DE2148717B2 - Verfahren zur reinigung von rohlactamen mit 6 bis 12 kohlenstoffatomen im ring - Google Patents
Verfahren zur reinigung von rohlactamen mit 6 bis 12 kohlenstoffatomen im ringInfo
- Publication number
- DE2148717B2 DE2148717B2 DE19712148717 DE2148717A DE2148717B2 DE 2148717 B2 DE2148717 B2 DE 2148717B2 DE 19712148717 DE19712148717 DE 19712148717 DE 2148717 A DE2148717 A DE 2148717A DE 2148717 B2 DE2148717 B2 DE 2148717B2
- Authority
- DE
- Germany
- Prior art keywords
- carbon atoms
- lactam
- raw
- solvents
- process according
- 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- Withdrawn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
- 238000000034 method Methods 0.000 title claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 4
- 150000003951 lactams Chemical class 0.000 claims description 42
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 17
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 10
- 125000004432 carbon atom Chemical group C* 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 125000001931 aliphatic group Chemical group 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 125000004429 atom Chemical group 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 2
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 claims description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims 2
- 238000010438 heat treatment Methods 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims 1
- 125000000217 alkyl group Chemical group 0.000 claims 1
- 239000000356 contaminant Substances 0.000 claims 1
- 150000001924 cycloalkanes Chemical class 0.000 claims 1
- 150000002170 ethers Chemical class 0.000 claims 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- 238000001953 recrystallisation Methods 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 27
- 230000005540 biological transmission Effects 0.000 description 14
- 239000000047 product Substances 0.000 description 9
- 238000005292 vacuum distillation Methods 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 5
- 241001550224 Apha Species 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 150000002576 ketones Chemical class 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 150000002923 oximes Chemical class 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- VEZUQRBDRNJBJY-UHFFFAOYSA-N cyclohexanone oxime Chemical compound ON=C1CCCCC1 VEZUQRBDRNJBJY-UHFFFAOYSA-N 0.000 description 2
- -1 methyl lactams Chemical class 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- PUMRUSBKNSBTAL-UHFFFAOYSA-N 3,4-dihydro-2h-chromene-2-carbaldehyde Chemical compound C1=CC=C2OC(C=O)CCC2=C1 PUMRUSBKNSBTAL-UHFFFAOYSA-N 0.000 description 1
- 238000006237 Beckmann rearrangement reaction Methods 0.000 description 1
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000002105 tongue Anatomy 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D201/00—Preparation, separation, purification or stabilisation of unsubstituted lactams
- C07D201/16—Separation or purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyrrole Compounds (AREA)
- Other In-Based Heterocyclic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Peptides Or Proteins (AREA)
- Cephalosporin Compounds (AREA)
- Extraction Or Liquid Replacement (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH1455070A CH547805A (de) | 1970-10-01 | 1970-10-01 | Verfahren zur reinigung von lactamen. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| DE2148717A1 DE2148717A1 (de) | 1972-04-06 |
| DE2148717B2 true DE2148717B2 (de) | 1976-02-05 |
Family
ID=4401749
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19712148717 Withdrawn DE2148717B2 (de) | 1970-10-01 | 1971-09-29 | Verfahren zur reinigung von rohlactamen mit 6 bis 12 kohlenstoffatomen im ring |
