CN104058920A - Separation method of propylene from propane by extractive rectification with alkane as extracting agent - Google Patents
Separation method of propylene from propane by extractive rectification with alkane as extracting agent Download PDFInfo
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- CN104058920A CN104058920A CN201310701140.7A CN201310701140A CN104058920A CN 104058920 A CN104058920 A CN 104058920A CN 201310701140 A CN201310701140 A CN 201310701140A CN 104058920 A CN104058920 A CN 104058920A
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Abstract
The invention discloses a separation method of propylene from propane by extractive rectification with an alkane as an extracting agent. A propylene-propane mixture, with a propylene content being 20%-80% by weight, is subjected to a heat transfer process with the extracting agent separated out from a separating column and then is fed into a middle part of an extractive rectifying column. An extraction process is carried out between the propylene-propane mixture and the extracting agent in a rectifying section in a countercurrent manner. Extracted propylene is condensed in an overhead condenser and a reflux process is carried out to the condensed propylene. A propylene product is partially extracted and is fed into a propylene product storage tank. A bottom product in the extractive rectifying column is fed into the middle ofthe separating column which is used for separating the extracting agent from the propane. A reboiler is arranged at the bottom of the separating column and a condenser is arranged at the top of the separating column. A top product is condensed through the condenser and is refluxed and a propane product is partially extracted and is fed into a propane product storage tank. The extracting agent in the bottom of the separating column is subjected to a heat transfer process through a reboiler at the bottom of the extractive rectifying column, is subjected to a heat transfer process with the fed propylene-propane mixture and is fed into the extractive rectifying column from the top. After the separation process, a purity of the propylene can reach 99.7% by weight. According to the invention, the extracting agent is subjected to a heat transfer process with the bottom product in the extractive rectifying column and the feedstock in a gradient manner so that energy consumption is reduced. To separate 1t of a product, only 1.0-1.2 Gcal of energy is needed while 1.8-2.0 Gcal of energy is needed in the prior art.
Description
Technical field
The invention belongs to vitochemical separation technology field, relate to a kind of method taking alkane as extraction agent separation of extractive distillation propylene-propane.
Background technology
Propylene is colourless inflammable gas at normal temperatures and pressures, is heavier than air, and forms explosive mixture with air, and limits of explosion (volume), dissolves in ethanol and ether, is slightly soluble in water.
Propylene is one of petrochemical complex basic raw material, can, in order to produce multiple important Organic Chemicals, can produce vinyl cyanide, propylene oxide, and epoxy chloropropane, Virahol, butanols, octanols etc., also can directly synthesize polypropylene, second propane etc.Third rare raw material that does polypropylene, Virahol, also can do the raw material of the product such as acrylic fibers, acrylonitrile, and propylene is very large in the requirement of China, and it is the important raw and processed materials of three large synthetic materialss.
The source of propylene is mainly by 3 approach: the by product (accounting for 68%) of ethylene plant's steam cracking, catalytic cracking by product (accounting for 29%), remaining 3% is to obtain by methods such as conversion of olefines, dehydrogenating propane and preparing olefin by conversion of methanols.Adopt the steam cracking gained propylene that petroleum naphtha is raw material to be generally 0.50-0.65 with the yield ratio of ethene, and the conventional yield of propylene of the fluid catalytic cracking of refinery (FCC) device by-product only have 3%-6%.So the problem that solves propylene shortage by conventional steam cracking and catalytic cracking unit is difficult to realize at short notice, dehydrogenating propane will become one of propylene important sources.
No matter be steam cracking and catalytic cracking or dehydrogenating propane, all there is the sepn process of propylene-propane, the separation method of propylene-propane is divided into low-pressure distillation, high-pressure rectification and 3 kinds of operating method of low pressure heat pump distillation according to working pressure difference conventionally at present.High-pressure process is because tower top temperature is higher than 40 DEG C, can produce and reflux by cooling water condensation, and tower reactor can be with low-pressure steam or hot water heating, and equipment is simple, and shortcoming is that reflux ratio is large, and stage number is many.Adopt low-pressure process, propylene propane relative volatility is high, thereby reduce stage number and reflux ratio, but tower top need adopt the cryogen condensation lower than water coolant, now often adopts heat pump, the low temperature hydrocarbon vapour steaming using tower top is as refrigeration cycle cryogen, after compressed raising pressure and temperature, send to tower reactor heat exchange, emit heat and the liquid that congeals into, part discharging, partial reflux, this flow process complexity.Propylene tower adopts high pressure and cooling water system mostly in recent years.Because high-pressure process exists the shortcoming that relative volatility is low, reflux ratio is large, stage number is many, someone adopts extracting rectifying flow process to improve and optimizate it, its ultimate principle is based on propane propylene electronic cloud mobility difference, extraction agent is also different to their interaction force, thereby they are separated to the moisture CH of solvent selection
3cN (acetonitrile), forms azeotrope containing water-acetonitrile and propylene, reaches separation of extractive distillation propylene-propane effect.This flow process is made up of 4 towers, and tower 1 is extractive distillation column, and tower top is isolated propane; Tower 2 is stripping towers, and tower reactor is extracted agent and recycles, and overhead gas major part is propylene; Tower 3 is water wash columns, washes the ACN containing in propylene off, and tower top obtains product propylene; Tower 4 is extraction agent recovery towers, and a small amount of ACN in recycle-water, to avoid ACN loss.But CH
3cN toxicity is large, adopts containing water-acetonitrile, and produce sewage and have a strong impact on environment, 4 towers of this requirements of process simultaneously, equipment is many, and investment is large.
In order to address these problems, the present invention adopts alkane to make extraction agent, thereby makes propane in alkane extraction propylene-propane mixture realize the separation of propylene-propane.
Summary of the invention
The present invention adopts alkane to make extraction agent, and two tower flow processs have realized propylene-propane high efficiency separation object.
technical scheme:
A kind of method taking alkane as extraction agent separation of extractive distillation propylene-propane, propylene content 20(wt) %-80(wt) enter extractive distillation column middle part after the extraction agent heat exchange through separating with knockout tower of propylene-propane mixture of %, propylene-propane mixture is in rectifying section and extraction agent adverse current, after overhead condenser condensation, reflux, part extraction propylene product is entered propylene product storage tank; Extracting rectifying tower reactor material enters extraction agent and propane knockout tower middle part, knockout tower tower reactor is equipped with reboiler, tower top has condenser, tower top material is after condenser condenses, reflux, part extraction propane product enters propane tank, the extraction agent of tower reactor after the heat exchange of extracting rectifying tower reactor reboiler, then with propylene-propane mixture heat exchange of charging after enter tower from extractive distillation column top.
In described propylene-propane mixture, propylene content is 50(wt) %-80(wt) %.
Described extraction agent is Skellysolve A, iso-pentane.
The theoretical plate number of described extractive distillation column is 40-60 piece.
The theoretical plate number of described knockout tower is 10-15 piece.
Described propylene-propane mixture and the weight ratio of extraction agent are 1:2-1:3.
Described extracting rectifying tower reactor temperature 50-55 DEG C.
Described extractive distillation column tower top temperature 40-45 DEG C, pressure is 1.2-1.5MPa.
Described separation tower reactor temperature 60-65 DEG C.
Described separation tower top temperature 46-50 DEG C, pressure is 1.1-1.3MPa.
Described extractive distillation column reflux ratio is 8-15.
Described knockout tower reflux ratio 2-3.
Described extractive distillation column propylene-propane mixture feed zone stage number is 10-15.
Described extractive distillation column extractant feed section stage number is 2-3.
Described knockout tower feed zone stage number is 4-7.
Described separation tower reactor reboiler is made thermal source by low-pressure steam.
Described extractive distillation column and knockout tower item condenser are made refrigerant with water coolant.
invention has feature and effect
The present invention uses alkane to make extraction agent, particularly uses Skellysolve A to make extraction agent, and the propane in extractive distillation column in counter-current extraction propylene-propane mixture reaches propylene and separates object with propane, and after separating, purified propylene reaches 99.7(wt) %.The present invention by extraction agent and rectifying tower reactor material and the heat exchange of charging step, has reduced energy consumption simultaneously, separates one ton of product energy consumption and only needs 1.0-1.2Gcal, and prior art needs 1.8-2.0 Gcal.
Embodiment
Below in conjunction with specific embodiment, invention is described further, but invention is not limited.
example 1
To be propylene-propane mixture of 20% enter the 12nd column plate place of the extractive distillation column of theoretical plate number as 50 taking 1250kg/h flow to weight concentration, from separate tower reactor out Skellysolve A rectifying tower reboiler and the heat exchange of rectifying tower bottoms, after feed exchanger and the heat exchange of propylene-propane mixture, enter tower from the 48th block of column plate of extractive distillation column again, carry out counter-current extraction with propylene-propane mixture, the flow of extraction agent Skellysolve A is 2500kg/h.Control tower item temperature 40-45 DEG C, pressure 1.2-1.5MPa, the propylene of tower top enters overhead condenser condensation and enters backflash and reflux through reflux pump, controls reflux ratio (weight ratio) 9-10, tower reactor temperature 50-55 DEG C.
It is the 5th block of column plates of 12 knockout towers that extracting rectifying tower reactor liquid dependence self pressure enters theoretical plate number, carry out the separation of propane-Skellysolve A, tower top temperature 46-50 DEG C, pressure is 1.1-1.3 MPa, the propane of tower top enters knockout tower backflash and refluxes after overhead condenser condensation, and reflux ratio (weight ratio) is 2-3; The reboiler of tower reactor heats by low-pressure steam, controls temperature 60-65 DEG C.After separating, extraction agent enters extractive distillation column top after step heat exchange.
Result of implementation, through gas chromatographic analysis, separation of propylene purity is 99.75(wt) %, meet polymerization-grade propylene requirement; Purified propylene oxide reaches 98(wt) more than %, contain propylene lower than 1(wt) %.
example 2
To be propylene-propane mixture of 40% enter the 10th column plate place of the extractive distillation column of theoretical plate number as 60 taking 1250kg/h flow to weight concentration, from separate tower reactor out Skellysolve A rectifying tower reboiler and the heat exchange of rectifying tower bottoms, after feed exchanger and the heat exchange of propylene-propane mixture, enter tower from the 58th block of column plate of extractive distillation column again, carry out counter-current extraction with propylene-propane mixture, the flow of extraction agent Skellysolve A is 3000kg/h.Control tower item temperature 40-45 DEG C, pressure 1.2-1.5MPa, the propylene of tower top enters overhead condenser condensation and enters backflash and reflux through reflux pump, controls reflux ratio (weight ratio) 9-10, tower reactor temperature 50-55 DEG C.
It is the 5th column plate places of 12 knockout towers that extracting rectifying tower reactor liquid dependence self pressure enters theoretical plate number, carry out the separation of propane-Skellysolve A, tower top temperature 46-50 DEG C, pressure is 1.1-1.3 MPa, the propane of tower top enters knockout tower backflash and refluxes after overhead condenser condensation, and reflux ratio (weight ratio) is 2-3; The reboiler of tower reactor heats by low-pressure steam, controls temperature 60-65 DEG C.After separating, extraction agent enters extractive distillation column top after step heat exchange.
