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US3886199A Expired / Lapsed US ⏱️ 0.0 years remaining

Manufacture of diesters of dicarboxylic acids with substantial waste water purification

Assignee: BASF SE
•
Filing: 1973-06-18
•
Granted: 1975-05-27
•
Expires: 1993-06-18
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Abstract

Abstract Manufacture of diesters of dicarboxylic acids from aliphatic or aromatic dicarboxylic acids or their anhydrides and alcohols of from three to 15 carbon atoms, in which substantial purification of the waste water is achieved by treating the waste water with the same alcohol as used in the ester synthesis.

Inventors

  • 👤 Hubert Suter
  • 👤 Rosemarie Berger
  • 👤 Hansjoerg Bipp
  • 👤 Gert Buerger
  • 👤 Kurt Hauptmann
  • 👤 Otto Kratzer
  • 👤 Willi Reimer

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 20:06
CPC Classifications
C; C02; C02F; C02F1/00; C02F1/26; C02F2101/00; C02F2101/30; C02F2101/34; C02F2101/345; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/582

Claims Analysis

Total Claims: 7
Claim 1
Independent Claim 249 words
IN A CONTINUOUS PROCESS FOR THE MANUFACTURE OF THE DIESTER OF A DICARBOXYLIC ACID BY ESTERIFICATION OF A DICARBOXYLIC ACID COMPONENT SELECTED FROM THE GROUP CONSISTING OF PHTHALIC ANHYDRICE, MALEIC ANHYDRIDE AND ACIDS OF THE FORMULA HOOC-(CH2)N-COOH IN WHICH N IS A WHOLE NUMBE OF 1 TO 8 WITH AN ALCOHOL SELECTED FROM THE GROUP CONSISTING OF NUTANOL, N-OCTANOL-1, N-OCTANOL-2, 2-ETHYLHEXANOL-1, N-NONYL ALCOHOL, DECANOL AND ISODECANOL, ESTERIFICATION BEING CARRIED OUT WITH RECYCLING OF THE ALCOHOL USED IN EXCESS AND IN THE ABSENCE OF AN ESTERIFICATION CATALYST AT A TEMPERATURE OF FROM 150* TO 150* C AND THE REACTION MIXTURE BEING SEPARATED FROM THE WATER OF REACTION, STEAMED OUT AND THEN MIXED WITH AN AQUEOUS ALKALI FOR SEPARATION OF THE MONOESTER, THE RESULTING AQUEOUS MONOESTER SALT SOLUTION BEING ACIDIFIED FOR THE RECOVERY OF THE MONOESTER, THE IMPROVEMENT WHICH COMPRISES: TREATING THE AQUEOUS MONOESTER SALT SOLUTION AFTER ACIDIFICATION WITH FROM0.5 TO 1 TIMES ITS WEIGHT OF THE SAME ALCOHOL AS USED IN THE ESTER SUNTHESIS; SEPARATING THE RESULTING MIXTURE INTO ALCOHOLIC ANC AQUEOUS PHASES AND THEN EXTRACTING THE SEPARATED AQUEOUS PHASE WITH FROM 1 TO 2 TIMES ITS WEIGHT OF THE SAME ALCOHOL; RECYCLING THE ALCOHOLIC PHASE FROM SAID SEPARATION AND SAID EXTRACTION TO THE ESTERIFICATION REACTION; COMBINING SAID WATER OF REACTON SEPARATED FROM THE ESTERIFICATION REACTION MIXTURE AS A WASTE WATER WITH SAID AQUEOUS PHASE RESULTING FROM THE EXTRACTION STEP; AND REMOVING THE ALCOHOL TRACES WHICH REMAIN IN THE RESULTING COMBINED WASTE WATER AND AQUEOUS PHASE BY BLOWING STEAM THERETHROUGH.
Claim 2
Dependent Claim 249 words
IN A CONTINUOUS PROCESS FOR THE MANUFACTURE OF THE DIESTER OF A DICARBOXYLIC ACID BY ESTERIFICATION OF A DICARBOXYLIC ACID COMPONENT SELECTED FROM THE GROUP CONSISTING OF PHTHALIC ANHYDRICE, MALEIC ANHYDRIDE AND ACIDS OF THE FORMULA HOOC-(CH2)N-COOH IN WHICH N IS A WHOLE NUMBE OF 1 TO 8 WITH AN ALCOHOL SELECTED FROM THE GROUP CONSISTING OF NUTANOL, N-OCTANOL-1, N-OCTANOL-2, 2-ETHYLHEXANOL-1, N-NONYL ALCOHOL, DECANOL AND ISODECANOL, ESTERIFICATION BEING CARRIED OUT WITH RECYCLING OF THE ALCOHOL USED IN EXCESS AND IN THE ABSENCE OF AN ESTERIFICATION CATALYST AT A TEMPERATURE OF FROM 150* TO 150* C AND THE REACTION MIXTURE BEING SEPARATED FROM THE WATER OF REACTION, STEAMED OUT AND THEN MIXED WITH AN AQUEOUS ALKALI FOR SEPARATION OF THE MONOESTER, THE RESULTING AQUEOUS MONOESTER SALT SOLUTION BEING ACIDIFIED FOR THE RECOVERY OF THE MONOESTER, THE IMPROVEMENT WHICH COMPRISES: TREATING THE AQUEOUS MONOESTER SALT SOLUTION AFTER ACIDIFICATION WITH FROM0.5 TO 1 TIMES ITS WEIGHT OF THE SAME ALCOHOL AS USED IN THE ESTER SUNTHESIS; SEPARATING THE RESULTING MIXTURE INTO ALCOHOLIC ANC AQUEOUS PHASES AND THEN EXTRACTING THE SEPARATED AQUEOUS PHASE WITH FROM 1 TO 2 TIMES ITS WEIGHT OF THE SAME ALCOHOL; RECYCLING THE ALCOHOLIC PHASE FROM SAID SEPARATION AND SAID EXTRACTION TO THE ESTERIFICATION REACTION; COMBINING SAID WATER OF REACTON SEPARATED FROM THE ESTERIFICATION REACTION MIXTURE AS A WASTE WATER WITH SAID AQUEOUS PHASE RESULTING FROM THE EXTRACTION STEP; AND REMOVING THE ALCOHOL TRACES WHICH REMAIN IN THE RESULTING COMBINED WASTE WATER AND AQUEOUS PHASE BY BLOWING STEAM THERETHROUGH.
Claim 3
Dependent Claim 27 words
A process as claimed in claim 1, wherein the dicarboxylic acid or dicarboxylic anhydride used is adipic acid or phthalic anhydride and the alcohol used is 2-ethylhexanol-1.
Claim 4
Dependent Claim 28 words
A process as claimed in claim 1, where the addition of alcohol to the aqueous monoester salt solution is carried out at temperatures of up to 100* C.
Claim 5
Dependent Claim 35 words
A process as claimed in claim 1, wherein the extraction of separated aqueous phase with from 1 to 2 times its weight of alcohol is carried out at temperatures of from 50* to 100* C.
Claim 6
Dependent Claim 15 words
A process as claimed in claim 1 wherein the dicarboxylic acid component is adipic acid.
Claim 7
Dependent Claim 15 words
A process as claimed in claim 1 wherein the dicarboxylic acid component is phthalic anhydride.

References Cited (Backward Citations)

US3843697A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1978-05-26 1978-11-25 1979-05-27 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-05-26 1982-11-25 1983-05-27 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-05-26 1986-11-25 1987-05-27 $7700.00 Window Closed / Lapsed

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