EP1406948A1 - Verfahren zur herstellung von hochviskosen oder hochstabilisierten polykondensaten und entmonomerisiertem pa6 - Google Patents
Verfahren zur herstellung von hochviskosen oder hochstabilisierten polykondensaten und entmonomerisiertem pa6Info
- Publication number
- EP1406948A1 EP1406948A1 EP02738083A EP02738083A EP1406948A1 EP 1406948 A1 EP1406948 A1 EP 1406948A1 EP 02738083 A EP02738083 A EP 02738083A EP 02738083 A EP02738083 A EP 02738083A EP 1406948 A1 EP1406948 A1 EP 1406948A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- reaction stage
- polycondensate
- reactor
- distributor
- reaction
- Prior art date
- Legal status (The legal status 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 status listed.)
- Withdrawn
Links
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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/46—Post-polymerisation treatment
-
- 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
-
- 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
- B01J19/2455—Stationary reactors without moving elements inside provoking a loop type movement of the reactants
- B01J19/2465—Stationary reactors without moving elements inside provoking a loop type movement of the reactants externally, i.e. the mixture leaving the vessel and subsequently re-entering it
-
- 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
- B01J19/247—Suited for forming thin films
-
- 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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/04—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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
- C08G69/18—Anionic polymerisation
-
- 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
- B01J2219/00164—Controlling or regulating processes controlling the flow
- B01J2219/00166—Controlling or regulating processes controlling the flow controlling the residence time inside 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
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00182—Controlling or regulating processes controlling the level of reactants in the reactor vessel
Definitions
- the invention relates to a method for producing highly viscous or highly stabilized polycondensates and demonomerized PA6 of the type mentioned in the preamble of claim 1 and to an apparatus for carrying out the method.
- twin-screw extruders For polycondensation, it is known to increase the viscosity by performing degassing in twin-screw extruders.
- twin-screw extruders represent complex and wear-prone components, and the extent of the degassing that can be achieved with them is limited.
- the invention has for its object to provide a method of the type mentioned and an apparatus for carrying out the method, which or with little effort enables a strong increase in viscosity.
- the reaction stage shown in the drawing comprises a vertical reactor 1 which has an inlet line 7 at the upper end for supplying the polycondensate melt supplied by a preliminary stage, with one in the course of the supply line 7
- Pump P1 can be arranged.
- a distributor 2 for supplying the polycondensate melt to the elements 3 is arranged, the inlet of which is connected to the inlet line 7.
- metering devices P2, P3 connected in series, for example in the form of controllable pumps, between which one end of a return line 6 is connected, the other end of which is connected to the inlet of the distributor 2, this connection can preferably also take place at a connection point 9 with the inlet line.
- Flow direction rear metering device P3 could also be formed by a control valve.
- connection point 9 it is expedient to use a static mixer 10 in the inlet line and to dimension the static mixer 10 including the line after the static mixer 10 up to a maximum of the distributor 2 such that the residence time for a viscosity increase due to polycondensation increases.
- the cross-sectional area of the line 7 after the connection point 9 is therefore larger than the sum of the cross sections of the line 7 before the connection point 9 plus the cross section of the return line 6.
- connection point 9 which is completely filled with polycondensate and through which the product flows through the connection point 10 until it enters the polycondensation stage.
- the inlet line 7 at the reactor discharge then ends before the distributor
- the reactor 1 further has at least one gas outlet 4 at the upper end and a level measuring device 5 in the sump, the output signal of which can be used to control the metering device P3 or alternatively the pump P1.
- the return line 6 enables a portion of the polycondensate melt located at the lower end of the reactor 1 to be recirculated and thus a portion of this melt to be pumped around, thereby increasing the viscosity and / or reducing the lactam in a simple manner since the melt is repeated several times via the surface-enlarging elements 3 is conducted and degassed intensively to effectively remove polycondensation waste products.
- the residence time in the reactor 1 is set to achieve the chemical polycondensate equilibrium and / or in the case of the production of PA 6 polycondensate or copolyamide polycondensates based on PA 6 to achieve a reduction in lactam, so that sufficient polycondensate product is simulated and in the degassing space above of the melt level can be removed via the gas outlet 4.
- the polycondensate product can be removed by introducing an inert gas via a line 8 into the vicinity of the surface of the melt or in a vacuum.
- the residence time of the melt in the reactor can be 3 hours, with a pumped amount of 50% of the throughput through the reactor 1 being able to be set via the control of the metering devices P2, P3 as an example.
- Useful volume can be increased by an increase of the fill level measured by the level measuring device 5 by 50%.
- Stabilizers can be added in the preliminary stage to obtain more stabilized polycondensate.
- the level is not raised and about 4.5% lactam reduction can be achieved by pumping 100% of the throughput.
