EP0837725A1 - Procede de rectification sous vide pousse pour extraire des substances pures contenues dans des melanges de substances a point d'ebullition eleve et a forte sensibilite a la temperature et a l'air, qui exigent un fort pourvoir de separation, et colonnes adaptees a ce procede - Google Patents

Procede de rectification sous vide pousse pour extraire des substances pures contenues dans des melanges de substances a point d'ebullition eleve et a forte sensibilite a la temperature et a l'air, qui exigent un fort pourvoir de separation, et colonnes adaptees a ce procede

Info

Publication number
EP0837725A1
EP0837725A1 EP96924820A EP96924820A EP0837725A1 EP 0837725 A1 EP0837725 A1 EP 0837725A1 EP 96924820 A EP96924820 A EP 96924820A EP 96924820 A EP96924820 A EP 96924820A EP 0837725 A1 EP0837725 A1 EP 0837725A1
Authority
EP
European Patent Office
Prior art keywords
rectification
column
distributors
air
columns
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.)
Withdrawn
Application number
EP96924820A
Other languages
German (de)
English (en)
Inventor
Horst Hartmann
Wolfram Burst
Wulf Kaiser
Harald Laas
Paul Grafen
Bernhard Bockstiegel
Kai-Uwe Baldenius
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Priority to EP01130402A priority Critical patent/EP1209156B1/fr
Publication of EP0837725A1 publication Critical patent/EP0837725A1/fr
Withdrawn legal-status Critical Current

Links

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
    • B01D3/141—Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall
    • 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
    • B01D3/008—Liquid distribution
    • 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
    • B01D3/146—Multiple effect distillation
    • 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
    • B01D3/16—Fractionating columns in which vapour bubbles through liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/32—Packing elements in the form of grids or built-up elements for forming a unit or module inside the apparatus for mass or heat transfer
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00—Preparation of halogenated hydrocarbons
    • C07C17/38—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
    • C07D311/70—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with two hydrocarbon radicals attached in position 2 and elements other than carbon and hydrogen in position 6
    • C07D311/72—3,4-Dihydro derivatives having in position 2 at least one methyl radical and in position 6 one oxygen atom, e.g. tocopherols
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/322—Basic shape of the elements
    • B01J2219/32203—Sheets
    • B01J2219/3221—Corrugated sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/322—Basic shape of the elements
    • B01J2219/32203—Sheets
    • B01J2219/32213—Plurality of essentially parallel sheets
    • B01J2219/3222—Plurality of essentially parallel sheets with sheets having corrugations which intersect at an angle different from 90 degrees
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/322—Basic shape of the elements
    • B01J2219/32203—Sheets
    • B01J2219/32224—Sheets characterised by the orientation of the sheet
    • B01J2219/32227—Vertical orientation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/322—Basic shape of the elements
    • B01J2219/32203—Sheets
    • B01J2219/32265—Sheets characterised by the orientation of blocks of sheets
    • B01J2219/32272—Sheets characterised by the orientation of blocks of sheets relating to blocks in superimposed layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/324—Composition or microstructure of the elements
    • B01J2219/32408—Metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/324—Composition or microstructure of the elements
    • B01J2219/32408—Metal
    • B01J2219/32416—Metal fibrous
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/326—Mathematical modelling
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S159/00—Concentrating evaporators
    • Y10S159/42—Seals
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S261/00—Gas and liquid contact apparatus
    • Y10S261/72—Packing elements

