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CN111228842A - Separation method - Google Patents

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Publication number
CN111228842A
CN111228842A CN202010188431.0A CN202010188431A CN111228842A CN 111228842 A CN111228842 A CN 111228842A CN 202010188431 A CN202010188431 A CN 202010188431A CN 111228842 A CN111228842 A CN 111228842A
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CN
China
Prior art keywords
reboiler
gas phase
tower
phase fraction
tower bottom
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Pending
Application number
CN202010188431.0A
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Chinese (zh)
Inventor
杨建春
朱荣欣
汪帆
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Beijing Nuowei New Material Technology Co ltd
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Beijing Nuowei New Material Technology Co ltd
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Priority to CN202010188431.0A priority Critical patent/CN111228842A/en
Publication of CN111228842A publication Critical patent/CN111228842A/en
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    • 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
    • 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
    • B01D3/42Regulation; Control
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/005Processes comprising at least two steps in series
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention provides a separation method, which comprises the steps of pressurizing gas phase fraction at the top of a distillation tower, and respectively feeding the pressurized gas phase fraction and tower bottom liquid into a reboiler connected with the bottom of the distillation tower; the gas phase fraction passes through a first reboiler and a second reboiler in sequence; the tower bottom liquid is respectively sent into a first reboiler and a second reboiler; in the reboiler, the pressurized gas phase fraction heats the bottoms. The method comprises the steps of pressurizing a gas phase fraction obtained at the top of a distillation tower to obtain a superheated gas phase fraction, and using the superheated gas phase fraction as a heat source of a reboiler of the distillation tower. The reboiler is heated under the condition of higher temperature in a step cooling mode, and then the reboiler is heated in the rest reboilers in a condensation mode.

Description

Separation method
Technical Field
The invention belongs to the technical field of separation, and particularly relates to a separation method, in particular to a method for separating C2-C4 hydrocarbon.
Background
The C2-C4 hydrocarbon is an important basic chemical raw material, and because the molecular structures are similar and the boiling points are not greatly different, the separation and purification are difficult, and the separation device is also a plate with the largest energy consumption in a chemical production device.
For example, propylene is mainly derived from by-products obtained from petroleum refining, and with the increasing demand for propylene and the breakthrough of catalyst research in selectivity and yield, the production of propylene by dehydrogenation of propane, which is low in cost, has been promoted. The process for preparing propylene by propane dehydrogenation generally comprises the following steps: propane dehydrogenation is used for preparing propylene, product gas is subjected to cryogenic separation, and a product is refined, wherein lighter components such as hydrogen, ethane, ethylene and the like can be well separated by cryogenic separation and conventional rectification, but propylene and propane are difficult to separate. The boiling points of the two are close, and the separation of the mixture by the traditional single-column rectification consumes a large amount of energy.
As another example, since isobutane and isobutene are in much greater demand than n-butane and n-butene, the conversion of n-paraffins to isoparaffins via isomerization at C4 represents an important step in the overall deep processing of C4. Like the separation of propylene and propane, because the properties of C4 normal paraffin and C4 isoparaffin are close, a large-scale rectifying tower is needed for the separation, and the energy consumption in the rectifying process is very high.
How to improve the separation efficiency of C2-C4 hydrocarbon and reduce the separation energy consumption is an important chemical process subject.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a separation method, wherein a superheated gas phase fraction is obtained by pressurizing a gas phase fraction obtained at the top of a distillation tower, and the superheated gas phase fraction is used as a heat source of a reboiler of the distillation tower. The reboiler is heated by a step cooling mode under the condition of higher temperature, and then the reboiler is heated by a condensation mode in the rest reboilers.
