US3390965A - Reactor for the manufacture of polyethylene phthalates - Google Patents

Reactor for the manufacture of polyethylene phthalates Download PDF

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US3390965A
US3390965A US437368A US43736865A US3390965A US 3390965 A US3390965 A US 3390965A US 437368 A US437368 A US 437368A US 43736865 A US43736865 A US 43736865A US 3390965 A US3390965 A US 3390965A
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reactor
chambers
chamber
adjustable
liquids
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US437368A
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Bachmann Ditmar
Hoyer Hans
Welfers Egidius
Fischer Wolfgang
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Hoechst AG
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Hoechst AG
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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
    • 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
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/2415—Tubular reactors
    • B01J19/242—Tubular reactors in series
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00121—Controlling the temperature by direct heating or cooling
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00162—Controlling or regulating processes controlling the pressure
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00168—Controlling or regulating processes controlling the viscosity
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00182—Controlling or regulating processes controlling the level of reactants in the reactor vessel
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/18—Details relating to the spatial orientation of the reactor
    • B01J2219/182—Details relating to the spatial orientation of the reactor horizontal

Description

y 2, 1968 o. BACHMANN ET AL 3,390,965
REACTOR FOR THE MANUFACTURE OF POLYETHYLENE PHTHALATES Filed March 5, 1965 mvzmons lu 0mm: BACHMANN HANS HOYER I EGIDIUS WELFERS WOLFGANG FISCHER ATTORNEYS United States Patent Office Patented July 2, 1968 2 Claims. ci. 23 285 The present invention'relates to a reactor for the continuous manufacture of pure or mixed esters of terephthalic acid and isophthalic acid, particularly polyethylene terephthalate and polyethylene isophthalate, from esters of terephthalic or isophthalic acid with lower alcohols, particularly methanol and ethylene glycol. These esters are referred to herein as polyethylene phthalates.
In the known processes for the continuous manufacture of polyethylene phthalates several separate apparatus are used of which the first, a vessel provided with a stirrer or an apparatus similar to the known fractionating columns, serves for the re-esterification. The second and the following apparatus serve for the polycondensation proper. In the first stage of the condensation, reactors provided with a stirrer or plate-type columns are used. For the next stage of the condensation, the so-called main condensation, film reactors are advantageously used in which the reaction mixture is distributed in thin layers. It has been proposed, for example, to carry out the main condensation in reactors constructed like film or falling film evaporators. It has also been proposed to use reactors in which the stream of liquid material is dammed up in steps by weirs.
The-three process steps differ not only in the apparatus that are advantageously used but also in the physical conditions under which they are carried out, such as pressure and temperature, and particularly in the flow propertiesof the material used.
The liquid mixture which is being reacted is conveyed from one apparatus to the next one through'pipes by means of mechanically driven devices, such as gear pumps or diaphragm pumps.
The use of separate apparatusfor each process step enables each apparatus to be well adapted to the respective process steps, but involves also great disadvantages. The large number of spots of packing in apparatus, pipes and conveying devices, particularly at the openings for the drives for the stirrers, scrapers and pump shafts, allow air to enter which alters the degree of whiteness of the product. Mere traces of air or oxygen lead to products of inferior quality or rejected products. This disadvantage of the known apparatus cannot even be overcome satisfactorily by thorough control of the process by the operator or by automatic devices. At best, the process can be interrupted prematurely.
Another disadvantage of such apparatus is that the control of the stream of material and the adjustment of the pressure and temperature to the course of the process is difiicult to achieve in apparatus of such dilferent type.
To avoid the above disadvantages in the continuous manufacture of polyethylene phthalates from dimethyl phthalates and ethylene glycol, it has been proposed to use a reactor which comprises several chambers arranged side by side which can be heated separately and which are provided with weirs. Each chamber communicates with the adjacent chamber through an adjustable opening disposed below the level of the overflow edge of the weirs. The gas chambers, i.e. the spaces above the liquid level in the individual chambers, are each connected with a separate steam ejector device or an adjustable stage of a common multistage steam ejector device so that the reactor can be operated with regulatable pressures graduated from the entrance to the outlet of the reactor.
Besides offering advantages as to arrangement, this reactor enables the known polycondensation process to be effectively adjusted so that any desired degree of polycondensation can be obtained. However, when changing over to another product, for example a product of lower degree of polymerization or lower viscosity, it takes some time until a steady state of operation is obtained.
Now we have found that the above disadvantage can be avoided by improving the said reactor by providing at least two of the chambers, advantageously the last ones, each with an adjustable discharge device with shutoff means through which the liquid space of the chamber communicates with a device disposed after the reactor, such as a conveying means, mixer, extruder, roll mill, spinning device or another device appropriate for forming the product.
This construction enables partial streams of polycondensate to be united with the product that issues from the last chamber, while omitting one or more chambers. The degree of viscosity of the mixture depends only on the viscosity and quantity of the individual partial streams. Any desired degree of viscosity can rapidly be adjusted within the limits given by the partial streams, without time-consuming readjustment of the reactor. This mode of working is particularly advantageous if the type of further treatment varies from case to case.
As discharge device it is advantageous to use a screw pump with a variable drive. It is also possible to use worm pumps or other known discharge devices. Such discharge devices enable the weight velocity of flow of the streams of polycondensate to be adjusted as desired. When the pumps stand still, they act as shut-off device. They can advantageously be used to overcome pressure ditferences between the place of drawing-ofi and the place where the partial streams are united, without differences in output occurring. With the help of such discharge devices known in themselves the streams of material can therefore be fed to a common conveying means, for example a collecting pipe or screw conveyor, or they may be directly introduced, without being collected, into a mixer or another apparatus, without the adjusted quantities being varied.
For example, the partial streams of polycondensate may be fed to a spinning device in a manner such that they are united in the spinning head. Such arrangement enables the manufacture of three-dimensionally crimped fibers and filaments of particularly good crimp retentivity.
An example of an improved reactor constructed in accordance with the invention will now be described in greater detail with reference to the accompanying drawing.
In the drawing which is a longitudinal section through the improved reactor constructed in accordance with the invention, the chambers are denoted by reference numerals 1 to 5 in the direction in which polycondensation proceeds. To simplify the drawing only the last chamber 5 and penultimate chamber 4 are each provided with a discharge device. Discharge devices 6 and 7 are screw pumps. Instead of screw pumps, worm pumps or other known discharge devices may be used. Through pipes 8 and 9 the polycondensate is conducted to a mixer 10. The said pipes 8 and 9 run separately and join only immediately before the inlet to the mixer.
Discharge devices 6 and 7 are of one and the same type and have identical dimensions. The viscosity is only insignificantly influenced by the mixing operation and is in the first place a function of the rate of the numbers of revolutions to which the pumps have been adjusted. In the reactor shown in the drawing, the limits within which the viscosity can be adjusted are given by the cosities of the two partial streams.
The lower limit of the range within which the viscosity may be adjusted can still be lowered if, contrary to the reactor shown in the drawing, further chambers are provided with discharge devices and connected accordingly.
We claim:
1. In a reactor for the continuous manufacture of polyethylene phthalates from dimethyl phthalates and ethylene glycol, which reactor is provided with several chambers where chambers are arranged side by side, each of which is provided with weirs, separate heating means, and each of which chambers communicates with the adjacent chambers through an adjustable opening placed below the level of the overflow edge of the weirs, and in which chamber the gas space above the liquid level is connected with a separate steam ejector device or for each chamber an individually adjustable and common steam ejector device, the improvement comprising of: at least two chambers, each with an adjustable discharge device having shut-off means, said devices communicating exteriorly of the reactor through the liquid space of each chamber from which visliquids are discharged and through a device in which the withdrawn liquids from each chamber are joined and discharged from the reactor; and means for regulating each of the adjustable discharge devices responsive to a preselected combination of liquids wtihdrawn from each of the chambers.
2. The reactor according to claim 1 wherein the discharge device is provided with a screw pump with a variable drive through which the liquid space of a chamber is connected with the device from which the liquids from each chamber are joined and discharged and means for regulating the operation of each of the discharge devices to withdraw a liquid of a preselected degree of condensation.
References Cited UNITED STATES PATENTS 3,251,657 5/1966 Bachmann et al. 23285 JAMES H. TAYMAN, JR., Primary Examiner. M. O. WOLK, Examiner.

Claims (1)

1. IN A REACTOR FOR THE CONTINUOUS MANUFACTURE OF POLYETHYLENE PHTHALATES FROM DIMETHYL PHTHALATES AND ETHYLENE GLYCOL, WHICH REACTOR IS PROVIDED WITH SEVERAL CHAMBERS WHERE CHAMBERS ARE ARRANGED SIDE BY SIDE, EACH OF WHICH IS PROVIDED WITH WEIRS, SEPARATE HEATING MEANS, AND EACH OF WHICH CHAMBERS COMMUNICATES WITH THE ADJACENT CHAMBERS THROUGH AN ADJUSTABLE OPENING PLACED BELOW THE LEVEL OF THE OVERFLOW EDGE OF THE WEIRS, AND IN WHICH CHAMBER THE GAS SPACE ABOVE THE LIQUID LEVEL IS CONNECTED WITH A SEPARATE STAM EJECTOR DEVICE OR FOR EACH CHAMBER AN INDIVIDUALLY ADJUSTABLE AND COMMON STEAM EJECTOR DEVICE, THE IMPROVEMENT COMPRISING OF: AT LEAST TWO CHAMBERS, EACH WITH AN ADJUSTABLE DISCHARGE DEVICE HAVING SHUT-OFF MEANS, SAID DEVICES COMMINICATING EXTERIORLY OF THE REACTOR THROUGH THE LIQUID SPACE OF EACH CHAMBER FROM WHICH LIQUIDS ARE DISCHARGED AND THROUGH A DEVICE IN WHICH THE WITHDRAWN LIQUIDS FROM EACH CHAMBER ARE JOINED AND DISCHARGED FROM THE REACTOR; AND MEANS FOR REGULATING EACH OF THE ADJUSTABLE DISCHARGE DEVICES RESPONSIVE TO A PRESELECTED COMBINATION OF LIQUIDS WITHDRAWN FROM EACH OF THE CHAMBERS.
US437368A 1962-05-11 1965-03-05 Reactor for the manufacture of polyethylene phthalates Expired - Lifetime US3390965A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DEF36779A DE1189271B (en) 1962-05-11 1962-05-11 Process for the continuous production of polyesters
DEF42219A DE1259565B (en) 1962-05-11 1964-03-06 Device for the continuous production of poly (ethylene glycol terephthalate)

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US3390965A true US3390965A (en) 1968-07-02

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US279132A Expired - Lifetime US3251657A (en) 1962-05-11 1963-05-09 Reactor for the manufacture of polyethylene phthalates
US437368A Expired - Lifetime US3390965A (en) 1962-05-11 1965-03-05 Reactor for the manufacture of polyethylene phthalates

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US (2) US3251657A (en)
BE (2) BE660780A (en)
CH (2) CH422338A (en)
DE (2) DE1189271B (en)
FR (1) FR88261E (en)
GB (2) GB1045343A (en)
NL (2) NL6502823A (en)

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3483151A (en) * 1966-06-10 1969-12-09 Melle Usines Sa Continuous process for the preparation of polyesters
NL1017260C2 (en) * 2001-02-01 2002-08-02 Dsm Nv Continuous production of thermoplastic polyesters, includes a polycondensation step in which the partial pressure of the volatile reaction products is higher at the start of polycondensation than at the end
US20080221296A1 (en) * 2007-03-08 2008-09-11 Debruin Bruce Roger Polyester production system employing an unagitated esterification reactor
US20080227931A1 (en) * 2000-12-07 2008-09-18 Debruin Bruce Roger Polyester process using a pipe reactor
US20090018281A1 (en) * 2007-07-12 2009-01-15 Eastman Chemical Company Multi-level tubular reactor with internal tray
WO2009009033A1 (en) * 2007-07-12 2009-01-15 Eastman Chemical Company Horizontal trayed reactor
US20090047186A1 (en) * 2005-03-22 2009-02-19 Epc Industrial Engineering Gmbh Modular device for the continuous degassing and production of polymer precondensate with high reaction product surface to volume ratio with gentle treatment of the reaction product mass
US7649109B2 (en) 2006-12-07 2010-01-19 Eastman Chemical Company Polyester production system employing recirculation of hot alcohol to esterification zone
US7842777B2 (en) 2007-07-12 2010-11-30 Eastman Chemical Company Sloped tubular reactor with divided flow
US7847053B2 (en) 2007-07-12 2010-12-07 Eastman Chemical Company Multi-level tubular reactor with oppositely extending segments
US7858730B2 (en) 2007-07-12 2010-12-28 Eastman Chemical Company Multi-level tubular reactor with dual headers
US7863477B2 (en) 2007-03-08 2011-01-04 Eastman Chemical Company Polyester production system employing hot paste to esterification zone
US7868130B2 (en) 2007-07-12 2011-01-11 Eastman Chemical Company Multi-level tubular reactor with vertically spaced segments
US7868129B2 (en) 2007-07-12 2011-01-11 Eastman Chemical Company Sloped tubular reactor with spaced sequential trays
US7872090B2 (en) 2007-07-12 2011-01-18 Eastman Chemical Company Reactor system with optimized heating and phase separation
US7943094B2 (en) 2006-12-07 2011-05-17 Grupo Petrotemex, S.A. De C.V. Polyester production system employing horizontally elongated esterification vessel

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE632261A (en) * 1962-05-11
NL294427A (en) * 1962-06-23
US3476521A (en) * 1967-01-20 1969-11-04 Joseph T Wise Polymerizing apparatus
US3927983A (en) * 1973-09-19 1975-12-23 Monsanto Co Continuous staged isobaric stirred polymerization apparatus
DE2645251C2 (en) * 1976-10-07 1983-12-01 Mobil Oil Ag In Deutschland, 2000 Hamburg Process for the preparation and recovery of diisopropanolamine from a mixture containing 1- (2-hydroxypropyl) -4-methyl-oxazolidone- (2)
DE2805915C3 (en) * 1978-02-13 1981-11-05 Dynamit Nobel Ag, 5210 Troisdorf Reactor for the oxidation of mixtures of p-xylene and p-toluic acid methyl ester with oxygen-containing gases in the liquid phase
FR2442794A1 (en) * 1978-12-01 1980-06-27 Obispo Miguel Alkaline orthophosphate soln. prodn. - by continuous neutralisation of phosphoric acid in single multicompartment reaction vessel
DE3514367A1 (en) * 1985-04-20 1986-10-23 Basf Ag, 6700 Ludwigshafen DEVICE FOR SOLID BED POLYMERIZATION OF MONOMERS
US5245057A (en) * 1990-07-20 1993-09-14 The Dow Chemical Company Horizontal continuous reactor and processes
US5372790A (en) * 1991-01-18 1994-12-13 The Dow Chemical Company Vertical continuous reactor

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3251657A (en) * 1962-05-11 1966-05-17 Hoechst Ag Reactor for the manufacture of polyethylene phthalates

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2768987A (en) * 1954-12-31 1956-10-30 Standard Oil Co Method and apparatus for hydrocarbon alkylation

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3251657A (en) * 1962-05-11 1966-05-17 Hoechst Ag Reactor for the manufacture of polyethylene phthalates

Cited By (28)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3483151A (en) * 1966-06-10 1969-12-09 Melle Usines Sa Continuous process for the preparation of polyesters
US7541423B2 (en) 2000-12-07 2009-06-02 Eastman Chemical Company Polyester process using a pipe reactor
US8114954B2 (en) 2000-12-07 2012-02-14 Grupo Petrotemex, S.A. De C.V. Polyester process using a pipe reactor
US20080227931A1 (en) * 2000-12-07 2008-09-18 Debruin Bruce Roger Polyester process using a pipe reactor
US20080312406A1 (en) * 2000-12-07 2008-12-18 Eastman Chemical Company Polyester process using a pipe reactor
US7842778B2 (en) 2000-12-07 2010-11-30 Eastman Chemical Company Polyester process using a pipe reactor
US7718759B2 (en) 2000-12-07 2010-05-18 Eastman Chemical Company Polyester process using a pipe reactor
US7531618B2 (en) 2000-12-07 2009-05-12 Eastman Chemical Company Polyester process using a pipe reactor
NL1017260C2 (en) * 2001-02-01 2002-08-02 Dsm Nv Continuous production of thermoplastic polyesters, includes a polycondensation step in which the partial pressure of the volatile reaction products is higher at the start of polycondensation than at the end
US20090047186A1 (en) * 2005-03-22 2009-02-19 Epc Industrial Engineering Gmbh Modular device for the continuous degassing and production of polymer precondensate with high reaction product surface to volume ratio with gentle treatment of the reaction product mass
US8124018B2 (en) 2005-03-22 2012-02-28 Epc Industrial Engineering Gmbh Modular device for the continuous degassing and production of polymer precondensate with high reaction product surface to volume ratio with gentle treatment of the reaction product mass
US8470250B2 (en) 2006-12-07 2013-06-25 Grupo Petrotemex, S.A. De C.V. Polyester production system employing horizontally elongated esterification vessel
US7649109B2 (en) 2006-12-07 2010-01-19 Eastman Chemical Company Polyester production system employing recirculation of hot alcohol to esterification zone
US7943094B2 (en) 2006-12-07 2011-05-17 Grupo Petrotemex, S.A. De C.V. Polyester production system employing horizontally elongated esterification vessel
US7863477B2 (en) 2007-03-08 2011-01-04 Eastman Chemical Company Polyester production system employing hot paste to esterification zone
US20080221296A1 (en) * 2007-03-08 2008-09-11 Debruin Bruce Roger Polyester production system employing an unagitated esterification reactor
US7892498B2 (en) 2007-03-08 2011-02-22 Eastman Chemical Company Polyester production system employing an unagitated esterification reactor
US20090018281A1 (en) * 2007-07-12 2009-01-15 Eastman Chemical Company Multi-level tubular reactor with internal tray
US7868130B2 (en) 2007-07-12 2011-01-11 Eastman Chemical Company Multi-level tubular reactor with vertically spaced segments
US7868129B2 (en) 2007-07-12 2011-01-11 Eastman Chemical Company Sloped tubular reactor with spaced sequential trays
US7872089B2 (en) 2007-07-12 2011-01-18 Eastman Chemical Company Multi-level tubular reactor with internal tray
US7872090B2 (en) 2007-07-12 2011-01-18 Eastman Chemical Company Reactor system with optimized heating and phase separation
US7858730B2 (en) 2007-07-12 2010-12-28 Eastman Chemical Company Multi-level tubular reactor with dual headers
US7847053B2 (en) 2007-07-12 2010-12-07 Eastman Chemical Company Multi-level tubular reactor with oppositely extending segments
US7842777B2 (en) 2007-07-12 2010-11-30 Eastman Chemical Company Sloped tubular reactor with divided flow
US7829653B2 (en) 2007-07-12 2010-11-09 Eastman Chemical Company Horizontal trayed reactor
RU2478424C2 (en) * 2007-07-12 2013-04-10 Групо Петротемекс, С.А. Де С.В., Horizontal plate reactor
WO2009009033A1 (en) * 2007-07-12 2009-01-15 Eastman Chemical Company Horizontal trayed reactor

Also Published As

Publication number Publication date
BE660780A (en) 1965-09-08
BE632261A (en)
GB1045343A (en) 1966-10-12
US3251657A (en) 1966-05-17
CH422338A (en) 1966-10-15
GB1085725A (en) 1967-10-04
NL292245A (en)
DE1259565B (en) 1968-01-25
NL6502823A (en) 1965-09-07
FR88261E (en) 1967-01-06
DE1189271B (en) 1965-03-18
CH465874A (en) 1968-11-30

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