← Back to Patent Explorer
US4353784A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of recovery of acetic acid

Assignee: Daicel Corp
•
Filing: 1981-09-21
•
Granted: 1982-10-12
•
Expires: 2001-09-21
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract Disclosed is a method of recovering acetic acid by extracting from an acetic acid-containing aqueous solution with an organic extracting agent and subjecting the extract to distillation, said method comprising the first step of performing extraction by using a tertiary amine having a boiling point higher than that of acetic acid and being capable of forming a non-aqueus phase as the organic extracting agent in combination with an oxygen-containing, high-boiling-point organic solvent selected from the group consisting of di-isobutylcarbinol, isophorene, methyl benzoate, tributyl phosphate, 3,3,5-trimethylcyclohexanone and 2-ethoxyethyl acetate, the second step of performing dehydration by subjecting the extract to distillation, and the third step of subjecting the dehydrated mixture to distillation in a reduced pressure distillation column at a column bottom temperature of 120° to 170° C. to distill acetic acid and separate it from the organic extracting agent. According to this method, water-free acetic acid can be recovered from an acetic acid-containing aqueous solution at a high separation efficiency with reduced energy consumption, and this recovery method is suitably applied to recovery of acetic acid from acetic acid-containing aqueous solutions discharged from various chemical industrial processes.

Inventors

  • 👤 Kunio Koga
  • 👤 Ryoichi Kishimoto

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 06:37
CPC Classifications
C; C07; C07C; C07C51/00; C07C51/42; C07C51/43; C07C51/44; C07C51/48

Claims Analysis

Total Claims: 14
Claim 1
Independent Claim 137 words
A method of recovering acetic acid by extracting an acetic acid-containing aqueous solution with an organic extracting agent and subjecting the extract to distillation, said method comprising the first step of performing extraction by using a tertiary amine having a boiling point higher than that of acetic acid and being capable of forming a non-aqueous phase as the organic extracting agent in combination with an oxygen-containing, high-boiling-point organic solvent selected from the group consisting of di-isobutyl carbinol, isophorone, methyl benzoate, tributyl phosphate, 3,3,5-trimethylcyclohexanone and 2-ethoxyethyl acetate, the second step of performing dehydration by subjecting the extract to distillation, and the third step of subjecting the dehydrated mixture to distillation in a reduced pressure distillation column at a column bottom temperature of 120° to 170° C. to distill acetic acid and separate it from the organic extracting agent.
Claim 2
Independent Claim 137 words
A method of recovering acetic acid by extracting an acetic acid-containing aqueous solution with an organic extracting agent and subjecting the extract to distillation, said method comprising the first step of performing extraction by using a tertiary amine having a boiling point higher than that of acetic acid and being capable of forming a non-aqueous phase as the organic extracting agent in combination with an oxygen-containing, high-boiling-point organic solvent selected from the group consisting of di-isobutyl carbinol, isophorone, methyl benzoate, tributyl phosphate, 3,3,5-trimethylcyclohexanone and 2-ethoxyethyl acetate, the second step of performing dehydration by subjecting the extract to distillation, and the third step of subjecting the dehydrated mixture to distillation in a reduced pressure distillation column at a column bottom temperature of 120° to 170° C. to distill acetic acid and separate it from the organic extracting agent.
Claim 3
Dependent Claim 37 words
A recovery method according to claim 1, wherein the organic extracting agent separated from acetic acid at the third step is used as a reflux liquid to be fed to the distillation column of the second step.
Claim 4
Dependent Claim 23 words
A recovery method according to claim 1, wherein the acetic acid concentration in the starting aqueous solution is 7 to 40% by weight.
Claim 5
Dependent Claim 26 words
A recovery method according to claim 1, wherein the extraction of the first step is carried out by using a mixer-settler type counter-current multi-stage extracting device.
Claim 6
Dependent Claim 50 words
A recovery method according to claim 1, wherein the tertiary amine has 12 to 40 carbon atoms and in the partial structure >N-CH 2 CR 1 R 2 - of said tertiary amine, R 1 is a hydrogen atom and R 2 is a hydrogen atom or a methyl group.
Claim 7
Dependent Claim 13 words
A recovery method according to claim 5, wherein the tertiary amine is tri-n-octylamine.
Claim 8
Dependent Claim 14 words
A recovery method according to claim 1, wherein the oxygen-containing organic solvent is 3,3,5-trimethylcyclohexanone.
Claim 9
Dependent Claim 29 words
A recovery method according to claim 1, wherein the oxygen-containing organic solvent is a member selected from the group consisting of isophorone, 2-ethoxethyl acetate, methyl benzoate and tributyl phosphate.
Claim 10
Dependent Claim 15 words
A recovery method according to claim 1, wherein the oxygen-containing organic solvent is di-isobutyl carbinol.
Claim 11
Dependent Claim 24 words
A recovery method according to claim 1, wherein the proportion of the tertiary amine in the extraction solvent is 10 to 80% by volume.
Claim 12
Dependent Claim 22 words
A recovery method according to claim 10, wherein the proportion of the tertiary amine in the extraction solvent is 50% by volume.
Claim 13
Dependent Claim 25 words
A recovery method according to claim 1, wherein the extraction of the first step is carried out at a temperature not higher than 50° C.
Claim 14
Dependent Claim 23 words
A recovery method according to claim 1, wherein the third step is conducted at a column bottom temperature of 120° to 150° C.

References Cited (Backward Citations)

US2588268A Cited
US2571919A Cited
US2568095A Cited
US2868832A Cited
US3394058A Cited
US3433831A Cited
US3692829A Cited
US3980702A Cited
US4143066A Cited
JPS55154935A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1985-10-11 1986-04-12 1986-10-12 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1989-10-11 1990-04-12 1990-10-12 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1993-10-11 1994-04-12 1994-10-12 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag