 1 t / h by using a reaction mixture containing alkylaryl carbonate obtained through the Transesterification reaction between dialkyl carbonate compounds and aromatic monohydroxyte was the starting material. Although a variety of offerings have been involved. The process for the production of aromatic carbonate reaction mixtures by means of reactive distillation methods, all of which have been done on a small scale and in short time of operation in Laboratory level, and no specific processes or equipment has been disclosed. That makes it possible to Mass produced on an industrial scale From the aforementioned mixture of high purity diaryl carbonate That can be used as a raw material of high quality and high performance polycarbonate in accordance with this invention. Has been prepared A unique process that makes high-purity diaryl carbonate so important is the raw material of high-quality, high-performance polycarbonate that is stably produced for a long period of time. At an industrial scale of not less than 1 t / h by using a reaction mixture containing alkyl aryl carbonate obtained through Transesterification reaction Between dialkyl carbonate and aromatic monohydroxy compounds as starting material, and through this starting material to transesterification by using a reactive distillation column. F Unique structure And later through the mixture of making High boiling point reactions Obtained from the bottom part of Reactive distillation columns to separation and purification using column A for the separation of high boiling point materials and column B, which yields a pure diaryl carbonate with multi-layer distillation columns connected. In particular It is the purpose of this invention to provide A specific process that makes high-purity diaryl carbonate that can be used as a raw material of High-quality, high-performance polycarbonate that will be produced stably for a long time. On an industrial scale At not less than 1 t / h by means of a reaction hair reagent containing alkylaryl carbonate obtained through the Transesterification reaction between dialkyl carbonate compounds and aromatic monohydroxyte was the starting material. Although a variety of offerings have been involved. The process for the production of aromatic carbonate reaction mixtures by means of reactive distillation methods, all of which have been done on a small scale and in short time of operation in Laboratory level, and no specific processes or equipment has been disclosed. That makes it possible to Mass produced on an industrial scale From the aforementioned mixture of high purity diaryl carbonate That can be used as a raw material of high quality and high performance polycarbonate in accordance with this invention. Has been prepared A unique process that makes high-purity diaryl carbonate so important is the raw material of high-quality, high-performance polycarbonate that is stably produced for a long period of time. At an industrial scale of not less than 1 t / h by using a reaction mixture containing alkyl aryl carbonate obtained through Transesterification reaction Between dialkyl carbonate and aromatic monohydroxy compounds as starting material, and through this starting material to transesterification by using a reactive distillation column. F Unique structure And later through the mixture of making High boiling point reactions Obtained from the bottom part of Reactive distillation column to separation and purification by using column A for the separation of high boiling point materials and column B, which yields a pure diaryl carbonate with multi-layer distillation columns connected. In particular

Claims (22)

1. Industrial Process for the Production of High-Purity Dialyl Carbonate: High-purity dialyl carbonate is produced using a reaction mixture with alkyl aryl carbonate as the starting material, obtained through a transesterification reaction between dialyl carbonate and aromatic monohydroxy compounds. The starting material is continuously fed into a reactive distillation column consisting of a series of continuous multi-stage distillation columns where a homogeneous catalyst is present. Transesterification and distillation reactions are performed simultaneously in the columns. The low-boiling point reaction mixture containing dialyl carbonate is continuously extracted from the top of the column in gaseous form, and the high-boiling point reaction mixture containing dialyl carbonate is extracted from the bottom of the column in liquid form. The high-boiling point reaction mixture is continuously introduced into column A for high-boiling point separation, and continuous separation is performed. By distillation into the upper mixture of column AT containing diaryl carbonate and the lower mixture of column AB containing the catalyst, and subsequently the continuous introduction of the upper mixture of column AT into column B for the purification of diaryl carbonate, the outlet for side cutting and continuous separation operation by distillation into the upper mixture of column BT, the side cutting mixture BS and the lower mixture of column BB. The improvement consists of: (a) such reactive distillation column consisting of a continuous multistage distillation column of length L(cm), inner diameter D(cm) inside with number of inner stages n, a gas outlet of inner diameter d1(cm) at the top of the column or in the upper part of the column near the top, a liquid outlet of inner diameter d2(cm) at the bottom of the column or in the lower part of the column near the bottom. At least one inlet is provided in the upper and/or middle section of the column below the gas outlet and at least one inlet is provided in (b) Column A for the separation of such high boiling point materials consists of a continuous multistage distillation column of length LA (cm), inner diameter DA (cm), and inside which there are nA layers, in which LA, DA, and nA satisfy the formulas (1) to (6) below: 1500 less than or equal to L less than or equal to 8000 (1) 100 less than or equal to D less than or equal to 2000 (2) 2 less than or equal to L/D less than or equal to 40 (3) 10 less than or equal to n less than or equal to 80 (4) 2 less than or equal to D/d1 less than or equal to 15 (5) 5 less than or equal to D/d2 less than or equal to 30 (6) (b) Column A for the separation of such high boiling point materials consists of a continuous multistage distillation column of length LA (cm), inner diameter DA (cm), and inside which there are nA layers, in which LA, DA, and nA satisfy the formulas (7) to (9) below: 800 less than or equal to LA less than or equal to 3000 (7) 100 less than or equal to DA less than or equal to 1000 (8) 20 less than or equal to nA less than or equal to 100 (9) (c) Column B for the purification of such diaryl, consisting of a series of continuous multistage distillation columns. which has length LB (cm), inner diameter DB (cm), inside of the inside of those things, entrance B1 at the inside of the column, and exit of the side cut B2 between entrance B1 and the bottom of the column, where the number of layers of the inside above entrance B1 is n1, the number of layers of the inside between entrance B1 and exit of side cut B2 is n2, the number of layers of the inside below exit of side cut B2 is n3, and the total number of layers is nB (=n1 + n2 + n3), where LB, DB, n1, n2, n3, and nb satisfy the following formulas (10) to (15): 1000 less than or equal to LB less than or equal to 5000 (10) 100 less than or equal to DB less than or equal to 1000 (11) 5 less than or equal to n1 less than or equal to 20 (12) 12 less than or equal to n2 Less than or equal to 40 (13) 3 Less than or equal to n3 Less than or equal to 15 (14) 20 Less than or equal to nB Less than or equal to 70 (15) and (d) not less than 1 ton/hr of high purity diaryl carbonate is continuously obtained as a mixture of BS side cutting. 2. The process under claim 1 shall be carried out where the distillation of column A for the separation of such high-boiling point materials is performed at a bottom temperature of column TA ranging from 185 to 280 °C and an upper pressure of column PA ranging from 1000 to 20000 Pa, and the distillation of column B for the purification of such diarylcarbonate is carried out at a bottom temperature of column TB ranging from 185 to 280 °C and an upper pressure of column PB ranging from 1000 to 20000 Pa. 3. A process in compliance with claim 1 or 2 where L, D, L/D, and n for such reactive columns satisfy the following formulas: 2000 ≤ L ≤ 6000, 150 ≤ D ≤ 1000, 3 ≤ L/D ≤ 30, and 15 ≤ n ≤ 60, respectively. LA, DA, and nA for column A for the separation of such high-boiling point materials. The following formulas apply to diaryl carbonate purification: 1000 ≤ or equal to LA ≤ or equal to 2500, 200 ≤ or equal to DA ≤ or equal to 600, and 30 ≤ or equal to nA ≤ or equal to 70, respectively. LB, DB, n1, n2, n3, and nB for column B for diaryl carbonate purification are as follows: 1500 ≤ or equal to LB ≤ or equal to 3000, 150 ≤ or equal to DB ≤ or equal to 500, 7 ≤ or equal to n1 ≤ or equal to 15, 12 ≤ or equal to n2 ≤ or equal to 30, 3 ≤ or equal to n3 ≤ or equal to 10, and 25 ≤ or equal to nB ≤ or equal to 55, respectively. TA ranges from 190 to 240 °C, and PA ranges from 2000 to... Temperatures in TB (Biochemical Oxygen Demand) range from 190 to 240°C, and temperatures in PB (Potty Leaping Body) range from 2000 to 15000 Pa. 4. Which of the following processes complies with the claims of Claims 1 through 3 where each of the aforementioned reactive distillation columns, Column A for the separation of such high-boiling material and Column B for the purification of such diaryl carbonate, is a distillation column with internal trays and/or packing? 