Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
  • B29B13/00—Conditioning or physical treatment of the material to be shaped
  • B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
• • 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
  • C08G64/40—Post-polymerisation treatment
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
  • B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
• • 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
  • C08G64/40—Post-polymerisation treatment
  • C08G64/406—Purifying; Drying
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
  • B29K2069/00—Use of PC, i.e. polycarbonates or derivatives thereof, as moulding material

Definitions

• the invention relates to an improved process for the production of products made of polycarbonate and the products themselves.
• phase interface dihydroxydiarylalkanes implemented in the form of their alkali metal salts with phosgene in heterogeneous phase in the presence of inorganic bases such as sodium hydroxide and an organic solvent in which the product polycarbonate is readily soluble.
• inorganic bases such as sodium hydroxide and an organic solvent in which the product polycarbonate is readily soluble.
• the aqueous phase distributed in the organic phase and after the reaction, the organic polycarbonate-containing phase is washed with an aqueous liquid, among other things, electrolytes are to be removed, and the washing liquid is then separated off.
• the solvent is removed and finally the polycarbonate in granulate form for later processing on products such as magneto-optical objects, in particular laser-readable data storage devices, lenses for the automotive industry, optical lenses, polycarbonate plates, foils etc. are provided.
• the granulate must then be melted again and the melt depending on the desired product, e.g. can be further processed in injection molding or extrusion technology.
• polycarbonate which has been produced by the melt transesterification process in which bisphenols are reacted with diaryl carbonates in the melt with the release of hydroxyarylene, is first processed into granules, which are then processed further, e.g. after the injection molding or extrusion process must be melted again.
• the object of the invention is to achieve quality improvements in polycarbonate products by means of an improved manufacturing process.
• the object is achieved in that the polycarbonate melt is used directly in production, without prior granulation, whereby, of course, usual cleaning steps, such as, for example, filtrations, can be interposed before processing.
• the reduced thermal load on the material leads to an improved quality of the products.
• the saving of an additional processing step also solves the task of making a simpler and accordingly more efficient process for the production of polycarbonate products available.
• the invention initially relates to a process for the production of polycarbonate products, in which one obtained by the phase interface process
• the polycarbonate solution is washed with an aqueous washing liquid, the washing liquid is separated off and the solvent is evaporated off, and the mixture of organic polycarbonate solution and the remaining washing liquid obtained after the washing liquid has been separated is heated by indirect heat exchange until a clear solution has been reached and for separating Solids is filtered, and then
• the solution with a polymer content of 5 to 20% by weight in a combination of a tube bundle heat exchanger and a thin-film evaporator or a snake tube evaporator or in a tube bundle heat exchanger, each with a downstream separator at a temperature of 150 is concentrated to 60 to 75% by weight to 250 ° C., the pressure in the separator being approximately 0.1 to 0.4 MPa, preferably ambient pressure (ie approximately 0.1 MPa),
• the solution is concentrated in a tube bundle heat exchanger with a downstream separator at a temperature of 250 to 350 ° C. from 60 to 75% by weight to at least 95% by weight, in particular to 98 to 99.9% by weight, the shell and tube heat exchanger being vertical, heated straight tubes with or without built-in static mixer with a has an inner diameter of 5 to 30 mm, preferably 5 to 15 mm, a length of 0.5 to 4 m, preferably 1 to 2 m, and the throughput per heat exchanger tube through the tubes is 0.5 to 10 kg / h, preferably 3 to 7 kg / h, based on the polymer and the pressure in the separator being 0.5 kPa to 0.1 MPa, in particular 3 kPa to 0.1 kPa, preferably 3 kPa to
• the throughput per heat exchanger tube through the tubes is 0.5 to 10 kg / h, preferably 3 to 7 kg / h, based on the polymer and wherein the pressure in the separator is 0.05 kPa to 0.1 MPa, preferably 0.1 kPa to 2 kPa,
• Temperatures advantageous because these are significantly lower than the temperatures that usually occur in the final evaporation in this step by means of extruders, which results in a lower thermal load on the product and thus also in a higher product quality.
