CN1324261A - Vacuum distillation system and use thereof the concentrating organic-aqueous solvent mixtures - Google Patents
Vacuum distillation system and use thereof the concentrating organic-aqueous solvent mixtures Download PDFInfo
- Publication number
- CN1324261A CN1324261A CN99812392A CN99812392A CN1324261A CN 1324261 A CN1324261 A CN 1324261A CN 99812392 A CN99812392 A CN 99812392A CN 99812392 A CN99812392 A CN 99812392A CN 1324261 A CN1324261 A CN 1324261A
- Authority
- CN
- China
- Prior art keywords
- end product
- condensate
- product
- described vacuum
- condensation
- 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.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0036—Multiple-effect condensation; Fractional condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/28—Evaporating with vapour compression
- B01D1/284—Special features relating to the compressed vapour
- B01D1/2856—The compressed vapour is used for heating a reboiler or a heat exchanger outside an evaporator
-
- 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
- B01D3/06—Flash distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
- B01D5/009—Collecting, removing and/or treatment of the condensate
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to a vacuum distillation system and a method for concentrating organic-aqueous solutions, especially of so-called spissum extracts using said system. The vacuum distillation system comprises a flash evaporator, a vent condenser and a multi-stage condenser downstream of the vent condenser. The inventive system is also provided with means for recovering at least a part of the condensate from any condenser step and returning it to the bottom product. The invention further relates to a method for concentrating organic-aqueous solutions such as concentrated extracts using said system.
Description
The present invention relates to a kind of vacuum distillation plant and use this kind equipment make organic-aqueous solvent mixture, especially a kind of method of concentrating of the solvent mixture of concentrated extract.
Manufacturing is exactly to extract vegetable material and the extract and the preserved material of gained further is processed into dry extracts based on the method for the medicine of plant.What make usually is moisture/alcoholic extract moisture, alcoholic or that mix, wherein uses ethanol as alcoholic content mostly.But extract also can contain other organic solvent, as methyl alcohol, propyl alcohol, butanols and ether and ketone (especially ether and acetone).Extract that is obtained or preserved material or be employed like this or be condensed to so-called concentrated extract like this.And then can be processed into dry extracts.Organic-aqueous solvent mixture normally concentrates by air blast evaporation or surface evaporation.May cause undesirable transformation owing to therefore the surface with heat comes in contact, this transformation may cause the minimizing of activator content.With regard to present distillation technique, because the volatile composition in the solvent mixture at first is evaporated, this increases certain percentage with regard to the content that causes water.The content of this water is said so from reason and is helped that the bacterium bud grows up.Stipulated that in relevant pharmacopeia the bacterium of bacterium, yeast and mould counts the limit.
When selected a kind of and non-sterile initial product, as existing inevitably when producing plant extracts, the bacterium number in the end product of having processed is directly relevant with the time that the processing processing continues.
Have a kind of method once to be used for concentrate drying, this method protectiveness ground has shortened drying time (DE19525026.5) greatly by means of a leafy agitator, but has proposed the problem of ability aspect.For fear of using such process to make concentrate, be preferably under the condition of identical protection and concentrate in advance.With commercial scale the unknown still such method is arranged.
Usually carry out thickening or evaporation and concentration by means of traditional distillation.But be used for that concentrated extract or general moisture, alcoholic solution are carried out altar traditional distillating method thick or evaporation and concentration and have various shortcoming.At first, for evaporating, the solution that makes strong polarization such as water or alcohol needs many energy.For example evaporating 1 kg water when traditional vapo(u)rization system needs big 1 kilowatt power, and this solvent that is equivalent to make polarization is 15 times of toluene distillation power demand for example.From the equipment aspect, this just requires heat exchange area big especially and must supply with heat again always.This shows that it is uneconomic especially not having heat to return existing process.
