CN102863306A - Slurry bed ft synthesis method - Google Patents

Slurry bed ft synthesis method Download PDF

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Publication number
CN102863306A
CN102863306A CN2011101840120A CN201110184012A CN102863306A CN 102863306 A CN102863306 A CN 102863306A CN 2011101840120 A CN2011101840120 A CN 2011101840120A CN 201110184012 A CN201110184012 A CN 201110184012A CN 102863306 A CN102863306 A CN 102863306A
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fischer
tropsch
catalyst
reaction
synthetic
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CN102863306B (en
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李�杰
袁长富
张舒冬
宋喜军
张喜文
倪向前
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/40—Ethylene production

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  • Catalysts (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a slurry bed ft synthesis method, which is characterized in that a proper amount of a reduced ft synthesis catalyst and a reaction solvent are weighted and placed in a slurry bed reactor, after airtight and gas displacement, the temperature and pressure are increased to reach the ft synthesis reaction condition, the synthesis catalyst and the reaction solvent are sealed and stirred for 1-5 hours and then synthetic gas is switched for the ft synthesis reaction, and the reaction solvent comprises 1-5% of water or an oxygen-containing organic matter by weight. The oxygen-containing organic matter comprises one or more of methanol, ethanol, propanol, ethylene oxide, acetone and epoxypropane. The ft synthesis reaction condition is characterized in that the reaction pressure is 1.5-2.2 MPa, the reaction temperature is 180-230 DEG C, and the volume air speed of the synthetic gas is 500-2500h<-1>. The method is used for keeping the high activity during the stable period of a cobalt-based Fischer-Tropasch synthetic catalyst, and reducing the initial activity of the catalyst.