• the saving of the otherwise usual re-melting of the granules leads to the simplification also to a lower thermal load on the product and thus to an improvement in product quality.
• polycarbonate melts obtained from the melt transesterification process, optionally cooled to a suitable temperature, can be processed directly.
• polycarbonate melts obtained from the melt transesterification process optionally cooled to a suitable temperature, can be directly processed further.
• step C the temperatures maintained there must be made possible by using special evaporator devices.
• an evaporator e.g. B. for the production of polycarbonate sheets.
• polycarbonate should include both homopolycarbonates and copolycarbonates and mixtures thereof.
• the polycarbonates according to the invention can be aromatic polyester carbonates or polycarbonates which are present in a mixture with aromatic polyester carbonates.
• the term polycarbonate is then used to represent the aforementioned polymers.
• the polycarbonate according to the invention is obtained by the so-called phase boundary process (H. Schnell “Chemistry and Physics of Polycarbonates", Polymer Review, Vol.IXS. 22ff, Interscience Publishers, New York 1964), in which the solution containing polycarbonate is then washed with a washing liquid , the washing liquid is separated off and the solvent is evaporated off.
• the polycarbonate can also be obtained by the so-called melt transesterification process (DG LeGrand et al., "Jlandbook of Polycarbonate Science and Technology", Marcel Dekker Verlag New York, Basel, 2000, p. 12ff.).
• melts obtained at the end of the respective manufacturing process are then not granulated, but processed directly for the end products.
• Compounds to be used preferably as starting compounds according to the invention are bisphenols of the general formula HO-Z-OH, in which Z is a divalent organic radical having 6 to 30 carbon atoms and one or more aromatic
• Examples of such compounds are bisphenols which belong to the group of the dihydroxydiphenyls, bis (hydroxyphenyl) alkanes, inganbisphenols, bis (hydroxyphenyl) ethers, bis (hydroxyphenyl) sulfones, bis (hydroxyphenyl) ketones and, ⁇ '-bis (hydroxyphenyl) diisopropylbenzenes belong.
• Particularly preferred bisphenols which belong to the abovementioned connecting groups are 2,2-bis (4-hydroxyphenyl) propane (bisphenol-A), tetraalkylbisphenol-A, 4,4- (meta-phenylenediisopropyl) diphenol (bisphenol M), 1,1-bis (4-hydroxyphenyl) - 3,3,5-trimethylcyclohexanone and, if appropriate, their mixtures.
• Particularly preferred copolycarbonates are those based on the monomers bisphenol-A and 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane.
• the bisphenol compounds to be used according to the invention are reacted with carbonic acid compounds, in particular phosgene and diphenyl carbonate.
• the polyester carbonates according to the invention are obtained by reacting the bisphenols already mentioned, at least one aromatic dicarboxylic acid and optionally carbonic acid.
• aromatic dicarboxylic acids are, for example, orthophthalic acid, terephthalic acid, isophthalic acid, 3,3'- or 4,4'-diphenyldicarboxylic acid and benzophenone dicarboxylic acids.
• Inert organic solvents used in the process are preferably dichloromethane or mixtures of dichloromethane and chlorobenzene.
• the reaction can be accelerated by catalysts such as tertiary amines, N-alkylpiperidines or onium salts.
• Tributylamine, triemylarnine and N-ethylpiperidine are preferably used.
• a monofunctional phenol such as phenol, cumylphenol, p-tert-butylphenol or 4- (l, l, 3,3-tetramethylbutyl) phenol, can be used as chain terminator and molecular weight regulator.
• isatin biscresol can be used as branching agent.
• the bisphenols are dissolved in an aqueous alkaline phase, preferably sodium hydroxide solution.
• the chain terminators which may be required for the production of copolycarbonates are dissolved in amounts of 1.0 to 20.0 mol% per mole of bisphenol, in the aqueous alkaline phase or added to them in bulk in an inert organic phase.
• phosgene is introduced into the mixer containing the other reaction components and the polymerization is carried out.