5. A process in compliance with any of the claims 1 through 4 where such reactive distillation column is a distillation column with packing in the upper part of the column and trays in the lower part of the column as the inner part and the inner part of each of column A for the separation of such high boiling point material and column B for the purification of such diaryl carbonate as the packing. 6. A process in accordance with claim 5 whereby the packing is structured as at least one of a group of packings selected from Mellapak, Gempak, Techno-Pak, Flexi-Pak, Sulzer packing, Goodroll packing, and Glitchgrid packing. 7. A process in accordance with claim 4 or 5 where such tray of the reactive distillation column is a tray of sif, which contains the sif portion and the reduced portion. 8. A process in compliance with claim number 7 where the said SIP tray has 100 to 1000 holes/sq.m in the SIP section. 9. Processes in compliance with claims 7 or 8 where the cross-sectional area of the hole of the zip tray is between 0.5 and 5 cm². 10. High-purity diphenyl carbonate, which is diaryl carbonate produced by a process in compliance with any one of Reputations 1 through 9; such diphenyl carbonate which is not replaced or replaced by lower hydrocarbons; and which contains no more than 0.1 ppm of halogen and no more than 100 ppm of by-products with boiling points higher than the boiling point of such diphenyl carbonate. 11. High-purity diphenyl carbonate in accordance with claim 10, where such diphenyl carbonate is non-replaceable diphenyl carbonate, and the amount of halogen present is not greater than 10 ppm, and the amount of each of phenyl salicylates, xanthones, phenyl methoxybenzoates, and 1-phenoxycarbonyl-2-phenoxycarboxy-phenylene, which are by-products with boiling points higher than the boiling point of diphenyl carbonate, is not greater than 30 ppm. 12. High-purity diphenyl carbonate in compliance with claim 11, where the amount of by-products with a boiling point higher than the boiling point of diphenyl carbonate is not greater than 50 ppm. 13. High-purity diphenyl carbonate in compliance with claim 12, where the amount of halogen present is not greater than 1 ppm and the amount of by-product with a boiling point higher than the boiling point of diphenyl carbonate is not greater than 10 ppm. 14. Equipment for the production of high-purity dialyl carbonate, consisting of: a reactive distillation column consisting of a series of continuous multistage distillation columns containing a homogeneous catalyst; this reactive distillation column, which receives a reaction mixture with alkyl aryl carbonate as the starting material, obtained through the transesterification reaction between dialyl carbonate compounds and aromatic minohydroxy, where the transesterification and distillation reactions are carried out simultaneously in the column; the low-boiling point reaction mixture containing dialyl carbonate produced is extracted from the top of the column in gaseous form, and the high-boiling point reaction mixture containing dialyl carbonate is extracted from the bottom of the column in liquid form; and column A for the separation of high-boiling points material, connected to the reactive distillation column, which receives the high-boiling point reaction mixture. Where separation and distillation are carried out into the upper mixture of column AT containing diaryl carbonate and the lower mixture of column AB containing the catalyst and column B for the purification of diaryl carbonate, which is provided with a side cut-off outlet and which is connected to column A for the separation of high boiling point materials and which receives the upper AT component of the column from the side cut-off outlet, where separation and distillation are carried out into the upper mixture BT of the column, the side cut-off mixture BS and the lower mixture BB of the column, where (a) such reactive distillation column consists of a continuous multistage distillation column of length L(cm), inner diameter D (cm) inside with the number of inner stages n, gas outlet of inner diameter d1(cm) at the top of the column or in the upper part of the column near the top. A liquid outlet with an inner diameter d2 (cm) is provided at the bottom of the column, or in the lower section of the column near the bottom. At least one inlet is provided in the upper and/or middle section of the column below the gas outlet, and at least one inlet is provided in the lower section. (b) Column A for the separation of such high boiling point materials consists of a continuous multistage distillation column of length LA (cm), inner diameter DA (cm), and inside which there are nA layers, in which LA, DA, and