Result of implementation, through gas chromatographic analysis, separation of propylene purity is 99.85(wt) %, meet polymerization-grade propylene requirement; Purified propylene oxide reaches 98(wt) more than %, contain propylene lower than 1(wt) %.
example 3
To be propylene-propane mixture of 50% enter the 12nd column plate place of the extractive distillation column of theoretical plate number as 40 taking 1250kg/h flow to weight concentration, from separate tower reactor out Skellysolve A rectifying tower reboiler and the heat exchange of rectifying tower bottoms, after feed exchanger and the heat exchange of propylene-propane mixture, enter tower from the 39th block of column plate of extractive distillation column again, carry out counter-current extraction with propylene-propane mixture, the flow of extraction agent iso-pentane is 1700kg/h.Control tower item temperature 40-45 DEG C, pressure 1.2-1.5MPa, the propylene of tower top enters overhead condenser condensation and enters backflash and reflux through reflux pump, controls reflux ratio (weight ratio) 9-10, tower reactor temperature 50-55 DEG C.
It is the 5th block of column plates of 10 knockout towers that extracting rectifying tower reactor liquid dependence self pressure enters theoretical plate number, carry out the separation of propane-iso-pentane, tower top temperature 46-50 DEG C, pressure is 1.1-1.3 MPa, the propane of tower top enters knockout tower backflash and refluxes after overhead condenser condensation, and reflux ratio (weight ratio) is 2-3; The reboiler of tower reactor heats by low-pressure steam, controls temperature 60-65 DEG C.After separating, extraction agent enters extractive distillation column top after step heat exchange.
Result of implementation, through gas chromatographic analysis, separation of propylene purity is 99.70(wt) %, meet polymerization-grade propylene requirement; Purified propylene oxide reaches 98(wt) more than %, contain propylene lower than 1(wt) %.
example 4
To be propylene-propane mixture of 80% enter the 12nd column plate place of the extractive distillation column of theoretical plate number as 50 taking 1250kg/h flow to weight concentration, from separate tower reactor out Skellysolve A rectifying tower reboiler and the heat exchange of rectifying tower bottoms, after feed exchanger and the heat exchange of propylene-propane mixture, enter tower from the 48th block of column plate of extractive distillation column again, carry out counter-current extraction with propylene-propane mixture, the flow of extraction agent Skellysolve A is 1250kg/h.Control tower item temperature 40-45 DEG C, pressure 1.2-1.5MPa, the propylene of tower top enters overhead condenser condensation and enters backflash and reflux through reflux pump, controls reflux ratio (weight ratio) 9-10, tower reactor temperature 50-55 DEG C.
It is the 5th block of column plates of 15 knockout towers that extracting rectifying tower reactor liquid dependence self pressure enters theoretical plate number, carry out the separation of propane-Skellysolve A, tower top temperature 46-50 DEG C, pressure is 1.1-1.3 MPa, the propane of tower top enters knockout tower backflash and refluxes after overhead condenser condensation, and reflux ratio (weight ratio) is 2-3; The reboiler of tower reactor heats by low-pressure steam, controls temperature 60-65 DEG C.After separating, extraction agent enters extractive distillation column top after step heat exchange.
Result of implementation, through gas chromatographic analysis, separation of propylene purity is 99.80(wt) %, meet polymerization-grade propylene requirement; Purified propylene oxide reaches 98(wt) more than %, contain propylene lower than 1(wt) %.
example 5
To be propylene-propane mixture of 70% enter the 12nd column plate place of the extractive distillation column of theoretical plate number as 50 taking 1250kg/h flow to weight concentration, from separate tower reactor out Skellysolve A rectifying tower reboiler and the heat exchange of rectifying tower bottoms, after feed exchanger and the heat exchange of propylene-propane mixture, enter tower from the 48th block of column plate of extractive distillation column again, carry out counter-current extraction with propylene-propane mixture, the flow of extraction agent Skellysolve A is 675kg/h.Control tower item temperature 40-45 DEG C, pressure 1.2-1.5MPa, the propylene of tower top enters overhead condenser condensation and enters backflash and reflux through reflux pump, controls reflux ratio (weight ratio) 9-10, tower reactor temperature 50-55 DEG C.
It is the 5th block of column plates of 10 knockout towers that extracting rectifying tower reactor liquid dependence self pressure enters theoretical plate number, carry out the separation of propane-Skellysolve A, tower top temperature 46-50 DEG C, pressure is 1.1-1.3 MPa, the propane of tower top enters knockout tower backflash and refluxes after overhead condenser condensation, and reflux ratio (weight ratio) is 2-3; The reboiler of tower reactor heats by low-pressure steam, controls temperature 60-65 DEG C.After separating, extraction agent enters extractive distillation column top after step heat exchange.
Result of implementation, through gas chromatographic analysis, separation of propylene purity is 99.75(wt) %, meet polymerization-grade propylene requirement; Purified propylene oxide reaches 98(wt) more than %, contain propylene lower than 1(wt) %.
Claims (10)
1. the method taking alkane as extraction agent separation of extractive distillation propylene-propane, propylene content 20(wt) %-80(wt) enter extractive distillation column middle part after the extraction agent heat exchange through separating with knockout tower of propylene-propane mixture of %, propylene-propane mixture is in rectifying section and extraction agent adverse current, after overhead condenser condensation, reflux, part extraction propylene product is entered propylene product storage tank; Extracting rectifying tower reactor material enters extraction agent and propane knockout tower middle part, knockout tower tower reactor is equipped with reboiler, tower top has condenser, tower top material is after condenser condenses, reflux, part extraction propane product enters propane tank, the extraction agent of tower reactor after the heat exchange of extracting rectifying tower reactor reboiler, then with propylene-propane mixture heat exchange of charging after enter tower from extractive distillation column top.
2. the method taking alkane as extraction agent separation of extractive distillation propylene-propane according to claim 1, is characterized in that in described propylene-propane mixture, propylene content is 50(wt) %-80(wt) %.
3. the method taking alkane as extraction agent separation of extractive distillation propylene-propane according to claim 1, is characterized in that described extraction agent is Skellysolve A, iso-pentane.
4. the method taking alkane as extraction agent separation of extractive distillation propylene-propane according to claim 1, is characterized in that the theoretical plate number of described extractive distillation column is 40-60 piece, and the theoretical plate number of described knockout tower is 10-15 piece.
5. the method taking alkane as extraction agent separation of extractive distillation propylene-propane according to claim 1, is characterized in that described propylene-propane mixture and the weight ratio of extraction agent are 1:2-1:3.
6. the method taking alkane as extraction agent separation of extractive distillation propylene-propane according to claim 1, is characterized in that described extracting rectifying tower reactor temperature 50-55 DEG C, tower top temperature 40-45 DEG C, and pressure is 1.2-1.5MPa.
7. the method taking alkane as extraction agent separation of extractive distillation propylene-propane according to claim 1, is characterized in that described separation tower reactor temperature 60-65 DEG C, tower top temperature 46-50 DEG C, and pressure is 1.1-1.3 MPa.
8. the method taking alkane as extraction agent separation of extractive distillation propylene-propane according to claim 1, is characterized in that described extractive distillation column reflux ratio is 8-15, knockout tower reflux ratio 2-3.
9. the method taking alkane as extraction agent separation of extractive distillation propylene-propane according to claim 1, is characterized in that described extractive distillation column propylene-propane mixture feed zone stage number is 10-15, and extractant feed section stage number is 2-3; Knockout tower feed zone stage number is 4-7.
10. the method taking alkane as extraction agent separation of extractive distillation propylene-propane according to claim 1, the separation tower reactor reboiler low-pressure steam described in it is characterized in that is made thermal source, and extractive distillation column and knockout tower item condenser are made refrigerant with water coolant.
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| CN112479801A (en) * | 2020-12-22 | 2021-03-12 | 福建久策气体股份有限公司 | Electronic-grade propylene rectification and purification method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108290852A (en) * | 2015-11-26 | 2018-07-17 | 赢创德固赛有限公司 | The method of epoxidation of propylene |
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| CN112479801A (en) * | 2020-12-22 | 2021-03-12 | 福建久策气体股份有限公司 | Electronic-grade propylene rectification and purification method |
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