Other problem is: volatile solvent is distilled, thereby is always changing in the mutual proportionate relationship of end product (sumpfprodukt) lining solvent.Alcohol is exactly volatile composition for moisture spirit solvent mixture, but the minimizing of its content can cause the deposition of extracting material for plant extracts, and this phenomenon is undesirable.This just means under extreme case, and the concentrated of end product has only by the following method and could realize: distilling with batch processes, at first is alcohol, in second step water is distilled out again.But this can cause the segregation of product.
In addition as top pointed, must supply with heat for traditional distillation always.The strong temperature sensitivity of this and most of vegetal activators is a contradiction, for fear of this situation this is protected, and great majority have been used vacuum distillation.Though can reduce the operating temperature of distillating method like this, also must continue to be defeated by heat, and just in the end product that will concentrate, cause very big interface load owing to be defeated by heat.
At last, when carrying out evaporation and concentration, the moisture alcoholic plant extracts to some plants also has the problem that generates foam in addition.For fear of generating foam, must reduce the surface tension of end product by interpolation alcohol.Alcohol distillation is gone out and has just been aggravated to generate the problem of foam.This foam causes the overflow of distillation equipment under extreme case, thereby interrupts this process and must stop production procedure.
In order to solve the problem of high energy consumption, by other science department known have variously have heat and return existing distillating method.In these methods, have the concentrated open type thermal pump of machinery best parameter is arranged.Need 50 watts/kilogram for the distillation of water so herein, it is equivalent to than energy consumption little 20 times when traditional distillation.By the known distillation equipment of present technology status is principle work by the open type thermal pump of the steam compressed device (compression of a product) with machinery more accurately.With extracting out from volume in compressor reducer in a product that discharges under the vacuum the evaporimeter, compress, continue heating and and then condensation in a condenser simultaneously.The condensation energy is directly flowed to evaporation.Realized the cyclic process of an energy thus, do not had heating and cooling and just this process is proceeded by compressor reducer power.This can reduce needed heat widely.
Relevant with the solution that will distill, this equipment can move with an explosive evaporation device or a flash evaporator.If then heat exchanger is in the chamber, the end of the medium that will distill for an explosive evaporation device, if flash evaporator then makes end Product transport by this heat exchanger with a circulating pump, heating is also introduced in the evaporimeter again, and is used for distillation in the there release.These equipment are used for concentrating pond groove and the shower water of for example handling and electroplating from degreasing, phosphatization, cooling and lubricating emulsion, grind emulsion, compressor condensate or from the cleaning solution of cleaning shop and high-pressure cleaning device.Distillate (waste water) can enter in traditional waste water, and the highly enriched concentrate that will discharge then is utilized as end product.Also produce following problem for solvent mixture when adopting this distillation: volatile solvent is at first distilled, thereby makes in the end product the mutual proportionate relationship with solvent that variation has taken place.Thereby at present these equipment under the technology status are also and be not suitable for moisture alcoholic solution such as plant extracts are concentrated.
Task of the present invention is to propose a kind of equipment and method, just can especially carry out concentrating and avoiding again some cited problems to plant extracts or concentrated extract to organic aqueous solution by this equipment and method.These preferably should carry out under for the harmless as far as possible condition of content, and should optionally set up the alcohol content of concentrating degree and solution as required.
Solve by a kind of vacuum distillation plant according to this task of the present invention, this equipment includes a) flash evaporator, b) steam compressed device, and c) is connected to the multistage condenser of steam compressed device after one, the rectifier unit that inserts in the middle of preferably being equipped with wherein has been equipped with and is used for from a condensation segment at least a portion condensate being back to device in the evaporimeter.
Condenser preferably is used as heat exchanger, and its layout should make end product before being back into evaporimeter, and the cooling liquid that was used as condenser in other words before injecting flash evaporator is thermal liquid in other words.This moment before sending into evaporimeter end product just as the cooling liquid condenser of flowing through.End this moment product has absorbed the condensation heat of distillate and has been used to improve vapo(u)rizing temperature again in exchange.Product is with regard to release at the bottom of when sending in the flash evaporator heavily again, and wherein a part of solvent has evaporated and made liquid cools under remaining.This produces end product again, and it can be reused for cooling.The guiding of " cooling liquid " is carried out according to the principle of heat exchange, wherein it at first with a product in the contacting of the colder condensation segment used of the most volatile component, back to back other the condensation segment that is that volatile order is arranged in the distillate composition according to condensation is arranged the condensation segment of the component that is used for the most difficult volatilization always.Water is the composition of difficult volatilization in the product for moisture spirit solvent mixture, and alcohol then is the composition of easy volatilization.The distillation condensate is by taking out separately respectively in the condensation segment.
Between condensation segment, preferably be provided with a rectifier unit, so that make the composition of end product realize better separation each other.Preferably according to the one-tenth mark of waiting to extract out in the solvent mixture two to four condensation segments are set, majority is preferably two condensation segments.
According to the present invention, before flowing to evaporation again, be defeated by end product again by means of the pipeline of design for this reason at least a portion condensate at least one stage.Just can substitute the volatile component part that the hypergeometric example in the end product is taken out by this method that condensate is added into end product, although and thereby make and have the mutual proportionate relationship of volatility that has nothing in common with each other between the solvent and remain unchanged.Volatile composition alcohol, is carried away water secretly in moisture spirit solvent mixture as the awkward entrainer that evaporates into part water by the present invention under azeotropic point.Condensate preferably is defeated by evaporimeter again more than the fluid level of end product.But can be defeated by end product to condensate equally, mix with other solution (concentrated extract) under certain condition with it and mixture is flowed to evaporimeter.
The efficient of cooling means can improve as follows: be provided with end product in other words substrate from the device of evaporimeter movement guide by condenser.Preferably use a kind of circulating pump in addition.
Preferably has feature described in claims by device of the present invention.
In addition by the invention allows for a kind of concentration technology method that moisture alcoholic solution is not damaged of being used for, wherein:
A) make solution release under vacuum,
B) by volume ground delivery head product and make its compression,
C) make product condensation on a plurality of stages, so that make this product be separated into its difficult composition and more volatile composition that volatilizees, and
D) be defeated by end product heavily again at least a portion condensate in a stage of major general, before condensate is applied in the step a) again again in this section, until realize till desired the concentrating.
Preferably end product is used the cooling liquid as condensation stage, its method is its each different condensation stage of motion process that makes as described above.
The method that concentrates that a kind of aqueous alcohol that makes combined type (preferably ethanol) solution does not damage is preferably proposed, wherein in step c), carry out two condensing steps, and make the condensate of second stage, wherein relate to volatile alcohol, especially ethanol is defeated by end product heavily again.The condensate of such quantity is returned, so that the water/alcohol of solution remains unchanged than (water/ethanol ratio) in the end product.
Evaporate by means of flash vaporization.Flash vaporization allows to carry out work when low temperature, has reduced the surface loading of product simultaneously, has shortened the time of staying, makes the energy uniform absorption.Therefore just avoided making the effective medical components in the plant extracts to be subjected to thermic load.In general be the solution that contains heat-sensitive material can be concentrated like this.
According to the present invention, this process preferably is used to having 20% volume ratio at least, and preferably the moisture plant extracts that contains ethanol of the ethanol content of 30%-70% volume ratio concentrates.The effective medical components of great majority in this scope, especially phenol and the flavonoids as plant origin all is soluble.Just can avoid making extract too far upwards to enter the state of water according to the present invention, thereby make concentrated extract not produce decomposition.
Can use by equipment of the present invention to carry out by process of the present invention.
Idea behind the present invention is, use alcohol as entrainer so that the water of difficult volatilization distills, and obtain the energy that alcohol need not to add from this process.Control temperature in the heat exchanger like this by the condensation of part in addition, thus under identical pressure condensation side by side with separate multiple different solvent (water and alcohol).
The steam of this method by volume transports and reaches.When the steam by volume transports the molecule of gaseous state just by (steam residual air) compressor reducer corresponding to reaction chamber in the forming or dividing potential drop and being drawn out of of composition.As defined of the present invention, if between evaporization process and condenser, insert compressor reducer induction system by volume in other words, for example a root's blower then just has a kind of clear and definite mixture that can be decomposed by the condensation of part in the compressor reducer back.
With according to present technology different be rectifying not to be used at vaporizer side according to the present invention, herein for degradation necessary backflow be form by outside heat extraction and therefore caused the loss of energy, and be on condensate one side after concentrating.Use condensation (and rectifying) like this according to the present invention, thereby not only utilize hydraulic pressure can separate steam pressure, and the condensation heat of condensate fraction can system be utilized inherently, so that end product is returned on the operating temperature.Alcohol is refluxed continuously as entrainer, do not need additionally to use to surpass to concentrate the required energy of operation for this reason.
More favourable effect is to make a part of condensate be back into evaporimeter in other words in the end product from energy balance, and the heat that the inside is contained then is used to heating again because release and at flash evaporator institute product of the chilled end.The entrainer of volatile solvent composition as higher boiling composition used in returning thereby not only allowing of condensate, and helps reducing the energy demand in the whole process.In addition owing to thereby returning of a part of condensate has been defeated by the interface load that heat has reduced end product, here owing to heat is not necessarily imported via the interface between container and the end product from the outside, but import with a kind of liquid.This helps the preparation of protectiveness to concentrate in other words.By keeping the alcohol concentration in the end product also just to stop formation to be decomposed simultaneously.
Using more volatile solvent (alcohol) makes it be back in the end product in other words as entrainer and keeps alcohol concentration therein, this has just further solved bubble-related issues, and this is because the appearance of this bubble-related issues is relevant with alcohol content decline in the solvent mixture to a great extent.
By the present invention the single component that a product is separated into it is just allowed individually it to be recycled in addition.Thereby just a product is decomposed in a plurality of condensation phase by partial condensation by the present invention.Can between single condensation phase, insert a rectifier unit in the centre in order to realize separating preferably for this reason.This rectifier unit preferably places between two heat exchangers for device of the present invention, thereby makes its form necessary steam weight, so as the composition (alcohol) of the composition (water) that makes higher fluidizing point and boiling easily respectively condensation go out.This effect preferably can improve in order to following method, is additional to compressor reducer exactly and uses a kind of fore pump.Here for example can refer to a kind of liquid annular pump that comes work with oil.Various condensates can be removed with pure relatively form, as long as they are not the words of returning by of the present invention.
Below according to accompanying drawing preferred form of implementation of the present invention is described.
As shown in Figure 1, at first include an evaporator unit 1 by a distillation equipment of the present invention, it comprises a base of evaporator 2 and the liquid to be evaporated position of circulation therein; Distillation equipment also includes a liquid separator 3, and the product that evaporation the time is carried secretly is separated and can be back to liquid condition through a liquid storage turn of bilge 4; Distillation equipment also has a suspended particulates separator 5, the steam residual air that in this separator, makes in advance cleaning in other words a product on evaporimeter top once more with a tangential separator cleaning, so that also isolate the suspended particulates that contained at this.
In evaporimeter central authorities a probe (not shown) from arranging is down arranged, can measure packed height in the evaporimeter with this probe.The end product that cools down owing to evaporation flows to pump 7 through an efferent duct 6 at base of evaporator.For fear of owing to product landing formation bumpy flow or obstruction, make the efferent duct lengthening with one section bend pipe, thereby can make evaporimeter and not exclusively dry run by this pipeline.In order to be emptied completely thereby to have adorned one section additional pipeline in its lowest position of base of evaporator, this section pipeline has been guaranteed remaining effluent inflow pump.Pump 7, preferably a kind of circulating pump, it transports by heat exchanger 8 bottom product.There with bottom product heating and through a circulation line 9 tangential spray mouth 10 in the Returning evaporimeter again.Also can flow to a kind of other solution (supply material) through same pipeline.Import circulation line through a prefill valve 11 by heat exchanger, wherein supply material input circulation line preferably carries out structural design like this, making it is flow controller simultaneously, and the product of circulation is through it and release and therefore the supply material is being mixed with the end product of this circulation to the pipeline of evaporimeter.