nA satisfy formulas (1) to (6) below: 1500 less than or equal to L less than or equal to 8000 (1) 100 less than or equal to D less than or equal to 2000 (2) 2 less than or equal to L/D less than or equal to 40 (3) 10 less than or equal to n less than or equal to 80 (4) 2 less than or equal to D/d1 less than or equal to 15 (5) 5 less than or equal to D/d2 less than or equal to 30 (6) (b) Column A for the separation of such high boiling point materials consists of a continuous multistage distillation column of length LA (cm), inner diameter DA (cm), and inside which there are nA layers, in which LA, DA, and nA satisfy formulas (7) to (9) 800 less than or equal to LA less than or equal to 3000 (7) 100 less than or equal to DA less than or equal to 1000 (8) 20 less than or equal to nA less than or equal to 100 (9) (c) Column B for the purification of such diaryl, consisting of a series of continuous multistage distillation columns. which has length LB (cm), inner diameter DB (cm), inside of the inside of those things, entrance B1 at the inside of the column, and exit of the side cut B2 between entrance B1 and the bottom of the column, where the number of layers of the inside above entrance B1 is n1, the number of layers of the inside between entrance B1 and exit of side cut B2 is n2, the number of layers of the inside below exit of side cut B2 is n3, and the total number of layers is nB (=n1 + n2 + n3), where LB, DB, n1, n2, n3, and nb satisfy the following formulas (10) to (15): 1000 less than or equal to LB less than or equal to 5000 (10) 100 less than or equal to DB less than or equal to 1000 (11) 5 less than or equal to n1 less than or equal to 20 (12) 12 less than or equal to n2 Less than or equal to 40 (13) 3 Less than or equal to n3 Less than or equal to 15 (14) 20 Less than or equal to nB Less than or equal to 70 (15) and 15. Equipment in accordance with claim 14 where the distillation operation of column A for the separation of such high boiling point materials is carried out at a temperature of the bottom of column TA in the range from 185 to 280 °C and at a pressure PA at the top of the column in the range from 1000 to 20000 Pa, and the distillation operation of column B for the purification of such diaryl carbonate is carried out at a temperature of the bottom of column TB in the range from 185 to 280 °C and at a pressure PB at the top of the column in the range from 1000 to 20000 Pa. 16. Equipment in accordance with claim 14 or 15 where L, D, L/D and n for such reactive column satisfy the following formulas: 2000 ≤ L ≤ 6000, 150 ≤ D ≤ 1000, 3 ≤ L/D ≤ 30 and 15 ≤ n ≤ 60, respectively. LA, DA and nA for column A for the separation of such high boiling point materials. The following formulas apply to diaryl carbonate purification: 1000 ≤ or equal to LA ≤ or equal to 2500, 200 ≤ or equal to DA ≤ or equal to 600, and 30 ≤ or equal to nA ≤ or equal to 70, respectively. LB, DB, n1, n2, n3, and nB for column B for diaryl carbonate purification are as follows: 1500 ≤ or equal to LB ≤ or equal to 3000, 150 ≤ or equal to DB ≤ or equal to 500, 7 ≤ or equal to n1 ≤ or equal to 15, 12 ≤ or equal to n2 ≤ or equal to 30, 3 ≤ or equal to n3 ≤ or equal to 10, and 25 ≤ or equal to nB ≤ or equal to 55, respectively. TA ranges from 190 to 240 °C, and PA ranges from 2000 to... Temperatures in TB (Biochemical Oxygen Demand) range from 190 to 240°C, and temperatures in PB (Potty Leaping Body) range from 2000 to 15000 Pa. 17. Equipment in accordance with any of the claims 14 to 16 where each such reactive distillation column, column A for the separation of such high-boiling material and column B for the purification of such diaryl carbonate, is a distillation column which has trays and/or packing as its inner part. 18. An apparatus in compliance with any of the claims 14 to 17 where such reactive distillation column is a distillation column which has packing in the upper part of the column and trays in the lower part of the column as the inner part and the inner part of each of column A for the separation of such high boiling point material and column B for the purification of such diaryl carbonate as packing. 19. Equipment in accordance with claim 18 where the packing is a structured packing which is at least one of the selected group of packings which includes Mellapak, Gempak, Techno-Pak, Flexi-Pak, Sulzer packing, Goodroll packing and Glitchgrid packing. 20. Equipment in accordance with claims 17 or 18 where such tray of the reactive distillation column is a sif tray containing the sif portion and the reduced portion. 21. Equipment in accordance with claim 20 where such SIP tray has 100 to 1000 holes/sq.m in the SIP section. 22. Equipment in accordance with claim 20 or 21 where the area of the cross-section to the hole of such shift tray is between 0.5 and 5 cm².