CN105087041A - Bifunctional catalyst-based short-process Fischer-Tropsch synthesis novel oil preparation process - Google Patents
Bifunctional catalyst-based short-process Fischer-Tropsch synthesis novel oil preparation process Download PDFInfo
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Abstract
The invention discloses a bifunctional catalyst-based short-process Fischer-Tropsch synthesis novel oil preparation process. The process comprises the steps: desulfurating and purifying coarse synthesis gas prepared by taking coal, natural gas or biomass as raw materials, and then adjusting the coarse synthesis gas to raw material synthesis gas with a proper H2/CO molar ratio through a water coal gas shift reaction; and feeding the raw material synthesis gas into a reactor for Fischer-Tropsch synthesis reaction in the presence of the bifunctional catalyst, separating the raw material synthesis gas to directly obtain a gasoline component with a high octane number, reforming methane steam, recovering hydrogen and low carbon hydrocarbon by treating tail gas, and carrying out wastewater treatment after removing alcohol substances from synthetic water, wherein the used catalyst is the bifunctional catalyst which comprises two parts: a molecular sieve and a metal active component, and the metal active component is embedded into a molecular sieve crystal. The Fischer-Tropsch synthesis oil preparation novel process provided by the invention can be used for directly obtaining gasoline which meets the purity and yield requirements with the high octane number through a one-step process, so that integration of Fischer-Tropsch synthesis reaction and product refining is realized, and the process is of great practicality and economical benefits.
Description
Technical field
The present invention relates to a kind of F-T synthesis oil-producing technique, relate to a kind of short route F-T synthesis new technology to prepare oil based on dual-function catalyst particularly.
Background technology
Along with the fast development of economy and improving constantly of people's living standard, the demand of countries in the world to processed oil increases sharply, and contradiction between oil supply and demand becomes increasingly conspicuous, the concussion of an International Crude Oil high position.Within the scope of our times, fuel oil obtains mainly through petroleum path, and prospective oil, produced quantity reduce gradually, and oil quality is progressively tending towards heaviness, in poor quality.In addition, along with increasingly sharpening of problem of environmental pollution, international and domestic environmental regulation is more and more stricter to the environmental protection standard of petroleum chemical industry, and for producing the oil product meeting environmental requirement, the benefit of refining of petroleum is subject to great effect, and production cost increases increasingly.Under these circumstances, countries in the world all utilize the Non oil-based route of Oil Production at active development, to slow down depending on unduly petroleum resources.In the fossil resources distribution of China, petroleum resources critical shortage, but the motor spirit of China about 80% is produced by the catalytic cracking process in petroleum refining industry, therefore needs a large amount of imported crude oil every year.On the other hand, the coal of China and natural gas reserves then relative abundance, strengthens the effective utilization to these resources, has great strategic significance to the sustainable development of China's economy and the safety control of power supply.At present, the non-oil resources such as coal, Sweet natural gas, biomass are converted into synthetic gas, then receive worldwide extensive attention and research via the indirect route producing liquefied hydrocarbon of F-T synthesis (Fischer-Tropschsynthesis).