The steam of telling when an evaporation product is in other words preferably extracted out, is compressed and be pressed into simultaneously in the heat exchanger 8a by a rocker-type piston pump or a roots-type compressor by steam compressed device 12.There is a connecting line 13 to lead to rectifier unit 14 from the lower portion of heat exchanger 8a, thereby uncooled steam in the heat exchanger is risen by rectifying and introduces in second heat exchanger 8b through the general tube connector 15 of rectifier unit thereupon.Make the surplus solution condensation there.Condensate is always gone out by pump drainage, preferably passes through membrane pump 16a and 16b output.The condensate of second heat exchanger then relevant with Flow-rate adjustment by means of a valve again spray go in the position, top of evaporimeter so that guarantee the proportionate relationship that refluxes here.
Extract that will be to be concentrated when this process operation is sent in the evaporimeter, and release is also incited somebody to action the gas that exists this moment via compressor reducer and taken away.Vinasse end product in other words falls in the bottom chamber also there as these heat exchangers of liquid process.Owing to can supply with new extract constantly through this pipe, and take out the extract that has concentrated, thereby this kind process can continuously be carried out through the bottom pipe.Also can stipulate a kind of batch process method selectively.Can continuously regulate control to the alcohol content of end product in both cases, that is to say the amount of the alcohol that returns by adjusting.The operating temperature of process is preferably 38 and 42 ℃ between 35 ℃ and 45 ℃.The vacuum of setting up reaches between 80 millibars and 150 millibars, is preferably 110 millibars and 130 millibars.The condensate that does not return can take out and be used for again extracting, and has been excluded as the very small product of stand under load in other words.
As a result, the cocnentration factor that can reach with process of the present invention is 1: 10.The absolute magnitude of the effective medicinal components that is contained in extract does not reduce, and precipitation do not occur or forms foam, perhaps only occurs in very little scope.
Claims (21)
1. vacuum distillation plant, it includes
A) flash evaporator,
B) steam compressed device and
C) be connected to the multistage condenser of steam compressed device after one,
Wherein disposed and be used at least a portion condensate being back to device in the end product from a condensation segment.
2. by the described vacuum distillation plant of claim 1, it includes the middle rectifier unit that inserts between condensation segment.
3. by claim 1 or 2 described vacuum distillation plants, wherein the layout of condenser should make end product be used as the thermal liquid of condenser before being back to evaporimeter.
4. steam equipment by any described vacuum in the claim 1 to 3, wherein be provided with two to four condensation segments, between them, have access to a rectifier unit respectively.
5. steam equipment by any described vacuum in the claim 1 to 4, wherein the condensate of last condensation segment is back in the evaporimeter in whole or in part.
6. by the described vacuum distillation plant of claim 5, have two condensation segments.
7. steam equipment by any described vacuum in the claim 1 to 6, wherein condensate is fed to the above evaporimeter in liquid plane of end product.
8. steam equipment by any described vacuum in the claim 1 to 6, wherein condensate is transfused to end product, mixes with it and mixture is defeated by evaporimeter.
9. steam equipment by any described vacuum in the claim 1 to 8, include in addition and initiatively guide the device of end product by condenser.
10. by the described vacuum distillation plant of claim 9, the device that wherein is used for initiatively guiding is a circulating pump.
11. steam equipment by any described vacuum in the claim 1 to 10, being additional to evaporimeter has a fore pump.
12. by the described vacuum distillation plant of claim 11, wherein fore pump is a liquid annular pump with the oil action.
13. steam equipment by any described vacuum in the claim 1 to 12, it has comprised the device of distillation aspect, when this device is used to be separated in flash distillation by a product institute's entrained solid and/or a liquid component.