Description

A kind of method for synthesizing Fischer Tropsch of slurry bed
Technical field
The present invention relates to a kind of method for synthesizing Fischer Tropsch of slurry bed.
Background technology
Synthetic synthetic gas (the CO+H that refers to of Fischer-Tropsch 2) catalyze and synthesize the reaction of liquid hydrocarbon fuel at catalyzer.Day by day exhaustion along with petroleum resources has been subject to the attention of countries in the world more with the Fischer-Tropsch synthesis prepare liquid fuel.
Be used for the synthetic technique of F-T fixed-bed process, Circulating Fluidized Bed Process, fixed fluidized bed technique and slurry attitude bed process are successively arranged.Fixed-bed reactor have the shortcomings such as focus, obstruction and throughput are low, and the fluid mapper process of circulating fluidized bed is restive, and catalyst utilization hangs down serious wear, and throughput is still on the low side.Fixed fluidized bed is the improved form of circulating fluidized bed, easy operation simple in structure not only, has also solved the problem of the low and wearing and tearing of catalyst utilization, and throughput improves greatly.The development of natural gas liquefaction has promoted the development of paste state bed reactor, and particularly in recent years, the syrup state bed Fischer Tropsch synthetic technology was greatly developed.
The synthetic used catalyzer of syrup state bed Fischer Tropsch mostly is the catalyzer after the prereduction outside device, if this is because the syrup state bed Fischer Tropsch synthesis technique carries out reducing in the device in the process that goes into operation, because the existence of reaction solvent, affect the mass transfer of hydrogen, cause the reduction effect of catalyzer often not reach the requirement of use.
The reduction process of typical catalyzer is in the presence of hydrogen, and the oxidation state precursor is activated by the high temperature reduction of hydrogen.Main purpose for the activity pursuing reduction effect and then improve catalyzer in the process of reduction.The disclosed method by reducing/oxidizing/reduction cyclic activation cobalt catalyst of US4492774, US4585798, US4088671, US4670414 and EP0253924 can improve the activity of F-T building-up reactions.The circulation of all oxidation/reduction/oxidations of describing in above-mentioned patent or reducing/oxidizing/reduction uses oxygen-containing gas at high temperature to process solid catalyst and carry out mostly, and the oxide compound that may cause forming most stable is Co for example 3O 4Generation, reduce the content of active ingredient in catalyzer, in addition, also to strictly control the exothermicity of oxidizing reaction and guarantee water partial pressure low between reduction period in order to avoid the sintering of cobalt.
European patent EP 0533228 discloses a kind of Co/Zr/Al 2O 3(SiO 2Or TiO 2) method of reducing of catalyzer.Being specially at pressure is under the condition of 100 ~ 350 ℃ of 1-10mbar and temperature, with hydrogen-containing gas (0 ~ 70%H 2/ rare gas element, V/V) reducing catalyst, H in hydrogen-containing gas during reduction 2Concentration and air speed progressively or increase continuously to guarantee H 2The dividing potential drop of O is lower than 200mbar.
For the synthetic load type cobalt-base catalyst of Fischer-Tropsch, although can improve the activity of catalyzer by different method of reducing, but inevitably in the process of a catalyzer rapid deactivation of initial reaction stage ubiquity, then reach active stabilization period, the higher initial activity of activity is also high often.Fischer-Tropsch building-up process reaction pressure is in the 0.5-4MPa scope, and pressure to increase synthetic to Fischer-Tropsch be favourable, so the reaction pressure that adopts is mostly more than 2.0MPa, and the pressure of system relies on the dividing potential drop of synthetic gas to keep mostly, catalyzer is too high activity and the rapid deactivation at initial stage in the early stage, very disadvantageous to industrial operation, and the conversion of the synthetic gas that the initial stage is too high, cause a large amount of generations of product water, and be difficult to be pulled away rapidly, thereby cause the increase of system water partial pressure, accelerated the inactivation of catalyzer.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of method for synthesizing Fischer Tropsch of slurry bed.Adopt the method can when keeping Co based Fischer-Tropsch synthesis catalyst high-activity stable stationary phase, reduce the initial activity of catalyzer.
A kind of method for synthesizing Fischer Tropsch of slurry bed, the fischer-tropsch synthetic catalyst and the reaction solvent that take by weighing after an amount of reduction are put into paste state bed reactor, increasing temperature and pressure is to the Fischer-Tropsch synthesis condition behind airtight and hydrogen exchange, sealing is stirred and to be switched synthetic gas behind the 1-5h and carry out Fischer-Tropsch synthesis, and described reaction solvent by weight content meter contains water or the oxygen-bearing organic matter of 1-5%.
Oxygen-bearing organic matter described in the inventive method comprises one or more in methyl alcohol, ethanol, propyl alcohol, oxyethane, acetone, the propylene oxide, particular methanol.
Fischer-Tropsch synthesis condition described in the inventive method is H in the synthetic gas 2The mol ratio of/CO is 1.0 ~ 4.0; Temperature of reaction is 180 ~ 350 ℃, and reaction pressure is 0.5 ~ 10MPa, and the volume space velocity of synthetic gas is 500 ~ 5000h -1, stirring velocity is 500-1200r/min.
