US20090114523A1 - Method for treating condensates form polycodensates - Google Patents
Method for treating condensates form polycodensates Download PDFInfo
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- US20090114523A1 US20090114523A1 US11/918,636 US91863606A US2009114523A1 US 20090114523 A1 US20090114523 A1 US 20090114523A1 US 91863606 A US91863606 A US 91863606A US 2009114523 A1 US2009114523 A1 US 2009114523A1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
- C08G64/30—General preparatory processes using carbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/785—Preparation processes characterised by the apparatus used
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/148—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/19—Hydroxy compounds containing aromatic rings
Definitions
- the invention relates to a method of treating vapors and condensates that are produced during the production of polycondensates from bisphenols or polyhydric phenols by esterification and/or transesterification with alkyl and/or aryl esters of at least divalent organic or inorganic acids.
- polycarbonates, polyarylates, and copolymers of polyethylene terephthalate, polypropylene terephthalate, or polybutylene terephthalate can be prepared by esterification and/or transesterification of alkyl or aryl esters of organic or inorganic, at least divalent acids with bisphenols and subsequent interfacial polycondensation or melt polycondensation.
- These polycondensates are known as engineering plastics for their outstanding properties.
- the water or other vapors released during condensation contain, apart from the main cleavage product from the transesterification or esterification that is preferably phenol, additional monomers, oligomers, or products that are produced through thermal decomposition or rearrangements.
- the decomposition or rearrangement products formed in the reaction contaminate the monomers and oligomers also still present in the vapors and make it impossible to return the monomers and oligomers unpurified to the polycondensation process when products that are not discolored and that do not sufficiently meet rheological and mechanical quality requirements are to be produced.
- the cleavage products produced by the polycondensation such as phenols, alcohols, and water, are also so contaminated by the mentioned decomposition and rearrangement products that they cannot be easily reused.
- reaction products arising during thermal decomposition interfere with the reutilization of phenols present in the vapors, for example, for the production of bisphenol A, diphenyl carbonate, triphenyl borate, or for any other phenyl ester of an organic or inorganic acid.
- the object arose to develop a method of treating vapors and condensates that are produced during the production of the above-described polycondensates, the method making it possible, on the one hand, to recover the entrained monomers and to return them to the polycondensation and, on the other, to produce the cleavage products arising in the polycondensation, primarily phenol, in such a pure form that they can be reused for other reactions without deterioration in the product quality.
- a method for treating vapors and condensates that are produced during the production of polycondensates from bisphenols or polyhydric phenols by esterification or transesterification with alkyl or aryl esters of at least divalent organic or inorganic acids the method in which the treatment occurs in several succeeding cascaded condensers and/or distillation columns with respective connected condensers, where in each condenser the dew point and pressure are established such that in the individual stages the specific monomers, oligomers, or the decomposition and rearrangement products are separated.
- This method enables the return of useful materials to the process, is especially economical and cost-effective, avoids environmental pollution by chemicals, and utilizes the inevitably forming by-products to generate energy.
- This method can be used especially well for the regeneration of phenol-containing vapors and condensates and for the recovery of monomers, as they arise, for example, in the production of polycarbonates, polyarylates, or in the melt-phase polycondensation of polymers and copolymers, such as polyethylene terephthalate, polypropylene terephthalate, or polybutylene terephthalate with diphenols and bisphenols or polyhydric phenols by esterification or transesterification with alkyl or aryl esters of organic or inorganic, at least divalent acids and/or the acids themselves.
- polycondensates are known as engineering plastics with outstanding properties and special fields of application. Their production occurs either by interfacial polycondensation as in the case of polycarbonate or by means of melt polycondensation in the direct polycondensation method from dicarboxylic acids or dialcohols or diphenols or by transesterification processes from the corresponding acid esters.
- aromatic dihydroxy compounds for example, bis(4-hydroxyphenyl)alkanes, particularly bisphenol A
- diphenyl carbonate or terephthalic diphenolate in the presence of catalysts with cleavage of phenols, oligomerized, and finally polymerized in multiple stages under a progressive vacuum.
- Methods of this type are described in the German patent publications DE-B-1 495 730 [U.S. Pat. No. 3,535,280] and DE-C-2 334 852 [U.S. Pat. No. 3,888,826].
- the international patent application WO 2002/044244 [U.S. Pat. No.
- 6,838,543 describes a method by which polycarbonates are prepared by reaction of a monomeric carbonate component with at least one diphenol or dialcohol in the presence of a transesterification catalyst; here, the melted components are mixed with the transesterification catalyst and a product is produced that is polycondensed.
