CN102503757B - Process flow for separating low-carbon hydrocarbons and separating gas during production of olefins (M-OS/MTO) from methanol - Google Patents
Process flow for separating low-carbon hydrocarbons and separating gas during production of olefins (M-OS/MTO) from methanol Download PDFInfo
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Abstract
The invention provides a non-cryogenic oil absorption separation method for a mixture of low-carbon hydrocarbons, which is used for separating the mixture of the hydrocarbons from gas during production of olefins from methanol. Methane/hydrogen can be separated from heavy components, namely C2 and above by absorbing fractions of the C2 and above by adopting two or more strands of absorbing agents. According to the method disclosed by the invention, an absorbing agent separating tower is increased before a demethanization tower, one strand of material flow, which is separated from the tower is taken as a main absorbing agent of the demethanization tower for absorbing the C2 and C3, the strand of the absorbing agent is the mixture of the fractions, which is from the former system and needs to be separated, and circulation is not required. The second strand of the absorbing agent of the demethanization tower is from a system including a depropanization tower and a debutanization tower, and the absorption effect is further enhanced. Compared with the prior art, the method can greatly reduce the using quantity of the circulating absorbing agents; moreover, the multiple strands of the absorbing agents are adopted, equipment investment and energy consumption are significantly reduced, the recovery rate of ethylene and propylene is further improved; and furthermore, the flow is simple, the operation cost is low, and the operation is safe and reliable.
Description
Technical field
This lower carbon number hydrocarbons separates and methanol-to-olefins (M-OS/MTO) gas separating technology flow process is applicable to oxide compound alkene processed, hydrocarbon cracking, and hydro carbons catalyzed reaction is produced alkene, is also adapted to traditional petrochemical complex ethene field simultaneously.
Background technology
In petrochemical industry, most of intermediates and the finished product are all take alkene and aromatic hydrocarbons as basic material.Ethylene unit is the main production plant of producing alkene (ethene, propylene, divinyl) and aromatic hydrocarbons.Past is mainly produced alkene by petroleum naphtha through pyrolysis in tubular furnace, and in recent years because petroleum resources are in short supply, methanol-to-olefins (MTO/MTP) technology is progressively developed, and has entered industrialization phase.Methanol-to-olefins technology is made up of reaction technology and isolation technique.Reaction technology is designed to core with development and the reactor development of catalyzer, take methyl alcohol as olefin production mixture; Isolation technique is take reaction product as raw material, produces polymer grade ethylene and propylene product through processes such as impurity removal, compression, separation, and its core is exploitation and the design of separation process.
Pass through converting methanol to prepare low carbon olefin gas, its product is similar to the product of petroleum naphtha, hydrocarbon cracking alkene processed in ethylene unit, all formed by hydrogen, methane, carbon two, carbon three, carbon four, carbon five and above composition, proportion of composing has certain difference, hydrogen in methanol-to-olefins (MTO/MTP) device, methane content are lower, and more than five hydro carbons of carbon is little.Therefore, the separation process scheme adopting flow process compared with existing ethylene unit is simple, equipment number of units is less, does not need low temperature separation process, does not need methane or ethylene refrigeration machine, only needs propylene refrigeration.Based on the gas composition feature of methanol-to-olefins (MTO/MTP), its separation process scheme is suitable for adopting once adopted ethylene unit 50, the sixties used oil absorption extraction technique.
What at present industrialized Shenhua packet header MTO device adopted at home is oily method for absorbing and separating.The method that difference between oil absorption extraction technique and low temperature separation process is mainly to remove hydrogen in gaseous mixture and methane is different.Low temperature separation process is to adopt the method for low temperature fractional condensation and low-temperature fractionation from splitting gas, to separate hydrogen and methane, and required cold condition can reach-90 ℃ following (high pressure demethanizer top temperature reaches-99 ℃, and low-pressure methane removing tower top temperature reaches-134 ℃).Oil-absorption process general using C3, C4, C5 and aromatic fraction absorb carbon two in splitting gas and above hydro carbons and from splitting gas, isolate methane and hydrogen as absorption agent, but required cold condition can be more than-40 ℃, therefore whole device only needs the propylene refrigeration system of-40 ℃ of configurations, refrigeration system is greatly simplified, can be avoided the low-temperature steel that uses low temperature separation process related simultaneously.
But because oil-absorption process adopts the absorption agents of a large amount of circulations, its energy consumption is higher, and in tower top methane, hydrogen cut ethene and propylene loss larger.According to the description about oily absorption techniques in Wang Songhan chief editor's the book such as " ethylene unit technology ", " ethylene process and technology ", the energy consumption of producing 1 ton of alkene oil absorption extraction method is about 1.5 times of Deep Cooling Method, secondly, in methane, hydrogen cut, ethene and propylene loss may be up to 3%～6%, and because cracking temperature is high, produce the diolefine of more easy coking.Therefore, oil-absorption process was almost all replaced by separation by deep refrigeration in the sixties in 20th century.
After the sixties in 20th century, the research to oil-absorption process and improvement are being carried out always.Beijing Chemical Research Institute carries out since 20 century 70s the research that in splitting gas, cold oil absorbs, the middle cold oil absorption techniques of exploitation was so incensed that ethene and propylene mainly for separating of regenerative furnace pyrolysis gas and pyrolysis in tubular furnace at that time, and Changzhou chemical industry factory, Beijing Chemical Factory No. 3 etc. have set up covering device more than 10 at home.This technical matters flow process comprises: cracking, compress, remove sour gas, except alkynes, C3 oil absorbs, C2 cut separates and separates with C3 cut.Its key point is that employing deethanizing column tower reactor carbon three is that main material absorbs C2 and above heavy constituent on absorption tower as absorption agent, isolates the noncondensable gas such as methane, hydrogen, adopts decompressor and ice chest to reclaim the lighter hydrocarbons in tail gas simultaneously.This technology has been done certain improvement to traditional oil-absorption process, the rate of recovery of ethene and propylene improves, the consumption of absorption agent has minimizing to a certain degree, but this technology is main or lean on the Matter Transfer of rear system (at the bottom of deethanizing column) as absorption agent, and energy consumption does not obtain substantial reduction.
The oily absorption extraction technique (ALCET) that Brown & Root proposes, the technique that before adopting, decarburization three front-end hydrogenations and solvent absorbing combine.What absorption agent adopted is take C5 as main absorption agent.This technique decreases with traditional oils absorption technique phase specific energy consumption, but the separation of demethanizing tower mainly relies on circulation absorption agent, and for guaranteeing good alkene specific absorption, the amount of the circulation absorption agent conventionally needing is all larger.
China global chemico chemical construction corporation developed a kind of separating hydrocarbons mixture solvent absorption patent (99122104.4), select a kind of hydrocarbon mixture that is major ingredient by C5 as absorption agent, carry out solvent absorbing and separate.The ALCET oil absorption technique of this method and Brown & Root is similar.In addition, absorption agent is also to lean on Analytic Tower below to parse.
Lee enclose tide and Wang Songhan in the nineties, oil-absorption process having been done to a large amount of research, and the paper that is entitled as " feasibility analysis of oily absorption extraction flow process and evaluation ", the main evaluation index of this paper to oil-absorption process: the assimilated efficiency result of study of energy consumption and alkene has been done disclosure on " ethylene industry ", are delivered in 1999.Its research adopts various absorption agents to comprise that C4, C5, C6, C4 and C5 the solvent mixture, aromatic hydrocarbons are that main solvent has all been done to calculate and research, and has listed the assimilated efficiency of the energy consumption, ethene and the propylene that adopt various absorption agents to draw.According to the conclusion of this paper, alkene assimilated efficiency and the energy consumption of C4 and C5 mixed solvent and C5 solvent are all better.
What current industrialized Shenhua packet header MTO device adopted is the top board that enters demethanizing tower take propane as main absorption agent, C2 and above component are absorbed, its assimilated efficiency is better, but absorption agent consumption is more and absorption agent from subsequent separation system (propylene rectification tower tower reactor), the route of circulation is longer, cause the equipment such as corresponding tower larger, invest high, energy consumption is higher.
Except the oily absorption technique of above-mentioned some that list, in recent years, also have some patent business to be studied the isolation technique of methanol-to-olefins, be substantially absorbed as master with oil, the sub-thread absorption agent that after adopting, systemic circulation is returned absorbs C2 and above heavy constituent.Be that ethane, propane or the ethane/propane mixture that after main absorption agent, Chinese patent 201010607679.2 adopts, systemic circulation is returned made absorption agent as Chinese patent 200780003084.2 adopts carbon four.The absorption agent that these technology adopt substantially all derives from rear system, enters into absorption tower (demethanizing tower) as sub-thread absorption agent.For obtaining higher olefin recovery, all need to guarantee the amount of certain circulation absorption agent, and investment and the energy consumption of the amount of circulation absorption agent on separation system there is larger impact.
Summary of the invention
The present invention is intended to overcome the defect of traditional oils absorption extraction technique and existing lighter hydrocarbons separating technology, and the lower carbon number hydrocarbons separation method of the non-deep cooling that a kind of facility investment is few, energy consumption is low, olefin recovery is high is provided.
The present invention absorbs with traditional oils and existing all kinds of lighter hydrocarbons isolation technique is compared, and its principal feature is:
(1) absorption tower adopts multiply absorption agent, adopts in an embodiment of the present invention two strands of absorption agents, and progressive absorption mode has not only strengthened the assimilation effect of absorption tower (demethanizing tower), has reduced investment and energy consumption simultaneously.
(2) one main absorber of the present invention from before demethanizing tower from splitting gas (or reaction gas) rough segmentation C3, C4 mixture be out the cut the led main absorber as demethanizing tower.This strand of absorption agent itself is fraction mixture to be separated, avoided the increase of the energy consumption that absorption agent mainly brings from rear systemic circulation.
(3) in order further to improve the rate of recovery of alkene, measure smaller absorption agent from depropanizing tower and/or debutanizing tower system for second strand of the present invention, major ingredient is the mixture of the above heavy constituent composition of C4, C5 and C5.The feature of this absorption agent is to go out according to the characteristic optimization of splitting gas (or reaction gas) absorption agent of different proportionings, strengthens the assimilation effect of alkene, reduces energy consumption.
The present invention is mainly used in lower carbon number hydrocarbons and separates, comprise light hydrocarbon cracking, hydro carbons catalyzed reaction, the gaseous mixture of the oxide compound such as alcohol, ether alkene processed separates, the compositing characteristic of its gaseous mixture is the yield of alkene high (take methanol-to-olefins as example, the mass yield of alkene approximately 80%), and generates a certain amount of butylene, produce a small amount of hydrogen, methane, carbon monoxide, carbonic acid gas, other oxide compounds simultaneously, and more than five hydro carbons of a small amount of carbon.After listed different methods preparing low-carbon olefins, gas delivery all can adopt method of the present invention above.Therefore, the present invention only describes with methanol-to-olefins gas separation unit, mainly comprises following steps:
(1) reaction gas of methyl alcohol being produced through catalyzed reaction boosts to 2.0MPaG step by step, is divided into gas-liquid two-phase after cooling, enters respectively dehumidification system and is dried.
(2) dried vapour, liquid phase enter an absorption agent knockout tower, send into the correct position on demethanizing tower top as the main absorber of demethanizing tower from tower reactor or side line extraction using C3, C4 mixture as main cut is cooling.After absorption agent knockout tower top is compressed, cooling compared with lighter-than-air gas, by separating tank isolate vapour, liquid two-phase is removed demethanizing tower as charging.
(3) second of demethanizing tower strand of absorption agent adopts depropanizing tower and/or C4, the C5 of debutanizing tower and above mixture, send into the top of demethanizing tower and further reclaim alkene, this strand of absorption agent can be provided by the self-produced hydrocarbon mixture of rear system, also can be provided by outside.
(4) second of demethanizing tower strand of absorption agent can circulate between demethanizing tower, depropanizing tower and/or debutanizing tower (seeing accompanying drawing 1).Also can parse by Analytic Tower (seeing accompanying drawing 2), between demethanizing tower and Analytic Tower, circulate.