Nineteen twenty-three, Germany scientist FransFischer and HansTropsch has invented Fischer-Tropsch synthesis method, through the development of nine more than ten years, has worldwide had some industrialized production equipments at present.The metal with F-T synthesis activity has Fe, Co, Ni, Ru etc., Ru due to reserves limited, expensive, be unsuitable for industrial applications; And though Ni activity is higher, primary product is methane, and easily forms volatilizable nickle carbonoxide under high pressure, and loss of active component is serious.Therefore current most study and what realize industrial applications is that Fe is catalyst based and Co is catalyst based.Compared to conventional petroleum derivative, in the liquid fuel that F-T synthesis is produced, the content of the material such as sulphur, nitrogen, aromatic hydrocarbons is extremely low, can meet the requirement of fuel spatter property.But F-T synthesis is a very complicated reaction system, and product species is various, obey Anderson-Schulz-Flory (ASF) regularity of distribution, all selective restriction of each cut, such as the theoretical selectivity of gasoline section cut hydrocarbon is only 48%.In addition, for synthetic gasoline process, according to the chainpropagation mechanism of product, F-T synthesis mainly forms straight-chain paraffin, and in product, the content of isoparaffin is lower, therefore directly can not be obtained the gasoline conformed to quality requirements by traditional Fischer-Tropsch synthesis.The main method that current technique adopts carries out corresponding post-treatment refinement treatment to Fischer-Tropsch synthesis oil, to obtain satisfactory processed oil, such as to synthetic oil application hydrocracking and isomerization process process, generate longer-chain hydrocarbons converting compounds can be made to be short chain normal paraffin or isoparaffin, to obtain the gasoline component that octane value is higher.Industrialized Fischer-Tropsch synthesis process process can be divided into synthetic gas preparation, Fischer-Tropsch synthesis and product purification three parts.The technical process of common with coal is raw material is mainly: first coal is obtained crude synthesis gas via vapourizing furnace gasification, crude synthesis gas first carries out desulfurization, scavenging process, is adjusted to H afterwards via water gas shift reaction
2the material synthesis gas that/CO mol ratio is suitable; Material synthesis gas enters reactor and carries out Fischer-Tropsch synthesis, is separated afterwards and obtains hydrocarbon compound, and produce a large amount of synthesis tail gas and water etc.; Products therefrom delivers to the product processing device in downstream, obtains the hydrocarbon fuel such as gasoline through follow-up refining process; Methane steam reforming, tail gas is recover hydrogen and low-carbon (LC) hydro carbons after treatment, and synthetic water carries out wastewater treatment after removing alcohols material.Fischer-Tropsch synthesis process process is very huge as can be seen here, needs the supporting technologies such as various post-treatment process.
The acid catalysis function of molecular sieve and the metal active centres of F-T synthesis are carried out effectively composite, single stage method can directly obtain the liquid fuel of composite quality requirement.At present, the research method reported mainly contains three kinds: (1) take acidic molecular sieve as support of the catalyst, dipping Fischer-Tropsch metal active constituent; (2) traditional fischer-tropsch synthetic catalyst and molecular sieve are carried out physical mixed; (3) molecular screen membrane is coated on fischer-tropsch synthetic catalyst, prepares molecular screen membrane coated catalyst.Although this several method can change the products distribution of F-T synthesis to a certain extent, but these catalyzer all fail fully to realize the synergy at acid catalysis function and fischer-tropsch activity center, the problems such as ubiquity catalytic activity is low, deactivation rate fast, methane and carbon dioxide selectivity is high, cannot be applied in industrialization actual procedure.
Chinese Patent Application No. 201210509729.2, " active ingredient nano particle embeds the catalyzer of crystallization of molecular sieves, method and application " discloses the catalyzer that a kind of active ingredient nano particle embeds crystallization of molecular sieves, comprise metal active constituent nano particle and molecular sieve, described metal active constituent nano particle embeds and is dispersed in molecular sieve, described metal active constituent nano particle in the catalyst content is 2 ~ 70wt%, active metal nano particle diameter is 4 ~ 200nm, and zeolite crystal size is 1 ~ 10 μm; Its preparation method is also disclosed in patent.In described catalyzer, metal active centres and acid site can effectively be mated, and heavy constituent product can effectively cracking; Molecular sieve can not break because of the difference of coefficient of thermal expansion, and physical strength is high.Catalytic activity is high, metallic reducing degree is high, methane selectively is low; Do not reduce fischer-tropsch reaction activity; Preparation process is simple, and cost is low.But this patent does not relate to the embody rule of this catalyzer in Fischer-Tropsch synthesis.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of short route F-T synthesis new technology to prepare oil based on dual-function catalyst, carries out integrated optimization, particularly improve product purification process traditional method.
For solving the problems of the technologies described above, the present invention adopts following technical proposals:
Based on a short route F-T synthesis new technology to prepare oil for dual-function catalyst, comprise the steps:
(1) by being that the crude synthesis gas that raw material obtains first carries out desulfurization, scavenging process by coal, Sweet natural gas or biomass, H is adjusted to via water gas shift reaction afterwards
2the material synthesis gas that/CO mol ratio is suitable;
(2) material synthesis gas enters reactor, carries out Fischer-Tropsch synthesis, directly obtain high-octane gasoline component after separation under dual-function catalyst exists;
(3) methane steam reforming, tail gas is recover hydrogen and low-carbon (LC) hydro carbons after treatment, and synthetic water carries out wastewater treatment after removing alcohols material;
Described dual-function catalyst has damascene structures, and comprise molecular sieve and metal active constituent two portions, wherein active metal nano particle is firmly embedded in crystallization of molecular sieves inside, and structure properties is excellent.