- the transesterification product is passed through a preliminary reactor, at least one intermediate reactor, and a final reactor, the reactors being connected in series and having a substantially horizontally driven shaft with mixing elements attached thereto.
- cleavage products 5 primarily phenol
- the distillate forming hereby is conveyed to a condenser 6 whose temperature is kept above the dew point of the cleavage products and that of monomers 1 and 2 , for example at a temperature above 200° C. and at 400 mbar.
- a condenser 6 whose temperature is kept above the dew point of the cleavage products and that of monomers 1 and 2 , for example at a temperature above 200° C. and at 400 mbar.
- high-boiling products 7 of the secondary reactions and present in vapors 5 of the first stage such as spiroidanes and indanes, can be separated out.
- the vapors continuing onward then pass through a rectification column 8 in which the lowest boiling cleavage products are stripped off at the top, but monomers 1 and 2 are drained off at different trays and returned to the first reaction stage 4 .
- the low-boiling cleavage product 10 is condensed in a condenser 11 and taken to a collection tank 28 .
- the first compressor stage 12 that, as indicated in FIG. 1 , may consist of a mechanical blower 12 , but also a jet exhaust, serves for generating the necessary low pressure.
- the condensates accumulating in the compression stage 12 in condenser 29 proceed to a collection tank 27 .
- the amount of low-boiling cleavage products 15 is even lower.
- more drastic measures such as a higher temperature and lower pressure than in stage 1 , are necessary to drive the reaction or the chain growth forward, thus, for example, 270 to 300° C. and 100 hPa to 10 hPa.
- the products from secondary reactions appear increasingly in the vapor gas stream 16 ; as a result, the amount of this product type, accumulating in condenser 6 ′, is also greater than in previous stage 4 .
- the condensate 7 accumulating in 6 ′, proceeds to a collection tank 24 .
- the amount of monomers 1 and 2 in the cleavage products has become so low that a separation is no longer worthwhile and everything is condensed in condenser 8 ′, before the lowest-boiling vapors are compressed in a compressor 16 .
- the vapors condensed in condenser 17 from the compressor 16 are combined with the stream 10 and taken to the collection tank 28 .
- Condensate 9 is supplied to the rectification stage 8 to increase the yield of monomers 1 and 2 and the cleavage products 10 .
- the lowest amount of cleavage products 20 accumulates.
- the most drastic measures such as the highest temperature and lowest pressure, are necessary to drive the reaction or the chain growth forward, thus, for example, 280 to 350° C. and 10 hPa to 0.1 hPa.
- the products in the secondary reaction occupy a large portion in the vapor gas stream 20 ; as a result, the amount accumulating in condenser 6 ′′ is also much higher than in the previous stages.
- the condensate 7 accumulating in 6 ′′ goes to collection tank 24 .
- the amount of monomers 1 and 2 in the cleavage products has become so low that a separation is no longer worthwhile and, for this reason, everything is condensed in condenser 8 ′′.
- the vapors condensed in condenser 22 from compression 21 are supplied as compressor condensate 22 to the collection tank 26 .
- the decision is made on the remaining amount of condensate 9 ′ after analysis in quality control (QC) whether it can still be supplied to rectification 8 to increase the yield of monomers 1 and 2 and cleavage products 10 , or is taken to collection tank 25 for special treatment according to FIG. 2 .
- the products collected in the tanks 24 to 28 are the results of a coarse fractionation or preliminary fractionation by selective choosing of the reaction and/or condensation conditions. They represent the first stage of an overall process that leads to an optimal and economic utilization of the monomers and cleavage products.
- the product from collection tank 24 has a high concentration of by-products, such as, for example, trisphenols, polymeric isopropenylphenols, dihydroxyindanes, dihydroxyspirobisindanes, alkyldistilbestrols, and polyhydroxyaryls, and only a minor effort is required to recover reusable products such as the monomers or cleavage product.
- Vapors 33 containing useful materials go to the top and proceed to rectification 34 , where they are rectified with product 9 and/or 9 ′ that stems from the middle fraction collected in collection tank 25 .
- a fraction each of monomers 1 and 2 is obtained from the lower trays; after passing quality control (QC), these are again taken either directly after purification by crystallization 41 , 43 and/or zone-melt process 42 , 44 as pure monomer 1 and/or 2 to the first stage with reactor 4 .
- the bottoms of stage 34 contain only high boilers, which proceed to incineration 32 .
