CN111013175A - Device and method for separating mixture of cyclohexane and isobutanol by partial heat integration double-tower pressure swing distillation - Google Patents
Device and method for separating mixture of cyclohexane and isobutanol by partial heat integration double-tower pressure swing distillation Download PDFInfo
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- CN111013175A CN111013175A CN201911142863.1A CN201911142863A CN111013175A CN 111013175 A CN111013175 A CN 111013175A CN 201911142863 A CN201911142863 A CN 201911142863A CN 111013175 A CN111013175 A CN 111013175A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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Abstract
The invention relates to the field of chemical separation and purification, and particularly discloses a device and a method for separating a mixture of cyclohexane and isobutanol by partial heat integration double-tower pressure swing rectification. The device for separating the mixture of cyclohexane and isobutanol by partial heat integration double-tower pressure swing distillation comprises a normal pressure tower communicated with a liquid inlet pipeline, and is characterized in that: the tower top outlet of the atmospheric tower is connected with a first reflux tank through a condenser, the reflux tanks are connected with a first reflux pipeline of the atmospheric tower and a liquid feeding pipeline of the high-pressure tower in parallel, and the tower bottom of the atmospheric tower is connected with a first reboiler and a second reboiler in parallel and circularly communicated; the tower bottom of the high-pressure tower is circularly connected with a reboiler III, the tower top reflux pipeline II of the high-pressure tower is communicated with a reflux tank II, a liquid inlet of the reflux tank II is communicated with a top outlet of the reboiler I, and a top outlet of the high-pressure tower is communicated with a bottom inlet of the reboiler I. The invention has the advantages of low investment cost, simple process, low energy consumption and obvious economic benefit, and simultaneously realizes the separation and recovery of important organic substances, namely isobutanol and cyclohexane.
Description
(I) technical field
The invention relates to the field of chemical separation and purification, in particular to a device and a method for separating a mixture of cyclohexane and isobutanol by partial heat integration double-tower pressure swing rectification.
(II) background of the invention
Isobutanol and cyclohexane are important chemical raw materials. Isobutanol is used as an organic synthetic raw material for the manufacture of petroleum additives, antioxidants, 2, 6-di-tert-butyl-p-cresol, isobutyl acetate (coating solvent), plasticizers, synthetic rubbers, artificial musks, fruit essences, synthetic drugs, etc. Also used as a higher solvent, and isobutanol is also a new biofuel with great potential, called second generation biofuel.
Cyclohexane can be used as monomers for nylon manufacture, adipic acid, hexamethylenediamine and caprolactam, and also as raw materials for cyclohexanol, cyclohexanone. And isobutanol is CO + H2Cyclohexane is an important component of synthesis gas for preparing low carbon alcohol, and is often used as an entrainer for dehydration of low carbon alcohol as an important organic solvent, so that the separation of cyclohexane and isobutanol is industrially significant.
Cyclohexane and isobutanol can form an azeotrope under normal pressure, the azeotropic composition contains 12.8 percent of isobutanol, the azeotropic point is 79.42 ℃, and the effective separation cannot be realized by adopting a simple rectification method due to the existence of the azeotrope in the mixture.
Chinese patent CN102942475B discloses a method for separating azeotrope of ethyl acetate and ethanol by pressure swing distillation and a production device thereof, wherein the purity of ethyl acetate separated and purified by the method reaches 99.7 percent, and the yield reaches 99.8 percent.
Chinese patent CN103102265B discloses a method for purifying methyl acetate by pressure swing distillation and a production device thereof, wherein the purity of methyl acetate separated and purified by the method reaches 99.9 percent.
Chinese patent CN105130742B discloses a method for separating a mixture of tert-butyl alcohol and benzene by pressure swing distillation, wherein the purity of the tert-butyl alcohol recovered by the method can reach 99.85%, and the purity of the benzene can reach 99.92%.
There are many papers and patents on heat-integrated pressure swing distillation, and no published data on pressure swing distillation separation of isobutanol-cyclohexane azeotropic system is found at present.
Disclosure of the invention
In order to make up for the defects of the prior art, the invention provides a device and a method for separating a mixture of cyclohexane and isobutanol by partial heat integration double-tower pressure swing distillation, which have the advantages of simple process, low energy consumption and high product purity.
The invention is realized by the following technical scheme:
the device for separating the mixture of cyclohexane and isobutanol by partial heat integration double-tower pressure swing distillation comprises a normal pressure tower communicated with a liquid inlet pipeline, and is characterized in that: the tower top outlet of the atmospheric tower is connected with a first reflux tank through a condenser, the reflux tanks are connected with a first reflux pipeline of the atmospheric tower and a liquid feeding pipeline of the high-pressure tower in parallel, and the tower bottom of the atmospheric tower is connected with a first reboiler and a second reboiler in parallel and circularly communicated; the tower bottom of the high-pressure tower is circularly connected with a reboiler III, the tower top reflux pipeline II of the high-pressure tower is communicated with a reflux tank II, a liquid inlet of the reflux tank II is communicated with a top outlet of the reboiler I, and a top outlet of the high-pressure tower is communicated with a bottom inlet of the reboiler I.
The invention utilizes the characteristic that the azeotropic composition of isobutanol and cyclohexane is greatly changed along with the change of pressure, adopts a two-tower pressure-variable rectification method, and particularly adopts the rectification of a normal pressure tower firstly and then the rectification and purification of a high pressure tower, and simultaneously adopts a method of partial heat integration that steam at the top of the high pressure tower provides a part of heat for a low pressure tower reboiler to separate an isobutanol and cyclohexane azeotropic system, so that a third component is not required to be introduced, the effective separation of the isobutanol and the cyclohexane is realized, the heat generated in the process is fully utilized, and the separation cost is reduced.
The more preferable technical scheme of the invention is as follows:
and a liquid outlet at the bottom of the reflux tank II is communicated with a liquid inlet of the atmospheric tower, and the refluxed isobutanol-cyclohexane mixture is fed back to the atmospheric tower for continuous rectification.
And the bottoms of the normal pressure tower and the high pressure tower are both provided with product extraction outlets, and the isobutanol and the cyclohexane are respectively recovered from the bottoms.
And the liquid outlets at the bottoms of the first reflux tank and the second reflux tank are respectively provided with a reflux pump, and the liquid conveying pipeline of the reflux tank communicated with the high-pressure tower is provided with a conveying pump for providing power for conveying liquid.
The tower bottom liquid outlet of the atmospheric tower is communicated with a reboiler I and a reboiler II in parallel, and the top outlets of the reboiler I and the reboiler II are communicated with the tower bottom inlet of the atmospheric tower, so that the circulating heat exchange of the reboiler I and the reboiler II on the atmospheric tower bottom flows is realized, and the separation yield is improved.
And the tower bottom outlet of the high-pressure tower is communicated with the bottom inlet of a reboiler III, and the top outlet of the reboiler III is communicated with the tower bottom inlet of the high-pressure tower, so that the circulating heat exchange of the tower bottom material flow of the high-pressure tower is realized.
The method for rectifying and separating the mixture of cyclohexane and isobutanol by adopting the device comprises the following steps:
(1) the isobutanol-cyclohexane mixture enters a low-pressure tower through a body fluid pipeline for rectification, a product at the top of the tower is condensed by a condenser and then enters a reflux tank I for collection, then a part of the product flows back to the normal-pressure tower for continuous rectification, and the other part of the product enters a high-pressure tower for rectification through a liquid delivery pipeline;
(2) part of tower bottom material flow of the atmospheric tower returns to the atmospheric tower after heat exchange by the reboiler I and the reboiler II, and part of tower bottom material flow is extracted from high-purity isobutanol products to realize separation of isobutanol;
(3) part of tower bottom material flow of the high-pressure tower is reboiled by a reboiler III and then returns to the high-pressure tower, and part of high-purity cyclohexane product is extracted to realize the separation of cyclohexane; the azeotrope of isobutanol and cyclohexane is extracted from the top of the high pressure tower in a gas form, enters a reboiler I through a pipeline for heat exchange and then is sent to a reflux tank II, one part of the azeotrope flows back to the high pressure tower, and the other part of the azeotrope enters an atmospheric tower for continuous rectification.
The preferred process conditions are:
the temperature of the top of the atmospheric tower is 71.12-87.36 ℃, and the temperature of the bottom of the atmospheric tower is 96.91-118.44 ℃; the temperature of the top of the high-pressure tower is 116.02-141.80 ℃, and the temperature of the bottom of the high-pressure tower is 120.61-147.41 ℃.
