FR2392010A1 - Purificn. of caprolactam prepd. from cyclohexanone oxime - by addn. of defined quantities of base, toluene and water - Google Patents
Purificn. of caprolactam prepd. from cyclohexanone oxime - by addn. of defined quantities of base, toluene and waterInfo
- Publication number
- FR2392010A1 FR2392010A1 FR7815780A FR7815780A FR2392010A1 FR 2392010 A1 FR2392010 A1 FR 2392010A1 FR 7815780 A FR7815780 A FR 7815780A FR 7815780 A FR7815780 A FR 7815780A FR 2392010 A1 FR2392010 A1 FR 2392010A1
- Authority
- FR
- France
- Prior art keywords
- caprolactam
- phase
- toluene
- water
- cyclohexanone oxime
- 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- Withdrawn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
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 title abstract 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 title abstract 9
- VEZUQRBDRNJBJY-UHFFFAOYSA-N cyclohexanone oxime Chemical compound ON=C1CCCCC1 VEZUQRBDRNJBJY-UHFFFAOYSA-N 0.000 title abstract 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title abstract 3
- 239000002585 base Substances 0.000 title 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract 3
- 230000008707 rearrangement Effects 0.000 abstract 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 abstract 2
- 239000004327 boric acid Substances 0.000 abstract 2
- 239000003054 catalyst Substances 0.000 abstract 2
- 239000012535 impurity Substances 0.000 abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- 238000000605 extraction Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 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)
- Other In-Based Heterocyclic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
Crude caprolactam contg. acid, obtd. in the rearrangement of cyclohexanone oxime, is mixed with: (i) 0.8-2 equivs. of a base, the pH being adjusted to 4-11; (ii) 3-6 pts. wt. toluene, w.r.t. the caprolactam; and (iii) 2-10 pts. wt. water w.r.t. the organic cpds. This forms a toluene phase and a water phase, the latter consisting of two layers. Substantially all the organic impurities are in the upper aq. layer, which is sepd. The crude caprolactam pref. contains 1-2 moles H2SO4 or 0.05-5 moles boric acid, depending on whether the cyclohexanone oxime rearrangement has been performed in the liq. phase with oleum as catalyst or the vapour phase with boric acid as catalyst. Purificn. of caprolactam, derived from rearrangement in oleum, by extraction with benzene is known, but there is a problem of supplementary treatment of the aqs. phase contg. all the impurities. The division of the aqs. phase into two in the present process solves this problem, the upper aqs. layer being easily sepd., e.g. by a siphon.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19772724361 DE2724361A1 (en) | 1977-05-28 | 1977-05-28 | CLEANING CAPROLACTAM |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| FR2392010A1 true FR2392010A1 (en) | 1978-12-22 |
Family
ID=6010216
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR7815780A Withdrawn FR2392010A1 (en) | 1977-05-28 | 1978-05-26 | Purificn. of caprolactam prepd. from cyclohexanone oxime - by addn. of defined quantities of base, toluene and water |
Country Status (7)
| Country | Link |
|---|---|
| JP (1) | JPS53147085A (en) |
| BE (1) | BE867528A (en) |
| DE (1) | DE2724361A1 (en) |
| ES (1) | ES470183A1 (en) |
| FR (1) | FR2392010A1 (en) |
| IT (1) | IT7849565A0 (en) |
| NL (1) | NL7805812A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0152843A2 (en) * | 1984-02-08 | 1985-08-28 | SNIA BPD S.p.A. | A method of purifying caprolactam |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3026538A1 (en) * | 1980-07-12 | 1982-02-11 | Basf Ag, 6700 Ludwigshafen | METHOD FOR CONTINUOUS EXTRACTION OF CAPROLACTAM AS SUCH AND AQUEOUS SOLUTIONS CONTAINING THE SAME OF THE OLIGOMER |
| JP2601946B2 (en) * | 1990-11-21 | 1997-04-23 | 宇部興産株式会社 | Method for purifying lactam-containing solution |
| JP2601945B2 (en) * | 1990-11-21 | 1997-04-23 | 宇部興産株式会社 | Lactam oil refining method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL7612486A (en) * | 1975-11-13 | 1977-05-17 | Bayer Ag | METHOD OF PURIFICATION OF CAPROLACTAM. |
-
1977
- 1977-05-28 DE DE19772724361 patent/DE2724361A1/en not_active Withdrawn
-
1978
- 1978-05-24 ES ES470183A patent/ES470183A1/en not_active Expired
- 1978-05-26 IT IT7849565A patent/IT7849565A0/en unknown
- 1978-05-26 JP JP6240978A patent/JPS53147085A/en active Pending
- 1978-05-26 BE BE188073A patent/BE867528A/en not_active IP Right Cessation
- 1978-05-26 FR FR7815780A patent/FR2392010A1/en not_active Withdrawn
- 1978-05-29 NL NL7805812A patent/NL7805812A/en not_active Application Discontinuation
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL7612486A (en) * | 1975-11-13 | 1977-05-17 | Bayer Ag | METHOD OF PURIFICATION OF CAPROLACTAM. |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0152843A2 (en) * | 1984-02-08 | 1985-08-28 | SNIA BPD S.p.A. | A method of purifying caprolactam |
| EP0152843A3 (en) * | 1984-02-08 | 1987-05-27 | SNIA BPD S.p.A. | A method of purifying caprolactam |
Also Published As
| Publication number | Publication date |
|---|---|
| IT7849565A0 (en) | 1978-05-26 |
| ES470183A1 (en) | 1979-01-01 |
| JPS53147085A (en) | 1978-12-21 |
| DE2724361A1 (en) | 1978-11-30 |
| NL7805812A (en) | 1978-11-30 |
| BE867528A (en) | 1978-11-27 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| RE | Withdrawal of published application |