- Product 35 escaping to the top of column 34 is rich in low-boiling cleavage products and enters the middle portion of column 36 , into which the main portion of the cleavage product from collection tanks 27 and 28 is also introduced.
- Pure cleavage product 37 , passing to the top, is recovered, which after condensation 39 is returned via return tank 40 and quality control (QC) either to column 36 or as the end product 45 is used for further reuse, for example, for the preparation of acid esters or of bisphenol A with acetone.
- the recovered product 45 meets the quality criteria of a product from the monomer synthesis.
- Quality control (QC) decides about the remaining bottom product 38 that is either again allocated to column 34 or to incineration 32 as waste.
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- Polymers & Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
Description
- The invention relates to a method of treating vapors and condensates that are produced during the production of polycondensates from bisphenols or polyhydric phenols by esterification and/or transesterification with alkyl and/or aryl esters of at least divalent organic or inorganic acids.
- It is known that polycarbonates, polyarylates, and copolymers of polyethylene terephthalate, polypropylene terephthalate, or polybutylene terephthalate can be prepared by esterification and/or transesterification of alkyl or aryl esters of organic or inorganic, at least divalent acids with bisphenols and subsequent interfacial polycondensation or melt polycondensation. These polycondensates are known as engineering plastics for their outstanding properties. The water or other vapors released during condensation contain, apart from the main cleavage product from the transesterification or esterification that is preferably phenol, additional monomers, oligomers, or products that are produced through thermal decomposition or rearrangements. The decomposition or rearrangement products formed in the reaction contaminate the monomers and oligomers also still present in the vapors and make it impossible to return the monomers and oligomers unpurified to the polycondensation process when products that are not discolored and that do not sufficiently meet rheological and mechanical quality requirements are to be produced. The cleavage products produced by the polycondensation, such as phenols, alcohols, and water, are also so contaminated by the mentioned decomposition and rearrangement products that they cannot be easily reused. The reaction products arising during thermal decomposition interfere with the reutilization of phenols present in the vapors, for example, for the production of bisphenol A, diphenyl carbonate, triphenyl borate, or for any other phenyl ester of an organic or inorganic acid.
- For this reason, the object arose to develop a method of treating vapors and condensates that are produced during the production of the above-described polycondensates, the method making it possible, on the one hand, to recover the entrained monomers and to return them to the polycondensation and, on the other, to produce the cleavage products arising in the polycondensation, primarily phenol, in such a pure form that they can be reused for other reactions without deterioration in the product quality.
- A method has now been found for treating vapors and condensates that are produced during the production of polycondensates from bisphenols or polyhydric phenols by esterification or transesterification with alkyl or aryl esters of at least divalent organic or inorganic acids, the method in which the treatment occurs in several succeeding cascaded condensers and/or distillation columns with respective connected condensers, where in each condenser the dew point and pressure are established such that in the individual stages the specific monomers, oligomers, or the decomposition and rearrangement products are separated.
- This method enables the return of useful materials to the process, is especially economical and cost-effective, avoids environmental pollution by chemicals, and utilizes the inevitably forming by-products to generate energy. This method can be used especially well for the regeneration of phenol-containing vapors and condensates and for the recovery of monomers, as they arise, for example, in the production of polycarbonates, polyarylates, or in the melt-phase polycondensation of polymers and copolymers, such as polyethylene terephthalate, polypropylene terephthalate, or polybutylene terephthalate with diphenols and bisphenols or polyhydric phenols by esterification or transesterification with alkyl or aryl esters of organic or inorganic, at least divalent acids and/or the acids themselves.
- The above-described polycondensates are known as engineering plastics with outstanding properties and special fields of application. Their production occurs either by interfacial polycondensation as in the case of polycarbonate or by means of melt polycondensation in the direct polycondensation method from dicarboxylic acids or dialcohols or diphenols or by transesterification processes from the corresponding acid esters. In the melt condensation for the production of polycarbonates and polyarylates, aromatic dihydroxy compounds, for example, bis(4-hydroxyphenyl)alkanes, particularly bisphenol A, are transesterified with diphenyl carbonate or terephthalic diphenolate in the presence of catalysts with cleavage of phenols, oligomerized, and finally polymerized in multiple stages under a progressive vacuum. Methods of this type are described in the German patent publications DE-B-1 495 730 [U.S. Pat. No. 3,535,280] and DE-C-2 334 852 [U.S. Pat. No. 3,888,826]. In addition, the international patent application WO 2002/044244 [U.S. Pat. No. 6,838,543] describes a method by which polycarbonates are prepared by reaction of a monomeric carbonate component with at least one diphenol or dialcohol in the presence of a transesterification catalyst; here, the melted components are mixed with the transesterification catalyst and a product is produced that is polycondensed. For the polycondensation, the transesterification product is passed through a preliminary reactor, at least one intermediate reactor, and a final reactor, the reactors being connected in series and having a substantially horizontally driven shaft with mixing elements attached thereto. Care is taken that a melt residence time of 5 minutes to 2 hours is maintained in the preliminary reactor and final reactor, the temperatures in the preliminary reactor are maintained within the range of from 220 to 300° C., and the pressure in the preliminary reactor is maintained in the range of from 100 to 800 mbar and in the final reactor in the range of from 0.1 to 50 mbar.
