CN102351629B - Method for producing propylene and high-octane gasoline from methanol - Google Patents
Method for producing propylene and high-octane gasoline from methanol Download PDFInfo
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- CN102351629B CN102351629B CN2011102425498A CN201110242549A CN102351629B CN 102351629 B CN102351629 B CN 102351629B CN 2011102425498 A CN2011102425498 A CN 2011102425498A CN 201110242549 A CN201110242549 A CN 201110242549A CN 102351629 B CN102351629 B CN 102351629B
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Abstract
The invention discloses a method for producing propylene and high-octane gasoline from methanol, which comprises steps as follows: methanol and water pass through an olefin preparation reactor and enters a deethanizing column; the separated C3+ material enters a depropanizing column, the separated C3 material enters a rectifying column, and the separated C4+ material enters an etherification reactor; the rectifying column separates out propane and propylene; the C4+ material enters the etherification reactor to react with methanol, the generated etherified gasoline is discharged out of the device, the unreacted C4+ material and C2 and C2- components are mixed to recoincide for dehydrocyclization; and the materials after reaction are separated to obtain dry gas, liquefied petroleum gas and a liquid material containing rich aromatic hydrocarbons. On the premise of obtaining high propylene yield, the byproduct containing rich olefins are subjected to etherification and coincidence dehydrocyclization reaction to coproduce the high-octane gasoline blended component; and the invention has the advantages of obvious economic benefit, simple overall process and low investment.
Description
Technical field
The present invention relates to a kind of method of utilizing methanol production propylene and stop bracket gasoline blend component.Especially when methyl alcohol generated propylene by catalyst reaction, utilization other reaction product except propylene carries out etherificate and the process that generates the stop bracket gasoline blend component is reacted in superimposed dehydrocyclization.
Background technology
Propylene is one of most important basic organic that is only second to by ethene, and its maximum purposes is to produce polypropylene, accounts for 52%.According to CMAI, global propylene demand year rate of rise has substantially exceeded ethene in recent years, and the major cause of propylene supply rapid growth is due to due to the rapid growth of the polyacrylic demand of derivative.In short supply due to the China's oil resource, utilize petroleum path to produce propylene and can not meet needs far away, and the propylene demand gap is very large, has had influence on the development of downstream chemical industry.Coal resources in China is relatively abundant, utilizes abundant coal to produce low-carbon alkene to China organic chemical industry sustainable development, and the energy safety of supply has great strategic importance.The olefin hydrocarbon making by coal technology is take coal as raw material, through technological processs such as gasification, synthesising gas systeming carbinol, methanol-to-olefins, wherein for representative be methanol-to-olefins technology (MTO) and preparing propylene from methanol technology (MTP), this two core technologies that technology is olefin hydrocarbon making by coal at present.
The methanol-to-olefins technology can be widened the propylene feedstocks channel, adjust raw material mix, reduces the dependence to petroleum resources.At present, the Industrial demonstration device that this technology is checked and approved through country has one, Shenhua Group MTO project, and the provincial project of checking and approving has two, is respectively the MTP project of Shenhua Ningxia Coal Industry Group and Datang derived energy chemical company limited.Various places have 28 (incomplete statistics) according to statistics in the project of planning, and the market temperature is very high.The technology that the methanol-to-olefins technology possesses industrialized condition has the MTO technique of UOP/Hydro company, Chinese Academy of Sciences's Dalian compound DMTO technique and oil of SPC research institute SMTO technology.The MTP technique that Lurgi is arranged of preparing propylene from methanol technical development maturation, the circulating fluidized bed preparing propylene from methanol FMTP technology of Tsing-Hua University.Wherein Lurgi company, the Dalian Chemistry and Physics Institute of Chinese Academy of Sciences Industrial demonstration device are driven, and Tsing-Hua University is just at the building industry testing apparatus.Under the level of soaring oil prices, MTO and MTP technique have the low economic advantages of cost than steam cracking and catalytic cracking volume increase propylene technique processed.
Oxygen-containing organic compound take methyl alcohol as representative comes the patent of process aspect of preparing ethylene and propylene a lot.
Chinese patent 96115333.4 has been introduced a kind of by methyl alcohol or dme preparing ethylene, the method of the low-carbon alkenes such as propylene adopts the SAPO-34 molecular sieve catalyst, carries out the method that this reacting middle catalyst continuous circulation reacts and regenerates on the ciculation fluidized reaction unit of dense bed;
Chinese patent 99815451.2 has been introduced by the reaction that continues-regeneration occurs on the micro-spherical catalyst based on the SAPO-34 zeolite, in fluidized-bed reactor-regenerator system, methanol conversion one-tenth is had the 93-100% degree of conversion and greater than 90% C optionally
2-C
4The method of low-molecular olefine;
Chinese patent 01144188.7 is a kind of processing method by dme or preparing low carbon olefin hydrocarbon with methanol and system thereof, and this process using silicoaluminophosphamolecular molecular sieves (SAPO-34), as catalyzer, utilizes gas-solid cocurrent flow descending formula fluidized-bed super short contact time reactor.By processing method and the system of using this invention, reduced the generation of by product alkane, reduce the difficulty of follow-up separation process, and then increased the output of product low-carbon alkene.
It is a kind of take methyl alcohol or/and dme is the method for waste low-carbon alkene that Chinese patent 200710064232.3 provides, the method is characterized in that methyl alcohol or/and dme is divided into three reaction zone feeds by a certain percentage, the ratio by regulating three reaction zone feeds and the reaction conditions of each reaction zone obtain required olefin product and distribute.
Chinese patent 200710037232.4 relates to a kind of method of methyl alcohol or dimethyl ether conversion producing light olefins, mainly solves the make charcoal problem of the bad control of degree, the bad assurance of catalyst in reactor average activity level of revivifier in prior art.
Chinese patent 200710037234.3 relates to a kind of method that improves selectivity of light olefin in methyl alcohol or dimethyl ether conversion process, mainly solves the lower problem of selectivity of light olefin in existing methanol-to-olefins technology.
Chinese patent 200480022527.9 provides and has been used for from comprising ethane, ethene, propylene, dme, and the effective separation method of novel high and the system of separation of polymeric level ethene and propylene in one or more the initial flow discharging stream in propane, acetylene, methylacetylene, propadiene, methane, hydrogen, carbon monoxide, carbonic acid gas and C4+ component.
The separation method that China 200610017775.5 discloses a kind of converting methanol to prepare low carbon olefin (DMTO) gas, the characteristics that form for DMTO gas, improve the flow process after four sections compressions in conventional front-end deethanization separation process.According to the present invention, arrange between five sections compressions and deethanizing column return tank and add the hydrogen-oxygen conversion, remove the oxygen that produces in acetylene and reaction regeneration process, material after condensing cooling is through the deethanizing column return tank, liquid phase refluxes as deethanizing column, and gas phase enters deep cooling demethanizing system, and material is after condensing cooling, do not need to arrange the front dehydrogenation system of loaded down with trivial details ice chest, directly enter high pressure demethanizer.Adopt the present invention to separate DMTO gas and can obtain Recovery rate of ethylene more than 99.5%.
To sum up patent is described, what relate generally to is that methanol conversion is catalyst research, reactor improvement, the optimization of process conditions that improves olefins yield and the improvement of product separation flow process of low-carbon alkene, prior art is with the further cracking of these components, be converted into propylene, to improve Propylene Selectivity and productive rate.Do not have and about utilization other reaction product except propylene, carry out the integrated patent of method of utilizing.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of utilizing methanol production propylene and stop bracket gasoline, the improved integrated flow that is generated propylene by methyl alcohol can be provided, particularly optimize methyl alcohol and generate integrated work flow and the scheme of the comprehensive utilization of by product after propylene.
In order to realize purpose of the present invention, a kind of method idiographic flow of methanol production propylene and stop bracket gasoline that utilizes of the present invention is:
(1), methyl alcohol and water charge ratio are 1.0～5.0(weight), by the beds of olefin hydrocarbon reactor processed olefine reaction processed, type of reactor is fixed-bed reactor, catalyzer is that ZSM-5 molecular sieve is the bar shaped catalyst of active ingredient, 400～600 ℃ of temperature of reaction, reaction pressure 0.1～2.0MPa, methyl alcohol weight space velocity are 0.5～5.0h
-1(weight), enter deethanizing column by the reaction product after olefin hydrocarbon reactor processed;
(2), enter deethanizing column from the reaction product of step (1) and separate, isolate material and be C2 and less than C2 component and C3
+Material, wherein C3
+Material goes out deethanizing column and enters depropanizing tower;
(3), from the C3 of step (2)
+Material enters depropanizing tower, isolates C3 material and C4
+Material, wherein isolated C3 material enters rectifying tower, isolated C4
+Material enters the etherification reaction device;
(4), from the C3 material of step (3), enter rectifying tower, isolate propane and propylene, these two kinds of materials go out respectively device; Purified propylene after rectifying can be adjusted as required, for example can reach the polymerization-grade standard, and propane weight purity can reach 90～99%;
(5), from the C4 of step (3)
+Material enters etherification reaction device and methyl alcohol reaction, and the etherified gasoline that reaction generates goes out device, has neither part nor lot in the C4 of reaction
+Material reenters superimposed dehydrocyclization device; Etherification reaction temperature is 60～80 ℃, and reaction velocity is 3.0～5.0h
-1(weight), reaction pressure are 0.50～1.0MPa;
(6), from having neither part nor lot in the C4 of reaction in step (5)
+Material and from step (2) material C2 and less than the C2 component, be mixed into superimposed dehydrocyclization reaction unit, carry out superimposed dehydrocyclization reaction, and reacting rear material is separated, and obtains dry gas, liquefied petroleum gas (LPG) and be rich in the liquid material of aromatic hydrocarbons; Superimposed dehydrocyclization temperature of reaction is that 350～450 ℃, reaction velocity are 0.5～2.0h
-1(weight), reaction pressure are 0.1～0.5 MPa.
It is 50～70% product liquid that reaction can obtain total aromaticity content, and in liquefied petroleum gas (LPG), propane content is 70～85%(weight).
Described olefin hydrocarbon apparatus catalyzer processed is the catalyzer take ZSM-5 molecular sieve as active ingredient, and this ZSM-5 belongs to high silica alumina ratio series.
Production propylene of the present invention and stop bracket gasoline flow process, its etherification reaction is identical with conventional etherification reaction, and the structure of reactor pattern is also identical with catalyzer with the etherification reaction device reaction type formula of routine with catalyzer.Concrete, described etherification reaction device, its reactor can be fixed-bed reactor, catalyzer can be Zeo-karb, molecular sieve, solid super-strong acid or the sulfuric acid catalyst of the etherification reaction of routine.
Concrete, described superimposed dehydrocyclization device, its reactor is fixed-bed reactor, catalyzer is that zeolite molecular sieve is the bar shaped catalyst in active centre.More specifically, this catalyzer is the commercial catalyst take the low silica-alumina ratio ZSM-5 molecular sieve as active ingredient, the Sinopec catalyst Co.
SKP-2Catalyzer.
Further concrete, in above-mentioned steps (5), the alfin ratio of reaction raw materials methyl alcohol/iso-butylene (mol/mol) is take 1.0～1.1 as best.
The described C2 material of this patent, C2 component, refer to that carbon atom number is 2 hydrocarbon component.
The described C3 of this patent
+Material, C3
+Component, refer to that carbon atom number is more than or equal to the hydrocarbon component of 3.
The described C4 of this patent
+Material, C4
+Component, refer to that carbon atom number is more than or equal to the hydrocarbon component of 4.
The above-mentioned steps flow process, the liquefied petroleum gas (LPG) mixing of materials that generates in the propane material that wherein separates in step (4) and step (6), can be used as motor liquified gas.What wherein in step (5), in reaction generation etherified gasoline and step (6), superimposed dehydrocyclization generated is rich in the arene liquid material through mixing, and can be used as the stop bracket gasoline blend component.
The main products that the present invention is based on methanol conversion and be propylene technique is propylene, while by-product fuel gas, liquefied petroleum gas (LPG) and petroleum naphtha (C5～C7), wherein be rich in ethene in fuel gas, be rich in C 4 olefin (especially iso-butylene is main) in liquefied petroleum gas (LPG), petroleum naphtha is rich in alkene (especially isopentene and dissident's alkene are main).This part by product that is rich in alkene can utilize machinery to process, and produces the stop bracket gasoline blend component to improve its added value.The machinery that relates generally to is that fuel gas advances superimposed dehydrocyclization device and generates the high component that contains aromatic hydrocarbons, liquefied petroleum gas (LPG) and petroleum naphtha enter ether-based device and the methyl alcohol reaction generates etherified gasoline, after etherificate, liquefied petroleum gas (LPG) enters the high component that contains aromatic hydrocarbons of the same generation of superimposed dehydrocyclization device, can be used as the stop bracket gasoline blend component after these three kinds of resultant of reaction material mix.
This patent is by the improvement of reaction process, in the situation that each device that relates to has maturing appts,, on guaranteed basis on product yield, several products of existing apparatus are comprised that in dry gas, liquefied gas, olefin component is reprocessed, form a new technical process.When obtaining high productivity of propylene, the by product that is rich in alkene can coproduction stop bracket gasoline blend component by etherificate, superimposed dehydrocyclization reaction, remarkable in economical benefits, whole flow process simply, less investment.
Description of drawings
Fig. 1 is the schematic flow sheet that utilizes methanol production propylene and stop bracket gasoline blend component.
In figure, 1, methyl alcohol, 2, the preparing propylene from methanol device, 3, deethanizing column, 4 ,≤the C2 component, 5, C3
+Component, 6, depropanizing tower, 7, the C3 rectifying tower, 8, C4
+Component, 9, the etherification reaction device, 10, C4 after etherificate
+Component, 11, superimposed dehydrocyclization device, 12, propylene, 13, propane, 14, dry gas, 15, motor liquified gas, 16, the stop bracket gasoline blend component.
Embodiment
Embodiment 1
As shown in Figure 1, raw material 1 and water access to plant 2 react, and processing condition are 400～600 ℃ of temperature of reaction, and reaction pressure 0.1～2.0MPa, methyl alcohol weight space velocity are 0.5～5.0h
-1(weight), catalysts is that high silica alumina ratio ZSM-5 is active constituent catalyst, reacting rear material enters 3, here the material 4 that forms of C2 and lighter gaseous fraction is transferred to and is entered follow-up device 11 and carry out superimposed dehydrocyclization reaction from tower top, and temperature of reaction is that 350～450 ℃, reaction velocity are 0.5～2.0h
-1(weight), reaction pressure is 0.1～0.5 Mpa, and catalysts is the Sinopec catalyst Co.
SKP-2Catalyzer, principal reaction material are ethene; Be admitted to device 6 from installing 3 bottoms material 5 out; The C3 component is left access to plant 7 from tower top, and the propylene of recovered overhead polymerization-grade, propane are incorporated follow-up material 15 pipe networks into.Comprise C4 hydro carbons and other heavier components from installing 6 bottoms material 8 out, this component and methyl alcohol access to plant 9 together carry out etherification reaction, and etherification reaction temperature is 60～80 ℃, and reaction velocity is 3.0～5.0h
-1(weight), reaction pressure are 0.50～1.0Mpa, and catalyzer can be Zeo-karb, molecular sieve, solid super-strong acid or the sulfuric acid catalyst of the etherification reaction of routine.In material, the etherification reaction of isomeric olefine and methyl alcohol generates etherified gasoline, part unreacted material 10 accesss to plant 11 carry out superimposed dehydrocyclization reaction, and after etherification reaction, gasoline and superimposed dehydrocyclization device high aromatic hydrocarbon content product liquid out mix rear component material 16.Material enters the fuel gas pipe network at the materials 14 that device 11 carries out producing after superimposed dehydrocyclization reaction, device 11 reactions produce liquefied petroleum gas (LPG) and device 7 materials that the separate 13 rear materials 15 of mixing as motor liquified gas.
After preparing propylene from methanol series of optimum reaction process, reaction product is dry gas, propylene, motor liquified gas, the stop bracket gasoline blend component, after the preparing propylene from methanol reaction, by product is fully used, added value is higher, remarkable in economical benefits of the present invention, whole flow process is simple, less investment, is the desirable integrated work flow of preparing propylene from methanol.
Table 1: the difference (raw material is methyl alcohol) of conventional MTP flow process and this integrated flow
Claims (4)
1. method of utilizing methanol production propylene and stop bracket gasoline is characterised in that idiographic flow is:
(1), methyl alcohol is 1.0～5.0 with water feed weight ratio, by the beds of olefin hydrocarbon reactor processed olefine reaction processed, type of reactor is fixed-bed reactor, catalyzer is that ZSM-5 molecular sieve is the bar shaped catalyst of active ingredient, 400～600 ℃ of temperature of reaction, reaction pressure 0.1～2.0MPa, methyl alcohol weight space velocity are 0.5～5.0h
-1, by the reaction product after olefin hydrocarbon reactor processed, enter deethanizing column;
(2), enter deethanizing column from the reaction product of step (1) and separate, isolate material and be C2 and less than C2 component and C3
+Material, wherein C3
+Material goes out deethanizing column and enters depropanizing tower;
(3), from the C3 of step (2)
+Material enters depropanizing tower, isolates C3 material and C4
+Material, wherein isolated C3 material enters rectifying tower, isolated C4
+Material enters the etherification reaction device;
(4), from the C3 material of step (3), enter rectifying tower, isolate propane and propylene, these two kinds of materials go out respectively device;
(5), from the C4 of step (3)
+Material enters etherification reaction device and methyl alcohol reaction, and the etherified gasoline that reaction generates goes out device, has neither part nor lot in the C4 of reaction
+Material reenters superimposed dehydrocyclization device; Etherification reaction temperature is 60～80 ℃, and the reaction weight space velocity is 3.0～5.0h
-1, reaction pressure is 0.50～1.0 MPa;
(6), from having neither part nor lot in the C4 of reaction in step (5)
+Material and from step (2) material C2 and less than the C2 component, be mixed into superimposed dehydrocyclization reaction unit, carry out superimposed dehydrocyclization reaction, and reacting rear material is separated, and obtains dry gas, liquefied petroleum gas (LPG) and be rich in the liquid material of aromatic hydrocarbons; Superimposed dehydrocyclization temperature of reaction is that 350～450 ℃, reaction weight space velocity are 0.5～2.0h
-1, reaction pressure is 0.1～0.5 MPa;
Described olefin hydrocarbon apparatus processed, its reactor are fixed-bed reactor, and catalyzer is the high silica alumina ratio catalyzer take ZSM-5 as active ingredient;
Described etherification reaction device, its reactor are fixed-bed reactor, and catalyzer is Zeo-karb, molecular sieve, solid super-strong acid or the sulfuric acid catalyst of etherification reaction;
The reactor of superimposed dehydrocyclization device is fixed-bed reactor, and catalyzer is that zeolite molecular sieve is the metal-modified bar shaped catalyst of process in active centre.
2. a kind of method of utilizing methanol production propylene and stop bracket gasoline according to claim 1, it is characterized in that: etherification reaction temperature is 60～80 ℃, the reaction weight space velocity is 3.0～5.0h
-1
3. a kind of method of utilizing methanol production propylene and stop bracket gasoline according to claim 1, is characterized in that, it is characterized in that: superimposed dehydrocyclization temperature of reaction is that 350～450 ℃, reaction weight space velocity are 0.5～2.0h
-1
4. a kind of method of utilizing methanol production propylene and stop bracket gasoline according to claim 1, it is characterized in that: the metallic element method of modifying is for employing is saturated or the solubility salt is flooded in supersaturation, will adopt the method for precipitation to deposit metal on molecular sieve, by roasting, metal is fixed on molecular sieve again after drying, reaches the modification to molecular sieve.
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| CN103242884B (en) * | 2013-05-20 | 2015-04-08 | 易高环保能源研究院有限公司 | Process for preparing high-octane high-cleanness gasoline with methanol by using multi-element catalysis method |
| CN105254462B (en) * | 2015-11-03 | 2018-06-29 | 中国石油大学(华东) | A kind of technique of methanol-to-olefins co-production gasoline and aromatic hydrocarbons |
| CN108404983B (en) * | 2018-03-23 | 2020-08-04 | 华东师范大学 | Preparation and application of ordered mesoporous phenolic resin polymer supported silver catalyst |
| CN110157480B (en) * | 2019-05-10 | 2021-04-20 | 国家能源投资集团有限责任公司 | Value-added utilization method of high-carbon byproduct in process of preparing propylene from coal-based methanol and application of value-added utilization method |
| CN114907178B (en) * | 2021-02-07 | 2024-09-27 | 中国石油天然气股份有限公司 | Method for producing C2-C3 olefin and high-octane gasoline blending component by using C4-C6 hydrocarbon as raw material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4826507A (en) * | 1987-12-08 | 1989-05-02 | Mobil Oil Corporation | Integrated etherification and oxygenates to gasoline process |
| CN101333461A (en) * | 2008-03-25 | 2008-12-31 | 北京惠尔三吉绿色化学科技有限公司 | Method for producing cleaning fuel oil form petroleum cracking dry gas and C4 component |
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|---|---|---|---|---|
| DE102009032915A1 (en) * | 2009-07-14 | 2011-03-31 | Lurgi Gmbh | Process and plant for the production of synthetic fuels |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4826507A (en) * | 1987-12-08 | 1989-05-02 | Mobil Oil Corporation | Integrated etherification and oxygenates to gasoline process |
| CN101333461A (en) * | 2008-03-25 | 2008-12-31 | 北京惠尔三吉绿色化学科技有限公司 | Method for producing cleaning fuel oil form petroleum cracking dry gas and C4 component |
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