The device for separating isobutanol and cyclohexane mixture by atmospheric distillation and pressurized distillation is suitable for separating isobutanol-cyclohexane mixture with the mass fraction of cyclohexane being more than 60 percent by distillation.
The pressure of the atmospheric tower is 1atm, the theoretical plate number is 10-30, the position of the feed plate is 8-16 plates, the reflux ratio is 2.0-4.0, the mass fraction of isobutanol at the tower bottom is more than 99.9%, and the yield is more than 99.9%; the pressure of the high-pressure tower is 4-6atm, the theoretical plate number is 10-35, the position of the feeding plate is 10-18 plates, the reflux ratio is 2.5-4.0, the mass fraction of the product cyclohexane at the bottom of the tower is more than 99.9%, and the yield is more than 99.9%.
The invention adopts a pressure swing distillation method to realize the effective separation of the mixture of the isobutanol and the cyclohexane, and impurities are not introduced in the separation process, thereby achieving higher purity; the invention has the advantages of low investment cost, simple process, low energy consumption and obvious economic benefit, and simultaneously realizes the separation and recovery of important organic substances, namely isobutanol and cyclohexane.
(IV) description of the drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic structural diagram of the present invention.
In the figure, a T1 atmospheric tower, a T2 high-pressure tower, a V1 reflux tank I, a V2 reflux tank II, a C1 condenser, a H1 reboiler I, a H2 reboiler II, a H3 reboiler III, a P1 reflux pump, a P2 delivery pump, a 1 liquid inlet pipeline, a 2 reflux pipeline I, a 3 liquid feeding pipeline and a 4 reflux pipeline II are arranged.
(V) detailed description of the preferred embodiments
The following further description, taken in conjunction with the accompanying drawings, is not intended to limit the scope of the present invention.
Example 1:
the feed temperature was 25 ℃. The feeding flow is 1000kg/h, the pressure is 1atm (absolute pressure), the feeding contains 50 percent of cyclohexane and 50 percent of isobutanol (mass fraction), the materials firstly enter a normal pressure tower T1 from a 15 th plate, the operation pressure is 1atm (absolute pressure), the number of theoretical plates is 25, the reflux ratio is 3.5, the temperature of the top of the tower is 79.45 ℃, and the temperature of the bottom of the tower is 107.68 ℃; a part of the product at the top of the atmospheric tower T1 enters a high-pressure tower T2 from the 14 th plate after being pressurized by a pump, the operating pressure is 4atm (absolute pressure), the theoretical plate number is 25, and the reflux ratio is 3; the steam at the top of the high-pressure tower T2 enters a reboiler I H1 at the bottom of the normal-pressure tower T1 for heat exchange and then flows back to the high-pressure tower T2 through a reflux tank II V2; the mass fraction of the isobutanol product obtained after separation is 99.9 percent, and the recovery rate is 99.9 percent; the mass fraction of the cyclohexane product is 99.9 percent, and the recovery rate is 99.9 percent.
TABLE 1 operating parameters of the rectification System
Example 2:
the feed temperature was 25 ℃. The feeding flow is 1000kg/h, the pressure is 1atm (absolute pressure), the feeding contains 60 percent of cyclohexane and 40 percent of isobutanol (mass fraction), the materials firstly enter a normal pressure tower T1 from the 16 th plate, the operation pressure is 1atm (absolute pressure), the number of theoretical plates is 25, and the reflux ratio is 3.3; pumping one part of the top product of the atmospheric tower T1 into a high-pressure tower T2 from a 12 th plate, wherein the operation pressure is 4atm (absolute pressure), the theoretical plate number is 24, and the reflux ratio is 3.5; the steam at the top of the atmospheric tower T1 returns to the atmospheric tower T1 through a first reflux tank V1, the steam at the top of the high-pressure tower T2 enters a first reboiler H1 at the bottom of the atmospheric tower T1 for heat exchange, and then returns to the high-pressure tower T2 through a second reflux tank V2; the mass fraction of the isobutanol product obtained after separation is 99.9 percent, and the recovery rate is 99.9 percent; the mass fraction of the cyclohexane product is 99.9 percent, and the recovery rate is 99.9 percent.