- If the operating conditions and process stages described in WO 2002/044244 are now applied to the production of polycarbonates, polyarylates, and other polymers or copolymers that were prepared from bisphenol A or other polyhydric phenols with at least divalent acids or the phenol-containing esters thereof, then different phenol-containing vapor and condensate compositions form depending on the residence time, catalyst, pressure, and temperature. Thus, for example, in a first stage primarily cleavage products from the esterification or transesterification arise such as water, phenols, or alcohols that still contain minor amounts of other monomers forming the polymer. Apart from the conventional cleavage products, depending on the selected reaction conditions, rearrangements and secondary reactions of the monomer compounds can also occur in this case, primarily of the polyhydric phenols and especially the bisphenols.
- Thus, for example, it is known from U.S. Pat. No. 4,294,994 that during treatment of bisphenol A with acids, formation of isopropenylphenol and its polymers, dihydroxyindanes, dihydroxyspirobisindanes, alkyldistilbestrols, trishydroxyphenyls, and polyhydroxyaryls occurs. These by-products because of their high molecular weight have high melting and boiling points and escape only under drastic reaction conditions, i.e. at high temperatures and low pressure. They cause, inter alia, discoloration and crosslinking in the polycondensate and disrupt the molecular structure. Other substances, such as, for example the monomers, also have high boiling points, but in the case of the raw materials employed for the production of engineering plastics these are far below those of the above-described secondary reaction products, so that they can be separated by fractional methods both from the high boilers and from the low boilers.
- The method of the invention will now be described in greater detail using the example of the reaction of diphenyl carbonate with bisphenol A in the presence of a catalyst, known for this reaction, according to
FIG. 1 andFIG. 2 . - The monomers, diphenyl carbonate 1 and
bisphenol A 2, introduced into a reactor 4, are reacted in the presence of acatalyst 3, so thatcleavage products 5, primarily phenol, accumulate in a large amount at the beginning of the reaction even at a low temperature and high pressure. The distillate forming hereby is conveyed to acondenser 6 whose temperature is kept above the dew point of the cleavage products and that ofmonomers 1 and 2, for example at a temperature above 200° C. and at 400 mbar. In this way, high-boilingproducts 7 of the secondary reactions and present invapors 5 of the first stage, such as spiroidanes and indanes, can be separated out. The vapors continuing onward then pass through arectification column 8 in which the lowest boiling cleavage products are stripped off at the top, butmonomers 1 and 2 are drained off at different trays and returned to the first reaction stage 4. - The product collected in the bottom of
column 8, withhigh boilers 30, which correspond substantially to the products of the secondary reaction, is combined with thebottom product 7 from the first condensation [6] and conveyed to acollection tank 24. - The low-boiling
cleavage product 10 is condensed in acondenser 11 and taken to acollection tank 28. Thefirst compressor stage 12 that, as indicated inFIG. 1 , may consist of amechanical blower 12, but also a jet exhaust, serves for generating the necessary low pressure. The condensates accumulating in thecompression stage 12 incondenser 29 proceed to acollection tank 27. - In the second reaction section (reactor 14, supplied with
product 13 from reactor 4), the amount of low-boiling cleavage products 15 is even lower. In this stage 14, however, because of the higher product viscosity, more drastic measures, such as a higher temperature and lower pressure than in stage 1, are necessary to drive the reaction or the chain growth forward, thus, for example, 270 to 300° C. and 100 hPa to 10 hPa. Because of the higher thermal loading, the products from secondary reactions appear increasingly in thevapor gas stream 16; as a result, the amount of this product type, accumulating incondenser 6′, is also greater than in previous stage 4. Thecondensate 7, accumulating in 6′, proceeds to acollection tank 24. The amount ofmonomers 1 and 2 in the cleavage products has become so low that a separation is no longer worthwhile and everything is condensed incondenser 8′, before the lowest-boiling vapors are compressed in acompressor 16. The vapors condensed incondenser 17 from thecompressor 16 are combined with thestream 10 and taken to thecollection tank 28. Condensate 9 is supplied to therectification stage 8 to increase the yield ofmonomers 1 and 2 and thecleavage products 10. - In the third reaction section (