• Some, up to 80 mol%, preferably from 20 to 50 mol%, of the carbonate groups in the polycarbonates can be replaced by aromatic dicarboxylic acid ester groups.
• thermoplastic polycarbonates have average molecular weights M w and a foreign particle index of less than
• the sodium content is preferably less than 30 ppb, measured by atomic absorption spectroscopy.
• the aqueous phase is emulsified in the organic phase. This creates droplets of different sizes.
• the organic phase containing the polycarbonate usually several times with a washed aqueous liquid and separated from the aqueous phase as far as possible after each wash.
• Diluted Müierals ⁇ ure such as HCl or H 3 PO and for further purification demineralized water are used as washing liquid for the separation of the catalyst.
• the concentration of HCl or H 3 PO 4 in the washing liquid can be, for example, 0.5 to 1.0% by weight.
• phase separation devices for separating the washing liquid from the organic phase.
• the solvent is evaporated off in stages A to C.
• solution PC also serve the SPC process (melt transesterification process PC).
• polycarbonate is produced in such a way that in the first stage of oligocarbonate synthesis quaternary
• Ammonium, phosphonium compounds in amounts of 10 "4 to 10 " 8 mol, based on 1 mol of bisphenol, the melting of the reactants being found at temperatures from 80 ° C. to 180 ° C., preferably at 100 ° C., in the first stage to 150 ° C under atmospheric pressure for up to 5 hours, preferably from 0.25 to
• the SPC process is carried out without a solvent. Therefore, in contrast to the LPC process, no tube / strand evaporator or extruder is required.
• the polycarbonate melts thus obtained from the various processes are then directly processed without an intermediate step, e.g. Granulation and remelting, further processed to the desired products, whereby, of course, usual cleaning steps, such as e.g. Filtration can be interposed.
• an intermediate step e.g. Granulation and remelting
• These products can e.g. be produced by the injection molding, extrusion or casting process (film).
• films include, but are not limited to, polycarbonate sheets such as for glazing greenhouses with double-wall sheets or twin-wall sheets, solid sheets, magneto-optical data storage / mini disk, compact disk, DVD, optical lenses and prisms, light guides, glazing for motor vehicles, headlights, foils , medical devices, packaging (eg for food and medical products etc.), housings for electrical and electronic articles (eg computer housings, mobile phone parts etc.), glasses and frames, household items (such as electrical articles, eg irons etc.), toys etc. to understand.
• polycarbonate sheets such as for glazing greenhouses with double-wall sheets or twin-wall sheets, solid sheets, magneto-optical data storage / mini disk, compact disk, DVD, optical lenses and prisms, light guides, glazing for motor vehicles, headlights, foils , medical devices, packaging (eg for food and medical products etc.), housings for electrical and electronic articles (eg computer housings
• the method according to the invention is particularly suitable for the production of products which have to meet high demands on the optical quality, ie transparency and colorlessness, for example glazing of greenhouses and motor vehicles, headlights, magneto-optical data storage / mini disk, compact disk, DVD, optical lenses and prisms, light guides, glasses etc.
• the method according to the invention is very particularly suitable for producing glazing for greenhouses and motor vehicles and headlights.
• Another very particularly suitable application is the production of magneto-optical data storage devices / mini disks, compact disks and DVDs.
• Another very particularly suitable application is the production of optical lenses and prisms, light guides and spectacle lenses.
• the preferred molecular weight range for the media is 12,000 to

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Mechanical Engineering (AREA)
• Health & Medical Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Polyesters Or Polycarbonates (AREA)
• Manufacture Of Macromolecular Shaped Articles (AREA)

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• 2000
  • 2000-08-23 DE DE10052873A patent/DE10052873A1/de not_active Withdrawn
• 2001
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  • 2001-08-10 CN CNB018144497A patent/CN100338114C/zh not_active Expired - Fee Related
  • 2001-08-10 WO PCT/EP2001/009245 patent/WO2002016470A1/de active Application Filing
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  • 2001-08-20 US US09/933,360 patent/US20020074683A1/en not_active Abandoned
• 2003
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