DE1208291B - Continuous process for the distillative purification of evaporable organic substances from difficult or non-evaporable substances - Google Patents
Continuous process for the distillative purification of evaporable organic substances from difficult or non-evaporable substancesInfo
- Publication number
- DE1208291B DE1208291B DEB47311A DEB0047311A DE1208291B DE 1208291 B DE1208291 B DE 1208291B DE B47311 A DEB47311 A DE B47311A DE B0047311 A DEB0047311 A DE B0047311A DE 1208291 B DE1208291 B DE 1208291B
- Authority
- DE
- Germany
- Prior art keywords
- evaporable
- substances
- distillation column
- difficult
- sump
- 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
- 239000000126 substance Substances 0.000 title claims description 16
- 238000010924 continuous production Methods 0.000 title claims description 3
- 238000000746 purification Methods 0.000 title claims description 3
- 238000004821 distillation Methods 0.000 claims description 18
- 239000010409 thin film Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 description 7
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000006356 dehydrogenation reaction Methods 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005194 fractionation Methods 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000011552 falling film Substances 0.000 description 1
- 210000003918 fraction a Anatomy 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- -1 nitrogenous organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000008262 pumice Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/148—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/06—Evaporators with vertical tubes
- B01D1/065—Evaporators with vertical tubes by film evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Description
Kontiunuierliches Verfahren zur destillativen Reinigung verdampfbarer organischer Stoffe von schwer oder nicht verdampfbaren Begleitstoffen Gemische aus verdampfbaren organischen Stoffen und schwer oder nicht verdampfbaren Begleitstoffen hat man bisher in einem Verdampfer oder in einer Destillationskolonne zerlegt, die dabei erhaltenen Rückstände gesammelt und periodisch hieraus weitere verdampfbare Anteile bei höheren Temperaturen ausgetrieben. Bei dieser Arbeitsweise wird ein verhältnismäßig großer Anteil der zu zerlegenden Stoffe zersetzt, Die Rückstände empfindlicher Stoffe hat man deshalb in Dünnschichtverdampfern aufgearbeitet, um so die Reste der verdampfbaren anteile abzutrennen. Da die in Verdampfern oder in Destillationskolonnen erhaltenen Rückstände oftmals eine große Menge verdampfbarer Anteile enthalten und daher einen hohen Anteil am Gesamtvolumen der Ausgangsstoffe ausmachen, ist es notwendig, mehrere Dünnschichtverdampfer zu verwenden, da die Verdampfungskapazität von Dünnschichtverdampfern bekanntermaßen klein ist.Continuous process for the purification of vaporizers by distillation of organic substances made up of mixtures that are difficult to evaporate or that cannot be evaporated Organic substances that can be evaporated and accompanying substances that are difficult or impossible to evaporate has so far been disassembled in an evaporator or in a distillation column, the residues obtained in the process are collected and periodically further vaporizable therefrom Shares expelled at higher temperatures. In this way of working, a Relatively large proportion of the substances to be broken down decomposed, the residues Sensitive substances have therefore been processed in thin-film evaporators in order to in this way to separate off the remnants of the vaporizable components. Since those in vaporizers or in Residues obtained in distillation columns often have a large amount of vaporizable material Contain proportions and therefore a high proportion of the total volume of the starting materials make up, it is necessary to use several thin film evaporators because the Evaporation capacity of thin film evaporators is known to be small.