The purpose of the invention is realized by the following technical scheme:
a method of separation, the method comprising the steps of:
(1) feeding the material to be separated into a distillation tower for distillation, obtaining gas phase fraction at the tower top of the distillation tower, and obtaining tower bottom liquid at the tower bottom of the distillation tower;
(2) pressurizing the gas phase fraction at the top of the distillation tower, and respectively feeding the pressurized gas phase fraction and tower bottom liquid into a reboiler connected with the bottom of the distillation tower;
wherein the reboiler comprises a first reboiler and a second reboiler; the gas phase fraction passes through a first reboiler and a second reboiler in sequence; the tower bottom liquid is respectively sent into a first reboiler and a second reboiler;
in the reboiler, the pressurized gas phase fraction heats the tower bottom liquid;
(3) and collecting tower bottoms flowing through the first reboiler, and/or collecting condensed fractions obtained by condensing gas-phase fractions flowing through the first reboiler and the second reboiler, so as to realize separation of components in the materials to be separated.
According to the invention, the method further comprises at least one of the following steps:
(4) heating the tower bottom liquid flowing through the first reboiler, and then returning all the obtained gas-phase materials to the tower bottom of the distillation tower, and extracting all the obtained liquid-phase materials;
(5) the tower bottom liquid flowing through the second reboiler is heated and then returns to the tower bottom of the distillation tower;
(6) and the gas phase fraction is sent into a reflux tank after being condensed by the first reboiler and the second reboiler, part of the gas phase fraction reflows to the distillation tower, and part of the gas phase fraction is extracted.
According to the invention, in the step (1), the material to be separated is selected from a mixture of C2-C4 hydrocarbons or a mixture of n-butyraldehyde and isobutyraldehyde, the mixture of C2-C4 hydrocarbons is selected from a mixture of propylene and propane, or one or two of a mixture of C4 normal alkane olefin and a mixture of C4 isomeric alkane olefin.
According to the present invention, in the step (1), the first reboiler is a tank heat exchanger.
According to the invention, in the step (1), the material to be separated is from materials such as petroleum cracking gas, propane dehydrogenation product, methanol-to-olefin product, butane isomerization product and the like.
According to the invention, in the step (2), the pressurization is performed by using a compressor, for example, and the compression ratio of the compressor is 1.5-3.0.
According to the invention, in step (2), the pressurized gas phase fraction is a superheated gas phase fraction. The pressurized gas phase fraction can be used as a heat source of a reboiler of the distillation column due to the high temperature, and the gas phase fraction is changed into a condensed fraction through heat exchange.
According to the invention, in the step (2), the first reboiler is used for cooling down the pressurized gas phase fraction. In the process, the supercharged overheated gas phase fraction preferentially enters a first reboiler, and because the supercharged gas phase fraction has overhigh temperature, in the first reboiler, the gas phase fraction heats the tower bottom liquid of a distillation tower flowing through the first reboiler in a cooling and cooling mode, all the obtained tower bottom gas phase materials return to a tower bottom of the distillation tower, and all the obtained tower bottom liquid phase materials are extracted; wherein, the concentration of light components in the gas phase material of the tower bottom liquid is improved, and the concentration of heavy components in the liquid phase material of the tower bottom liquid is improved, namely, the tower bottom liquid of the distillation tower is further separated in the first reboiler.
According to the present invention, in step (2), the number of the first reboiler is at least one, for example, 1 to 10, for example, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10. When a plurality of first reboilers are provided, the plurality of first reboilers may be connected in series (the series refers to the gas-phase fraction passing through the plurality of first reboilers in sequence) or in parallel (the parallel refers to the gas-phase fraction being divided and passing through the plurality of first reboilers).
According to the invention, in step (2), the second reboiler is adapted to condense the pressurized gas phase fraction. In the process, the temperature of the pressurized superheated gas phase fraction is reduced because the superheated gas phase fraction is cooled by the first reboiler, but the gas phase state is still kept; in the second reboiler, the gas phase fraction heats the tower bottom liquid mainly in a condensation mode, the heated tower bottom liquid returns to the tower bottom, and the condensed gas phase fraction is sent to a reflux tank, part of the gas phase fraction refluxes to the distillation tower and part of the gas phase fraction is extracted.
According to the invention, in step (2), the number of the second reboilers is at least one, such as 1-10, such as 1, 2, 3, 4, 5, 6, 7, 8, 9, 10. When a plurality of second reboilers are provided, the plurality of second reboilers may be connected in series (the series refers to that the gas-phase fraction passes through the plurality of second reboilers in sequence), or in parallel (the parallel refers to that the gas-phase fraction is divided and passes through the plurality of second reboilers).