Reaction solvent described in the inventive method is paraffin, and the volume ratio of paraffin and fischer-tropsch synthetic catalyst is 4-5.
Fischer-tropsch synthetic catalyst described in the inventive method is the fischer-tropsch synthetic catalyst after reduction of this area routine.Preferred fischer-tropsch synthetic catalyst is for take Co as active ingredient, and one or more in Zr, Hf, Ce and Th, Pt, Ru, Ni, Mo and the W are as auxiliary agent, with ZrO 2, TiO 2, SiO 2And Al 2O 3One or more are mixed into carrier.
Compared with prior art, a kind of method for synthesizing Fischer Tropsch of slurry bed of the present invention has following advantage:
1, in the Fischer-Tropsch synthesis process, the initial activity of catalyzer is high, easily cause the fluctuation of the reaction conditionss such as temperature, pressure, make reaction restive, even sintering of catalyst is lost activity, the inventive method adds a small amount of weak oxidant (water or oxygen-bearing organic matter) in reaction solvent, can reduce the initial activity of catalyzer, and reaction process is steadily carried out;
2, the inventive method water or oxygen-bearing organic matter in temperature-rise period becomes steam, make whole system have certain steam partial pressure or oxygen-bearing organic matter partial vapor pressure, the oxide treatment that catalyzer is relaxed, simultaneously because the existence of hydrogen, only reduced the initial activity of catalyzer, other performance to catalyzer can not exert an influence, and is easy to separate from reaction system;
3, the inventive method is before carrying out Fischer-Tropsch synthesis, pass into the mixed air that contains water vapor or oxygen-bearing organic matter steam and hydrogen in the paste state bed reactor, particularly passing under the condition of water vapour, can impel reaction system to carry out hydro-thermal reaction, suppress hydrothermal in the Fischer-Tropsch synthesis process, improve the stability of catalyzer, reduce the selectivity of methane.
Embodiment
Further specify process and the effect of the inventive method below in conjunction with embodiment.
Example 1
Take by weighing the 20%Co0.8%Pt3%Zr/SiO after an amount of reduction 2(Wt.) fischer-tropsch synthetic catalyst and paraffin, contain massfraction in the paraffin and be 2.5% water, catalyzer and paraffin volume ratio are 1:4, put into paste state bed reactor, increasing temperature and pressure to 220 ℃, 2.0 MPa switch H after 2.5h is stirred in the 800r/min sealing behind airtight and hydrogen exchange 2/ CO=2(mol ratio) synthetic gas carries out Fischer-Tropsch synthesis, and synthetic gas volume air speed is 1500h -1Reaction effluent is collected by hot trap, cold-trap respectively.The transformation efficiency of catalyzer, the results are shown in Table 1 for methane selectively and stability test.
Example 2
Take by weighing the 20%Co1%Ni3%Zr/TiO after an amount of reduction 2(Wt.) fischer-tropsch synthetic catalyst and paraffin, contain massfraction in the paraffin and be 1% acetone, catalyzer and paraffin volume ratio are 1:5, put into paste state bed reactor, increasing temperature and pressure to 240 ℃, 2.5 MPa switch H after 1h is stirred in the 600r/min sealing behind airtight and hydrogen exchange 2/ CO=2(mol ratio) synthetic gas carries out Fischer-Tropsch synthesis, and synthetic gas volume air speed is 2000h -1Reaction effluent is collected by hot trap, cold-trap respectively.The transformation efficiency of catalyzer, the results are shown in Table 1 for methane selectively and stability test.
Example 3
Take by weighing the 20%Co0.05%Ru3%Zr/Al after an amount of reduction 2O 3(Wt.) fischer-tropsch synthetic catalyst and paraffin, contain massfraction in the paraffin and be 5% methyl alcohol, catalyzer and paraffin volume ratio are 1:5, put into paste state bed reactor, increasing temperature and pressure to 220 ℃, 2.0 MPa switch H after 5h is stirred in the 800r/min sealing behind airtight and hydrogen exchange 2/ CO=2(mol ratio) synthetic gas carries out Fischer-Tropsch synthesis, and synthetic gas volume air speed is 1500h -1。Reaction effluent is collected by hot trap, cold-trap respectively.The transformation efficiency of catalyzer, the results are shown in Table 1 for methane selectively and stability test.
The reactivity worth of table 1 catalyzer.
Catalyzer Initial activity and selectivity, CO transformation efficiency (%) Initial activity and selectivity, CH 4Selectivity (wt%) 100h, CO transformation efficiency (%) 100h ,CH 4Selectivity (wt%) 200h, CO transformation efficiency (%) 200h ,CH 4Selectivity (wt%)
Embodiment 1 75.5 7.5 69.8 8.5 67.8 9.5
Embodiment 2 79.2 7.2 70.5 8.2 68.5 9.8
Embodiment 3 72.6 7.7 67.7 8.7 65.7 9.1
Comparative example 86.4 8.1 66.3 9.8 64.2 10.2
Comparative example:
Take by weighing the 20%Co0.05%Ru3%Zr/Al after an amount of reduction 2O 3(Wt.) fischer-tropsch synthetic catalyst and paraffin, catalyzer and paraffin volume ratio are 1:5, put into paste state bed reactor, pass into hydrogen and open whipping appts in the airtight and backward reactor of gas displacement, being warming up to 220 ℃, control pressure is 2.0 MPa, switches H 2/ CO=2(mol ratio) synthetic gas carries out Fischer-Tropsch synthesis, and synthetic gas volume air speed is 1500h -1, stirring velocity is 800r/min.Reaction effluent is collected by hot trap, cold-trap respectively.The transformation efficiency of catalyzer, the results are shown in Table 1 for methane selectively and stability test.

Claims (6)

1. method for synthesizing Fischer Tropsch of slurry bed, the fischer-tropsch synthetic catalyst and the reaction solvent that take by weighing after an amount of reduction are put into paste state bed reactor, increasing temperature and pressure is to the Fischer-Tropsch synthesis condition behind airtight and hydrogen exchange, sealing is stirred and to be switched synthetic gas behind the 1-5h and carry out Fischer-Tropsch synthesis, it is characterized in that: described reaction solvent by weight content meter contains water or the oxygen-bearing organic matter of 1-5%.
2. method according to claim 1, it is characterized in that: described oxygen-bearing organic matter comprises one or more in methyl alcohol, ethanol, propyl alcohol, oxyethane, acetone, the propylene oxide.
3. method according to claim 1, it is characterized in that: described Fischer-Tropsch synthesis condition is H in the synthetic gas 2The mol ratio of/CO is 1.0 ~ 4.0; Temperature of reaction is 180 ~ 350 ℃, and reaction pressure is 0.5 ~ 10MPa, and the volume space velocity of synthetic gas is 500 ~ 5000h -1
4. method according to claim 1, it is characterized in that: described reaction solvent is paraffin, the volume ratio of paraffin and fischer-tropsch synthetic catalyst is 4-5.
5. method according to claim 1 is characterized in that: described fischer-tropsch synthetic catalyst is the fischer-tropsch synthetic catalyst after reduction of this area routine.
6. method according to claim 1 or 5 is characterized in that: described fischer-tropsch synthetic catalyst is for take Co as active ingredient, and one or more in Zr, Hf, Ce and Th, Pt, Ru, Ni, Mo and the W are as auxiliary agent, with ZrO 2, TiO 2, SiO 2And Al 2O 3One or more are mixed into the Co based Fischer-Tropsch synthesis catalyst of carrier.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107405607A (en) * 2014-12-12 2017-11-28 英国石油有限公司 Use the fischer-tropsch process of reduction Co catalysts
CN107406775A (en) * 2014-12-12 2017-11-28 英国石油有限公司 Use the fischer-tropsch process of the Co catalysts of reduction activation

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107405607A (en) * 2014-12-12 2017-11-28 英国石油有限公司 Use the fischer-tropsch process of reduction Co catalysts
CN107406775A (en) * 2014-12-12 2017-11-28 英国石油有限公司 Use the fischer-tropsch process of the Co catalysts of reduction activation
US10717075B2 (en) 2014-12-12 2020-07-21 Bp P.L.C. Fischer-Tropsch process using reduced cobalt catalyst
CN107406775B (en) * 2014-12-12 2020-10-16 英国石油有限公司 Fischer-tropsch process using a reduction-activated cobalt catalyst
CN107405607B (en) * 2014-12-12 2020-12-08 英国石油有限公司 Fischer-tropsch process using a reduced cobalt catalyst

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