- the gas outlet 4 can be connected to devices for the recovery of monomer, the inert gas and water, which are only indicated schematically.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyamides (AREA)
- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10126133 | 2001-05-29 | ||
DE2001126133 DE10126133B4 (de) | 2001-05-29 | 2001-05-29 | Verfahren und Vorrichtung zur Herstellung von hochviskosen oder hochstabilisierten Polykondensaten und entmonomerisiertem PA 6 |
PCT/EP2002/005441 WO2002096975A1 (de) | 2001-05-29 | 2002-05-17 | Verfahren zur herstellung von hochviskosen oder hochstabilisierten polykondensaten und entmonomerisiertem pa6 |
Publications (1)
Publication Number | Publication Date |
---|---|
EP1406948A1 true EP1406948A1 (de) | 2004-04-14 |
Family
ID=7686512
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP02738083A Withdrawn EP1406948A1 (de) | 2001-05-29 | 2002-05-17 | Verfahren zur herstellung von hochviskosen oder hochstabilisierten polykondensaten und entmonomerisiertem pa6 |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP1406948A1 (ru) |
CN (1) | CN1249125C (ru) |
DE (1) | DE10126133B4 (ru) |
RU (1) | RU2295545C2 (ru) |
UA (1) | UA76471C2 (ru) |
WO (1) | WO2002096975A1 (ru) |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6906164B2 (en) | 2000-12-07 | 2005-06-14 | Eastman Chemical Company | Polyester process using a pipe reactor |
US7943094B2 (en) | 2006-12-07 | 2011-05-17 | 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 |
US7863477B2 (en) | 2007-03-08 | 2011-01-04 | Eastman Chemical Company | Polyester production system employing hot paste to esterification zone |
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 |
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 |
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 |
US7868130B2 (en) | 2007-07-12 | 2011-01-11 | Eastman Chemical Company | Multi-level tubular reactor with vertically spaced segments |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19506407A1 (de) * | 1995-02-23 | 1996-08-29 | Polymer Eng Gmbh | Verfahren und Vorrichtung zur Herstellung von hochviskosen oder hochstabilisierten, reaktionsstabilen Polyamiden und zur kontinuierlichen Entmonomerisierung von Polyamiden |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1313592A (en) * | 1970-04-28 | 1973-04-11 | Toray Industries | Method and apparatus of a continuous polymerization |
DE2461902A1 (de) * | 1974-12-31 | 1976-07-08 | Zimmer Ag | Verfahren und vorrichtung zum entfernen von verdampfbaren bestandteilen aus polyamidschmelzen |
DD265151A1 (de) * | 1987-09-30 | 1989-02-22 | Schwarza Chemiefaser | Schmelzentgaser zur kontinuierlichen polymerisation von polyamid-6 aus epsilon-kaprolaktam |
DE4039857A1 (de) * | 1990-10-19 | 1992-04-23 | Inventa Ag | Verfahren und vorrichtung zur direkten, kontinuierlichen modifizierung von polymerschmelzen |
DE19531989A1 (de) * | 1995-08-30 | 1997-05-15 | Polymer Eng Gmbh | Verfahren zur kontinuierlichen Herstellung eines dimerarmen Polyamid 6 |
DE19607723C2 (de) * | 1996-02-29 | 2002-10-24 | Polymer Eng Gmbh | Verfahren und Vorrichtung zur kontinuierlichen Extraktion von polymeren Granulaten |
DE19841376A1 (de) * | 1998-09-10 | 2000-03-16 | Lurgi Zimmer Ag | Verfahren zur Einspeisung von Additiven in einen Polymerschmelzestrom |
-
2001
- 2001-05-29 DE DE2001126133 patent/DE10126133B4/de not_active Expired - Lifetime
-
2002
- 2002-05-17 CN CN 02814690 patent/CN1249125C/zh not_active Expired - Fee Related
- 2002-05-17 EP EP02738083A patent/EP1406948A1/de not_active Withdrawn
- 2002-05-17 UA UA20031212941A patent/UA76471C2/uk unknown
- 2002-05-17 RU RU2003137774/04A patent/RU2295545C2/ru not_active IP Right Cessation
- 2002-05-17 WO PCT/EP2002/005441 patent/WO2002096975A1/de active Application Filing
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19506407A1 (de) * | 1995-02-23 | 1996-08-29 | Polymer Eng Gmbh | Verfahren und Vorrichtung zur Herstellung von hochviskosen oder hochstabilisierten, reaktionsstabilen Polyamiden und zur kontinuierlichen Entmonomerisierung von Polyamiden |
Non-Patent Citations (1)
Title |
---|
See also references of WO02096975A1 * |
Also Published As
Publication number | Publication date |
---|---|
RU2003137774A (ru) | 2005-05-20 |
RU2295545C2 (ru) | 2007-03-20 |
UA76471C2 (en) | 2006-08-15 |
CN1535291A (zh) | 2004-10-06 |
CN1249125C (zh) | 2006-04-05 |
DE10126133A1 (de) | 2003-01-02 |
WO2002096975A1 (de) | 2002-12-05 |
DE10126133B4 (de) | 2007-03-29 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
17P | Request for examination filed |
Effective date: 20031229 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR |
|
RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: LAUSMANN, PETER Owner name: WILTZER, KARL-HEINZ |
|
17Q | First examination report despatched |
Effective date: 20091030 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
|
18D | Application deemed to be withdrawn |
Effective date: 20100511 |