According to the invention, the distillation column is a rectification column.
The invention has the beneficial effects that:
the invention provides a separation method, which is characterized in that a gas phase fraction obtained at the top of a distillation tower is pressurized to obtain a superheated gas phase fraction, and the superheated gas phase fraction is used as a heat source of a reboiler of the distillation tower. The reboiler is heated under the condition of higher temperature in a step cooling mode, and then the reboiler is heated in the rest reboilers in a condensation mode.
Drawings
FIG. 1 is a flow diagram of a distillation process according to a preferred embodiment of the present invention.
The reference signs are: A. a rectifying tower; B. a compressor; C. a reflux tank; D. a first reboiler; E. a second reboiler; F. a pressure regulating valve; 1. a hydrocarbon feed line; 2. ejecting a gas phase out of the rectifying tower; 3. the compressed overhead gas phase; 4. the overhead gas phase after being cooled by the first reboiler; 5. cooling the condensate by a second reboiler; 7. refluxing liquid; 8. extracting the fraction at the top of the tower; 9. removing the tower bottom liquid from a reboiler; 10. the tower bottom liquid is heated by a second reboiler and then returns to the tower; 11. the tower bottom liquid is heated by a first reboiler, and then the gas phase returns to the tower; 12. and (4) extracting liquid from a tower kettle.
Detailed Description
The preparation method of the present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
In the description of the present invention, it should be noted that the terms "first", "second", etc. are used for descriptive purposes only and do not indicate or imply relative importance.
Example 1
The distillation process flow diagram is shown in fig. 1, and the distillation system for realizing the process comprises a rectifying tower A, a compressor B, a reflux tank C, a first reboiler D, a second reboiler E and a pressure regulating valve F. The method comprises the following steps that materials to be separated enter a rectifying tower A through a hydrocarbon feeding pipeline 1, distillation treatment is carried out, gas phase 2 is ejected out of the rectifying tower, gas phase components are compressed to obtain tower top gas phase 3 through a compressor B, the compressed tower top gas phase 3 enters a first reboiler D for heat exchange, the tower top gas phase 4 cooled by the first reboiler enters a second reboiler E for continuous heat exchange, condensate 5 cooled by the second reboiler enters a reflux tank C, part of the reflux tank C is reflux liquid 7, and part of tower top fraction is extracted 8; the tower bottom liquid of the rectifying tower A is sent to a reboiler 9, the tower bottom liquid is heated by a second reboiler E and then returned to the tower 10, the tower bottom liquid is heated by a first reboiler D, the gas phase is returned to the tower 11, and the liquid phase is extracted from the tower 12.
Example 2
The process flow of example 1 was used to separate propane and propylene by distillation, wherein the number of plates in the rectification column was 158, the overhead temperature was 10.6 ℃, the overhead pressure was 0.79MPa, the bottom temperature was 22 ℃, the bottom pressure was 0.88MPa, and the reflux ratio was 21. 15000kg/h of material to be separated (propylene content 27.7 mol%; propane content 72.3 mol%), feeding temperature 18 ℃ and pressure 0.85 MPa. The compression ratio of the overhead vapor compressor was 1.7, and the temperature of the compressed overhead vapor fraction was 37.3 ℃. The compressed tower top gas phase fraction is first fed into the first reboiler (kettle type heat exchanger) to control the operation temperature of the first reboiler to 24 deg.c, the tower bottom liquid is vaporized and phase separated in the first reboiler, the gas phase in the tower bottom liquid is controlled via the pressure control valve and returned to the rectifying tower, and the liquid phase in the tower bottom liquid is propane phase and cooled in the auxiliary cooler before being fed out of the apparatus. The temperature of the gas phase fraction at the top of the tower which is out of the first reboiler is reduced to 35 ℃, and the gas phase fraction enters the second reboiler to be condensed and then returns to the reflux tank. And the tower bottom liquid entering the second reboiler returns to the tower bottom after being heated. The reflux tank is filled with propylene liquid, optionally, the propylene liquid flows back to the rectifying tower after passing through an auxiliary cooler, part of the propylene liquid is sent out, and the content of propylene in the propylene liquid is 99.7 mol%.
The heat pump rectification reduces the energy consumption of the rectification operation; the tower bottom liquid (propane phase) is heated and vaporized by a first reboiler, volatile propylene is enriched in the gas phase, and the gas phase returns to the rectifying tower; the bottom propane phase withdrawn from the first reboiler had a propylene content of less than 0.8 mol%.
Comparative example 1
The process flow scheme of example 1 was employed with the exception that the first reboiler was not included and the compressed overhead vapor fraction was fed directly to the second reboiler, with the specific process parameters and flow scheme as follows: the number of tower plates of the rectifying tower is 158, the temperature at the top of the tower is 10.6 ℃, the pressure at the top of the tower is 0.79MPa, the temperature at the bottom of the tower is 22 ℃, the pressure at the bottom of the tower is 0.88MPa, and the reflux ratio is 21. 15000kg/h of material to be separated (propylene content 27.7 mol%; propane content 72.3 mol%), feeding temperature 18 ℃ and pressure 0.85 MPa. The compression ratio of the overhead vapor compressor is 1.7, the temperature of the compressed overhead gas phase fraction is 37.3 ℃, the compressed overhead gas phase fraction enters a second reboiler to exchange heat with tower bottom liquid, and the tower bottom liquid heated by the second reboiler returns to the tower bottom. The gas phase fraction at the top of the tower after heat exchange in the second reboiler optionally flows back to the rectifying tower after passing through an auxiliary cooler, and part of the gas phase fraction is sent out, wherein the content of propylene in the fraction at the top of the tower (propylene liquid) is 99.7 mol%.
The tower bottom liquid is directly extracted from the tower bottom, and the content of the propylene in the extracted tower bottom liquid propane phase is 1.1 mol%.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A separation method, wherein the method comprises the steps of:
(1) feeding the material to be separated into a distillation tower for distillation, obtaining gas phase fraction at the tower top of the distillation tower, and obtaining tower bottom liquid at the tower bottom of the distillation tower;
(2) pressurizing the gas phase fraction at the top of the distillation tower, and respectively feeding the pressurized gas phase fraction and tower bottom liquid into a reboiler connected with the bottom of the distillation tower;
wherein the reboiler comprises a first reboiler and a second reboiler; the gas phase fraction passes through a first reboiler and a second reboiler in sequence; the tower bottom liquid is respectively sent into a first reboiler and a second reboiler;
in the reboiler, the pressurized gas phase fraction heats the tower bottom liquid;
(3) and collecting the bottom liquid flowing through the first reboiler, and/or collecting the condensed fraction after the gas phase fraction flowing through the first reboiler and the second reboiler is condensed.
2. The separation method according to claim 1, wherein the method further comprises at least one of the following steps:
(4) heating the tower bottom liquid flowing through the first reboiler, and then returning all the obtained gas-phase materials to the tower bottom of the distillation tower, and extracting all the obtained liquid-phase materials;
(5) the tower bottom liquid flowing through the second reboiler is heated and then returns to the tower bottom of the distillation tower;
(6) and the gas phase fraction is sent into a reflux tank after being condensed by the first reboiler and the second reboiler, part of the gas phase fraction reflows to the distillation tower, and part of the gas phase fraction is extracted.
3. The separation process according to claim 1 or 2, wherein in step (1), the material to be separated is selected from a mixture of C2-C4 hydrocarbons, or from a mixture of n-butyraldehyde and isobutyraldehyde, and the mixture of C2-C4 hydrocarbons is selected from a mixture of propylene and propane, or from a mixture of C4 normal paraffins and a mixture of C4 isoparaffins, or from a mixture of two or more thereof.
4. The separation process according to any one of claims 1 to 3, wherein in step (1), the first reboiler is a tank heat exchanger.
5. The separation method according to any one of claims 1 to 4, wherein in the step (1), the material to be separated is at least one of cracked petroleum gas, olefin products from methanol, propane dehydrogenation products or butane isomerization products.
