DE2350567A1 - RECOVERY OF GLYCOL FROM SALT WASTE WATER - Google Patents
RECOVERY OF GLYCOL FROM SALT WASTE WATERInfo
- Publication number
- DE2350567A1 DE2350567A1 DE19732350567 DE2350567A DE2350567A1 DE 2350567 A1 DE2350567 A1 DE 2350567A1 DE 19732350567 DE19732350567 DE 19732350567 DE 2350567 A DE2350567 A DE 2350567A DE 2350567 A1 DE2350567 A1 DE 2350567A1
- Authority
- DE
- Germany
- Prior art keywords
- glycol
- salt
- waste water
- recovery
- production
- 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.)
- Pending
Links
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims description 64
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 title claims description 32
- 150000003839 salts Chemical class 0.000 title claims description 19
- 239000002351 wastewater Substances 0.000 title claims description 13
- 238000011084 recovery Methods 0.000 title claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 5
- 238000005115 demineralization Methods 0.000 claims description 4
- 230000002328 demineralizing effect Effects 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 238000001223 reverse osmosis Methods 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 229920002301 cellulose acetate Polymers 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000004821 distillation Methods 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- KVIPHDKUOLVVQN-UHFFFAOYSA-N ethene;hydrate Chemical group O.C=C KVIPHDKUOLVVQN-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
FARBWERKE HOECHST AG vormals Meister Lucius & Brüning WERK GENDORFFARBWERKE HOECHST AG formerly Master Lucius & Brüning WERK GENDORF
HOE 73/F 914HOE 73 / F 914
Gendorf, den 3.10.1973 Gd. 1569 ~r>cnt:e>n Gendorf, October 3rd, 1973 Gd. 1569 ~ r> cnt: e> n
n /mi /350567 n / mi / 350567
Aktenzeichen: Dr· Br/HH File number: Dr Br / HH
"Wiedergewinnung von Glykol aus salzhaltigem Abwasser""Recovery of glycol from saline wastewater"
Gegenstand der Erfindung ist ein Verfahren zur Wiedergewinnung von Glykol aus salzhaltigem Abwasser aus Anlagen zur Herstellung von.Äthylenoxid nach dem Direktoxidationsverfahren, welches dadurch gekennzeichnet ist, daß man das mit Salz und Glykol belastete Abwasser mit Hilfe der Umkehrosmose unter einem Druck von 30 bis 100 atü durch semipermeable Membranen aus Celluloseacetat oder Kunststoffen, vorzugsweise aus Polyamid, leitet, die dabei erhaltene, nur noch Spuren von Salz enthaltende Glykollösung entweder direkt oder nach Vollentsalzung mittels Ionentauschern wieder in die Oxid- bzw. Glykolproduktion zurückführt und die abgeschiedene Salzlösung verwirft.The invention relates to a method of recovery of glycol from saline wastewater from plants for the production of.Ethylenoxid after the direct oxidation process, which thereby is characterized by the fact that the wastewater contaminated with salt and glycol is pressurized with the help of reverse osmosis from 30 to 100 atü through semipermeable membranes made of cellulose acetate or plastics, preferably made of polyamide, conducts the glycol solution obtained, which only contains traces of salt either directly or after full demineralization using ion exchangers returns to the oxide or glycol production and discards the separated salt solution.
Bei der Herstellung von Äthylenoxid nach dem Direktoxidationsverfahren wird bereits in einer Nebenr'eaktionIn the production of ethylene oxide using the direct oxidation process is already in a side reaction
C2H4 + 3 O2 > 2 CO2 + 2 H2OC 2 H 4 + 3 O 2 > 2 CO 2 + 2 H 2 O
Kohlendioxid und Wasser gebildet, in geringem Umfang auch organische Säuren, die neutralisiert und zusammen mit dem Wasser ausgeschleust werden. Gleichzeitig wird dabei auchNatriumbicarbonat gebildet. Die auf diese Weise entstehende Salzlösung enthält auch Glykol, das durch Hydrolyse von im Wasser gelösten Äthylenoxid gebildet wird. Während das außerdem in der Salzlösung befindliche Äthylenoxid leicht durch Destillation entfernt werden kann, verbleibt das Glykol zusammen mit dem Salz im Wasser, das die Anlagen als zwar mengenmäßig kleiner, aber mit organischer Substanz hoch belasteter Abwasserstrom verläßt. Carbon dioxide and water are formed, also organic to a small extent Acids that are neutralized and discharged together with the water. At the same time, sodium bicarbonate is also used educated. The resulting salt solution also contains glycol, which is produced by hydrolysis of dissolved in the water Ethylene oxide is formed. While the ethylene oxide also contained in the salt solution is easily removed by distillation can be, the glycol remains together with the salt in the water, which the systems as though quantitatively smaller, but with organic matter highly contaminated wastewater flow leaves.