Es ist vorteilhaft, nach Art der bekannten Zwei stufenfraktionierung solche Gemische kontinuierlich destillativ von den Begleitstoffen zu reinigen indem man die Gemische, gegebenenfalls nadi Vorerhitzung, in eine Destillationskolonne einführt, in welcher ein erheblicller Teil der verdampfbaren Bestandteile verdampft wird. Der verdampfte Anteil wird am Kopf der Kolonne als gereinigt abgezogen. Der flüssige Anteil (Sumpf) wird dabei m Umlaul erhitzt. Wenigstens die dadurch gebildeten Dämpfe werden oberhalb des Sumpfes in die Destillationskolonne zurückgeführt. Gleichzeitig wird stetig aus einem kleinen Teil der Sumpffraktion In einer zw ten Trennstufe der Rest der verdampfbaren Bestandtile abgetrieben. It is advantageous to use the known two-stage fractionation to continuously purify such mixtures from the accompanying substances by distillation the mixtures, optionally after preheating, in a distillation column introduces, in which a significant part of the vaporizable constituents evaporates will. The vaporized portion is withdrawn as purified at the top of the column. Of the The liquid part (sump) is heated in the umlaul. At least those formed by it Vapors are returned to the distillation column above the bottom. Simultaneously becomes steadily from a small part of the bottom fraction in a second separation stage the rest of the vaporizable components are driven off.
Dieser Rest wird, vorzugsweise nach Kondensation, der Destillationskolonne wieder zugeführt.This remainder becomes the distillation column, preferably after condensation fed back.
Bei bekannten Verfahren dieser Art hat man sich bemüht, von Stufe zu Stufe die Abtrennttrg der verdampfbaren Stoffe möglichst weit zu treiben. Hierbei sind Zersetzungen bzw. Flogereaktionen unve-meidsich, so daß der erfindungsgemäß angestrebte Zweck, den verdampfbaren Hauptbestandteil in möglichst reiner Form in möglichst hoher Ausbeute zu erhalten, nicht erreicht wird. In known processes of this type, efforts have been made from stage to stage the separation of the vaporizable substances as far as possible. Here decomposition or float reactions are unavoidable, so that according to the invention intended purpose, the vaporizable main constituent in as pure a form as possible in To obtain the highest possible yield is not achieved.
Erfindungsgemäß lassen sich dies Nachteile meiden, indem man die Hauptverdampfung in der Destillationskolonne nur so weit treibt, daß in der Sumpffraktion ein Gehalt an schwer oder nicht veerdampfbaren Bestandteilen von 30 bis 75 %, insbesondere von 40 bis 60 %, aufrechterhalten wird und dann die Trennung in der zweiten Stufe nicht wie nach dem bekannten Stand der Technik in einer Fraktionierkolonne, in der Regel mit Umlaufverdampfer, son- dem durch Dünnschichtverdampfung vorgenommen wird. According to the invention, these disadvantages can be avoided by the Main evaporation in the distillation column only drives so far that in the bottom fraction a content of constituents which are difficult to evaporate or which cannot be evaporated from 30 to 75%, in particular from 40 to 60%, is maintained and then the separation in the second stage not as in the known prior art in a fractionation column in which Usually with a circulation evaporator, but which is carried out by thin film evaporation.
Auf diese Weise wird durch Aufrechterhaltung eines gewissen Mindestgehaltes an verdampfbaren Anteilen im Sumpf die thermische Zersetzung weitgehend zurückgedrängt. Die Dünnschichtverdampfung ermöglicht auf schonende Weise die Austreibung des Restes der verdampfbaren Stoffe. Der apparative Aufwand für diese Verfahreusstufe ist dabei durch die Vornahme der Hauptverdampfung iii der Destillationskolonne auf ein erträgliches Maß zurückgeführt, und die Dünnschichtverdampfung stellt so keinen. Engpaß für das Gesamtreiningungsverfahren dar. This is done by maintaining a certain minimum salary the thermal decomposition largely suppressed in the evaporable parts in the sump. The thin-film evaporation enables the remainder to be expelled in a gentle manner of vaporizable substances. The outlay on equipment for this process stage is included by undertaking the main evaporation iii of the distillation column to a tolerable level Measure back, and thin-film evaporation does not provide any. Bottleneck for that Overall cleaning process.
Es ist vorteilhaft, bei einer Reinigung von organischen Syntheseprodukten exothermer Reaktionen die frei werdende Wärmemenge oder die Wärme der Reaktionsprodukte solcher Reaktionen durch Wänneaustausch zur Aufheizung des zu reinigenden Gemischer, vor dessen Einführen in die Destillafionskolonne zu verwenden. Der Kreislauf zwischen Destillationskolonne und nebengeschaltetem Röhrenerhitzer kann mit Hilfe einer Pumpe betrieben werden. It is advantageous when purifying organic synthesis products exothermic reactions the amount of heat released or the heat of the reaction products such reactions through heat exchange to heat the mixture to be cleaned, to be used before introducing it into the distillation column. The cycle between The distillation column and the adjacent tube heater can be operated with the help of a pump operate.
Man kann zusätzlich in die Destillationskolonne Wasserdampf einführen. Steam can also be introduced into the distillation column.
Die im Erhitzer angereicherten Begleitstoffe gelangen über den Sumpf der Kolonne oder unmittelbar in kleinen ANteilen, z. B. 0,5 bis 15%, insbesondere 0,5 bis 5 %, bezogen auf das Ausgangsgemisch, in den Dünnschichtverdampfer, der gegebenenfalls bei einem tieferen Druck als die Kolonne betrieben wird. The accompanying substances enriched in the heater reach the sump the column or directly in small parts, e.g. B. 0.5 to 15%, in particular 0.5 to 5%, based on the starting mixture, in the thin-film evaporator, the is optionally operated at a lower pressure than the column.
Zweckmäßig läßt man den dem Sumpf entnommenen Teil etwa 10- bis 100mal in der Stunde über den Erhitzer umlaufen. The part removed from the sump is expediently left about 10 to 100 times circulate over the heater per hour.
Als Dünnschichtverdampfer bewährt sich ein Fallstromverdampfer gut, bei dem die zu verdampfende Flüssigkeit von oben nach unten an den beheizten Rohren herunterfließt und die entstandenen Dämpfe nach oben entweichen. As a thin film evaporator, a falling film evaporator has proven itself well, in which the liquid to be evaporated from top to bottom on the heated pipes flows down and the resulting vapors escape upwards.
Das Verfahren eignet sich für die Zerlegung von Rohprodukten aus organischen Synthesen, z. B. The process is suitable for the decomposition of raw products organic syntheses, e.g. B.
Chlorierungsprodukten, stickstoffhaltigen organischen Verbindungen, wie Nitrilen, und Oxydationsprodukten.Chlorination products, nitrogenous organic compounds, such as nitriles, and oxidation products.
Auch in der Ölindustrie kann das Verfahren Verwendung finden.The process can also be used in the oil industry.
Beispiel 3200kg Cyclohexanol, das durch Umsetzung von Anilin mit Wasser und Wasserstoff hergestellt und aus dem Reaktionsgemisch abgetrennt wurde und etwa 1 °/o höhersiedende stickstoffhaltige Verbindungen enthält, werden stündlich über die Leitungl dem Wärmeaustauscher 2, in dem sie auf 160"C aufgeheizt werden, zugeführt, wobei 700/o verdampfen. Das dampfförmig-flüssige Gemisch wird der Destillationskolonne 3, die im mittleren Teil Füllkörper enthält, zugeführt. Aus dem oberen Teil der Kolonne entweichen die Dämpfe über einen Dephlegmator 6 durch die Leitung 10. Am Boden der Kolonne sammelt sich der flüssige Teil des Ausgangsgutes als Sumpf. Example 3200kg cyclohexanol, which by reacting aniline with Water and hydrogen were produced and separated from the reaction mixture and contains about 1% higher-boiling nitrogen-containing compounds every hour Via the line to the heat exchanger 2, in which they are heated to 160 "C, supplied, with 700 / o evaporating. The vapor-liquid mixture becomes the distillation column 3, which contains packing in the middle part, is supplied. From the top of the Column, the vapors escape via a dephlegmator 6 through line 10. Am At the bottom of the column, the liquid part of the starting material collects as a sump.
Etwa 1100 kg dieser Flüssigkeit werden stündlich durch Leitung 7 in den dampfbeheizten Röhrenerhitzer 8 mit 15 m2 Heizfläche geleitet, in dem die Flüssigkeit auf 160"C erhitzt wird und teilweise verdampft. Die Dämpfe und der unverdampfte Teil gelangen durch Leitung 9 oberhalb des Flüssigkeitsspiegels in die Kolonne. Im kontinuierlichen Betrieb hat der Sumpf 4 ein konstantes Volumen. Er besteht zu 350/, aus den hochsiedenden stickstoffhaltigen Begleitstoffen und zu 6501o aus Cyclohexanol. Der Stand des Sumpfes wird durch einen automatischen Regler 16 mit Regulierventil 15 konstant gehalten.About 1100 kg of this liquid are passed hourly through line 7 in the steam-heated tube heater 8 with 15 m2 heating surface, in which the liquid is heated to 160 "C and partially evaporated. The vapors and the unevaporated Part pass through line 9 above the liquid level in the column. In continuous operation, the sump 4 has a constant volume. He insists 350 /, from the high-boiling nitrogen-containing accompanying substances and 6501o from cyclohexanol. The level of the sump is controlled by an automatic regulator 16 with a regulating valve 15 held constant.
Von der Sumpffraktion werden stündlich 100 kg über die Leitungen 7 und 11 in einen Dünnschichtverdampfer 12 geführt, in dem die schwer verdampfbaren Begleitstoffe vom dampfförmigen Cyclohexanol getrennt werden. Die Dämpfe werden durch Leitung 14 oberhalb des Flüssigkeitsspiegels in die Destillationskolonne eingeführt, während durch Leitung 13 stündlich 32 kg nicht verdampfbarer Rückstand abgezogen werden.100 kg of the sump fraction are transferred every hour via lines 7 and 11 fed into a thin film evaporator 12, in which the difficult to evaporate Accompanying substances are separated from the vaporous cyclohexanol. The fumes will introduced into the distillation column through line 14 above the liquid level, while 32 kg per hour of non-evaporable residue is drawn off through line 13 will.
Das aus der Kolonne entweichende dampfförmige Cyclohexanol wird in einem Wärmeaustauscher auf 250"C erhitzt und einem beheizten Röhrenofen, dessen Rohre mit geformtem, aus Kupfer und Bimsstein bestehendem Katalysator gefüllt sind, zugeführt. Bei einmaligem Durchgang erhält man 750/o Cyclo- hexanon. Der Katalysator besitzt 4 Monate seine volle Aktivität und wird dann regeneriert. The vaporous cyclohexanol escaping from the column is in a heat exchanger heated to 250 "C and a heated tube furnace, its Tubes are filled with shaped catalyst made of copper and pumice stone, fed. With a single pass you get 750 / o Cyclo- hexanone. The catalyst is fully active for 4 months and is then regenerated.
Läßt man den Dünnschichtverdampfer weg, so ergibt sich, daß bei sonst gleicher Arbeitsweise aus dem Sumpf stündlich 106 kg (mehr als dreimal soviel wie erfindungsgemäß) abgezogen werden müssen, um ebenfalls zu einer Lebensdauer des Dehydrierkatalysators in der Cyclohexanonstufe von 4 Monaten zu kommen. Reduziert man die Mengen des endgültig abgenommenen Rückstandes auf 52 kg stündlich, so weist der Dehydrierungskatalysator in der Cyclohexanonstufe nur noch eine Lebensdauer von einer Woche auf. If the thin-film evaporator is omitted, the result is that otherwise same working method from the sump 106 kg per hour (more than three times as much as according to the invention) must be deducted in order also to a service life of the Dehydrogenation catalyst in the cyclohexanone stage of 4 months. Reduced if the quantities of the residue finally removed are 52 kg per hour, it is shown the dehydrogenation catalyst in the cyclohexanone stage only has one lifetime from a week up.
Führt man die Sumpffraktion der ersten Kolonne in eine zweite Kolonne gleicher Bauart und führt man die in der zweiten Kolonne erhaltenen Dämpfe in die erste Kolonne zurück, so kann man im Röhrenerhitzer der zweiten Kolonne die Konzentration der schwer und der nicht verdampfbaren Begleitstoffe so weit steigern, daß nur 60 kg als endgültiger Rückstand abgezogen werden müssen, ohne daß Stauungen infolge Dickflüssigkeit im Röhrenerhitzer eintreten. Allerdings beträgt die Lebensdauer des Dehydrierkatalysators dann ebenfalls nur 1 Woche. If the bottom fraction of the first column is fed into a second column of the same design and the vapors obtained in the second column are fed into the first column back, you can see the concentration in the tube heater of the second column the difficult and non-evaporable accompanying substances so much that only 60 kg must be deducted as the final residue, without jams as a result Thick liquid enter the tube heater. However, the service life is of the dehydrogenation catalyst then also only 1 week.
Claims (1)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEB47311A DE1208291B (en) | 1957-12-31 | 1957-12-31 | Continuous process for the distillative purification of evaporable organic substances from difficult or non-evaporable substances |
| GB4199358A GB900457A (en) | 1957-12-31 | 1958-12-30 | Improvements in the separation of liquid mixtures into their components |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEB47311A DE1208291B (en) | 1957-12-31 | 1957-12-31 | Continuous process for the distillative purification of evaporable organic substances from difficult or non-evaporable substances |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1208291B true DE1208291B (en) | 1966-01-05 |
Family
ID=6968226
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEB47311A Pending DE1208291B (en) | 1957-12-31 | 1957-12-31 | Continuous process for the distillative purification of evaporable organic substances from difficult or non-evaporable substances |
Country Status (2)
| Country | Link |
|---|---|
| DE (1) | DE1208291B (en) |
| GB (1) | GB900457A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2628763A1 (en) * | 1975-09-02 | 1977-03-03 | Unitech Chemical Inc | METHOD AND DEVICE FOR RECYCLING USED LUBRICATING OIL |
| US4016048A (en) * | 1975-07-17 | 1977-04-05 | Hoechst Aktiengesellschaft | Distillative purification of 2,5-dioxo-1-oxa-2-phospholanes |
| DE3338488A1 (en) * | 1982-10-29 | 1984-05-03 | Basf Ag, 6700 Ludwigshafen | Process for recovering temperature-sensitive products by thermally mild distillation using a thin layer evaporator connected to a distillation column and an arrangement for carrying out the process |
| EP1090904A3 (en) * | 1999-10-07 | 2003-01-29 | Nippon Shokubai Co., Ltd. | Purification process for hydroxyalkyl (meth)acrylate |
| EP1459794A3 (en) * | 2003-03-18 | 2004-10-20 | Nippon Shokubai Co., Ltd. | Apparatus and process for purification of acrylic acid family |
| EP1576995A3 (en) * | 2004-03-17 | 2006-08-09 | Saltigo GmbH | Method for continual separation of substance mixtures |
| WO2022106685A1 (en) * | 2020-11-23 | 2022-05-27 | Covestro Deutschland Ag | Distillation unit and method for separating a liquid substance mixture into two to six liquid product flows with different compositions |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1488994A (en) * | 1965-09-10 | 1967-07-21 | Rhone Poulenc Sa | Chlorosilane purification process |
| US3476656A (en) * | 1968-06-07 | 1969-11-04 | Universal Oil Prod Co | Fractional distillation and recovery of styrene containing sulfur with subsequent bottoms separation |
| US3515647A (en) * | 1968-12-06 | 1970-06-02 | Universal Oil Prod Co | Method for distilling styrene and subjecting bottoms to thin film evaporation |
| CN102666371B (en) | 2009-11-13 | 2015-01-07 | 巴斯夫欧洲公司 | Method for purifying a chlorine supply |