6. The separation method according to any one of claims 1 to 5, wherein in the step (2), the pressurization is performed by using a compressor, and the compression ratio of the compressor is 1.5 to 3.0.
7. The separation process according to any one of claims 1 to 6, wherein in the step (2), the first reboiler is used for cooling down the pressurized gas phase fraction; in the first reboiler, heating tower bottom liquid of a distillation tower flowing through the first reboiler by the gas-phase fraction in a cooling and cooling mode, returning all obtained tower bottom gas-phase materials to a tower bottom of the distillation tower, and extracting all obtained tower bottom liquid-phase materials; wherein, the concentration of light components in the gas phase material of the tower bottom liquid is improved, and the concentration of heavy components in the liquid phase material of the tower bottom liquid is improved, namely, the tower bottom liquid of the distillation tower is further separated in the first reboiler.
8. The separation process according to any one of claims 1 to 7, wherein in the step (2), the number of the first reboilers is at least one, for example, 1 to 10, and wherein, when a plurality of first reboilers are provided, the plurality of first reboilers are connected in series or in parallel.
9. The separation process according to any one of claims 1 to 8, wherein in step (2) the second reboiler is used to condense the pressurized gas phase fraction; in the second reboiler, the gas phase fraction heats the tower bottom liquid mainly in a condensation mode, the heated tower bottom liquid returns to the tower bottom, and the condensed gas phase fraction is sent to a reflux tank, part of the gas phase fraction refluxes to the distillation tower and part of the gas phase fraction is extracted.
10. The separation process according to any one of claims 1 to 9, wherein in step (2), the number of the second reboilers is at least one, such as 1 to 10, and wherein when a plurality of second reboilers are provided, the plurality of second reboilers are connected in series or in parallel.
CN202010188431.0A 2020-03-17 2020-03-17 Separation method Pending CN111228842A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112169364A (en) * 2020-09-29 2021-01-05 江苏博颂化工科技有限公司 Fractionating tower heat pump system adopting external circulating working medium
CN112321382A (en) * 2020-09-23 2021-02-05 山东齐鲁石化工程有限公司 1-butene refining energy-saving process and device with heat pump heat integration
CN114432721A (en) * 2020-11-03 2022-05-06 北京诺维新材科技有限公司 Method for concentrating polymer solution and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101502721A (en) * 2009-02-12 2009-08-12 南京工业大学 Adsorption type heat pump rectification system
CN107814679A (en) * 2016-09-13 2018-03-20 河北新欣园能源股份有限公司 The heat-pump rectifying process separated for carbon four
CN209361889U (en) * 2018-11-28 2019-09-10 天津乐科节能科技有限公司 Organic silicon monomer is from backheat rectifier unit
WO2019176188A1 (en) * 2018-03-15 2019-09-19 東洋エンジニアリング株式会社 Non-heat-insulated distillation column

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101502721A (en) * 2009-02-12 2009-08-12 南京工业大学 Adsorption type heat pump rectification system
CN107814679A (en) * 2016-09-13 2018-03-20 河北新欣园能源股份有限公司 The heat-pump rectifying process separated for carbon four
WO2019176188A1 (en) * 2018-03-15 2019-09-19 東洋エンジニアリング株式会社 Non-heat-insulated distillation column
CN209361889U (en) * 2018-11-28 2019-09-10 天津乐科节能科技有限公司 Organic silicon monomer is from backheat rectifier unit

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112321382A (en) * 2020-09-23 2021-02-05 山东齐鲁石化工程有限公司 1-butene refining energy-saving process and device with heat pump heat integration
CN112169364A (en) * 2020-09-29 2021-01-05 江苏博颂化工科技有限公司 Fractionating tower heat pump system adopting external circulating working medium
CN112169364B (en) * 2020-09-29 2021-12-24 江苏博颂化工科技有限公司 Fractionating tower heat pump system adopting external circulating working medium
CN114432721A (en) * 2020-11-03 2022-05-06 北京诺维新材科技有限公司 Method for concentrating polymer solution and application thereof
CN114432721B (en) * 2020-11-03 2023-09-15 北京诺维新材科技有限公司 Polymer solution concentration method and application thereof

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