Die Konzentration an Glykol und Salz in diesem Abwasser schwankt je zwischen 1,5 und 3 Gew.-?l>. Diese hohe organische Belastung verursacht einerseits hohe Aufbereitungskosten in den biologischen Kläranlagen, andererseits einen Verlust an Glykol, derThe concentration of glycol and salt in this wastewater fluctuates each between 1.5 and 3 wt .-? l>. This high organic load on the one hand causes high processing costs in the biological Sewage treatment plants, on the other hand, a loss of glycol that
-Z--Z-
509815/1324509815/1324
in etwa 0,5 % der Äthylenoxid-Produktion beträgt. Es ist deshalb wünschenswert, das in diesem Abwasser enthaltene Glykol wiederzugewinnen, was aber infolge des gleichzeitig hohen Salzgehaltes äußerst schwierig ist.is about 0.5 % of ethylene oxide production. It is therefore desirable to recover the glycol contained in this waste water, but this is extremely difficult due to the high salt content at the same time.
Versuche, das Glykol durch Destillation wiederzugewinnen, scheitern daran, daß nach der Entfernung des größten Teils des Wassers ein glykolhaltiger Salzbrei zurückbleibt, aus dem sich das Glykol nicht abdestillieren läßt. Auch durch Extraktion ist das Problem wirtschaftlich nicht zu lösen, da polare Lösungsmittel Glykol und Salz zugleich extrahieren und nichtpolare Lösungsmittel kein.en der beiden Stoffe.Attempts to recover the glycol by distillation fail because after the majority of it has been removed a glycol-containing salt paste remains from the water from which the glycol cannot be distilled off. The problem cannot be solved economically by extraction either, since polar solvents extract glycol and salt at the same time and non-polar solvents extract none of the two substances.
Es wurde nun gefunden, daß eine weitgehende Trennung von Glykol und Salz möglich ist, wenn man die glykolhaltige Salzlösung der Umkehrosmose unterwirft. Die semipermeablen Membranen lassen Glykol und Wasser durch und halten das Salz weitgehend zurück.It has now been found that an extensive separation of glycol and salt is possible if the glycol-containing Reverse osmosis saline solution. The semi-permeable membranes let glycol and water through and hold that Salt largely back.
Nach diesem Verfahren lassen sich mindestens 60 % des im Abfallwasser enthaltenen Glykols wiedergewinnen. Man erhält auf diese Weise eine ca.1- bis 1,5-prozentige Lösung von Glykol in Wasser, die nur noch Spuren von Salz enthält und entweder direkt in eine Glykolanlage eingespeist werden kann, wo der nur noch geringe Salzgehalt in den Sümpfen der Glykoldestillation nicht stört, oder nach Vollentsalzung mit Ionentauschern innerhalb der Äthylenoxid- bzw. Glyko!produktion wieder eingesetzt werden kann. Somit kann ein großer Teil des sonst mit dem Abwasser verlorenen Glykols auf einfache Weise wiedergewonnen werden, was aus wirtschaftlichen Gründen nur erwünscht ist.Using this process, at least 60 % of the glycol contained in the waste water can be recovered. In this way, an approximately 1 to 1.5 percent solution of glycol in water is obtained, which only contains traces of salt and can either be fed directly into a glycol system, where the only low salt content in the sumps of the glycol distillation does not interfere, or can be used again after complete demineralization with ion exchangers within the ethylene oxide or glyco! production. Thus, a large part of the glycol otherwise lost with the wastewater can be recovered in a simple manner, which is only desirable for economic reasons.
-3--3-
509815/1324509815/1324
ORIGINAL INSPECTEDORIGINAL INSPECTED
Abwasser aus einer Äthylenoxid-Anlage nach dem Direktoxidationsverfahren wird mit Hilfe einer Hochdruckpumpe durch im Handel erhältliche Membraneinheiten zur Umkehrosmose, ausgerüstet mit Hohlfasern aus Polyamid, kontinuierlich durchgefahren.Waste water from an ethylene oxide plant using the direct oxidation process is commercially available with the help of a high pressure pump available membrane units for reverse osmosis, equipped with hollow fibers made of polyamide, passed through continuously.
Einsatz: 700 kg/h AbwasserUse: 700 kg / h wastewater
Konsentration an Glykol: 1,5 Gew.-?a = 10,5 kg/h
Konzentration an Salz: 1,2 Gew.-2'ό = 8,4 kg/hGlycol concentration: 1.5 wt .-? A = 10.5 kg / h
Concentration of salt: 1.2% by weight = 8.4 kg / h
gereinigte Lösung: 521 kg/hpurified solution: 521 kg / h
Konzentration an Glykol: 1,28 Gew.-$ = 6,67 kg/h Konzentration an Salz: 0,05 Gevt.-% = 0,26 kg/hConcentration of glycol: 1.28% by weight = 6.67 kg / h Concentration of salt: 0.05 % by weight = 0.26 kg / h
Rückstand: 179 kg/h "Residue: 179 kg / h "
Konzentration an Glykol: 2,13 Gew.-% = 3,82 kg/h Konzentration an Salz: 4,56 Gevr.-% =8,14 kg/hConcentration of glycol: 2.13% by weight = 3.82 kg / h Concentration of salt: 4.56 % by weight = 8.14 kg / h
In der gereinigten Lösung sind somit 63,6 % des in der Rohlösung enthaltenen Glykols, aber nur noch 3»1 % des in der Rohlösung enthaltenen Salzes vorhanden.The purified solution thus contains 63.6 % of the glycol contained in the raw solution, but only 3 »1 % of the salt contained in the raw solution.
Die gereinigte Lösung wird direkt oder nach Vollentsalzung mit lonentauschern in die Oxid- bzw. Glykolproduktion zurückgefahren. Der salzhaltige Rückstand wird verworfen.The cleaned solution is returned to oxide or glycol production directly or after complete demineralization with ion exchangers. The salt-containing residue is discarded.
-4--4-
5098 15/13245098 15/1324
Claims (1)
Priority Applications (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19732350567 DE2350567A1 (en) | 1973-10-09 | 1973-10-09 | RECOVERY OF GLYCOL FROM SALT WASTE WATER |
| NL7413125A NL7413125A (en) | 1973-10-09 | 1974-10-04 | METHOD FOR RECOVERING GLYCOL FROM OLD WASTEWATER. |
| IT28146/74A IT1022659B (en) | 1973-10-09 | 1974-10-07 | GLYCOL RIOLPER FROM SOARTO WATERS CONTAINING SALT |
| JP49115259A JPS5064205A (en) | 1973-10-09 | 1974-10-08 | |
| BE149347A BE820856A (en) | 1973-10-09 | 1974-10-09 | METHOD FOR RECOVERING ETHYLENE-GLYCOL FROM SALINE WASTEWATER |
| FR7433972A FR2246527B1 (en) | 1973-10-09 | 1974-10-09 | |
| GB4368274A GB1463324A (en) | 1973-10-09 | 1974-10-09 | Process for recovering glycol from waste water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19732350567 DE2350567A1 (en) | 1973-10-09 | 1973-10-09 | RECOVERY OF GLYCOL FROM SALT WASTE WATER |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE2350567A1 true DE2350567A1 (en) | 1975-04-10 |
Family
ID=5894879
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19732350567 Pending DE2350567A1 (en) | 1973-10-09 | 1973-10-09 | RECOVERY OF GLYCOL FROM SALT WASTE WATER |
Country Status (7)
| Country | Link |
|---|---|
| JP (1) | JPS5064205A (en) |
| BE (1) | BE820856A (en) |
| DE (1) | DE2350567A1 (en) |
| FR (1) | FR2246527B1 (en) |
| GB (1) | GB1463324A (en) |
| IT (1) | IT1022659B (en) |
| NL (1) | NL7413125A (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4427507A (en) | 1982-03-22 | 1984-01-24 | Shell Oil Company | Process for the separation of glycol from an electrolyte-containing aqueous solution |
| FR2564458B1 (en) * | 1984-05-15 | 1986-09-12 | Atochem | PROCESS FOR SEPARATING ETHYLENEGLYCOL IN CONCENTRATED FORM IN A PROCESS FOR PRODUCING ETHYLENE OXIDE |
| US5194159A (en) * | 1989-12-27 | 1993-03-16 | Union Carbide Chemicals & Plastics Technology Corporation | Treatment of lower glycol-containing operative fluids |
| US5034134A (en) * | 1989-12-27 | 1991-07-23 | Union Carbide Chemicals And Plastics Technology Corporation | Treatment of impurity-containing liquid streams in ethylene oxide/glycol processes with semi-permeable membranes |
| US5102549A (en) * | 1989-12-27 | 1992-04-07 | Union Carbide Chemicals & Plastics Technology Corporation | Treatment of lower glycol-containing operative fluids |
| DE4326345A1 (en) * | 1993-08-05 | 1995-02-09 | Hoechst Ag | Process for the reprocessing of used glycolic aircraft de-icing agents |
| GB9411020D0 (en) * | 1994-06-02 | 1994-07-20 | Britannia Natural Products Ltd | Juice and juice aroma concentrate production |
-
1973
- 1973-10-09 DE DE19732350567 patent/DE2350567A1/en active Pending
-
1974
- 1974-10-04 NL NL7413125A patent/NL7413125A/en unknown
- 1974-10-07 IT IT28146/74A patent/IT1022659B/en active
- 1974-10-08 JP JP49115259A patent/JPS5064205A/ja active Pending
- 1974-10-09 FR FR7433972A patent/FR2246527B1/fr not_active Expired
- 1974-10-09 GB GB4368274A patent/GB1463324A/en not_active Expired
- 1974-10-09 BE BE149347A patent/BE820856A/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| NL7413125A (en) | 1975-04-11 |
| GB1463324A (en) | 1977-02-02 |
| IT1022659B (en) | 1978-04-20 |
| BE820856A (en) | 1975-04-09 |
| FR2246527A1 (en) | 1975-05-02 |
| FR2246527B1 (en) | 1978-05-05 |
| JPS5064205A (en) | 1975-05-31 |
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