reactor 19, supplied withproduct 18 from reactor 14), the lowest amount ofcleavage products 20 accumulates. Here, however, because of the highest product viscosity, the most drastic measures, such as the highest temperature and lowest pressure, are necessary to drive the reaction or the chain growth forward, thus, for example, 280 to 350° C. and 10 hPa to 0.1 hPa. Because of the high thermal loading, the products in the secondary reaction occupy a large portion in thevapor gas stream 20; as a result, the amount accumulating incondenser 6″ is also much higher than in the previous stages. Thecondensate 7 accumulating in 6″ goes tocollection tank 24. The amount ofmonomers 1 and 2 in the cleavage products has become so low that a separation is no longer worthwhile and, for this reason, everything is condensed incondenser 8″. The vapors condensed incondenser 22 fromcompression 21 are supplied ascompressor condensate 22 to thecollection tank 26. The decision is made on the remaining amount ofcondensate 9′ after analysis in quality control (QC) whether it can still be supplied torectification 8 to increase the yield ofmonomers 1 and 2 andcleavage products 10, or is taken tocollection tank 25 for special treatment according toFIG. 2 . - The products collected in the
tanks 24 to 28 are the results of a coarse fractionation or preliminary fractionation by selective choosing of the reaction and/or condensation conditions. They represent the first stage of an overall process that leads to an optimal and economic utilization of the monomers and cleavage products. The product fromcollection tank 24 has a high concentration of by-products, such as, for example, trisphenols, polymeric isopropenylphenols, dihydroxyindanes, dihydroxyspirobisindanes, alkyldistilbestrols, and polyhydroxyaryls, and only a minor effort is required to recover reusable products such as the monomers or cleavage product. This is achieved by anotherrectification 31 to increase the yield of monomers and cleavage products, before the high-boiling and discoloredbottom product 32 is subjected to a thermal recovery. Or otherwise disposed of. The content ofmonomers 1 and 2 and low-boilingcleavage product 10 is less than 1% by weight in theoutgoing product 32. -
Vapors 33 containing useful materials go to the top and proceed torectification 34, where they are rectified withproduct 9 and/or 9′ that stems from the middle fraction collected incollection tank 25. In this case, a fraction each ofmonomers 1 and 2 is obtained from the lower trays; after passing quality control (QC), these are again taken either directly after purification bycrystallization melt process stage 34 contain only high boilers, which proceed toincineration 32. -
Product 35 escaping to the top ofcolumn 34 is rich in low-boiling cleavage products and enters the middle portion ofcolumn 36, into which the main portion of the cleavage product fromcollection tanks Pure cleavage product 37, passing to the top, is recovered, which aftercondensation 39 is returned viareturn tank 40 and quality control (QC) either tocolumn 36 or as theend product 45 is used for further reuse, for example, for the preparation of acid esters or of bisphenol A with acetone. The recoveredproduct 45 meets the quality criteria of a product from the monomer synthesis. Quality control (QC) decides about the remainingbottom product 38 that is either again allocated tocolumn 34 or toincineration 32 as waste. -
- 1 monomer A diphenyl carbonate
- 2 monomer B bisphenol A
- 3 catalyst
- 4 first reactor stage (first reaction of monomers)
- 5 vapors (cleavage products, oligomers, monomers)
- 6 high-boiler condensation first stage
- 6′ high-boiler condensation second stage
- 6″ high-boiler condensation third stage
- 7 condensate (highest boiling points)
- 8 rectification first stage
- 8′ condensation second stage
- 8″ condensation third stage
- 9 middle condensate fraction
- 9′ middle condensate fraction, not suitable for return to 8
- 10 condensate (lowest boiling point), cleavage product condensate of monomer A and/or monomer B
- 11 condenser
- 12 compressor (1st pressure stage, highest pressure)
- 13 product with a short chain length (1 to 10)
- 14 second reactor stage (precondensation, medium chain length)
- 15 vapors (cleavage products, oligomers, monomers)
- 16 compressor (2nd pressure stage, reduced pressure)
- 17 gas cooler/compressor-condenser
- 18 product with a medium chain length (5 to 50)
- 19 third reactor stage (polycondensation, long chain length)
- 20 vapors (cleavage products, oligomers, monomers)
- 21 compressor (3rd pressure stage, lowest pressure)
- 22 gas cooler/compressor-condenser
- 23 end product chain length (50 to 300)
- 24 collection tank condensate highest boilers
- 25 collection tank condensate high boilers
- 26 collection tank compressor condensate, lowest pressure
- 27 collection tank compressor condensate, highest pressure
- 28 condensate collection tank compressor condensate, 1st compressor stage
- condenser, 1st compressor stage
- 30 bottom product rectification
- 31 evaporator for products with highest boiling point
- 32 waste for incineration
- 33 evaporation product
- 34 rectification for products with middle boiling point
- 35 evaporation product
- 36 cleavage product rectification
- 37 pure cleavage product for further processing
- 38 bottom product, after
analysis waste 32 or back to 34 - 39 cleavage product cooler
- 40 collection tank cleavage products
- 41 fractional crystallization monomer 1
- 42 zone-melt purification method monomer 1
- 43
fractional crystallization monomer 2 - 44 zone-melt
purification method monomer 2 - 45 pure cleavage product for further reaction
- QC analysis site, quality control, and branching
Claims (8)
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102005017427A DE102005017427A1 (en) | 2005-04-15 | 2005-04-15 | Process for the treatment of condensates from polycondensation |
DE102005017427.2 | 2005-04-15 | ||
PCT/EP2006/001772 WO2006108469A1 (en) | 2005-04-15 | 2006-02-27 | Method for treating condensates from polycodensates |
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US20090114523A1 true US20090114523A1 (en) | 2009-05-07 |
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US11/918,636 Abandoned US20090114523A1 (en) | 2004-05-15 | 2006-02-27 | Method for treating condensates form polycodensates |
US12/268,516 Active 2030-03-22 US8029079B2 (en) | 2005-04-15 | 2008-11-11 | Safety cabinet |
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US12/268,516 Active 2030-03-22 US8029079B2 (en) | 2005-04-15 | 2008-11-11 | Safety cabinet |
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EP (1) | EP1869102A1 (en) |
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KR (1) | KR20080015406A (en) |
CN (1) | CN101160341A (en) |
DE (1) | DE102005017427A1 (en) |
WO (1) | WO2006108469A1 (en) |
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US7946665B2 (en) * | 2008-11-11 | 2011-05-24 | Dueperthal Sicherheitstechnik GmbH | Safety cabinet with multipanel folding door |
CN102126958B (en) * | 2010-12-30 | 2013-12-04 | 江苏淮河化工有限公司 | Device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization |
US8727459B2 (en) * | 2011-07-08 | 2014-05-20 | SSI Schäfer Noell GmbH Lager- und Systemtechnik | Multiple-door switchgear cabinet |
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CN104109101B (en) * | 2013-06-06 | 2016-12-28 | 上海志诚化工有限公司 | A kind of quasiconductor ultra-pure electronic grade chemical reagent purification devices |
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2006
- 2006-02-27 WO PCT/EP2006/001772 patent/WO2006108469A1/en active Application Filing
- 2006-02-27 EP EP06707287A patent/EP1869102A1/en not_active Withdrawn
- 2006-02-27 CN CNA2006800126037A patent/CN101160341A/en active Pending
- 2006-02-27 US US11/918,636 patent/US20090114523A1/en not_active Abandoned
- 2006-02-27 KR KR1020077026506A patent/KR20080015406A/en not_active Application Discontinuation
- 2006-02-27 JP JP2008505746A patent/JP2008535980A/en not_active Withdrawn
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2008
- 2008-11-11 US US12/268,516 patent/US8029079B2/en active Active
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US3888826A (en) * | 1972-07-10 | 1975-06-10 | Mitsubishi Gas Chemical Co | Process for preparing aromatic polycarbonates |
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Also Published As
Publication number | Publication date |
---|---|
WO2006108469A1 (en) | 2006-10-19 |
US8029079B2 (en) | 2011-10-04 |
JP2008535980A (en) | 2008-09-04 |
DE102005017427A1 (en) | 2006-10-19 |
EP1869102A1 (en) | 2007-12-26 |
US20090134756A1 (en) | 2009-05-28 |
KR20080015406A (en) | 2008-02-19 |
CN101160341A (en) | 2008-04-09 |
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