Definitions

  • the invention relates to a method for obtaining pure substances from mixtures of high-boiling air and / or temperature-sensitive substances which require high separation efficiency by rectification in a fine vacuum, in particular a method for rectifying raw vitamin E acetate for cleaning of low-boiling and higher-boiling impurities, and columns suitable for this process.
  • rectification columns are generally used which, in regular geometry, have systematically structured packings with defined passage areas for the countercurrent phases, since structured packings in relation to packing elements regularly emerge Characterize higher resilience and a better separating effect, a lower specific pressure loss and a lower required packing volume and therefore also have a smaller necessary material and heat exchanging height. They are therefore used for all vacuum rectifications in which it is of the mixture to be separated is particularly important to limit the loss of column pressure.
  • Particularly suitable column packs are metal fabric packs of the type BX and CY from Sulzer (see company publication "Separating columns for distillation and absorption" from Sulzer) and similarly effective metal fabric packs from other companies, such as Montz GmbH.
  • the highest product temperature occurs in the bottom of a column. In addition to the head pressure, it is largely determined by the pressure drop in the column internals which is necessary for the required separation performance. In rectification columns, lowering the top pressure to below 0.5 mbar has no significant influence on the bottom temperature.
  • the thermal stability is so low that, despite the use of the metal mesh packings described with an ordered structure and top pressures in the column of only 0.5 to 1 mbar, the pressure drop at the fabric packs required for the required separation performance in the sump results in temperatures would occur, which lies above the decomposition range of the compounds to be separated.
  • distillative separation of such mixtures has generally been carried out in a high vacuum range (approx. IO -1 to IO " 5 mbar), ie short path distillations or molecular distillations are used. In mixtures with low relative volatilities, these distillations are high However, purities can only be achieved with low distillation yields.
  • VEA synthetic vitamin E acetate
  • acetic anhydride acetic anhydride
  • VEA synthetic vitamin E acetate
  • the rectification which is generally very advantageous for the purification of products on an industrial scale, prepares at VEA due to its high boiling point. Big problems associated with its fragility at higher temperatures. For this reason, distillations in high vacuum or even molecular distillation have hitherto been carried out essentially in order to be able to distil VEA at the lowest possible temperatures.
  • the object of the invention was to provide a process for to develop distillative separation of high-boiling air- and / or temperature-sensitive substances that require a high separation performance, in which no high vacuum distillation or even molecular distillation are necessary, ie a process in which a head vacuum of 0.1 to 2 mbar is sufficient and as a result much less complex vacuum generation processes are necessary and a high distillation yield is achieved.
  • the invention now relates to a process for obtaining pure substances from mixtures of high-boiling air- and / or temperature-sensitive substances which require a high separation performance, by rectification in a fine vacuum in columns containing metal tissue packs with an ordered structure is characterized in that the rectification is carried out in a mass exchange column in which
  • the column is designed in such a way that it is practically possible to work in the absence of air.
  • the method according to the invention is particularly advantageous when working with fabric packs in which the angle of inclination of the teeth of the individual fabric layers of the pack against the column axis is as small as possible in order to minimize the specific pressure loss of the pack.
  • the angle of inclination of the teeth in the usual BX sulfon packs is generally 30 °
  • tissue packs are preferred in the process according to the invention, the angle of inclination of the teeth of the fabric layers against the column axis being 0 to 25 °, preferably 3 to 10 °.
  • the angle of inclination of the toothing of the fabric layers against the column axis is illustrated in FIG. 1.
