ZA200106583B - Method for producing polyamide 6 of a low extract content, high viscosity stability and low remonomerization rate. - Google Patents
Method for producing polyamide 6 of a low extract content, high viscosity stability and low remonomerization rate. Download PDFInfo
- Publication number
- ZA200106583B ZA200106583B ZA200106583A ZA200106583A ZA200106583B ZA 200106583 B ZA200106583 B ZA 200106583B ZA 200106583 A ZA200106583 A ZA 200106583A ZA 200106583 A ZA200106583 A ZA 200106583A ZA 200106583 B ZA200106583 B ZA 200106583B
- Authority
- ZA
- South Africa
- Prior art keywords
- pressure
- bar
- reaction mixture
- water
- aminonitrile
- Prior art date
Links
- 229920002292 Nylon 6 Polymers 0.000 title description 6
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000000284 extract Substances 0.000 title description 2
- 239000011541 reaction mixture Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000004952 Polyamide Substances 0.000 claims description 23
- 239000003054 catalyst Substances 0.000 claims description 23
- 229920002647 polyamide Polymers 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000012632 extractable Substances 0.000 claims description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 238000000926 separation method Methods 0.000 claims description 20
- 229910044991 metal oxide Inorganic materials 0.000 claims description 18
- 150000004706 metal oxides Chemical class 0.000 claims description 18
- 125000005219 aminonitrile group Chemical group 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 14
- 238000001704 evaporation Methods 0.000 claims description 13
- 230000008020 evaporation Effects 0.000 claims description 13
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- FHKPTEOFUHYQFY-UHFFFAOYSA-N 2-aminohexanenitrile Chemical compound CCCCC(N)C#N FHKPTEOFUHYQFY-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000010457 zeolite Substances 0.000 claims description 7
- 239000007791 liquid phase Substances 0.000 claims description 6
- 239000002638 heterogeneous catalyst Substances 0.000 claims description 5
- 239000007848 Bronsted acid Substances 0.000 claims description 4
- 229910021536 Zeolite Inorganic materials 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- 238000010924 continuous production Methods 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052615 phyllosilicate Inorganic materials 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 24
- 239000000047 product Substances 0.000 description 21
- 229920000642 polymer Polymers 0.000 description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000012071 phase Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000000605 extraction Methods 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 239000004408 titanium dioxide Substances 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
- 239000000470 constituent Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000000155 melt Substances 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 230000032683 aging Effects 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 239000008188 pellet Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000006286 aqueous extract Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- -1 copper(I) halides Chemical class 0.000 description 2
- 239000000539 dimer Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000005501 phase interface Effects 0.000 description 2
- 238000003303 reheating Methods 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 238000010626 work up procedure Methods 0.000 description 2