Country Status (18)
| Country | Link |
|---|---|
| US (1) | US3794647A (enExample) |
| JP (1) | JPS4915276B1 (enExample) |
| AT (1) | AT311376B (enExample) |
| AU (1) | AU457339B2 (enExample) |
| BE (1) | BE773264A (enExample) |
| BG (1) | BG26000A3 (enExample) |
| CA (1) | CA962676A (enExample) |
| CH (1) | CH547805A (enExample) |
| CS (1) | CS176170B2 (enExample) |
| DE (1) | DE2148717B2 (enExample) |
| ES (1) | ES395584A1 (enExample) |
| FR (1) | FR2112238B1 (enExample) |
| GB (1) | GB1318459A (enExample) |
| IE (1) | IE35686B1 (enExample) |
| NL (1) | NL7113365A (enExample) |
| PL (1) | PL88944B1 (enExample) |
| RO (1) | RO57818A (enExample) |
| YU (1) | YU34507B (enExample) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE794622A (fr) * | 1972-01-28 | 1973-07-26 | Bayer Ag | Procede de purification du caprolactame |
| DE2641454A1 (de) * | 1976-09-15 | 1978-03-23 | Bayer Ag | Verfahren zur reinigung von epsilon-caprolactam |
| JPS5341599A (en) * | 1976-09-28 | 1978-04-15 | Minoru Ban | Polymerizating method for grafting to cloth |
| DE2845075A1 (de) * | 1978-10-17 | 1980-05-08 | Basf Ag | Verfahren zur reinigung von rohcaprolactam |
| DE3729853A1 (de) * | 1987-09-05 | 1989-03-23 | Basf Ag | Verfahren zur aufarbeitung von destillationsrueckstaenden, die bei der reinigung von caprolactam anfallen |
| TW215084B (en) * | 1992-04-17 | 1993-10-21 | Sumitomo Chemical Co | Process for producing a high purity caprolactam |
| JP4182273B2 (ja) * | 2000-06-27 | 2008-11-19 | 住友化学株式会社 | ε−カプロラクタムの製造方法 |
| US20090182139A1 (en) * | 2006-04-06 | 2009-07-16 | Basf Se | Process for the preparation of an n-alkyl lactam with improved colour quality |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2861988A (en) * | 1958-11-25 | Caprolactam manufacture |
-
1970
- 1970-10-01 CH CH1455070A patent/CH547805A/xx not_active IP Right Cessation
-
1971
- 1971-09-22 US US00182830A patent/US3794647A/en not_active Expired - Lifetime
- 1971-09-24 CS CS6825A patent/CS176170B2/cs unknown
- 1971-09-29 GB GB4540671A patent/GB1318459A/en not_active Expired
- 1971-09-29 BG BG018643A patent/BG26000A3/xx unknown
- 1971-09-29 PL PL1971150800A patent/PL88944B1/pl unknown
- 1971-09-29 NL NL7113365A patent/NL7113365A/xx unknown
- 1971-09-29 YU YU2459/71A patent/YU34507B/xx unknown
- 1971-09-29 DE DE19712148717 patent/DE2148717B2/de not_active Withdrawn
- 1971-09-29 BE BE773264A patent/BE773264A/xx unknown
- 1971-09-29 AT AT842571A patent/AT311376B/de active
- 1971-09-30 RO RO68322A patent/RO57818A/ro unknown
- 1971-09-30 CA CA124,069A patent/CA962676A/en not_active Expired
- 1971-09-30 FR FR7135350A patent/FR2112238B1/fr not_active Expired
- 1971-09-30 AU AU34063/71A patent/AU457339B2/en not_active Expired
- 1971-09-30 IE IE1228/71A patent/IE35686B1/xx unknown
- 1971-09-30 ES ES395584A patent/ES395584A1/es not_active Expired
- 1971-10-01 JP JP46077028A patent/JPS4915276B1/ja active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| JPS4915276B1 (enExample) | 1974-04-13 |
| CA962676A (en) | 1975-02-11 |
| YU245971A (en) | 1979-02-28 |
| FR2112238A1 (enExample) | 1972-06-16 |
| AU457339B2 (en) | 1975-01-23 |
| BE773264A (fr) | 1972-01-17 |
| PL88944B1 (enExample) | 1976-10-30 |
| BG26000A3 (bg) | 1979-01-12 |
| ES395584A1 (es) | 1974-02-16 |
| NL7113365A (enExample) | 1972-04-05 |
| DE2148717A1 (de) | 1972-04-06 |
| IE35686L (en) | 1972-04-01 |
| AT311376B (de) | 1973-11-12 |
| YU34507B (en) | 1979-09-10 |
| FR2112238B1 (enExample) | 1974-03-15 |
| IE35686B1 (en) | 1976-04-28 |
| CH547805A (de) | 1974-04-11 |
| AU3406371A (en) | 1973-04-05 |
| GB1318459A (en) | 1973-05-31 |
| CS176170B2 (enExample) | 1977-06-30 |
| US3794647A (en) | 1974-02-26 |
| RO57818A (enExample) | 1975-03-15 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| BHN | Withdrawal |