| AU2011316139B2 (en) * | 2010-10-13 | 2016-07-07 | Cognis Ip Management Gmbh | Device and method for distilling temperature-sensitive substances |
| CN112827204A (en) * | 2021-02-07 | 2021-05-25 | 吉林凯莱英医药化学有限公司 | Vacuum purification device and purification system |
| CN115228120B (en) * | 2022-08-17 | 2024-02-27 | 山东宏旭化学股份有限公司 | Vacuum pump condensate recycling mechanism |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR523445A (en) * | 1920-01-27 | 1921-08-18 | Barbet Et Fils Et Cie E | Improvements to evaporative devices with intensive circulation intended for all liquids |
| DE851635C (en) * | 1950-03-02 | 1952-10-06 | Heinrich Dr Ratte | Method and device for heating distillation columns |
| DE902005C (en) * | 1951-09-18 | 1954-01-18 | Metallgesellschaft Ag | Process for the recovery of the solvent by distillation from phenol-containing solutions |
| DE1006394B (en) * | 1952-04-24 | 1957-04-18 | Bayer Ag | Distillation device |
| US2795536A (en) * | 1955-03-29 | 1957-06-11 | California Research Corp | Liquid control for a fractionating column |
| GB787688A (en) * | 1954-09-20 | 1957-12-11 | Ruetgerswerke Ag | Process and apparatus for the evaporation of heterogeneous liquid mixtures |
-
1957
- 1957-12-31 DE DEB47311A patent/DE1208291B/en active Pending
-
1958
- 1958-12-30 GB GB4199358A patent/GB900457A/en not_active Expired
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR523445A (en) * | 1920-01-27 | 1921-08-18 | Barbet Et Fils Et Cie E | Improvements to evaporative devices with intensive circulation intended for all liquids |
| DE851635C (en) * | 1950-03-02 | 1952-10-06 | Heinrich Dr Ratte | Method and device for heating distillation columns |
| DE902005C (en) * | 1951-09-18 | 1954-01-18 | Metallgesellschaft Ag | Process for the recovery of the solvent by distillation from phenol-containing solutions |
| DE1006394B (en) * | 1952-04-24 | 1957-04-18 | Bayer Ag | Distillation device |
| GB787688A (en) * | 1954-09-20 | 1957-12-11 | Ruetgerswerke Ag | Process and apparatus for the evaporation of heterogeneous liquid mixtures |
| US2795536A (en) * | 1955-03-29 | 1957-06-11 | California Research Corp | Liquid control for a fractionating column |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4016048A (en) * | 1975-07-17 | 1977-04-05 | Hoechst Aktiengesellschaft | Distillative purification of 2,5-dioxo-1-oxa-2-phospholanes |
| DE2628763A1 (en) * | 1975-09-02 | 1977-03-03 | Unitech Chemical Inc | METHOD AND DEVICE FOR RECYCLING USED LUBRICATING OIL |
| DE3338488A1 (en) * | 1982-10-29 | 1984-05-03 | Basf Ag, 6700 Ludwigshafen | Process for recovering temperature-sensitive products by thermally mild distillation using a thin layer evaporator connected to a distillation column and an arrangement for carrying out the process |
| EP1090904A3 (en) * | 1999-10-07 | 2003-01-29 | Nippon Shokubai Co., Ltd. | Purification process for hydroxyalkyl (meth)acrylate |
| EP1459794A3 (en) * | 2003-03-18 | 2004-10-20 | Nippon Shokubai Co., Ltd. | Apparatus and process for purification of acrylic acid family |
| US7014736B2 (en) | 2003-03-18 | 2006-03-21 | Nippon Shokubai Co., Ltd. | Apparatus and process for purification of acrylic acid family |
| EP1576995A3 (en) * | 2004-03-17 | 2006-08-09 | Saltigo GmbH | Method for continual separation of substance mixtures |
| WO2022106685A1 (en) * | 2020-11-23 | 2022-05-27 | Covestro Deutschland Ag | Distillation unit and method for separating a liquid substance mixture into two to six liquid product flows with different compositions |
| US12508519B2 (en) | 2020-11-23 | 2025-12-30 | Covestro Deutschland Ag | Distillation unit and method for separating a liquid substance mixture into two to six liquid product flows with different compositions |
Also Published As
| Publication number | Publication date |
|---|---|
| GB900457A (en) | 1962-07-04 |
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