CN109096039A - A method of ethane and carbon dioxide are separated using ion liquid abstraction rectifying - Google Patents

A method of ethane and carbon dioxide are separated using ion liquid abstraction rectifying Download PDF

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Publication number
CN109096039A
CN109096039A CN201810958617.2A CN201810958617A CN109096039A CN 109096039 A CN109096039 A CN 109096039A CN 201810958617 A CN201810958617 A CN 201810958617A CN 109096039 A CN109096039 A CN 109096039A
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China
Prior art keywords
ethane
carbon dioxide
extractant
extractive distillation
distillation column
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Pending
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CN201810958617.2A
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Chinese (zh)
Inventor
王英龙
亓鹏超
戴姚
朱兆友
崔培哲
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Qingdao University of Science and Technology
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Qingdao University of Science and Technology
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Priority to CN201810958617.2A priority Critical patent/CN109096039A/en
Publication of CN109096039A publication Critical patent/CN109096039A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • C07C7/05Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
    • C07C7/08Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Epoxy Compounds (AREA)

Abstract

The present invention provides the methods using ion liquid abstraction rectifying separation ethane and carbon dioxide, high, complex process the status for ethane and carbon dioxide binary azeotrope prior art separating energy consumption, using 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ionic liquid as extractant, the target that product ethane and carbon dioxide are separated from binary mixture is realized.It is operated using single column extracting rectifying, compared with traditional separation method, significantly reduces energy consumption, save cost of equipment.Using the fixedness of extractant 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ionic liquid, realize high-purity separation, can reuse to extractive distillation column, save cost of material.

Description

A method of ethane and carbon dioxide are separated using ion liquid abstraction rectifying
[technical field]
The invention belongs to rectifying separation technology fields, and in particular to a kind of ion liquid abstraction rectifying separation ethane and dioxy Change the method for carbon.
[background technique]
Ethane is the common composition in oil recovery processes, is the important source material for producing ethylene.In chemical engineering industry, ethane master Be used for steam cracking production ethylene, to the growing of ethylene requirements, the research of making ethylene from ethane oxidative dehydrogenation increasingly by To concern, and it can be used as refrigerant in refrigeration.Carbon dioxide is as one of main greenhouse gases, carbon dioxide Capture it is extremely important.
The normal boiling point of ethane and carbon dioxide is respectively 194.7K and 184.55K, and two kinds of compounds are at various pressures The homogeneous binary azeotrope for forming minimum boiling point, cannot achieve using traditional separation method and efficiently separates.
Patent (CN201810020014) is related to a kind of device and method of carbon dioxide removal from ethane gas, the hair The consumption of the bright sodium hydroxide that downstream unit can be greatly lowered, while the purity of ethane product is greatlyd improve, but technique Process and process unit are complicated, and energy consumption consumption is big.
Patent (CN201210288030) is related to the method for carbon dioxide recovery in a kind of extraction of petroleum, simple process, It is easy to operate, but the rate of recovery of carbon dioxide is low.
Patent (CN201710418571) is related to recycling device and the side of ethane carbon dioxide removal in a kind of pipe natural gas The process flow of method, carbon dioxide removal of the present invention is relative complex.
The present invention realizes efficiently separating for ethane and carbon dioxide mixture using extractive distillation column-flash tank, with 1- Ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ionic liquid is extractant, and the carbon dioxide purity after realizing separation is up to The purity of 99.90%-99.99%, ethane reach 99.90%-99.99%;By the flash distillation of flash tank, keep extractant real Existing recycling and reusing, reduces separation costs;Height just is isolated from the binary mixture formed containing azeotropic merely with single column Purity component, compared to traditional technique, low energy consumption, simple process and at low cost.
[summary of the invention]
[technical problems to be solved]
The object of the present invention is to provide a kind of methods using ion liquid abstraction rectifying separation ethane and carbon dioxide.
[technical solution]
The present invention is directed to ethane and carbon dioxide binary mixture, and prior art separating energy consumption is high, complex process status, The method of separation of extractive distillation ethane and carbon dioxide is provided.With 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ion Liquid is extractant, and the carbon dioxide purity after realizing separation is up to 99.90%-99.99%, and the purity of ethane reaches 99.90%-99.99%.By the flash distillation of flash tank, extractant is made to can be realized recycling and reusing, reduces separation costs;Only High-purity component is just isolated from the binary mixture formed containing azeotropic using single column, compared to traditional technique, substantially Reduce energy consumption and simple for process.
The present invention is a kind of method using ion liquid abstraction rectifying separation ethane and carbon dioxide, it is characterised in that should Method equipment therefor is as follows:
Extractive distillation column (T), condenser (C1), condenser (C2) reboiler (R), heat exchanger (H), flash tank (F), discharging Pump (P1), discharging pump (P2);Wherein reboiler (R) and condenser (C) are connected to extractive distillation column (T) tower bottom and tower top;
A kind of method using ion liquid abstraction rectifying separation ethane and carbon dioxide, comprising the following steps:
(1) ethane and carbon dioxide mixture 1 enter in tower by the road from the lower part of extractive distillation column (T), extractant warp Pipeline 6 enters in tower from the top of extractive distillation column (T), and the ethane product of high-purity 3 produces by the road from overhead stream, tower reactor Logistics 2 entrance flash tank (F) by the road;
(2) extractive distillation column (T) tower reactor logistics is flashed in the flash tank (F), and product carbon dioxide is from flash tank (F) Top produces after condenser (C2) condensation through pipeline 4;
(3) extractant flows through pipeline 5 and mixes after heat exchanger (H) heat exchange with the fresh extractant of supplement, is delivered to extraction Rectifying column (T) is taken, is recycled;
Extractive distillation column (T) operating pressure is 24atm, and reflux ratio 1.0-5.0, the number of plates is 33 pieces, mixture charging Plate is 19-25 block, and extractant feed plate is 1-5 block, and tower top temperature is 252-255 DEG C, and column bottom temperature is 131-133 DEG C.
In accordance with another preferred embodiment of the present invention, it is characterised in that: the extractant is 1- ethyl-3-methylimidazole Bis-trifluoromethylsulfoandimide ionic liquid.
In accordance with another preferred embodiment of the present invention, it is characterised in that: the extractant and ethane and carbon dioxide are mixed The charging molar flow ratio for closing object is 0.3-0.6.
In accordance with another preferred embodiment of the present invention, it is characterised in that: in the ethane and carbon dioxide mix liquid Ethane 0.538mol%, carbon dioxide 0.462mol%.
In accordance with another preferred embodiment of the present invention, it is characterised in that: the purity of isolated ethane and carbon dioxide point It Gao Da not 99.90%-99.99% and 99.90%-99.99%.
In accordance with another preferred embodiment of the present invention, it is characterised in that: the ionic liquid that extractant is recycled through flash tank (F) Body is reusable in extractive distillation column (T).
The method of separation of extractive distillation ethane and carbon dioxide of the invention is described in detail below:
At 47 DEG C, ethane and carbon dioxide mixture 1 enter in tower by the road from the lower part of extractive distillation column (T), extract Agent 6 enters in tower by the road from the top of extractive distillation column (T), and product ethane is from tower top 3 extraction by the road, and tower reactor logistics is through pipe Road 2 enters flash tank (F);Extractive distillation column (T) tower reactor logistics is flashed in the flash tank (F), and product carbon dioxide is from top Portion's 4 extraction by the road;Extractant 5 mixes after heat exchanger (H) heat exchange with the fresh extractant of supplement by the road, is delivered to extraction Rectifying column (T) is taken, is recycled.
[beneficial effect]
Compared with prior art, the present invention mainly have it is following the utility model has the advantages that
(1) the separating high-purity component from binary mixture, work are realized using simple single column and flash unit operation Skill is simple and easy;
(2) the ethane purity after separating is up to 99.90%-99.99%, and carbon dioxide purity is up to 99.90%- 99.99%;
(3) extractant realizes recycling and reusing well, reduces separation costs.
[Detailed description of the invention]
Fig. 1 is flow diagram of the invention, in which:
P1, P2- discharging pump;F- flash tank;T- extractive distillation column;C- condenser;R- reboiler;H- heat exchanger;Digital table Show each logistics pipeline.
[specific embodiment]
Embodiment 1
(number of plates is from top to bottom with 33 blocks of theoretical trays for extractive distillation column in extracting rectifying process as shown in Figure 1 Number), it is added using ionic liquid 1- ethyl-3-methylimidazole as extractant from the 2nd block of plate, flow 1.6kmol/s, ethane and two The mixture of carbonoxide is added from the 22nd piece of theoretical plate, forms ethane 0.538mol%, carbon dioxide 0.462mol%, and flow is 4kmol/s.Extractive distillation column is operated at 24atm, and overhead reflux ratio is 4.0.
The pressure of flash tank is 10kPa, and flash temperature is 100 DEG C, and the molar fraction of ethane is 99.2% after separation, dioxy The molar fraction for changing carbon is 99.93%.
Embodiment 2
(number of plates is from top to bottom with 33 blocks of theoretical trays for extractive distillation column in extracting rectifying process as shown in Figure 1 Number), it is added using ionic liquid 1- ethyl-3-methylimidazole as extractant from the 4th block of plate, flow 1.6kmol/s, ethane and two The mixture of carbonoxide is added from the 20th piece of theoretical plate, forms ethane 0.538mol%, carbon dioxide 0.462mol%, and flow is 4kmol/s.Extractive distillation column is operated at 24atm, and overhead reflux ratio is 4.0.
The pressure of flash tank is 10kPa, and flash temperature is 100 DEG C, and the molar fraction of ethane is 99.0% after separation, dioxy The molar fraction for changing carbon is 99.96%.
Embodiment 3
(number of plates is from top to bottom with 33 blocks of theoretical trays for extractive distillation column in extracting rectifying process as shown in Figure 1 Number), it is added using ionic liquid 1- ethyl-3-methylimidazole as extractant from the 3rd block of plate, flow 1.6kmol/s, ethane and two The mixture of carbonoxide is added from the 24th piece of theoretical plate, forms ethane 0.538mol%, carbon dioxide 0.462mol%, and flow is 4kmol/s.Extractive distillation column is operated at 24atm, and overhead reflux ratio is 4.0.
The pressure of flash tank is 10kPa, and flash temperature is 100 DEG C, and the molar fraction of ethane is 99.1% after separation, dioxy The molar fraction for changing carbon is 99.93%.
Embodiment 4
(number of plates is from top to bottom with 33 blocks of theoretical trays for extractive distillation column in extracting rectifying process as shown in Figure 1 Number), it is added using ionic liquid 1- ethyl-3-methylimidazole as extractant from the 1st block of plate, flow 1.6kmol/s, ethane and two The mixture of carbonoxide is added from the 23rd piece of theoretical plate, forms ethane 0.538mol%, carbon dioxide 0.462mol%, and flow is 4kmol/s.Extractive distillation column is operated at 24atm, and overhead reflux ratio is 4.0.
The pressure of flash tank is 10kPa, and flash temperature is 100 DEG C, and the molar fraction of ethane is 99.3% after separation, dioxy The molar fraction for changing carbon is 99.95%.

