WO2007098637A1 - Réacteur de prépolycondensation - Google Patents

Réacteur de prépolycondensation Download PDF

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Publication number
WO2007098637A1
WO2007098637A1 PCT/CN2006/000290 CN2006000290W WO2007098637A1 WO 2007098637 A1 WO2007098637 A1 WO 2007098637A1 CN 2006000290 W CN2006000290 W CN 2006000290W WO 2007098637 A1 WO2007098637 A1 WO 2007098637A1
Authority
WO
WIPO (PCT)
Prior art keywords
chamber
lower chamber
reactor according
precondensation
heater
Prior art date
Application number
PCT/CN2006/000290
Other languages
English (en)
Chinese (zh)
Inventor
Wende Luo
Huatang Zhou
Chun Zhang
Huishu Zhang
Xiuheng Zhou
Original Assignee
China Textile Industrial Engineering Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Textile Industrial Engineering Institute filed Critical China Textile Industrial Engineering Institute
Priority to PCT/CN2006/000290 priority Critical patent/WO2007098637A1/fr
Publication of WO2007098637A1 publication Critical patent/WO2007098637A1/fr

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Classifications

    • 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
    • B01J19/0053—Details of the reactor
    • B01J19/006—Baffles
    • 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
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • 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
    • B01J19/18—Stationary reactors having moving elements inside
    • 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
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
    • B01J2219/00081—Tubes
    • 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
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
    • B01J2219/00083—Coils
    • 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
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
    • B01J2219/00085—Plates; Jackets; Cylinders
    • 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
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00092—Tubes
    • 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
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • 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
    • B01J2219/00159—Controlling the temperature controlling multiple zones along the direction of flow, e.g. pre-heating and after-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
    • B01J2219/00761—Details of the reactor
    • B01J2219/00763—Baffles
    • B01J2219/00765—Baffles attached to the reactor wall
    • B01J2219/0077—Baffles attached to the reactor wall inclined