- FTVFPPFZRRKJIH-UHFFFAOYSA-N 2,2,6,6-tetramethylpiperidin-4-amine Chemical compound CC1(C)CC(N)CC(C)(C)N1 FTVFPPFZRRKJIH-UHFFFAOYSA-N 0.000 description 1
- SCEIUGQQBYRBPP-UHFFFAOYSA-N 2,3,4,5-tetrahydro-1h-azepine Chemical compound C1CCC=CNC1 SCEIUGQQBYRBPP-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 241000257303 Hymenoptera Species 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000008045 alkali metal halides Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 208000010587 benign idiopathic neonatal seizures Diseases 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000003951 lactams Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- C08G69/02—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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19905754A DE19905754A1 (de) | 1999-02-11 | 1999-02-11 | Verfahren zur Herstellung von Polyamid 6 mit geringem Extraktgehalt, hoher Viskositätsstabilität und kleiner Remonomerisierungsrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| ZA200106583B true ZA200106583B (en) | 2002-08-12 |
Family
ID=7897207
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| ZA200106583A ZA200106583B (en) | 1999-02-11 | 2001-08-10 | Method for producing polyamide 6 of a low extract content, high viscosity stability and low remonomerization rate. |
Country Status (23)
| Country | Link |
|---|---|
| US (1) | US6525167B1 (fr) |
| EP (1) | EP1165660B1 (fr) |
| JP (1) | JP3428584B2 (fr) |
| KR (1) | KR20010102034A (fr) |
| CN (1) | CN1175026C (fr) |
| AR (1) | AR022564A1 (fr) |
| AT (1) | ATE229047T1 (fr) |
| AU (1) | AU3279800A (fr) |
| BG (1) | BG105809A (fr) |
| BR (1) | BR0008116A (fr) |
| CA (1) | CA2362510A1 (fr) |
| CZ (1) | CZ20012883A3 (fr) |
| DE (2) | DE19905754A1 (fr) |
| ES (1) | ES2188514T3 (fr) |
| HU (1) | HUP0105495A2 (fr) |
| ID (1) | ID30049A (fr) |
| IL (1) | IL144522A0 (fr) |
| MY (1) | MY133350A (fr) |
| PL (1) | PL350053A1 (fr) |
| SK (1) | SK10962001A3 (fr) |
| TR (1) | TR200102317T2 (fr) |
| WO (1) | WO2000047651A1 (fr) |
| ZA (1) | ZA200106583B (fr) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19962573A1 (de) * | 1999-12-23 | 2001-07-05 | Basf Ag | Verfahren zur Herstellung von Polyamiden |
| DE10021191A1 (de) * | 2000-05-03 | 2001-11-08 | Basf Ag | Verfahren zur Herstellung eines Polymers unter Verwendung von Caprolactam |
| DE10047657B4 (de) * | 2000-09-26 | 2005-02-10 | Basf Ag | Verfahren zur Herstellung von Polycaprolactam, ein Polycaprolactam und dessen Verwendung |
| DE10251798A1 (de) * | 2002-11-07 | 2004-05-19 | Bayer Ag | Verfahren zur Herstellung von Polyamid 6 mit geringem Dimergehalt |
| US6875838B2 (en) | 2003-04-28 | 2005-04-05 | Invista North Americal S.A.R.L. | Process for reducing caprolactam and its oligomers in nylon-6 pre-polymer |
| US20100227973A1 (en) * | 2009-03-06 | 2010-09-09 | Honeywell International Inc. | Low viscosity polyamides |
| HUE033035T2 (hu) | 2010-04-14 | 2017-11-28 | Wingspeed Ag | Eljárás módosított poliamid 6 elõállítására |
| EP2784102B1 (fr) * | 2013-03-26 | 2015-12-09 | Uhde Inventa-Fischer GmbH | Procédé et dispositif pour le retour en continu d'eaux d'extraction dans un processus de fabrication de polyamide |
| CN107619476B (zh) * | 2017-10-27 | 2020-11-24 | 万华化学集团股份有限公司 | 一种十二内酰胺的聚合方法 |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2245129A (en) | 1935-01-02 | 1941-06-10 | Du Pont | Process for preparing linear polyamides |
| US4568736A (en) * | 1984-09-17 | 1986-02-04 | The Standard Oil Company | Preparation of polyamide from omega-aminonitrile with oxygen containing phosphorus catalyst |
