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 distillationInfo
- 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
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
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/36—Azeotropic 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
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/40—Extractive 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.
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)
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.
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.
- 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.
- 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.
- 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.
- 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.
- 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.
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) |
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US8779169B2 (en) | 2010-05-27 | 2014-07-15 | Basf Se | Process for the preparation of 2 substituted tetrahydropyranols |
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US3142016A (en) * | 1961-12-18 | 1964-07-21 | Clarke C Minter | Ratio-measuring apparatus utilizing a capacitance bridge circuit |
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US4419188A (en) * | 1980-06-02 | 1983-12-06 | Mccall Thomas F | Thermally coupled extractive distillation process |
-
1983
- 1983-08-03 DE DE19833327952 patent/DE3327952A1/en not_active Withdrawn
-
1984
- 1984-07-24 DE DE8484108721T patent/DE3460936D1/en not_active Expired
- 1984-07-24 EP EP84108721A patent/EP0133510B1/en not_active Expired
- 1984-07-30 CA CA000459954A patent/CA1222717A/en not_active Expired
- 1984-07-30 JP JP59157715A patent/JPS6075304A/en active Pending
Cited By (10)
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 |
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