(5) while utilizing two strands of absorption agents to absorb for current methanol-to-olefins gaseous mixture, demethanizing tower can be only with absorption agent, and tower top does not need to arrange the systems such as condenser, return tank, reflux pump again.If but gas composition changes greatly, after improving compared with light constituent content, the systems such as condenser, return tank, reflux pump can be set as required.For the separation of current methanol to olefins reaction gas, when particularly propylene content is high, that demethanizing tower top can not established is conventionally cooling, condensation, return-flow system.
(6) when second of demethanizing tower strand of absorption agent provided by rear systemic circulation mode, demethanizing tower tower reactor material is sent into deethanizing column, isolates carbon two components go ethylene rectification tower rectifying to produce qualified ethylene product through deethanizer overhead.Deethanizing column tower reactor material is sent into depropanizing tower, isolates carbon three components send into propylene rectification tower rectifying and produce qualified propylene product by depropanizing tower tower top.Depropanizing tower tower reactor material is sent into debutanizing tower and is removed carbon four.Depropanizing tower and debutanizing tower remove demethanizing tower (seeing accompanying drawing 1) as second strand of absorption agent above-mentioned after extracting respectively shallow bid material out and mixing according to a certain percentage.
(7) when second of demethanizing tower strand of absorption agent parsed by Analytic Tower, demethanizing tower reactor material is directly sent into Analytic Tower, and one absorption agent that Analytic Tower tower reactor parses is got back to demethanizing tower top after cooling, and rest materials is sent into debutanizing tower.Desorption tower tower top material is sent into deethanizing column, isolates C-2-fraction go ethylene rectification tower to obtain qualified ethylene product by deethanizer overhead, and tower reactor material goes propylene rectification tower to obtain propylene product.(seeing accompanying drawing 2)
Accompanying drawing explanation
Fig. 1: a kind of low-carbon (LC) separation of hydrocarbons and methanol-to-olefins (M-OS/MTO) gas separating technology flow process one, second strand of absorption agent of demethanizing tower is by separating out at depropanizing tower and/or debutanizing tower circulant solution.Wherein, D1: absorption agent knockout tower; D2: demethanizing tower; D3: deethanizing column; D4: depropanizing tower; D5: debutanizing tower.
Fig. 2: a kind of low-carbon (LC) separation of hydrocarbons and methanol-to-olefins (M-OS/MTO) gas separating technology flow process two, second strand of absorption agent of demethanizing tower parses by Analytic Tower.Wherein, D1: absorption agent knockout tower; D2: demethanizing tower; D3: Analytic Tower.
Fig. 3: methanol-to-olefins (MTO) gas separating technology flow implementation illustration.Wherein, D1: absorption agent knockout tower; D2: demethanizing tower; D3: deethanizing column; D4: depropanizing tower; D5: debutanizing tower; D6: ethylene rectification tower; D7: propylene rectification tower.
Embodiment
Be below embodiments of the invention, produce the methanol to olefins reaction gas composition of 600,000 tons of alkene per year as the foundation of charging using certain factory, the wherein ratio of ethene and propylene approximately 1: 1, adopts the technical process of accompanying drawing 3 to separate.Protection scope of the present invention is not limited to following embodiment.
In the present embodiment, the reaction gas that methyl alcohol is produced through catalyzed reaction boosts to 2.0MPaG step by step, is divided into gas-liquid two-phase after cooling, enters respectively dehumidification system and is dried.Dried reaction gas enters in absorption agent knockout tower D1, and absorption agent knockout tower tower top is mainly methane, hydrogen, carbon two and part carbon three, and the main ingredient of tower reactor is carbon three, carbon four and more than four heavy constituent of carbon, is a unintelligible splitter.Absorption agent knockout tower top gaseous phase enters compressor compresses to about 3.2MPaG, then in E3, E4, E5, condense to step by step-21 ℃～-37 ℃ through circulating water, the heat exchange of demethanizing tower tower reactor, propylene refrigerant, gas phase, the liquid phase fluid separated enter demethanizing tower from different position, the middle part of demethanizing tower D2 respectively as the charging of demethanizing tower, absorption agent knockout tower tower reactor liquid phase is cooled to-21 ℃～-37 ℃ through recirculated water and propylene refrigerant, enters into demethanizing tower D2 as absorption agent from demethanizing tower top.
