US4254246A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Column system process for polyester plants
Assignee: LL Plant Engineering AG
•
Filing: 1979-03-26
•
Granted: 1981-03-03
•
Expires: 1999-03-26
Abstract
Abstract A new process for use with continuously operated plants for the production of polyester polymers suitable for producing fibers, bottles and film, by reacting ethylene glycol and terephthalic acid in the presence of a catalyst so that the vapour by-products from the esterification, prepolycondensation and polycondensation stages are continuously rectified in two in-line columns yielding ethylene glycol of high purity (99.85%) which is returned to the process, waste water with 400 ppm ethylene glycol, and a heavy fraction containing oligomers, diethylene glycol, etc. Moreover, an improvement in the quality of the esterified product is attained as it contains less than 0.6% diethylene glycol without the use of diisopropylamine, a poisonous additive.
Inventors
- 👤 Ovidiu Dicoi
- 👤 Hans Wewer
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 16:17
CPC Classifications
C; C07; C07C; C07C29/00; C07C29/74; C07C29/76; C07C29/80; Y; Y10; Y10S; Y10S203/00; Y10S203/06
Claims Analysis
Total Claims: 9
Claim 1
Independent Claim
289 words
A continuous process for purifying and recovering at least 99% ethylene glycol from the vapour by-products generated in three reactors (esterification, prepolycondensation and polycondensation) during the reaction of ethylene glycol and terephthalic acid to produce polyethylene glycol terephthalate polymer, said by-products being contamined with aldehydes, water, diethylene glycol and oligomers, which comprises: (a) providing an enriching column and a rectification column, (b) introducing a first stream of ethylene glycol vapours from the esterification stage into the bottom of said enriching column, said first stream containing at least about 90% ethylene glycol, (c) introducing a second stream of ethylene glycol condensate from the pre- and polycondensation reactors into said enriching column above said first stream for flow countercurrent to the upward flow of said first stream, thereby condensing said diethylene glycol and oligomers, (d) removing the resulting mixture of ethylene glycol, diethylene glycol and oligomers from the bottom of said enriching column at a rate which maintains some liquid in the bottom of said column into which liquid said first stream is introduced, (e) charging the resulting mixture of aqueous ethylene glycol vapour and aldehydes rising from the top of said enriching column into said rectification column, (f) condensing a portion of said aqueous ethylene glycol vapour and refluxing the condensate in the rectification column to condense ethylene glycol from said aqueous ethylene glycol vapour, (g) removing from the top of said rectification column a portion of said aqueous vapours containing less than 440 ppm ethylene glycol, condensing the vapours and discharging the condensate directly to waste, (h) withdrawing from the bottom of said rectification column ethylene glycol of at least 99.85% purity, and (i) recycling at least a portion of said pure ethylene glycol directly into said esterification reactor.
Claim 2
Dependent Claim
289 words
A continuous process for purifying and recovering at least 99% ethylene glycol from the vapour by-products generated in three reactors (esterification, prepolycondensation and polycondensation) during the reaction of ethylene glycol and terephthalic acid to produce polyethylene glycol terephthalate polymer, said by-products being contamined with aldehydes, water, diethylene glycol and oligomers, which comprises: (a) providing an enriching column and a rectification column, (b) introducing a first stream of ethylene glycol vapours from the esterification stage into the bottom of said enriching column, said first stream containing at least about 90% ethylene glycol, (c) introducing a second stream of ethylene glycol condensate from the pre- and polycondensation reactors into said enriching column above said first stream for flow countercurrent to the upward flow of said first stream, thereby condensing said diethylene glycol and oligomers, (d) removing the resulting mixture of ethylene glycol, diethylene glycol and oligomers from the bottom of said enriching column at a rate which maintains some liquid in the bottom of said column into which liquid said first stream is introduced, (e) charging the resulting mixture of aqueous ethylene glycol vapour and aldehydes rising from the top of said enriching column into said rectification column, (f) condensing a portion of said aqueous ethylene glycol vapour and refluxing the condensate in the rectification column to condense ethylene glycol from said aqueous ethylene glycol vapour, (g) removing from the top of said rectification column a portion of said aqueous vapours containing less than 440 ppm ethylene glycol, condensing the vapours and discharging the condensate directly to waste, (h) withdrawing from the bottom of said rectification column ethylene glycol of at least 99.85% purity, and (i) recycling at least a portion of said pure ethylene glycol directly into said esterification reactor.
Claim 3
Dependent Claim
29 words
The process of claim 1 in which said refluxing condensate of step (f) is a portion of aqueous ethylene glycol vapour discharged from the top of the rectification column.
Claim 4
Dependent Claim
23 words
The process of claim 1 in which another portion of pure ethylene glycol is charged into said enriching column above said second stream.
Claim 5
Dependent Claim
56 words
The process of claim 3 in which said second stream contains at least 90% ethylene glycol and said another portion of pure ethylene glycol is maintained at a temperature below about 170° C. to condense traces of diethylene glycol in the ascending aqueous vapour mixture and reduce the diethylene glycol content to less than 100 ppm.
Claim 6
Dependent Claim
40 words
The process of claim 3 in which said another portion of pure ethylene glycol is charged between 160° and 170° C. and at a ratio of 0.2 to 0.4 with respect to the quantity of ethylene glycol in said stream.
Claim 7
Dependent Claim
31 words
The process of claim 1 in which said ethylene glycol condensate of step (c) is condensed prior to forming said second stream by contacting with pure ethylene glycol from step (g).
Claim 8
Dependent Claim
38 words
The process of claim 6 in which said contacting step is carried out under vacuum and said pure ethylene glycol is a motion fluid for carrying the vapours from the pre- and polycondensation reactors through said contacting step.
Claim 9
Dependent Claim
26 words
The process of claim 1 in which the pressure prevailing in said prepolycondensation reactor ranges from 250-50 mbar and in said polycondensation reactor from 1-2 mbar.
References Cited (Backward Citations)
US3367847A
Cited
US4146729A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-03-02 | 1984-09-01 | 1985-03-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-03-02 | 1988-09-01 | 1989-03-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-03-02 | 1992-09-01 | 1993-03-03 | $7700.00 | Window Closed / Lapsed |