CA1222717A - Separation of an azeotropic mixture by distillation in a distillation column by a procedure similar to extractive distillation - Google Patents

Separation of an azeotropic mixture by distillation in a distillation column by a procedure similar to extractive distillation

Info

Publication number
CA1222717A
CA1222717A CA000459954A CA459954A CA1222717A CA 1222717 A CA1222717 A CA 1222717A CA 000459954 A CA000459954 A CA 000459954A CA 459954 A CA459954 A CA 459954A CA 1222717 A CA1222717 A CA 1222717A
Authority
CA
Canada
Prior art keywords
column
take
distillation
mixture
section
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.)
Expired
Application number
CA000459954A
Other languages
French (fr)
Inventor
Gerd Kaibel
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
Application granted granted Critical
Publication of CA1222717A publication Critical patent/CA1222717A/en
Expired legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/141Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/36Azeotropic distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/40Extractive distillation

Abstract

Abstract of the Disclosure: A mixture which is azeo-tropic or which behaves almost azeotropically and is difficult to separate by distillation, is separated into two pure or substantially pure fractions by distillation, by adding a further component, using a procedure which is similar to extractive distillation and is carried out in a distillation column, a section of which is divided into a feed part and a take off part by means of a separating unit which is effective in the longitudinal direction and completely or partially prevents cross-mixing of liquid streams and/or vapor streams. In this process, the azeo-tropic mixture is fed as bleed streams to the feed part and to the take off part, in each case at or near the top, and one of the two pure or substantially pure fractions is removed as a top product from the distillation column while the other is removed as a side product from the take off part.

Description

;n a d;stillation column by a Droeedure sim;Lar to extrartive distillation ~.
The present inven~ion rel3tes to a process for separating a mixture which is azeotrop;c or behaves almost azeotrop;cally and ;s d;ff;cult to separate ~~ by d;stillat;on~ into two pure or substant;a~ly pure fractions by dist;llation, by adding a further compo-nent, using a procedure wh;ch is similar to extract;ve d;stillation and is carr;ed out in a d;st;llation column, a section of wh;ch is divided into a feed part and a take o~f part by means of a separating unit ~h;ch is effective in the longitudinal direction and completely or partially prevents cross-m;x;ng of liquid streams and/or vapor streams.
It is known that a two-component azeotropic mixture can be separated into its individual components by means of various distillation methodc~ These are essentiaLly t~o~pressure distillation9 azeotropic dis-ZO tillation and extractive d;st;llation~ These three dis-tillation rnethods are descr;bed in detail by R. 8illet in Distillation Industrielle, 1972, pages 223-231.
All three distillation methods have the disad-vantage that two or more distiLlat;on columns are re-quired for separating the two-component azeotrop;c mix-ture, enta;l;ng high costs in terms of apparatus and ;n-strumentation.
It is an object of the present invention to sim-plify the separation by distillat;on of two-component azeo-tropic mixtures ;e. to carry out the procedure in a single-stage d;st;llation process us;ng one distillation columnN
It has been found that this object is achieved, in accordance with the invention, if the azeotropic mixture is fed as bleed streams to the feed part and to the take off part, in each case at or near the top, and one of the two pure or substantially pure fractions is removed as a top product from the distillation column while the , ....