Second strand of absorption agent of demethanizing tower provided by depropanizing tower and debutanizing tower system.Demethanizing tower tower reactor material is sent into deethanizing column D3, and isolating carbon two components through deethanizer overhead, to go ethylene rectification tower D6 rectifying to produce purity be 99.96% ethylene product.Deethanizing column tower reactor material is sent into depropanizing tower D4, isolates carbon three components send into propylene rectification tower D7 rectifying to produce purity be 99.6% propylene product by depropanizing tower tower top.Propylene rectification tower adopts single tower in this embodiment.Depropanizing tower D4 tower reactor material is sent into debutanizing tower and is removed carbon four.Depropanizing tower tower reactor and debutanizing tower tower reactor are extracted separately one material out and are mixed according to a certain percentage as second strand of absorption agent of demethanizing tower and enter from the top of demethanizing tower, utilize the assimilation effect of absorption agent further to reduce the loss of ethene and propylene.
In this embodiment, the main absorber of demethanizing tower is one cut to be separated from absorption agent knockout tower, has compared with prior art greatly reduced the consumption of circulation absorption agent, has reduced corresponding facility investment and energy consumption; And multiply absorption agent has strengthened the assimilated efficiency of alkene, reduce the loss of ethene and propylene; In addition, because absorption agent does not circulate by propylene rectification tower, propylene rectification tower can adopt single tower, has further reduced facility investment.For these reasons, save approximately 10% with existing industrialized 600,000 tons of MTO Olefin Separation Technology phase specific investments, energy consumption saves approximately 5%.The assimilated efficiency of alkene improves 5～10%.The calculation result of the present embodiment is as in table 1.
The calculation result of table 1 embodiment
| Mole composition | D1 charging | D1 charging | D2 charging | D2 charging | Ethylene product | Propylene product |
| H2 | 4.95 | 0.12 | 26.61 | 1.25 | 0.00 | 0.00 |
| C0 | 0.48 | 0.00 | 1.70 | 0.21 | 0.00 | 0.00 |
| 02 | 0.00 | 0.00 | 0.01 | 0.00 | 0.00 | 0.00 |
| N2 | 0.41 | 0.00 | 1.65 | 0.15 | 0.00 | 0.00 |
| CH4 | 5.89 | 0.89 | 13.31 | 3.74 | 0.00 | 0.00 |
| C2H4 | 61.34 | 32.44 | 50.31 | 60.48 | 99.96 | 0.00 |
| C2H6 | 1.02 | 0.77 | 0.66 | 1.15 | 0.04 | 0.01 |
| C3H6 | 22.28 | 45.50 | 5.47 | 30.98 | 0.00 | 99.60 |
| C3H8 | 1.44 | 3.42 | 0.29 | 1.93 | 0.00 | 0.38 |
| C4H6 | 0.04 | 0.32 | 0.00 | 0.00 | 0.00 | 0.00 |
| C4H8 | 1.94 | 12.33 | 0.00 | 0.09 | 0.00 | 0.00 |
| C4H10 | 0.08 | 0.58 | 0.00 | 0.00 | 0.00 | 0.00 |
| C5 and more than | 0.12 | 3.63 | 0.00 | 0.03 | 0.00 | 0.00 |
Claims (3)
1. a methanol-to-olefins gas separating technology flow process, it is characterized in that: demethanizing tower has been selected two strands of different absorption agents, enter from top different positions, and wherein one main absorber is before isolated from demethanizing tower, do not need circulation, comprise the following steps:
(1) compressed, dry, cooled methanol to olefins reaction gas enters an absorption agent knockout tower, from tower reactor or side line extraction take C3, C4 mixture sends into demethanizing tower top correct position as main cut, as the main absorber of demethanizing tower, after absorption agent knockout tower top is compressed, cooling compared with lighter-than-air gas, by separating tank isolate vapour, liquid two-phase is removed demethanizing tower as charging;
(2) another burst of absorption agent main component of demethanizing tower is C4, C5 and above mixture, this strand of absorption agent can be provided by outside, also can extract out from depropanizing tower side line or tower reactor, or extract out from debutanizing tower side line or tower reactor, or provided by a certain percentage by depropanizing tower side line or tower reactor and debutanizing tower side line or tower reactor, alkene is further reclaimed at the top that this strand of absorption agent enters demethanizing tower.