Definitions

  • This invention relates to novel precondensation reactors for the production of prepolymers, particularly novel precondensation reactors for the production of polyethylene terephthalate (PET) prepolymers.
  • PET polyethylene terephthalate
  • a conventional polycondensation method for producing polyethylene terephthalate (PET) is that the ester compound undergoes two stages of pre-condensation and final polycondensation.
  • the pre-condensation section is a transitional stage of the material from the esterification reaction to the polycondensation reaction, which will complete the esterification reaction of the oligomer from the esterification section, and increase the esterification rate to 99% or more, and at the same time, start polycondensation. reaction. Since the pressure change during the pre-polycondensation reaction is a depressurization process from positive pressure to vacuum, two separate reactors are currently used to complete the pre-polycondensation process, or a tower reactor to treat the pressure reduction process.
  • the average prepolymerization reactor has an average degree of polymerization of 20 to 30. Since the pressure of the pre-polycondensation reaction is a decompression process from positive pressure to vacuum, most processes use two independent reactors to complete the pre-polycondensation process, and some manufacturers use a tower reactor to treat this decompression process. process.
  • the two-stage precondensation reactor has many control points, large floor space, and increased operating costs; the two reactors have a large investment.
  • the novel pre-polycondensation reactor of the invention has the advantages of simple process, low investment, low energy consumption, low operating cost, simple operation control and excellent product quality, and has the disadvantages of the above two types of reactors. Summary of the invention
  • the pre-polycondensation reaction is completed, which solves the problem that the two-stage pre-polycondensation reactor in the prior art has many control points, large floor space, large operation cost and large investment, and also solves the prior art tower type.
  • the reactor consumes a lot of metal materials, a long reaction process, a lot of waste when parking, a large investment and a large consumption problem.
  • the novel precondensation reactor of the invention adopts a double chamber vertical structure, including an upper chamber, a lower chamber and an external power driving device, wherein:
  • the upper chamber includes a material inlet, an upper chamber material outlet, an upper chamber heater located in the upper chamber, and upper and lower chamber liquid pipelines connecting the upper chamber and the lower chamber;
  • the lower chamber includes a lower chamber material inlet, the upper portion has an exhaust passage extending outside the reaction vessel, a prepolymer outlet, and a lower chamber heater;
  • annular vapor-phase orifices in the upper and lower chamber separators.
  • damper chamber at the upper portion of the lower chamber and the upper chamber, wherein a plurality of damper plates are disposed in the damper chamber.
  • the upper chamber heater is a tube-and-tube heater.
  • the lower chamber heater is a plate heater.
  • the lower portion of the lower end of the exhaust passage outside the reaction vessel in the lower portion of the polycondensation reactor has a gas collection enthalpy.
  • the polycondensation reactor external power drive includes a stirring drive, agitating blades, a seal, and a stirrer shaft.
  • the agitating drive of the external power drive is located outside of the bottom of the lower chamber.
  • the upper chamber heater of the polycondensation reactor employs a vapor phase heat medium.
  • the polycondensation reactor lower chamber heater employs a vapor phase heat medium.
  • the polycondensation reactor further comprises a reaction vessel holding and heating device.
  • the reaction vessel holding and heating device of the polycondensation reactor employs a vapor phase heat medium.
  • the polycondensation reactor has a regulating valve on the upper and lower chamber liquid phase lines.
  • the precondensation reactor of the present invention has a simple structure, and the precondensation reaction can be completed by only one apparatus, and has the advantages of simple operation, easy control, and stable production.
  • Figure 1 is a longitudinal cross-sectional view showing a preferred embodiment of the precondensation reactor of the present invention
  • Figure 2 is a schematic cross-sectional view of a preferred embodiment of the precondensation reactor of the present invention. detailed description
  • the novel precondensation reactor of the present invention is a vertical apparatus of a double chamber structure, including a closed reaction vessel 100, and the upper chamber 6 and the lower chamber 7 are combined in a closed reaction vessel through the upper and lower chamber separators 17.
  • the upper chamber 6 is located at the top of the outer side of the lower chamber 7, the upper chamber is a flash chamber, the operating pressure is a vacuum, the lower chamber is a polycondensation chamber, and the operating pressure is a low vacuum.
  • the reaction vessel insulation heating device 16 employs a vapor phase heat medium.
  • an external power drive unit 200 is provided at the bottom of the lower chamber.
  • the upper chamber 6 includes a material inlet 1, an upper chamber material outlet 9, a upper chamber heater 14 and an upper and lower chamber liquid phase conduit 4 at the bottom of the upper chamber.
  • the upper chamber material outlet 9 is connected to the lower chamber material inlet 10 of the lower chamber 7 via the upper and lower chamber liquid phase lines 4, so that the upper chamber liquid material passes through the upper chamber material outlet 9 through the lower chamber liquid phase line 4 through the lower chamber material inlet 10 Flow into the lower chamber 7.
  • a regulating valve 300 is provided on the upper and lower chamber liquid phase lines 4 for controlling the flow rate of the material entering the lower chamber 7 from the upper chamber 6, thereby controlling the liquid level difference in the upper chamber 6 and the lower chamber 7, so that the reactor Simple control and smooth production.
  • the upper chamber heater 14 is a tubular heater and uses a vapor phase heat medium to provide heat to the upper chamber.
  • the discharge of the generated gas will promote the reaction to proceed, so that preferably, the generated gas is continuously discharged out of the precondensation reactor through the exhaust passage 21 through the annular vapor-phase orifice 2.
  • the lower chamber 7 includes an upper portion having an exhaust passage 21 extending outside the reaction vessel, a lower chamber material inlet 10, a prepolymer outlet 5, a lower chamber heater 13, and an external power drive unit 200.
  • the upper portion has an exhaust passage 21 extending outside the reaction vessel to discharge the gas generated by the reaction in the upper chamber 6 and the lower chamber 7 out of the reaction vessel.
  • the reaction product is discharged through the prepolymer outlet 5 to the precondensation reactor.
  • the lower chamber heater 13 located at the bottom of the lower chamber is preferably a plate heater.
  • the heater has an annular shape and is internally divided into a plurality of annular flow passages to ensure that the heat medium has a sufficient flow velocity in the heater to increase the heat transfer rate. .
  • the heater preferably uses a vapor phase heat medium.
  • the external power drive unit 200 includes an agitation drive 204, agitator blades 201, a seal 203, and an agitator shaft 202. Since the reaction of the material in the chamber 6 of the pre-polycondensation reactor is carried out under the condition of gradually reducing pressure, the material enters the upper chamber 6 of the reactor and is boiled under the influence of the pressure difference, and the material is boiled for mixing. The bubble generation process is agitated, so there is no need to provide an external power drive. When the material enters the lower chamber of the reactor 7, the viscosity of the material is increased, and the generated gas needs to be removed under mechanical agitation to facilitate the reaction. Therefore, a higher viscosity material is disposed in the lower chamber 7 of the precondensation reactor.
  • External power drive unit 200 the agitating drive 204 located at the bottom of the lower chamber 7 outside the reaction vessel 100 drives the agitator blades 201 through the agitator shaft 202 for agitation.
  • the agitator blade 201 employs a scraper wall agitator blade which allows the material fluid to flow down the reactor edge, increasing the area of the material to remove volatiles and increasing the renewal of the reactor wall material.
  • the external power drive unit located at the bottom of the lower chamber 7 has a shorter shaft and a smaller swing during agitation than the upper external power drive unit, and a better stirring efficiency can be obtained under the same stirring power.
  • the upper and lower chamber partitions have annular vapor-phase flow holes 2 for flowing the gas in the upper chamber 6 in a given direction.
  • a damping chamber 19 is further disposed at an upper portion of the lower chamber and the upper chamber, wherein a plurality of damping plates I 8 are disposed in the damping chamber 19, and the damping chamber 19 is a key component for maintaining a pressure difference between the upper and lower chambers, and the high-speed airflow passes through the plurality of damping plates. 18 After decompression, it flows into the lower chamber 7, and the gas-liquid separation causes the droplets to fall into the lower chamber liquid phase.
  • the polycondensation reactor further comprises a reaction vessel insulation heating device 16, and the reaction vessel insulation heating device uses a vapor phase heat medium.
  • the vapor phase heat medium enters the polycondensation reactor from the heat medium inlet 11 and exits the polycondensation reactor from the heat medium outlet 12.
  • the pre-polycondensation reactor of the invention has the advantages of simple and novel structure and simple process, and the pre-polycondensation reaction can be completed by using only one device, and the defects in the prior art are overcome, and the product outlet viscosity of the product can reach 0.20 ⁇ 0.29, which fully satisfies the pre-polycondensation process. Requires, and has the advantages of simple operation, easy control and smooth production.
  • the ethylene terephthalate with a material esterification rate of 96% enters the pre-polycondensation reactor through the material inlet 1 and operates in the upper chamber 6 where the pressure is normal, and flows along the peripheral phase and is heated by the vapor-phase heat medium.
  • the tube heater 14 is heated, and at the same time, two reactions of esterification and polycondensation are carried out.
  • the gas flows through the annular vapor phase guiding hole 2 through the annular vapor phase guiding hole 2 under the pressure difference to the damping including the plurality of damping plates 18.
  • the chamber 19 After the chamber 19 is depressurized, it enters the lower chamber 7 where the operating pressure is vacuum.
  • the pressure difference between the upper and lower chambers is controlled in the range of 15 mbar to 50 mbar.
  • the droplets carried therein fall into the lower chamber liquid.
  • the gas entering the lower chamber merges with the vaporized gas of the lower chamber, and the precondensation reaction vessel 100 is discharged through the exhaust passage 21 extending from the upper portion of the lower chamber to the outside of the reaction vessel through the gas collection ⁇ 20.
  • the obtained liquid phase material flows from the reactor upper chamber 6 through the upper and lower chamber liquid phase conduits 4 through the lower valve material inlet 10 into the lower chamber 7 through the upper chamber liquid phase conduit 4, and is heated by the vapor phase heat medium in the lower chamber 7
  • the lower chamber plate heater 13 is heated and further reacted by the lower outdoor power driving device 200.
  • the reaction material is pre-polycondensed at 270 ⁇ 278 Torr, and the total residence time of the material in the pre-polycondensation reactor can be controlled from 60 to 110 minutes.
  • the product obtained by the reaction exits the precondensation reactor through the prepolymer outlet 5.
  • the material Since the reaction of the material in the upper chamber of the precondensation reactor is carried out under the condition of gradually reducing pressure, the material enters the upper chamber of the reactor and is boiled under the influence of the pressure difference. The material itself boils and mixes, and the material is stirred by the bubble generation process, so there is no need to set up a mechanical agitator.
  • an external power drive for the higher viscosity material is disposed in the lower chamber of the reactor.
  • Device 200 The agitation drive located at the bottom of the lower chamber 7 outside the reaction vessel 100 drives the agitator blades 201 through the agitator shaft 202 to agitate the material.
  • the precondensation reactor is provided with a vapor phase heat medium heat insulating device 16 .

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

Le réacteur de prépolycondensation à double chambre verticale comprend une chambre supérieure, une chambre inférieure et un dispositif d'entraînement à puissance externe. La chambre supérieure comprend une entrée supérieure de matière, une sortie supérieure de matière, un échangeur thermique supérieur, des tubes de liquide reliant la chambre supérieure et la chambre inférieure, cette dernière comprenant une entrée inférieure de matière, des tuyaux d'évacuation sortant du réacteur, une sortie de prépolymère et un échangeur thermique inférieur. La chambre supérieure et la chambre inférieure sont assemblées dans le réacteur étanche par un organe de séparation.
PCT/CN2006/000290 2006-02-28 2006-02-28 Réacteur de prépolycondensation WO2007098637A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2006/000290 WO2007098637A1 (fr) 2006-02-28 2006-02-28 Réacteur de prépolycondensation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2006/000290 WO2007098637A1 (fr) 2006-02-28 2006-02-28 Réacteur de prépolycondensation

Publications (1)

Publication Number Publication Date
WO2007098637A1 true WO2007098637A1 (fr) 2007-09-07

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PCT/CN2006/000290 WO2007098637A1 (fr) 2006-02-28 2006-02-28 Réacteur de prépolycondensation

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105536679A (zh) * 2016-01-29 2016-05-04 扬州惠通化工技术有限公司 一种酯化反应系统
CN110869413A (zh) * 2017-07-06 2020-03-06 德希尼布吉玛股份有限公司 制备可生物降解聚酯的方法和设备
CN114588839A (zh) * 2021-12-03 2022-06-07 江苏傲赛工业密封有限公司 一种聚酯合成真空系统及其密封件的在线更换方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1583821A (zh) * 2004-06-02 2005-02-23 中国纺织工业设计院 生产聚对苯二甲酸乙二醇酯的高效简化连续工艺及装置

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1583821A (zh) * 2004-06-02 2005-02-23 中国纺织工业设计院 生产聚对苯二甲酸乙二醇酯的高效简化连续工艺及装置

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105536679A (zh) * 2016-01-29 2016-05-04 扬州惠通化工技术有限公司 一种酯化反应系统
CN105536679B (zh) * 2016-01-29 2017-07-07 扬州惠通化工科技股份有限公司 一种酯化反应系统
CN110869413A (zh) * 2017-07-06 2020-03-06 德希尼布吉玛股份有限公司 制备可生物降解聚酯的方法和设备
EP3649176B1 (fr) * 2017-07-06 2021-08-25 Technip Zimmer GmbH Procédé et appareil pour préparer des polyesters biodégradables
US11427677B2 (en) 2017-07-06 2022-08-30 Technip Zimmer Gmbh Process and apparatus for preparing biodegradable polyesters
CN114588839A (zh) * 2021-12-03 2022-06-07 江苏傲赛工业密封有限公司 一种聚酯合成真空系统及其密封件的在线更换方法

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