$~

other is removed as a side product from the take off part.
More particularly, the present invention proposes a process for separating by distillation a mixture which is a~eotropic or behaves almost azeotropically and is difficult to separate by distillation into two pure or substantially pure fractions, wherein:
a) use is made of a single distilation column having a section divided into a feed part and a take off part by means of a separating unit which is effective in the longitudinal direction and prevents cross-mixing of liquid stream, vapor stream or both of them;
b) a further component in which one of the two fractions to be separated is readily soluble, is added as an extraction agent into the mixture;
c) the mixture to be separated is fed as a bleed stream to the feed part of the distillation column, at or near the top of said feed part;
d) the fraction readily soluble in the further component added to the mixture is removed as a side product from the take-off part of the column, and e) the other fraction sparingly soluble in the further component is removed as a top product from the column.
In accordance with a first ~referred embodiment of the invention:
- the column has an undivided section located above the divided section;
- the take-off part of the divided section of the column has its top sealed off tightly from the undivided upper sections; and - the top of said take-off part is equipped with a condenser for partial or total condensation of the readily soluble fraction of the mixture, which is removed from said take-off part.
In accordance with another preferred embodiment of - 2a -the invention, the mixture to be separated is also fed as a bleed stream to the take-off part of the distillation column, at or near the top of said take-off part.
These two preferred embodiments of the invention are illustrated in the accompanying drawing, and are described in detail below.
Figure 1 shows a process flowchart for a distilla-tion column in which the two-component azeotropic mixture is fed as bleed streams to the feed part and to the take oEf part, in each case at the top.
Figure 2 shows a process flowchart for a distilla-tion column in which the two-component azeotropic mixture is fed exclusively to the feed part.
In Figure 1, a distillation column 1 (referred to below as column 1) is divided into a feed part 3 and a take off part 4 by means of a separating unit 2 which is effective in the longitudinal direction. The take off part 4 is closed at the upper end of the separatin~ unit 2 by means of a liquid collector 5 of conventional construction, so thatthe liquid flowing downward from the undivided upper section 6 of column 1 is conducted completely into the feed part 3 of the column, with the result that the further component E ~extraction agent) cannot pass from the undivided upper section 6 into the take off part 4. The two-component azeotropic mixture A, B is fed as bleed streams to the top of the feed part 3, which is open at the top, and the top of the take off part 4, which allows the vapor to pass through the top but prevents liquid from doing so. The bleed stream is fed in at the top of the take off part 4 in an amount corresponding to the amount of liquid required for mass transfer within the take off part 4. Because it has this function, this feed is preferably introduced in liquid form and at a very low temperature, in order to keep ,;
~, . i - 2b _ ~ 2 ~ 71 7 the amount very small. Accordingly, in Figure 1, the two-component azeotropic mixture A, B is fed as bleed streams to the feed part and to the take off part, in each case at or near the top, while that component, A, of the said mixture which is sparingly soluble in the `'''i ~ '~
~, ~.. .

lZ227~L~

- 3 - OOZ. 0~50/36670 further component E is distilled off via the top of the column in a conventional manner, and that component, B, of the stated mixture which is readily soluble in the further component E is removed from t~e take off part, in the form of vapor or liquid. As in the conventional extractive distillation, the further component E is fed ;nto the upper, und;vided section of the column, and is removed as a bottom product, either in pure form or containing small residual amounts of the read;ly soluble component B, and, if required, is recycled to the column.
In Figure 2, the top of the take off part 4 is sealed off tightly from the undivided upper section 6.
Furthermore, the top of the take off part 4 is equipped with a condenser 7 for partial or total condensation of the readily soluble component ~ of the two-component mixture, which is to be removed from the take off part 4. In this case, ~he take off part 4 corresponds to the downstream rect;fication column in the convent;onal ex-tractive distillation, for separatin~ the componentwh;ch is readily soluble in the further component from this component ~extraction agent).
In contrast to s;mple distillations ln columns divided lengthwise, in the novel procedure for extractive d;st;llation the side fract;on removed from the take off part passes from the feed part ;nto the take off part only at the lower end of the long;tudinal partition.
Apart from the special case where the vapor rising ;n the take off part undergoes total condensation at the upper end of the longitudinal partit;on, ;t ;s even possible for flow to take place in the oppos;te direct;on, ie.
some of the fract;on to be removed as a s;de str~am passes, at the upper end of the long;tud;nal part;tion, from the take off part back into the upper, common column sect;on or ;nto the feed part.
The decisive advantage of the novel process is that the separat;on of a two-component azPotrop;c mix-4 ~ture ;nto ;ts ;nd;v;dual components can be carr;ed out by means of one d;st;llat;on column.

Claims (7)

The embodiments of the invention in which an ex-clusive property or privilege is claimed are defined as follows:
1. A process for separating by distillation a mixture which is azeotropic or behaves almost azeotropically and is difficult to separate by distillation into two pure or substantially pure fractions, wherein:
a) use is made of a single distilation column having a section divided into a feed part and a take off part by means of a separating unit which is effective in the longitudinal direction and prevents cross-mixing of liquid stream, vapor stream or both of them;
b) a further component in which one of the two fractions to be separated is readily soluble, is added as an extraction agent into the mixture;
c) the mixture to be separated is fed as a bleed stream to the feed part of the distillation column, at or near the top of said feed part;
d) the fraction readily soluble in the further component added to the mixture is removed as a side product from the take-off part of the column, and e) the other fraction sparingly soluble in the further component is removed as a top product from the column.
2. The process of claim 1, wherein:
- the column has an undivided section located above the divided section;
- the take-off part of the divided section of the column has its top sealed off tightly from the undivided upper sections; and - the top of said take-off part is equipped with a condenser for partial or total condensation of the readily soluble fraction of the mixture, which is removed from said take-off part.
3. The process of claim 2, wherein:
- the further component used as an extraction agent is removed from the bottom of the column up and recycled up to the undivided upper section of said column.
4. The process of claim 1, wherein the mixture to be separated is also fed as a bleed stream to the take-off part of the distillation column, at or near the top of said take-off part.
5. The process of claim 4, wherein:
- the column has an undivided section located above the divided section;
- the take-off part of the divided section of the column has its top designed to allow the vapors to pass therethrough but to prevent the liquids from doing so; and - the mixture fed as a bleed stream at or near the top of said take-off part is introduced in an amount corres-ponding to the amount of liquid required for mass transfer within said take-off part.
6. The process of claim 5, wherein:
- the mixture fed as a bleed stream at or near the top of the take-off of the column is in liquid form and at a very low temperature.
7. The process of claim 6, wherein:
- the further component used as an extraction agent is removed from the bottom of the column up and recycled up to the undivided upper section of said column.
CA000459954A 1983-08-03 1984-07-30 Separation of an azeotropic mixture by distillation in a distillation column by a procedure similar to extractive distillation Expired CA1222717A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19833327952 DE3327952A1 (en) 1983-08-03 1983-08-03 METHOD FOR THE DISTILLATIVE DISASSEMBLY OF AN AZEOTROPIC MIXTURE MIXTURE - ANALOGUE OF AN EXTRACTIVE DISTILLATION - BY MEANS OF A DISTILLATION COLUMN
DEP3327952.7 1983-08-03

Publications (1)

Publication Number Publication Date
CA1222717A true CA1222717A (en) 1987-06-09

Family

ID=6205624

Family Applications (1)

Application Number Title Priority Date Filing Date
CA000459954A Expired CA1222717A (en) 1983-08-03 1984-07-30 Separation of an azeotropic mixture by distillation in a distillation column by a procedure similar to extractive distillation

Country Status (4)

Country Link
EP (1) EP0133510B1 (en)
JP (1) JPS6075304A (en)
CA (1) CA1222717A (en)
DE (2) DE3327952A1 (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6387222B1 (en) 1999-04-01 2002-05-14 Basf Aktiengesellschaft Continuous isolation of a high-melting material by distillation
US7090748B2 (en) 2001-12-21 2006-08-15 Basf Aktiengesellschaft Dividing-wall column with feed in whole or in part in the vaporous state and/or side stream take off in whole or in part in the vaporous state
US8092655B2 (en) 2000-02-24 2012-01-10 Basf Aktiengesellschaft Dividing wall column for fractionation of a multicomponent mixture
US8414744B2 (en) 2007-09-11 2013-04-09 Basf Se Continuous process for preparing menthol in pure or enriched form
US8653313B2 (en) 2010-11-02 2014-02-18 Basf Se Process for preparing a phenylcyclohexane
US8674140B2 (en) 2008-09-17 2014-03-18 Basf Se Devices and method for continuous distillative separation of a mixture containing one or more alkanolamine(s)
US8933277B2 (en) 2009-01-12 2015-01-13 Basf Se Process for preparing polymethylols
US10889547B2 (en) 2016-06-29 2021-01-12 Basf Se Method for the purification of ethoxyquin

Families Citing this family (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3510365C2 (en) * 1984-03-28 1996-09-12 Basf Ag Process for the distillation of a mixture by means of a distillation column
DE4418488A1 (en) * 1994-05-27 1995-11-30 Basf Ag Method and device for separating mixtures of substances by distillation
DE19849651C2 (en) * 1998-10-29 2003-01-16 Krupp Uhde Gmbh Rectifying column for the extractive distillation of closely or azeotropically boiling mixtures
DE19958464C2 (en) * 1999-12-03 2002-02-28 Krupp Uhde Gmbh Extractive distillation process and column for carrying out the process
US6240744B1 (en) * 1999-12-13 2001-06-05 Air Products And Chemicals, Inc. Process for distillation of multicomponent fluid and production of an argon-enriched stream from a cryogenic air separation process
DE10002806A1 (en) * 2000-01-24 2001-07-26 Basf Ag Chemical column stripper inlet feed separated by gap from strengthened inlet chamber adjacent to stripper chamber
DE10123066A1 (en) 2001-05-11 2002-11-14 Basf Ag Process for the production of higher alpha, beta-unsaturated alcohols
US6749668B2 (en) 2001-06-18 2004-06-15 Degussa Ag Process for the recovery of combustible components of a gas stream
US6720436B2 (en) 2002-03-18 2004-04-13 Degussa Ag Process for the epoxidation of olefins
US7141683B2 (en) 2002-05-02 2006-11-28 Degussa Ag Process for the epoxidation of olefins
DE10233388A1 (en) 2002-07-23 2004-02-12 Basf Ag Process for continuously operating pure distillation of the solvent methanol used in the coupling product-free propylene oxide synthesis with simultaneous removal of the methoxypropanols and the high boilers
DE10233382A1 (en) 2002-07-23 2004-01-29 Basf Ag Process for continuously operating pure distillation of the 1,2-propylene glycol obtained in the coupling product-free synthesis of propylene oxide
DE10233385A1 (en) 2002-07-23 2004-02-12 Basf Ag Process for the continuous production of propylene glycols
DE10233387A1 (en) 2002-07-23 2004-02-12 Basf Ag Process for the continuous distillation of oxiranes, especially propylene oxide
US6838572B2 (en) 2002-09-30 2005-01-04 Degussa Ag Process for the epoxidation of olefins
US7722847B2 (en) 2002-09-30 2010-05-25 Evonik Degussa Gmbh Aqueous hydrogen peroxide solutions and method of making same
US7169945B2 (en) 2002-11-26 2007-01-30 Degussa Ag Process for the epoxidation of olefins
DE10361516A1 (en) 2003-12-23 2005-07-28 Basf Ag Process for the separation of trioxane from a trioxane / formaldehyde / water mixture by pressure swing rectification
DE102004022735A1 (en) * 2004-05-07 2005-12-01 Vinnolit Gmbh & Co. Kg Divided EDC column
DE102004022734A1 (en) * 2004-05-07 2005-12-01 Vinnolit Gmbh & Co. Kg Process for the distillation of product mixtures
DE102005002129A1 (en) 2005-01-17 2006-07-20 Basf Ag Reactor and process in a reactor with a reactor interior, which is divided into two or more separate reaction spaces
US8461356B2 (en) 2007-03-23 2013-06-11 Basf Se Process for obtaining maleic anhydride by distillation
EP2008989A1 (en) 2007-06-26 2008-12-31 Basf Se Continuous method for manufacturing neral in pure or enriched form
CN101932543B (en) 2007-11-30 2014-07-30 巴斯夫欧洲公司 Method for producing optically active, racemic menthol
US8779169B2 (en) 2010-05-27 2014-07-15 Basf Se Process for the preparation of 2 substituted tetrahydropyranols
CN103003258B (en) 2010-06-10 2014-12-10 巴斯夫欧洲公司 Process for the preparation and isolation of 2-substituted tetrahydropyranols
US8791276B2 (en) 2010-06-10 2014-07-29 Basf Se Process for the preparation and isolation of 2-substituted tetrahydropyranols
ES2532540T3 (en) 2010-11-02 2015-03-27 Basf Se Procedure for the preparation of a phenylcyclohexane
EP2854977A1 (en) * 2012-06-05 2015-04-08 Akzo Nobel Chemicals International B.V. Dehydration of dilutions of compounds forming an azeotrope with water
EP3301089A1 (en) 2016-09-28 2018-04-04 Basf Se Method for purifying ethoxyquin