| WO1998008889A2 (fr) * | 1996-08-30 | 1998-03-05 | Basf Aktiengesellschaft | Procede pour la preparation de polyamides a partir d'aminonitriles |
| DE19804020A1 (de) * | 1998-02-02 | 1999-08-05 | Basf Ag | Verfahren zur Herstellung von Polyamiden aus Aminonitrilen |
| DE19804033A1 (de) * | 1998-02-02 | 1999-08-05 | Basf Ag | Kontinuierliches Verfahren zur Herstellung von Polyamiden aus Aminonitrilen |
| DE19808442A1 (de) * | 1998-02-27 | 1999-09-02 | Basf Ag | Verfahren zur Extraktion von Polyamidteilchen |
| DE19808407A1 (de) * | 1998-02-27 | 1999-09-09 | Basf Ag | Herstellung von Polyamiden durch Reaktivdestillation |
| DE19808490A1 (de) * | 1998-02-27 | 1999-09-02 | Basf Ag | Verfahren zur Herstellung von Polyamiden aus Aminocarbonsäureverbindungen |
-
1999
- 1999-02-11 DE DE19905754A patent/DE19905754A1/de not_active Withdrawn
- 1999-02-11 HU HU0105495A patent/HUP0105495A2/hu unknown
-
2000
- 2000-02-10 AR ARP000100582A patent/AR022564A1/es unknown
- 2000-02-10 CN CNB00803706XA patent/CN1175026C/zh not_active Expired - Fee Related
- 2000-02-10 AT AT00910666T patent/ATE229047T1/de not_active IP Right Cessation
- 2000-02-10 MY MYPI20000464A patent/MY133350A/en unknown
- 2000-02-10 KR KR1020017010115A patent/KR20010102034A/ko active IP Right Grant
- 2000-02-10 CZ CZ20012883A patent/CZ20012883A3/cs unknown
- 2000-02-10 PL PL00350053A patent/PL350053A1/xx not_active Application Discontinuation
- 2000-02-10 EP EP00910666A patent/EP1165660B1/fr not_active Expired - Lifetime
- 2000-02-10 ID IDW00200101975A patent/ID30049A/id unknown
- 2000-02-10 BR BR0008116-7A patent/BR0008116A/pt not_active IP Right Cessation
- 2000-02-10 ES ES00910666T patent/ES2188514T3/es not_active Expired - Lifetime
- 2000-02-10 IL IL14452200A patent/IL144522A0/xx unknown
- 2000-02-10 DE DE50000872T patent/DE50000872D1/de not_active Expired - Lifetime
- 2000-02-10 SK SK1096-2001A patent/SK10962001A3/sk unknown
- 2000-02-10 CA CA002362510A patent/CA2362510A1/fr not_active Abandoned
- 2000-02-10 TR TR2001/02317T patent/TR200102317T2/xx unknown
- 2000-02-10 JP JP2000598565A patent/JP3428584B2/ja not_active Expired - Fee Related
- 2000-02-10 US US09/913,122 patent/US6525167B1/en not_active Expired - Fee Related
- 2000-02-10 WO PCT/EP2000/001089 patent/WO2000047651A1/fr not_active Application Discontinuation
- 2000-02-10 AU AU32798/00A patent/AU3279800A/en not_active Abandoned
-
2001
- 2001-08-09 BG BG105809A patent/BG105809A/bg unknown
- 2001-08-10 ZA ZA200106583A patent/ZA200106583B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| JP2002536517A (ja) | 2002-10-29 |
| AU3279800A (en) | 2000-08-29 |
| JP3428584B2 (ja) | 2003-07-22 |
| BG105809A (bg) | 2002-03-29 |
| DE19905754A1 (de) | 2000-08-17 |
| KR20010102034A (ko) | 2001-11-15 |
| DE50000872D1 (de) | 2003-01-16 |
| CN1340073A (zh) | 2002-03-13 |
| EP1165660B1 (fr) | 2002-12-04 |
| BR0008116A (pt) | 2001-11-06 |
| ID30049A (id) | 2001-11-01 |
| WO2000047651A1 (fr) | 2000-08-17 |
| CZ20012883A3 (cs) | 2001-12-12 |
| CN1175026C (zh) | 2004-11-10 |
| TR200102317T2 (tr) | 2001-12-21 |
| MY133350A (en) | 2007-11-30 |
| SK10962001A3 (sk) | 2002-04-04 |
| IL144522A0 (en) | 2002-05-23 |
| EP1165660A1 (fr) | 2002-01-02 |
| ES2188514T3 (es) | 2003-07-01 |
| HUP0105495A2 (en) | 2002-05-29 |
| PL350053A1 (en) | 2002-11-04 |
| US6525167B1 (en) | 2003-02-25 |
| CA2362510A1 (fr) | 2000-08-17 |
| AR022564A1 (es) | 2002-09-04 |
| ATE229047T1 (de) | 2002-12-15 |
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