TABLE 2 operating parameters of the rectification System
Example 3:
the feed temperature was 25 ℃. The feeding flow is 1000kg/h, the pressure is 1atm (absolute pressure), the feeding contains 70 percent of cyclohexane and 30 percent of isobutanol (mass fraction), the material firstly enters a normal pressure tower T1 from the 10 th plate, the operation pressure is 1atm (absolute pressure), the number of theoretical plates is 18, and the reflux ratio is 3; a part of the product at the top of the atmospheric tower T1 enters a high-pressure tower T2 from the 7 th plate after being pressurized by a pump, the operating pressure is 4atm (absolute pressure), the number of theoretical plates is 19, and the reflux ratio is 3.2; the steam at the top of the high-pressure tower T2 enters a reboiler I H1 at the bottom of the normal-pressure tower T1 for heat exchange and then flows back to the high-pressure tower T2 through a reflux tank II V2; the mass fraction of the isobutanol product obtained after separation is 99.9 percent, and the recovery rate is 99.9 percent; the mass fraction of the cyclohexane product is 99.9 percent, and the recovery rate is 99.9 percent.
TABLE 3 operating parameters of the rectification System
Example 4:
the feed temperature was 25 ℃. The feeding flow is 1000kg/h, the pressure is 1atm (absolute pressure), the feeding contains 80 percent of cyclohexane and 20 percent of isobutanol (mass fraction), the materials firstly enter a normal pressure tower T1 from the 9 th plate, the operation pressure is 1atm (absolute pressure), the number of theoretical plates is 19, and the reflux ratio is 3.3; a part of the product at the top of the atmospheric tower T1 enters a high-pressure tower T2 from the 8 th plate after being pressurized by a pump, the operating pressure is 4atm (absolute pressure), the number of theoretical plates is 18, and the reflux ratio is 3.1; the steam at the top of the high-pressure tower T2 enters a reboiler I H1 at the bottom of the normal-pressure tower T1 for heat exchange and then flows back to the high-pressure tower T2 through a reflux tank II V2; the mass fraction of the isobutanol product obtained after separation is 99.9 percent, and the recovery rate is 99.9 percent; the mass fraction of the cyclohexane product is 99.9 percent, and the recovery rate is 99.9 percent.
TABLE 4 operating parameters of the rectification System
The above disclosure is only for the preferred embodiments of the present invention, but the present invention is not limited thereto, and any modifications that are insubstantial to those skilled in the art should fall within the scope of the present invention.
Claims (10)
1. The device for separating the mixture of cyclohexane and isobutanol by partial heat integration double-tower pressure swing distillation comprises a normal pressure tower communicated with a liquid inlet pipeline, and is characterized in that: the tower top outlet of the atmospheric tower is connected with a first reflux tank through a condenser, the reflux tanks are connected with a first reflux pipeline of the atmospheric tower and a liquid feeding pipeline of the high-pressure tower in parallel, and the tower bottom of the atmospheric tower is connected with a first reboiler and a second reboiler in parallel and circularly communicated; the tower bottom of the high-pressure tower is circularly connected with a reboiler III, the tower top reflux pipeline II of the high-pressure tower is communicated with a reflux tank II, a liquid inlet of the reflux tank II is communicated with a top outlet of the reboiler I, and a top outlet of the high-pressure tower is communicated with a bottom inlet of the reboiler I.
2. The apparatus for partially thermally integrated double column pressure swing distillation separation of a mixture of cyclohexane and isobutanol according to claim 1, wherein: and a liquid outlet at the bottom of the second reflux tank is communicated with a liquid inlet of the atmospheric tower.
3. The apparatus for partially thermally integrated double column pressure swing distillation separation of a mixture of cyclohexane and isobutanol according to claim 1, wherein: and product extraction outlets are formed at the bottoms of the normal pressure tower and the high pressure tower.
4. The apparatus for partially thermally integrated double column pressure swing distillation separation of a mixture of cyclohexane and isobutanol according to claim 1, wherein: and the liquid outlets at the bottoms of the first reflux tank and the second reflux tank are respectively provided with a reflux pump, and the reflux tank is communicated with a liquid conveying pipeline of the high-pressure tower and is provided with a conveying pump.
5. The apparatus for partially thermally integrated double column pressure swing distillation separation of a mixture of cyclohexane and isobutanol according to claim 1, wherein: and a tower bottom liquid outlet of the atmospheric tower is communicated with a first reboiler and a second reboiler in parallel, and top outlets of the first reboiler and the second reboiler are communicated with a tower bottom inlet of the atmospheric tower.
6. The apparatus for partially thermally integrated double column pressure swing distillation separation of a mixture of cyclohexane and isobutanol according to claim 1, wherein: and the tower bottom outlet of the high-pressure tower is communicated with the bottom inlet of a reboiler III, and the top outlet of the reboiler III is communicated with the tower bottom inlet of the high-pressure tower.
7. A method for separating a mixture of cyclohexane and isobutanol by rectification using the device of claim 1, comprising the steps of: (1) the isobutanol-cyclohexane mixture enters a low-pressure tower through a body fluid pipeline for rectification, a product at the top of the tower is condensed by a condenser and then enters a reflux tank I for collection, then a part of the product flows back to the normal-pressure tower for continuous rectification, and the other part of the product enters a high-pressure tower for rectification through a liquid delivery pipeline; (2) part of tower bottom material flow of the atmospheric tower returns to the atmospheric tower after heat exchange by a reboiler I and a reboiler II, and part of tower bottom material flow is extracted from a high-purity isobutanol product; (3) part of tower bottom material flow of the high-pressure tower is reboiled by a reboiler III and then returns to the high-pressure tower, and part of high-purity cyclohexane product is extracted; the azeotrope of isobutanol and cyclohexane is extracted from the top of the high pressure tower in a gas form, enters a reboiler I through a pipeline for heat exchange and then is sent to a reflux tank II, one part of the azeotrope flows back to the high pressure tower, and the other part of the azeotrope enters an atmospheric tower for continuous rectification.
8. The method of claim 7, wherein: the temperature of the top of the atmospheric tower is 71.12-87.36 ℃, and the temperature of the bottom of the atmospheric tower is 96.91-118.44 ℃; the temperature of the top of the high-pressure tower is 116.02-141.80 ℃, and the temperature of the bottom of the high-pressure tower is 120.61-147.41 ℃.
9. The method of claim 7, wherein: the mass fraction of cyclohexane in the isobutanol-cyclohexane mixture to be separated is more than 60%.
10. The method of claim 7, wherein: the pressure of the atmospheric tower is 1atm, the theoretical plate number is 10-30, the position of the feeding plate is 8-16 plates, and the reflux ratio is 2.0-4.0; the pressure of the high-pressure tower is 4-6atm, the theoretical plate number is 10-35, the position of the feeding plate is 10-18 th plate, and the reflux ratio is 2.5-4.0.
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Cited By (4)
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| CN111499496A (en) * | 2020-04-21 | 2020-08-07 | 青岛科技大学 | Energy-saving process for separating n-heptane-isobutanol by variable-pressure batch rectification-stripping |
| CN113200822A (en) * | 2021-05-08 | 2021-08-03 | 青岛科技大学 | Method for separating ethyl acetate and ethanol by double-tower pressure swing rectification |
| CN113214048A (en) * | 2021-05-08 | 2021-08-06 | 青岛科技大学 | Method for separating isobutanol, isobutyl acetate and ethanol by three-tower heat integration pressure swing rectification |
| CN114853607A (en) * | 2021-02-04 | 2022-08-05 | 万华化学集团股份有限公司 | Monomer-containing solvent refining system and process |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111499496A (en) * | 2020-04-21 | 2020-08-07 | 青岛科技大学 | Energy-saving process for separating n-heptane-isobutanol by variable-pressure batch rectification-stripping |
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| CN113200822A (en) * | 2021-05-08 | 2021-08-03 | 青岛科技大学 | Method for separating ethyl acetate and ethanol by double-tower pressure swing rectification |
| CN113214048A (en) * | 2021-05-08 | 2021-08-06 | 青岛科技大学 | Method for separating isobutanol, isobutyl acetate and ethanol by three-tower heat integration pressure swing rectification |
| CN113214048B (en) * | 2021-05-08 | 2022-08-12 | 青岛科技大学 | Method for separating isobutanol, isobutyl acetate and ethanol by three-tower heat integration pressure swing rectification |
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Application publication date: 20200417 |