Claims (6)

1. a kind of method using ion liquid abstraction rectifying separation ethane and carbon dioxide, it is characterised in that this method dress used It sets as follows:
Extractive distillation column (T), condenser (C1), condenser (C2), reboiler (R), heat exchanger (H), flash tank (F), discharging pump (P1), discharging pump (P2);Wherein reboiler (R) and condenser (C) are connected to extractive distillation column (T) tower bottom and tower top;
A kind of method using ion liquid abstraction rectifying separation ethane and carbon dioxide, comprising the following steps:
(1) ethane and carbon dioxide mixture 1 enter in tower by the road from the lower part of extractive distillation column (T), extractant by the road 6 Enter in tower from the top of extractive distillation column (T), product ethane from overhead stream by the road 3 extraction, tower reactor logistics by the road 2 into Enter flash tank (F);
(2) extractive distillation column (T) tower reactor logistics is flashed in flash tank (F), and product carbon dioxide is at the top of flash tank (F) It is produced after condenser (C2) condensation through pipeline 4;
(3) extractant 5 mixes after heat exchanger (H) heat exchange with the fresh extractant of supplement by the road, is delivered to extracting rectifying Tower (T), is recycled;
Extractive distillation column (T) operating pressure is 24atm, and reflux ratio 1.0-5.0, the number of plates is 33 pieces, and mixture feedboard is 19-25 block, extractant feed plate are 1-5 block, and tower top temperature is 252-255 DEG C, and column bottom temperature is 131-133 DEG C.
2. a kind of method using ion liquid abstraction rectifying separation ethane and carbon dioxide according to claim 1, Be characterized in that: the extractant is 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ionic liquid.
3. a kind of method using ion liquid abstraction rectifying separation ethane and carbon dioxide according to claim 1, Be characterized in that: the charging molar flow ratio of the extractant and ethane and carbon dioxide mix liquid is 0.3-0.6.
4. a kind of method using ion liquid abstraction rectifying separation ethane and carbon dioxide according to claim 1, It is characterized in that: ethane 0.538mol%, carbon dioxide 0.462mol% in the ethane and carbon dioxide mix liquid.
5. a kind of method using ion liquid abstraction rectifying separation ethane and carbon dioxide according to claim 1, Be characterized in that: the purity of isolated ethane and carbon dioxide is up to 99.90%-99.99% and 99.90%-99.99% respectively.
6. a kind of method using ion liquid abstraction rectifying separation ethane and carbon dioxide according to claim 1, Be characterized in that: the ionic liquid that extractant is recycled through flash tank (F) is reusable in extractive distillation column (T).
CN201810958617.2A 2018-08-22 2018-08-22 A method of ethane and carbon dioxide are separated using ion liquid abstraction rectifying Pending CN109096039A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0036733A1 (en) * 1980-03-18 1981-09-30 Koch Process Systems, Inc. Distillative separation of carbon dioxide from light hydrocarbons
CN1678412A (en) * 2002-08-27 2005-10-05 国际壳牌研究有限公司 Method of removing solid carbon dioxide
CN102471188A (en) * 2009-07-30 2012-05-23 埃克森美孚上游研究公司 Systems and methods for removing heavy hydrocarbons and acid gases from a hydrocarbon gas stream
CN108067012A (en) * 2018-01-17 2018-05-25 中国科学院过程工程研究所 A kind of extractant for being used for separation of extractive distillation methanol and dimethyl carbonate azeotrope and application thereof and processing method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0036733A1 (en) * 1980-03-18 1981-09-30 Koch Process Systems, Inc. Distillative separation of carbon dioxide from light hydrocarbons
CN1678412A (en) * 2002-08-27 2005-10-05 国际壳牌研究有限公司 Method of removing solid carbon dioxide
CN102471188A (en) * 2009-07-30 2012-05-23 埃克森美孚上游研究公司 Systems and methods for removing heavy hydrocarbons and acid gases from a hydrocarbon gas stream
CN108067012A (en) * 2018-01-17 2018-05-25 中国科学院过程工程研究所 A kind of extractant for being used for separation of extractive distillation methanol and dimethyl carbonate azeotrope and application thereof and processing method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZHU ZHAOYOU,ET AL: "Process design of carbon dioxide and ethane separation using ionic liquid by extractive distillation", 《JOURNAL OF CHEMICAL TECHNOLOGY & BIOTECHNOLOGY》 *

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Application publication date: 20181228