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3142016A (en) * 1961-12-18 1964-07-21 Clarke C Minter Ratio-measuring apparatus utilizing a capacitance bridge circuit
US3881994A (en) * 1974-04-11 1975-05-06 Universal Oil Prod Co Distillation column reboiler control system
US4419188A (en) * 1980-06-02 1983-12-06 Mccall Thomas F Thermally coupled extractive distillation process

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6387222B1 (en) 1999-04-01 2002-05-14 Basf Aktiengesellschaft Continuous isolation of a high-melting material by distillation
US8092655B2 (en) 2000-02-24 2012-01-10 Basf Aktiengesellschaft Dividing wall column for fractionation of a multicomponent mixture
US7090748B2 (en) 2001-12-21 2006-08-15 Basf Aktiengesellschaft Dividing-wall column with feed in whole or in part in the vaporous state and/or side stream take off in whole or in part in the vaporous state
US7264696B2 (en) 2001-12-21 2007-09-04 Basf Aktiengesellschaft Dividing-wall column with feed in whole or in part in the vaporous state and/or side stream take off in whole or in part in the vaporous state
US8414744B2 (en) 2007-09-11 2013-04-09 Basf Se Continuous process for preparing menthol in pure or enriched form
US8674140B2 (en) 2008-09-17 2014-03-18 Basf Se Devices and method for continuous distillative separation of a mixture containing one or more alkanolamine(s)
US9345988B2 (en) 2008-09-17 2016-05-24 Basf Se Devices and method for continuous distillative separation of a mixture containing one or more alkanolamine(s)
US8933277B2 (en) 2009-01-12 2015-01-13 Basf Se Process for preparing polymethylols
US8653313B2 (en) 2010-11-02 2014-02-18 Basf Se Process for preparing a phenylcyclohexane
US10889547B2 (en) 2016-06-29 2021-01-12 Basf Se Method for the purification of ethoxyquin

Also Published As

Publication number Publication date
DE3460936D1 (en) 1986-11-20
DE3327952A1 (en) 1985-02-14
EP0133510B1 (en) 1986-10-15
JPS6075304A (en) 1985-04-27
EP0133510A1 (en) 1985-02-27

Similar Documents

Publication Publication Date Title
CA1222717A (en) Separation of an azeotropic mixture by distillation in a distillation column by a procedure similar to extractive distillation
CA2134849A1 (en) Process to recover benzene from mixed hydrocarbons
ES2322049T3 (en) PURIFICATION OF N, N-DIMETHYLETAMETAMIDE.
KR100466771B1 (en) Process for Separating Medium Boiling Substances from a Mixture of Low, Medium and High Boiling Substances
KR101203805B1 (en) Method for the Distillative Separation of Mixtures Containing Ethyleneamines
PL264303A1 (en) Method of continuously separating water from its mixture with organic matter
GB1139282A (en) Process for purifying ethylene glycol
US3844898A (en) Fractionation apparatus having plural, integral and concentric fractionating units
US2350256A (en) Extractive distillation process
KR930023052A (en) Separation Method of Multi-Component Flows
FR2836396B1 (en) METHOD AND DEVICE FOR CHROMATOGRAPHY WITH SOLVENT RECOVERY
CA2082291A1 (en) Inter-column heat integration for multi-column distillation system
US2679472A (en) Separation of hydrocarbons by azeotropic distillation
JP7114492B2 (en) Method for purifying ethoxyquin
US6264800B1 (en) Purification process
US4412887A (en) Evaporation process with liquid entrainment separation
US3686077A (en) Process and apparatus for separating liquids
US2335162A (en) Process for the separation of hydrocarbon gases
US3855077A (en) Distillation drying process
CN100391917C (en) Process for the separation of mixtures containing m-and p-dichlorobenzene
US4402797A (en) Separation of chlorosilanes by extractive distillation
US20020130077A1 (en) Separation of azeotropic mixtures
Rao et al. Production of motor fuel grade alcohol by concentration swing adsorption
KR830001016B1 (en) Separation of volatile and nonvolatile components from solution components
US4019979A (en) Fractionation of hydrocarbons

Legal Events

Date Code Title Description
MKEX Expiry