  • 1 means the angle of inclination of the toothing of the fabric layers against the column axis and the second fabric layer.
  • the process according to the invention is of particular importance for the fine purification of VEA, ie for the case where a VEA contaminated with colored low-boiling and higher-boiling substances is rectified as a mixture of high-boiling air and / or temperature-sensitive substances.
  • a VEA contaminated with colored low-boiling and higher-boiling substances is rectified as a mixture of high-boiling air and / or temperature-sensitive substances.
  • VEA has a boiling temperature of approx. 240 ° C at a pressure of 1 mbar. Due to the limited thermal stability of VEA, the temperature in the column bottom is limited to approx. 260 to 270 ° C. A rectification column may therefore only be operated with a maximum sump pressure of only 4 mbar. This means that only a pressure loss of about 3 to 3.5 mbar between the top and bottom of the column can be tolerated. This is very difficult to achieve since a separation performance of about 10 to 30 separation stages is required for the fine cleaning of VEA and a pressure loss of 0.3 to 0.5 mbar per separation stage must normally be expected. In the work areas according to the invention, there were no measurements regarding the pressure losses.
  • a liquid distribution with channel distributors with the same or more than 500 draining points is claimed. Similar, but also called “capillary distributors” but round distributors are sold by the Sulzer and Montz companies and are described, for example, in EP 512 277. Known channel distributors generally have only 50 to 60 drip points per 2 .
  • channel distributors brings about a reduction in the so-called pressure loss in two different ways. On the one hand, they require rapid, extremely fine distribution and thus ultimately better use of the packing to distribute the mixture to be separated and, on the other hand, a very low sprinkling density.
  • liquid loads from approx. 0.2 m 3 / m 2 -h are specified as the lower load limit.
  • a layer of a tissue pack generally consists of a large number of usually individual, 170 mm high layers of tissue.
  • Each packing sheet is installed by 90 ° with respect to the previous one.
  • the arrangement of the distributors is also rotated by 90 ° with respect to the packing element located directly below the distributors, or the packing position located there.
  • the liquid now spreads on one of these layers of fabric at a certain angle. After an inlet length which is dependent on the spreading angle and the distance between two drip dividers, a uniform film has formed over a fabric layer.
  • 2 or more packing elements with a height of only 20 to 100 mm, preferably 25 to 50 mm, in particular 35 to 45 mm, the fabric layers of which are each rotated through 90 ° to one another, are therefore used below the liquid distributor.
  • the inlet length is approx. 340 mm, which means that with a packing height of 2 meters, approx. 17% of the packing is not fully used for the actual separating operation.
  • the rectification should be carried out practically in the absence of air.
  • VEA fine purification of VEA according to the invention
  • head pressures of 0.2 to 1 mbar, preferably 0.5 to 1 mbar and with bottom pressures of 1 to 4 mbar, preferably 1.5 to 3.5 mbar , in particular 2 to 3 mbar, works.
  • the packing columns are loaded with a liquid load between 0.03 and 0.3 m 3 / m 2 -h in the rectifying section of the column and with a liquid load between 0.03 and 1.0 m 3 / m 2 -h operated in the stripping section of the columns.
  • a separating plate column is generally understood to be a combination of two separate column packs within an outer column jacket, on which there are inlet and side draws.
  • FIG. 2c Such a dividing plate column is shown schematically in FIG. 2c.
  • 1, 2, 3 and 5 have the same meaning as in FIGS. 2a and 2b and 9 means dividing plate column.
  • the invention also relates to the packed columns equipped for the process according to the invention and to their use for the fine purification of contaminated V ⁇ A by rectification in the pressure range between 0.1 and 2 mbar.
  • packing columns with stripping section and reinforcing section containing metal fabric packs with an ordered structure which are each rotated through 90 ° to one another for rectifying mixtures of high-boiling air and / or temperature-sensitive substances which require a high separation performance at head pressures of 0.1 to 2 mbar, which are characterized by
  • the channels of the liquid distributors are arranged at an angle of approximately 90 ° to the fabric layers of the packing elements located directly below the distributor,