14. the process that moisture alcoholic solution is concentrated with being used for not damaging, wherein:
A) make solution release in a vacuum;
B) by volume ground delivery head product and make its compression;
C) make product condensation on a plurality of stages, so that make this product separate difficult composition and more volatile composition, and
D) be defeated by end product heavily again at least a portion condensate in a stage of major general, before condensate is applied in the step a) again again in this section, until realize till desired the concentrating.
15., wherein end product is used thermal liquid as condensation phase by the described process of claim 14.
16., wherein set out and in step c), carry out two condensing steps, and at least a portion condensate of second stage is defeated by end product again by composite solution by claim 14 or 15 described processes.
17. by each described process in the claim 14 and 16, a certain amount of condensate is returned so that in the end product ratio of the water/alcohol of solution remain unchanged.
18. by each described process in the claim 14 to 17, wherein product distills by means of flash vaporization at the end.
19. by each described process in the claim 14 to 18, be used to make the concentrating again of plant medical agent extract of moisture ethanol, the ethanol content of extract is at least 20% volume ratio, is preferably the 30-70% volume ratio.
20. by each described process in the claim 14 to 19, it is characterized in that, finish by any described vacuum distillation plant in the claim 1 to 13 with a kind of.
21. use and a kind ofly the organic-aqueous solvent that contains extract concentrated by any described equipment in the claim 1 to 13.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19849010.0 | 1998-10-23 | ||
DE19849010 | 1998-10-23 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1324261A true CN1324261A (en) | 2001-11-28 |
CN1211145C CN1211145C (en) | 2005-07-20 |
Family
ID=7885473
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB998123927A Expired - Fee Related CN1211145C (en) | 1998-10-23 | 1999-10-20 | Vacuum distillation system and use thereof the concentrating organic-aqueous solvent mixtures |
Country Status (7)
Country | Link |
---|---|
JP (1) | JP3577461B2 (en) |
CN (1) | CN1211145C (en) |
AU (1) | AU6341699A (en) |
CA (1) | CA2342982C (en) |
DE (1) | DE19905323C2 (en) |
HK (1) | HK1043069B (en) |
WO (1) | WO2000024488A1 (en) |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2016188176A (en) * | 2013-08-30 | 2016-11-04 | 住友ベークライト株式会社 | Separation, enrichment, and/or recovery method of phenol, and system thereof |
JP6199192B2 (en) * | 2014-01-14 | 2017-09-20 | 日本化学機械製造株式会社 | Heat recovery system in evaporator |
CN106582050B (en) * | 2016-11-03 | 2019-02-26 | 江苏海雷德蒙新能源有限公司 | A kind of downward film evaporator liquid feeding control system |
JP6850000B2 (en) * | 2017-05-18 | 2021-03-31 | 株式会社ササクラ | Anticorrosion method for roots blower |
AT17768U3 (en) * | 2022-09-27 | 2023-03-15 | Gig Karasek Gmbh | Plant and process for the concentration of substance-containing liquids by multi-stage evaporation |
CN115888141A (en) * | 2022-11-04 | 2023-04-04 | 石家庄博欧金属制品有限公司 | Wax liquid recovery processing device for precision casting |
WO2024173304A1 (en) * | 2023-02-16 | 2024-08-22 | Cargill, Incorporated | Oilseed extraction plant comprising an installation suitable for evaporating a solvent from a solvent-containing mixture |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2435521A1 (en) * | 1978-09-11 | 1980-04-04 | Tournaire Sa | Extn. of essential oils by hydro:distillation - with separate boiler vaporising recycled mother water for live stream injection to still |
US4305790A (en) * | 1980-01-31 | 1981-12-15 | Kramer Sr Edward F | Multiple effect distillation method and apparatus |
DE4129076C2 (en) * | 1991-09-02 | 2001-11-15 | Domo Caproleuna Gmbh | Process for the purification of caprolactam |
DE4218451A1 (en) * | 1992-06-04 | 1993-12-09 | Transferon Waeschereimasch | Process for the preparation of contaminated higher-boiling solvents and device for carrying out the process |
CH684057A5 (en) * | 1992-11-30 | 1994-07-15 | Buss Ag | Methods for further processing the vacuum residue in a crude oil refinery. |
DE19507126A1 (en) * | 1995-03-01 | 1996-09-12 | Esa Tech Dr Baumann Gmbh | Regeneration of contaminated solvents from dry cleaning of textiles |
IT1281057B1 (en) * | 1995-12-06 | 1998-02-11 | Cit S R L | PROCEDURE AND DEVICE FOR WATER PURIFICATION. |
-
1999
- 1999-02-09 DE DE19905323A patent/DE19905323C2/en not_active Expired - Fee Related
- 1999-10-20 WO PCT/EP1999/007968 patent/WO2000024488A1/en active Application Filing
- 1999-10-20 CN CNB998123927A patent/CN1211145C/en not_active Expired - Fee Related
- 1999-10-20 CA CA002342982A patent/CA2342982C/en not_active Expired - Fee Related
- 1999-10-20 JP JP2000578087A patent/JP3577461B2/en not_active Expired - Fee Related
- 1999-10-20 AU AU63416/99A patent/AU6341699A/en not_active Abandoned
-
2002
- 2002-05-24 HK HK02103902.9A patent/HK1043069B/en not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
CA2342982A1 (en) | 2000-05-04 |
CN1211145C (en) | 2005-07-20 |
HK1043069B (en) | 2006-03-03 |
AU6341699A (en) | 2000-05-15 |
JP3577461B2 (en) | 2004-10-13 |
HK1043069A1 (en) | 2002-09-06 |
DE19905323A1 (en) | 2000-04-27 |
DE19905323C2 (en) | 2000-09-14 |
WO2000024488A1 (en) | 2000-05-04 |
JP2002528244A (en) | 2002-09-03 |
CA2342982C (en) | 2005-01-04 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US4770780A (en) | Liquid CO2 /cosolvent extraction | |
US4877530A (en) | Liquid CO2 /cosolvent extraction | |
CA2194668C (en) | Vacuum distillation of a petroleum product | |
RU2422185C1 (en) | Spirit rectification column | |
EP3983104B1 (en) | Process for distilling a crude composition in a rectification plant including an indirect heat pump | |
US20060135826A1 (en) | Process for recovering methanol | |
EP2197562A1 (en) | Liquid separation by membrane assisted vapor process | |
GB2457186A (en) | Installation for the distillation of drinking alcohol,especially whiskey | |
CN104853840A (en) | Device for preparing alkanol | |
CN1211145C (en) | Vacuum distillation system and use thereof the concentrating organic-aqueous solvent mixtures | |
US8337672B2 (en) | Method and device for producing vacuum in a petroleum distillation column | |
US11629109B2 (en) | Extractive distillation column system and the use thereof in the separation of butenes from C4-hydrocarbon streams | |
TW202239741A (en) | Process for the energy-efficient production of alkali metal alkoxides | |
CN110256202A (en) | A kind of refining crude methanol process of four towers quadruple effect | |
US2152164A (en) | Distillation process | |
US6086721A (en) | Facility for distilling a liquid product | |
US4303478A (en) | Process for distillatively separating liquid mixtures | |
JPS6253702A (en) | Distillation accompanied by energy recovery by re-compression of steam used in ejector | |
CN107641083A (en) | A kind of power-saving technology of azeotropic joint variable-pressure rectification separating ethyl acetate and n-hexane | |
WO2017179026A1 (en) | Method and unit for reducing dioxane produced as a result of sulfonation of alcohol ether sulfates | |
CN208726769U (en) | A kind of solvent recovery unit | |
JPS61254177A (en) | Extraction of ethanol from ethanol-containing liquid | |
RU2392028C1 (en) | Method for pulling vacuum in vacuum column of oil stock refining and installation for method realisation | |
CN108129265A (en) | The separator and method of a kind of methanol and mixed ester | |
CN108129264A (en) | A kind of device and method of transformation separation methanol and acetate esters |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20050720 Termination date: 20171020 |
|
CF01 | Termination of patent right due to non-payment of annual fee |