Preferably, the active ingredient of described dual-function catalyst is one or both in following active ingredient: Fe, Co.
Preferably, the addible auxiliary agent of described dual-function catalyst is one or more in following auxiliary agent: Zr, Mg, Ni, Mn, Cu, Ti, Ag, Mo, Zn, Ru, Pt, Pd, Rh, Ce.
Preferably, the molecular sieve of described dual-function catalyst is one or more in following molecular sieve: HZSM-5 molecular sieve, H beta-molecular sieve, MCM-41 molecular sieve, HMS molecular sieve, MCM-22 molecular sieve, SAPO-34 molecular sieve, HY molecular sieve, SBA-15 molecular sieve, TS-1 molecular sieve.
Preferably, described reactor adopts fixed-bed reactor, fluidized-bed reactor or paste state bed reactor.
Preferably, in described material synthesis gas, H
2/ CO mol ratio is 2 ~ 5 ︰ 1.
Beneficial effect of the present invention is as follows:
1, short route F-T synthesis new technology to prepare oil of the present invention, optimize traditional method, significantly simplify Fischer-Tropsch synthesis process process, integrated optimization has been carried out to whole set process flow process, provide a kind of Fischer-Tropsch synthesis process of simplification, eliminate the following process treating process of Fischer-Tropsch synthetic, as hydrocracking, isomerization etc.Achieve the integration of Fischer-Tropsch synthesis and product purification, single stage method can directly obtain the clean gasoline fuel meeting purity and yield requirement, hardly containing sulphur, nitrogen, aromatic hydrocarbons in products obtained therefrom gasoline.The stop bracket gasoline obtained both can directly as finished fuels oil, also can as gasoline blending component, complementary with other gasoline products.Fischer-Tropsch synthesis method of the present invention considerably reduces facility investment, power consumption and process cost, improves the production efficiency of reaction process, has very large practicality and economy.
2, short route F-T synthesis new technology to prepare oil of the present invention, based on a kind of dual-function catalyst, preferably there is the dual-function catalyst of damascene structures, effective coupling of molecular sieve acid catalysis function and active ingredient fischer-tropsch reaction function can be realized, the acid catalysis character of the hydrocarbon polymer that active ingredient generates by molecular sieve excellence and the further reaction and separation processes of pore passage structure of high-sequential, this synergy can realize the coupling of polystep reaction process, directly obtains high-octane gasoline component.And all right absorption reaction liberated heat of scission reaction, slow down the deactivation rate of catalyzer; This catalyst structure excellent performance, reactive behavior is high, and preparation process is simple, and stability is good, and physical strength is high, and suitability for mass industrializedization is applied.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 illustrates typical Fischer-Tropsch synthesis process schema.
Fig. 2 illustrates the short route F-T synthesis new technology to prepare oil schema based on dual-function catalyst.
Embodiment
In order to be illustrated more clearly in the present invention, below in conjunction with preferred embodiments and drawings, the present invention is described further.Parts similar in accompanying drawing represent with identical Reference numeral.It will be appreciated by those skilled in the art that specifically described content is illustrative and nonrestrictive, should not limit the scope of the invention with this below.
Embodiment 1
A kind of short route F-T synthesis new technology to prepare oil based on dual-function catalyst, comprise the steps: that (1) is by being that the crude synthesis gas that raw material obtains first carries out desulfurization, scavenging process by coal, Sweet natural gas or biomass, is adjusted to H via water gas shift reaction afterwards
2/ CO mol ratio is the material synthesis gas of 2 ~ 5 ︰ 1; (2) material synthesis gas enter reactor dual-function catalyst exist under carry out Fischer-Tropsch synthesis, directly obtain high-octane gasoline component after separation; (3) methane steam reforming, tail gas is recover hydrogen and low-carbon (LC) hydro carbons after treatment, and synthetic water carries out wastewater treatment after removing alcohols material; Wherein selected catalyzer is the Co/HZSM-5 dual-function catalyst with damascene structures, and metal active constituent Co is embedded in HZSM-5 molecular sieve, is applied to Fischer-Tropsch synthesis.This F-T synthesis new technology to prepare oil end reaction the results are shown in Table 1.