  • a packing column which can be used according to the invention for the rectification of VEA is shown schematically in FIG. 3.
  • Degassed, synthetically produced raw vitamin E acetate with a content of about 96% VEA is at a temperature between 200 and 250 degrees Celsius through inlet 10 into the middle of the first rectification column with a packing height of 3 to 5 m of the Sulzer type BX or Montz A3 entered.
  • the liquid is distributed uniformly over the column cross-section at the top and at the inlet of the column using the newly developed high-performance channel distributors 6.
  • the packing elements 7 with a height of only 20 to 100 mm are located below the newly developed channel distributors.
  • the fabric layers of the packing elements arranged directly under the channel distributors 6 are to the channels of the Liquid distributor twisted at an angle of 90 °.
  • the column is equipped with a protective heater 9 and is operated adiabatically. Flanges and sockets are provided with welding lip seals or high-quality metal seals.
  • the top pressure of the column is 0.5 to 1 mbar.
  • the reflux ratio is 2 to 4.
  • the liquid returning in the column has a temperature between 170 and 220 degrees Celsius. 5 to 20% of the feed stream is taken off at the bottom of the column.
  • the product removed at the top of the first column was conveyed at a temperature of 200 to 250 ° C. into the middle of the second rectification column with a packing height of 3 to 5 m of the Sulzer BX or Montz A3 type.
  • the liquid is distributed over the column cross-section at the top and at the inlet using the newly developed high-performance channel distributors.
  • This column is also equipped with protective heating and is operated adiabatically. Flanges and sockets are provided with welding lip seals or high-quality metal seals.
  • the top pressure of the column is approximately 0.5 mbar.
  • the reflux ratio is 5 to 15.
  • the liquid returning to the column has a temperature between 170 and 220 ° C. 5 to 20% of the feed stream are taken off at the top and bottom of the column.
  • the vitamin E acetate removed in the side draw immediately above the evaporator of the second column is almost colorless (color number less than 2) and has pharmaceutical quality with a purity of more than 99%.
  • the yield of such a pure product is about 50% of theory.
  • the residue is separated off from the bottom draw of the first rectification column at a pressure of between 1 and 5 mbar.
  • the distillate obtained in this way can be sold as vitamin E acetate for cattle feed purposes (feed quality). These products generally contain 90 to 99% VEA.
  • the total distillation yield of feed and pharmaceutical VEA is between 95 and 98%.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne un procédé pour extraire des substances pures de mélanges à point d'ébullition élevé et à forte sensibilité à la température et à l'air, par rectification sous vide poussé dans des colonnes contenant des garnitures en toile métallique de structure ordonnée. Ce procédé met en oeuvre des répartiteurs à canaux destinés à la séparation du fluide et pourvus d'un nombre supérieur ou égal à 500 points d'égouttage/m2, lesquels sont disposés à 90° par rapport aux couches de tissu des éléments de garniture (7,8) se trouvant directement sous les répartiteurs. Deux ou une pluralité d'éléments de garniture (7,8) situés sous le répartiteur (6) ont seulement une faible hauteur, ce qui garantit quasiment l'exclusion de l'air. Ces éléments de garniture sont conçus de telle façon qu'aucun échange de chaleur ne puisse se produire à travers la paroi de la colonne pendant la rectification. L'invention concerne également les colonnes à garniture utilisées pour ce procédé ainsi que l'application de ce procédé et l'utilisation de ces colonnes pour une purification fine par distillation d'acétate de vitamine E
EP96924820A 1995-07-08 1996-06-29 Procede de rectification sous vide pousse pour extraire des substances pures contenues dans des melanges de substances a point d'ebullition eleve et a forte sensibilite a la temperature et a l'air, qui exigent un fort pourvoir de separation, et colonnes adaptees a ce procede Withdrawn EP0837725A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP01130402A EP1209156B1 (fr) 1995-07-08 1996-06-29 Procédé d extraction de l acétate de la vitamine E pur ou des tocophéroles pures par rectification pour enlever des substances contaminantes à point d ébullition supérieure et inférieures

