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)

Publications (1)

Family

ID=7686512

Family Applications (1)

Country Status (6)

Families Citing this family (12)

Citations (1)

Family Cites Families (7)

• 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)

Non-Patent Citations (1)

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