The transformation efficiency of table 1CO and each matter selective
αiso-C
5-C
12for C
5-C
12the selectivity of middle isoparaffin.Known according to table 1, embodiment 1 Fischer-Tropsch synthesis method used can directly obtain the gasoline products conformed to quality requirements, and considerably reduces facility investment, power consumption and process cost, improves production efficiency and the economy of reaction process.
Embodiment 2
Repeat embodiment 1, its difference is only: select the Co-Zr/HZSM-5 dual-function catalyst with damascene structures, and metal active constituent Co and auxiliary agent Zr is embedded in HZSM-5 molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 3
Repeat embodiment 1, its difference is only: select the Co/H β dual-function catalyst with damascene structures, metal active constituent Co is embedded in H beta-molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 4
Repeat embodiment 1, its difference is only: select the CoZr/H β dual-function catalyst with damascene structures, metal active constituent Co and auxiliary agent Zr is embedded in H beta-molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 5
Repeat embodiment 1, its difference is only: select the FeMn/HZSM-5 dual-function catalyst with damascene structures, and metal active constituent Fe and auxiliary agent Mn is embedded in HZSM-5 molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 6
Repeat embodiment 1, its difference is only: select the FeCuMn/HZSM-5 dual-function catalyst with damascene structures, and metal active constituent Fe and auxiliary agent Cu, Mn are embedded in HZSM-5 molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 7
Repeat embodiment 1, its difference is only: select the FeMn/H β dual-function catalyst with damascene structures, metal active constituent Fe and auxiliary agent Mn is embedded in H beta-molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 8
Repeat embodiment 1, its difference is only: select the FeCuMnH β dual-function catalyst with damascene structures, metal active constituent Fe and auxiliary agent Cu, Mn are embedded in H beta-molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 9
Repeat embodiment 1, its difference is only: select the Co/MCM-41 dual-function catalyst with damascene structures, and metal active constituent Co is embedded in MCM-41 molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 10
Repeat embodiment 1, its difference is only: select the Co/HMS dual-function catalyst with damascene structures, and metal active constituent Co is embedded in HMS molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 11
Repeat embodiment 1, its difference is only: select the Co/MCM-22 dual-function catalyst with damascene structures, and metal active constituent Co is embedded in MCM-22 molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 12
Repeat embodiment 1, its difference is only: select the Co/SAPO-34 dual-function catalyst with damascene structures, and metal active constituent Co is embedded in SAPO-34 molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 13
Repeat embodiment 1, its difference is only: select the Co/HY dual-function catalyst with damascene structures, and metal active constituent Co is embedded in HY molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 14
Repeat embodiment 1, its difference is only: select the Co/SBA-15 dual-function catalyst with damascene structures, and metal active constituent Co is embedded in SBA-15 molecular sieve, its technical process and quality product and embodiment 1 close.
Embodiment 15
Repeat embodiment 1, its difference is only: select the Co/TS-1 dual-function catalyst with damascene structures, and metal active constituent Co is embedded in TS-1 molecular sieve, its technical process and quality product and embodiment 1 close.
Obviously; the above embodiment of the present invention is only for example of the present invention is clearly described; and be not the restriction to embodiments of the present invention; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description; here cannot give exhaustive to all embodiments, every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (6)
1., based on a short route F-T synthesis new technology to prepare oil for dual-function catalyst, it is characterized in that: comprise the steps:
(1) will be that the crude synthesis gas that raw material obtains carries out desulfurization, scavenging process by coal, Sweet natural gas or biomass, then be adjusted to H via water gas shift reaction
2the material synthesis gas that/CO mol ratio is suitable;
(2) under dual-function catalyst exists, carry out Fischer-Tropsch synthesis after material synthesis gas enters reactor, after separation, directly obtain high-octane gasoline component;
(3) methane steam reforming, tail gas is recover hydrogen and low-carbon (LC) hydro carbons after treatment, and synthetic water carries out wastewater treatment after removing alcohols material;
Described dual-function catalyst has damascene structures, and comprise molecular sieve and metal active constituent two portions, metal active constituent is embedded in crystallization of molecular sieves.
2. according to claim 1 based on the short route F-T synthesis new technology to prepare oil of dual-function catalyst, it is characterized in that: preferably, the active ingredient of described dual-function catalyst is one or both in Fe, Co.
3. according to claim 1 based on the short route F-T synthesis new technology to prepare oil of dual-function catalyst, it is characterized in that: preferably, the molecular sieve of described dual-function catalyst is one or more in following molecular sieve: HZSM-5 molecular sieve, H beta-molecular sieve, MCM-41 molecular sieve, HMS molecular sieve, MCM-22 molecular sieve, SAPO-34 molecular sieve, HY molecular sieve, SBA-15 molecular sieve, TS-1 molecular sieve.
4. according to claim 1 based on the short route F-T synthesis new technology to prepare oil of dual-function catalyst, it is characterized in that: preferably, in described dual-function catalyst, addible auxiliary agent is one or more in following auxiliary agent: Zr, Mg, Ni, Mn, Cu, Ti, Ag, Mo, Zn, Ru, Pt, Pd, Rh, Ce.
5. according to claim 1 based on the short route F-T synthesis new technology to prepare oil of dual-function catalyst, it is characterized in that: described reactor adopts fixed-bed reactor, fluidized-bed reactor or paste state bed reactor.
6., according to claim 1 based on the short route F-T synthesis new technology to prepare oil of dual-function catalyst, it is characterized in that: in described material synthesis gas, H
2/ CO mol ratio is 2 ~ 5 ︰ 1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2630308C1 (en) * | 2016-06-02 | 2017-09-07 | Публичное акционерное общество "Газпром" | Method and installation for producing high-octane synthetic gasoline fraction from hydrocarbon-containing gas |
| CN107572481A (en) * | 2017-09-14 | 2018-01-12 | 武汉凯迪工程技术研究总院有限公司 | Methods and applications and its synthesis oil system based on gasification of bio-oil for synthesis gas |
| CN108017480A (en) * | 2016-11-03 | 2018-05-11 | 中国石油化工股份有限公司 | Using coal as apparatus and method of the raw material through the direct producing light olefins of synthesis gas |
| CN109762589A (en) * | 2019-03-21 | 2019-05-17 | 北京大学 | The method for preparing hydrocarbon product using CO and water |
| CN111215125A (en) * | 2018-11-26 | 2020-06-02 | 北京化工大学 | The target product of the Fischer-Tropsch reaction for the synthesis gas is C5-12And a process for preparing the same |
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| CN103100415A (en) * | 2012-12-03 | 2013-05-15 | 北京化工大学 | Catalyst with active component nano particles embedded in molecular sieve to crystallize, method and application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2630308C1 (en) * | 2016-06-02 | 2017-09-07 | Публичное акционерное общество "Газпром" | Method and installation for producing high-octane synthetic gasoline fraction from hydrocarbon-containing gas |
| CN108017480A (en) * | 2016-11-03 | 2018-05-11 | 中国石油化工股份有限公司 | Using coal as apparatus and method of the raw material through the direct producing light olefins of synthesis gas |
| CN107572481A (en) * | 2017-09-14 | 2018-01-12 | 武汉凯迪工程技术研究总院有限公司 | Methods and applications and its synthesis oil system based on gasification of bio-oil for synthesis gas |
| CN107572481B (en) * | 2017-09-14 | 2019-11-08 | 武汉凯迪工程技术研究总院有限公司 | Methods and applications and its synthesis oil system based on gasification of bio-oil for synthesis gas |
| CN111215125A (en) * | 2018-11-26 | 2020-06-02 | 北京化工大学 | The target product of the Fischer-Tropsch reaction for the synthesis gas is C5-12And a process for preparing the same |
| CN109762589A (en) * | 2019-03-21 | 2019-05-17 | 北京大学 | The method for preparing hydrocarbon product using CO and water |
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