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19524928 1995-07-08
DE19524928A DE19524928A1 (de) 1995-07-08 1995-07-08 Verfahren zur Rektifikation von Gemischen hochsiedender luft- und/oder temperaturempfindlicher Substanzen, die eine hohe Trennleistung erfordern, im Feinvakuum, sowie für dieses Verfahren geeignete Kolonnen
PCT/EP1996/002852 WO1997002880A1 (fr) 1995-07-08 1996-06-29 Procede de rectification sous vide pousse pour extraire des substances pures contenues dans des melanges de substances a point d'ebullition eleve et a forte sensibilite a la temperature et a l'air, qui exigent un fort pourvoir de separation, et colonnes adaptees a ce procede

Related Child Applications (1)

Application Number Title Priority Date Filing Date
EP01130402A Division EP1209156B1 (fr) 1995-07-08 1996-06-29 Procédé d extraction de l acétate de la vitamine E pur ou des tocophéroles pures par rectification pour enlever des substances contaminantes à point d ébullition supérieure et inférieures

Publications (1)

Publication Number Publication Date
EP0837725A1 true EP0837725A1 (fr) 1998-04-29

Family

ID=7766346

Family Applications (2)

Application Number Title Priority Date Filing Date
EP96924820A Withdrawn EP0837725A1 (fr) 1995-07-08 1996-06-29 Procede de rectification sous vide pousse pour extraire des substances pures contenues dans des melanges de substances a point d'ebullition eleve et a forte sensibilite a la temperature et a l'air, qui exigent un fort pourvoir de separation, et colonnes adaptees a ce procede
EP01130402A Expired - Lifetime EP1209156B1 (fr) 1995-07-08 1996-06-29 Procédé d extraction de l acétate de la vitamine E pur ou des tocophéroles pures par rectification pour enlever des substances contaminantes à point d ébullition supérieure et inférieures

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP01130402A Expired - Lifetime EP1209156B1 (fr) 1995-07-08 1996-06-29 Procédé d extraction de l acétate de la vitamine E pur ou des tocophéroles pures par rectification pour enlever des substances contaminantes à point d ébullition supérieure et inférieures

Country Status (7)

Country Link
US (2) US6111117A (fr)
EP (2) EP0837725A1 (fr)
JP (1) JPH11508818A (fr)
CN (1) CN1048910C (fr)
DE (2) DE19524928A1 (fr)
ES (1) ES2240322T3 (fr)
WO (1) WO1997002880A1 (fr)

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WO1999001215A1 (fr) * 1997-07-04 1999-01-14 Kühni Ag Chicanes pour colonnes d'echange de substance
US7097890B1 (en) * 1998-07-31 2006-08-29 Chevron Phillips Chemical Co. Lp Polymer with pendent cyclic olefinic functions for oxygen scavenging packaging
DE19903459A1 (de) 1999-01-28 2000-08-03 Basf Ag Verfahren zur Herstellung von hochreinem Phytantriol
DE10010810A1 (de) * 2000-03-08 2001-09-13 Montz Gmbh Julius Flüssigkeitsverteiler und Verfahren zum Betreiben
DE10135714A1 (de) * 2001-07-21 2003-02-06 Basf Ag Verbessertes Verfahren zur Aufarbeitung eines Vitamin-E-Acetat-haltigen Produktstromes
TWI351306B (en) * 2003-05-16 2011-11-01 Sulzer Chemtech Ag Method of mass transfer of a material or heat
US20050115819A1 (en) * 2003-12-01 2005-06-02 Ching-Piau Lai System for desalinating and purifying seawater and devices for the system (II type)
ATE502931T1 (de) * 2004-08-19 2011-04-15 Dsm Ip Assets Bv Verfahren zur rektifikation von vitamin e acetat
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ES2240322T3 (es) 2005-10-16
DE59611228D1 (de) 2005-06-16
US6554965B1 (en) 2003-04-29
EP1209156A3 (fr) 2002-10-30
EP1209156A2 (fr) 2002-05-29
DE19524928A1 (de) 1997-01-09
EP1209156B1 (fr) 2005-05-11
WO1997002880A1 (fr) 1997-01-30
JPH11508818A (ja) 1999-08-03
CN1048910C (zh) 2000-02-02
CN1190354A (zh) 1998-08-12
US6111117A (en) 2000-08-29

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