2. a kind of methanol-to-olefins gas separating technology flow process according to claim 1, it is characterized in that: demethanizing tower has two strands of absorption agents, respectively from the hydrocarbon mixture of absorption agent knockout tower and rear system, and enter demethanizing tower from demethanizing tower top different positions respectively.
3. a kind of methanol-to-olefins gas separating technology flow process according to claim 1, it is characterized in that: the source from the absorption agent of rear system is: the mixture of the different proportionings of the material of the material of depropanizing tower side line or tower reactor extraction or debutanizing tower side line or tower reactor extraction or depropanizing tower side line or tower reactor and debutanizing tower side line or tower reactor extraction, this absorption agent can parse from Analytic Tower, also can parse by rear system local circulation.
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| CN102965143B (en) | 2011-09-01 | 2015-01-21 | 富德（北京）能源化工有限公司 | Absorption separation method of cracking gas in low-carbon olefin preparation process |
| CN103467231B (en) * | 2013-08-15 | 2015-02-11 | 上海河图工程股份有限公司 | Process for absorption and recycling of ethylene in olefin reaction products prepared from methanol |
| CN105272812B (en) * | 2014-06-05 | 2017-06-20 | 中国石化工程建设有限公司 | The system and method for ethene is reclaimed in a kind of product gas from preparing propylene from methanol |
| CN106316759B (en) * | 2015-06-24 | 2018-08-24 | 中石化广州工程有限公司 | The separation method of preparing propylene by methanol transformation gas |
| CN106316758B (en) * | 2015-06-24 | 2018-07-27 | 中石化广州工程有限公司 | The separation method of preparing propylene by methanol transformation reaction product |
| CN106316752B (en) * | 2015-06-24 | 2018-08-24 | 中石化广州工程有限公司 | A kind of separation method of preparing propylene by methanol transformation reaction product |
| CN106316757B (en) * | 2015-06-24 | 2018-07-27 | 中石化广州工程有限公司 | The separating technology of preparing propylene by methanol transformation gas |
| CN112760120B (en) * | 2019-11-01 | 2022-04-15 | 中国石化工程建设有限公司 | Oil gas recovery method and device |
| CN112760134B (en) * | 2019-11-04 | 2022-04-12 | 中国石化工程建设有限公司 | Oil gas recovery method and device |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| DD01 | Delivery of document by public notice |
Addressee: Wang Songhan Document name: the First Notification of an Office Action |
|
| ASS | Succession or assignment of patent right |
Owner name: SINOPEC SHANGHAI ENGINEERING CO., LTD. Free format text: FORMER OWNER: WANG SONGHAN Effective date: 20130815 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Chen Minghui Inventor after: Wang Songhan Inventor after: Zhou Ying Inventor after: Zhang Hong Inventor after: Shao Yufang Inventor after: He Kun Inventor after: Li Li Inventor after: Pei Xuemei Inventor before: Wang Songhan Inventor before: Li Li Inventor before: Pei Xuemei |
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| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 100101 CHAOYANG, BEIJING TO: 200120 PUDONG NEW AREA, SHANGHAI Free format text: CORRECT: INVENTOR; FROM: WANG SONGHAN LI LI PEI XUEMEI TO: CHEN MINGHUI WANG SONGHAN ZHOU YING ZHANG HONG SHAO YUFANG HE KUN LI LI PEI XUEMEI |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20130815 Address after: 200120 Galaxy Building, 769 Zhang Yang Road, Shanghai, Pudong New Area Applicant after: SINOPEC Shanghai Engineering Company Limited Applicant after: Beijing Maxstone Petrochemical Engineering Co., Ltd. Address before: 100101 Beijing City, Chaoyang District Road No. 10 Xiaoying Yangming Plaza South 16B1 Applicant before: Wang Songhan Applicant before: Beijing Maxstone Petrochemical Engineering Co., Ltd. |
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| DD01 | Delivery of document by public notice |
Addressee: Li Li Document name: Notification of Passing Examination on Formalities |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |