CN108722327A - A kind of biomass membrane type micro-wave reactor and its experimental provision and method applied to methane reforming - Google Patents
A kind of biomass membrane type micro-wave reactor and its experimental provision and method applied to methane reforming Download PDFInfo
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- CN108722327A CN108722327A CN201810351374.6A CN201810351374A CN108722327A CN 108722327 A CN108722327 A CN 108722327A CN 201810351374 A CN201810351374 A CN 201810351374A CN 108722327 A CN108722327 A CN 108722327A
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- 239000002028 Biomass Substances 0.000 title claims abstract description 93
- 239000012528 membrane Substances 0.000 title claims abstract description 73
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000002407 reforming Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003610 charcoal Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000002474 experimental method Methods 0.000 claims abstract description 17
- 239000010453 quartz Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229910017709 Ni Co Inorganic materials 0.000 claims abstract description 15
- 229910003267 Ni-Co Inorganic materials 0.000 claims abstract description 15
- 229910003262 Ni‐Co Inorganic materials 0.000 claims abstract description 15
- 239000003708 ampul Substances 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 9
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 17
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- 229910001868 water Inorganic materials 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000011148 porous material Substances 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 11
- 239000004014 plasticizer Substances 0.000 claims description 10
- 239000000080 wetting agent Substances 0.000 claims description 10
- 239000012018 catalyst precursor Substances 0.000 claims description 8
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 230000007547 defect Effects 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical group CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 4
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 4
- 238000005470 impregnation Methods 0.000 claims description 4
- 230000001404 mediated effect Effects 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 235000021419 vinegar Nutrition 0.000 claims description 4
- 239000000052 vinegar Substances 0.000 claims description 4
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 210000002268 wool Anatomy 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 11
- 238000011049 filling Methods 0.000 abstract description 3
- 229910017052 cobalt Inorganic materials 0.000 abstract description 2
- 239000010941 cobalt Substances 0.000 abstract description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 43
- 210000004379 membrane Anatomy 0.000 description 27
- 239000000243 solution Substances 0.000 description 10
- 229910002651 NO3 Inorganic materials 0.000 description 6
- 238000003763 carbonization Methods 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000000505 pernicious effect Effects 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 238000006057 reforming reaction Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 229910026161 MgAl2O4 Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 210000002469 basement membrane Anatomy 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002153 concerted effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011552 falling film Substances 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000001480 isothermal pyrolysis Methods 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
- B01J35/59—Membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
- C01B3/40—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts characterised by the catalyst
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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
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Abstract
The invention discloses a kind of biomass membrane type micro-wave reactors, the internal quartz ampoule for filling biomass-based charcoal film catalyst is fixed on microwave heating equipment central area with flange and screw rod, the new-type biomass membrane type micro-wave reactor is made, wherein, using biomass carbon membrane made from sawdust as carrier, using the active component of nickel and cobalt as catalyst, the load biomass-based charcoal film catalyst of Ni-Co active components is made；The biomass membrane type micro-wave reactor is assembled and is applied in the experimental provision of methane reforming, and carries out methane reforming experiment.The invention has the advantages that new-type biomass membrane type micro-wave reactor substitutes conventional heating device, methane reforming is carried out using the methane reforming experimental provision, strengthens reaction collaboration and carries out, the H of synthesis gas2With CO ratios 1.10, CH are increased to by 0.834And CO2High conversion rate is up to 95%, and experimental method of the invention is at low cost, reaction-ure conversion-age is high.
Description
Technical field
The present invention relates to the technical field of methane reforming more particularly to a kind of biomass membrane type micro-wave reactor and its applications
In the experimental provision and method of methane reforming.
Background technology
CH4And CO2It is the small-molecule substance of stable structure, CH4-CO2Reformation will carry out under catalytic condition.Catalyst master
There are noble metal catalyst, transition-metal catalyst and carbon-supported catalysts.Noble metal catalyst activity is high, and main bottleneck is price
It is big to promote difficulty for costliness；Transition-metal catalyst better performances mainly have the problems such as carbon distribution inactivation, active material sintering；It is carbon-based
Catalyst has a clear superiority in raw material sources and in price, and carbon distribution can be directly used as carrier.
Carbon membrane be it is a kind of by carbonaceous material through membrane material made of high temperature pyrolysis, have high temperature resistant, anticorrosive, acid and alkali-resistance, good
The characteristics such as good chemical stability and higher mechanical strength.Carbon membrane can be improved to carbon membrane oxidation modification and carrying active substance
Surface chemical property and catalytic performance.Microwave heating has the features such as instantaneity, globality, high efficiency and controllability, carbon-based to urge
The rise of agent promotes microwave technology in CH4-CO2Application in reforming reaction.
Patent CN102416328A discloses catalyst and its preparation side of a kind of synthesizing gas by reforming methane with co 2
Method, the catalyst are made of nickel, iron, cerium oxide, U.S. aluminate；Preparation method is first to prepare mesoporous MgAl2O4Spinelle carries
Body, then prepare nickel-base catalyst suspension is finally filtered, washed, dries, roasting and be made.
Patent CN101637726A discloses a kind of synthesizing gas by reforming methane with co 2 method for preparing catalyst, pass through by
Carrier impregnation obtains modified component in the mixed solution of cerous nitrate and lanthanum nitrate.Modified component is impregnated into nickel salt again
In soluble solution, catalyst precursor is obtained through drying, roasting.
Patent CN102464299A discloses a kind of method of producing hydrogen through fluidized-bed methane steam reforming, including by low accumulation
Pyrolytic regenerates the adsorption catalyst of density in a regenerator, and regenerative adsorption catalyst is conveyed in reactor bottom and outer circulation
High-bulk-density reforming catalyst mixing.Wherein realize the regeneration of catalyst, but the CO that catalyst regeneration generates2Directly
It connects and is drained into air, and complex process, energy consumption is relatively more.
Currently, conventional microwave technology is applied to CH4-CO2Reform in experiment, that there are reaction efficiencies is low, conversion ratio is low, at
The problem of this height, high energy consumption.
Invention content
The present invention against the above deficiency, proposes a kind of biomass membrane type micro-wave reactor and its reality applied to methane reforming
Experiment device and method.
To achieve the above object, the present invention uses following technical proposals：
A kind of biomass membrane type micro-wave reactor, including microwave heating equipment, biomass-based charcoal film catalyst and quartz ampoule,
The internal quartz ampoule for filling biomass-based charcoal film catalyst microwave is fixed on the flange of polytetrafluoroethylene (PTFE) material and screw rod to add
A cell quartz plate, biomass-based charcoal film catalyst is arranged at 28~32mm of quartzy bottom of the tube in thermal central area
It is separated with silica wool between quartz plate.
Using biomass carbon membrane as carrier, load Ni-Co is made by co-impregnation in Ni and the catalyst that Co is active component
The biomass-based charcoal film catalyst of active component.
The preparation process of the biomass carbon membrane is as follows：
(1) pug mixes：Sawdust, reagent are mixed according to a certain percentage, mediated in malaxator uniformly；
(2) extrusion forming：Pug is put into molding machine hopper, pug is squeezed into mold under compression bar effect, another at its
Product just can be obtained in end, and the shape of product depends on the interior shape of mold nozzle, obtains being former film in this experiment, and batch is raw
Production capacity power is strong, by adjusting the technological parameters such as extrusion pressure, obtains that surface is smooth, zero defect original film of regular shape.
(3) dry：Using freeze-day with constant temperature mode, drying process is to allow former film to be solidified into remove the solvent in former film
Skeleton improves former film strength, and in order to carry and carbonize, in the drying process with the volatilization of solvent, former film will will appear
It shrinks, it is therefore necessary to strictly control drying program, defect is generated when to avoid drying.
(4) it carbonizes：Former film after drying is put into retort, is warming up to 940~960 DEG C under nitrogen protection, constant temperature
Afterwards, room temperature is naturally cooled to, you can obtain biomass carbon membrane.Former film after drying is put into retort, to keep former film to exist
Smooth carbon membrane is made in natural shrinking under the conditions of thermal decomposition, between the former film pre-processed is lain against two panels flag, is placed in self-control folder
It is imposed in tool and with powder compressing machine and is fastened with bolt after normal pressure 5MPa is uniformly compressed, be then charged into reactor, will react
Device is fixed in the middle part of tubular type burner hearth flat-temperature zone, in N2Heat up charing under gas shielded；Gas is thermally decomposed at high temperature with carrier gas from anti-
Device export is answered successively to enter 20%H2SO4, copper ammon solution and 10% ferrous sulfate solution, to eliminate, there may be NH in tail gas3、
The pernicious gases such as CO and HCN are finally passed through in draught cupboard and discharge.
Technical scheme of the present invention further includes that the reagent in step (1) is binder, pore creating material, wetting agent and plasticizer
Intermixture, wherein binder is carboxymethyl cellulose, and pore creating material is polyvinyl butyral, and plasticizer is phthalic acid
Two fourth vinegar, wetting agent are dodecyl benzene sulfonic acid.
Technical scheme of the present invention further includes the sawdust in step (1) and binder, pore creating material, wetting agent and plasticizer
Proportioning be 8~10:1:1:1:1.
Technical scheme of the present invention further includes that the carbonization process of step (4) is：N2Gas velocity control is 320~350mL
min-1, heating rate is 2.5~3.5 DEG C of min-1, 280~300 DEG C are first warming up to, 55~65min of constant temperature is then heated to
550 DEG C, and 110~130min of constant temperature, it is continuously heating to different 940~950 DEG C of charing final temperatures, and 120~150min of constant temperature, most
Afterwards in N2The lower cooled to room temperature of protection.
The preparation process for loading the biomass-based charcoal film catalyst of Ni-Co active components is as follows：
(1) dipper precipitation：By biomass carbon film immersion obtained in Ni (NO3)2·6H2O and Co (NO3)2·6H2O is mixed
Then CO (NH are added in 1.5~2.5h in solution2) 0.4~0.6h is stirred at room temperature, which is put into 92~96 DEG C of perseverance
In tepidarium, start to precipitate after 0.4~0.6h of synthesis under normal pressure, continues constant temperature and handle 3~5h, obtain gel precipitation；
(2) it dries：Gel precipitation is filtered, and successively deionized water and absolute ethyl alcohol wash with remove it is unreacted instead
Object is answered, 110~130 DEG C of dry 10~12h in drying box are subsequently placed at, water is combined to remove Free water and part, is made
Catalyst precursor；
(3) it calcines：Catalyst precursor is placed in N in Muffle furnace2In atmosphere, 4 are calcined under conditions of 500~550 DEG C
~6h obtains the biomass carbon membrane of load Ni-Co active components；
(4) it restores：In a hydrogen atmosphere, biomass-based carbon membrane step (3) obtained carries out activating and reducing to get load
The biomass-based charcoal film catalyst of Ni-Co active components.
It is a kind of that biomass membrane type micro-wave reactor is applied to the experimental provision of methane reforming, including be linked in sequence successively
Reactor, biomass membrane type micro-wave reactor, three stub tuner, directional coupler, circulator, magnetron and power supply and
The top of control device, the reactor connects methane tank by pipeline and carbon dioxide tank, nitrogen gas tank access institute by pipeline
It states in reactor, the outlet at bottom pipeline of the reactor is also connected with steam generation facility, the biomass membrane type micro-wave reaction
Device is also connected with gas chromatograph.
A kind of experimental method of methane reforming is applied to methane reforming using above-mentioned biomass membrane type micro-wave reactor
Experimental provision, by CH4：CO2：N2：H2O is with 1:1:3:3~1.5:1.5:3:3 ratios enter reactor, and gas enters group after reaction
In the biomass membrane type micro-wave reactor installed, biomass membrane type micro-wave reactor is controlled at 950 DEG C, and gas is in biomass
Membrane type microwave reactor is detained 5s, you can obtains synthesis gas H2With CO.
The invention has the advantages that in traditional methane reforming experiment, heating is all conventional heating device, and of the invention
Using new-type biomass membrane type micro-wave reactor, using biomass carbon membrane made from sawdust as carrier, using nickel and cobalt as activearm
It is divided into catalyst, the biomass-based charcoal film catalyst of load Ni-Co active components is made, which overcomes conventional urge
The defect that agent mechanical performance is weak, stability is poor, while new catalyst absorbing property is good；New catalyst obtained is contained
It is put in quartz ampoule, assembles new-type biomass membrane type micro-wave reactor, which is assembled in methane reforming reality
Experiment device, the methane reforming experimental provision are applied to methane reforming experimental method, the more conventional reaction unit of experiment reaction efficiency
20% is improved, without apparent carbon distribution, strengthens concerted reaction and carries out, H21.10, energy saving 27% are increased to by 0.83 with CO ratios, at
This reduction by 10%, CH4And CO2Conversion ratio can reach 95%, significantly improve methane and carbon dioxide conversion ratio, energy conservation and environmental protection.
Description of the drawings
Fig. 1 is the biomass carbon membrane carbonization process schematic diagram in the present invention；
Fig. 2 is methane reforming Experimental equipment；
Wherein, 1-methane tank；2-carbon dioxide tanks；3-nitrogen gas tanks；4-steam generation facilities；5-mass flow controls
Device processed；6-reactors；7-biomass membrane type micro-wave reactors；8-three stub tuners；9-directional couplers；10—
Circulator；11-magnetrons；12-power supplys and control device；13-microwave power meters；14-gas chromatographs；15—MS,
FID, TCD detector；16-computers.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without creative efforts
Embodiment shall fall within the protection scope of the present invention.
A kind of biomass membrane type micro-wave reactor, including microwave heating equipment, biomass-based charcoal film catalyst and quartz ampoule,
The internal quartz ampoule for filling biomass-based charcoal film catalyst microwave is fixed on the flange of polytetrafluoroethylene (PTFE) material and screw rod to add
A cell quartz plate, biomass-based charcoal film catalyst is arranged at 28~32mm of quartzy bottom of the tube in thermal central area
It is separated with silica wool between quartz plate.
Using biomass carbon membrane as carrier, load Ni-Co is made by co-impregnation in Ni and the catalyst that Co is active component
The biomass-based charcoal film catalyst of active component.
As shown in Fig. 2, the preparation process of biomass carbon membrane is as follows：
(1) pug mixes：Sawdust, reagent are mixed according to a certain percentage, mediated in malaxator uniformly, reagent is
The intermixture of binder, pore creating material, wetting agent and plasticizer, binder are carboxymethyl cellulose, and pore creating material contracts for polyvinyl alcohol
Butyraldehyde, plasticizer are two fourth vinegar of phthalic acid, and wetting agent is dodecyl benzene sulfonic acid, and sawdust and binder, pore creating material, profit
The proportioning of humectant and plasticizer is 8~10:1:1:1:1.
(2) extrusion forming：Pug is put into molding machine hopper, pug is squeezed into mold under compression bar effect, another at its
Product just can be obtained in end, and the shape of product depends on the interior shape of mold nozzle, obtains being former film in this experiment, and batch is raw
Production capacity power is strong, by adjusting the technological parameters such as extrusion pressure, obtains that surface is smooth, zero defect original film of regular shape.
(3) dry：Using freeze-day with constant temperature mode, drying process is to allow former film to be solidified into remove the solvent in former film
Skeleton improves former film strength, and in order to carry and carbonize, in the drying process with the volatilization of solvent, former film will will appear
It shrinks, it is therefore necessary to strictly control drying program, defect is generated when to avoid drying.
(4) it carbonizes：Former film after drying is put into retort, is warming up to 940~960 DEG C under nitrogen protection, constant temperature
Afterwards, room temperature is naturally cooled to, you can obtain biomass carbon membrane, as shown in Figure 1.Former film after drying is put into retort, is
Keep former film natural shrinking under the conditions of thermal decomposition that smooth carbon membrane is made, between the former film pre-processed is lain against two panels flag,
It is placed in self-made clamp and is imposed with powder compressing machine and fastened with bolt after normal pressure 5MPa is uniformly compressed, be then charged into reactor
In 6, reactor 6 is fixed in the middle part of tubular type burner hearth flat-temperature zone, in N2Heat up charing under gas shielded；Thermally decompose gas at high temperature
Successively enter 20%H from the export of reactor 6 with carrier gas2SO4, copper ammon solution and 10% ferrous sulfate solution, can in tail gas to eliminate
NH can be generated3, the pernicious gases such as CO and HCN, be finally passed through in draught cupboard and discharge.
Wherein, the carbonization process of step (4) is：The carbonization process of step (4) is：N2Gas velocity control for 320~
350mL·min -1, heating rate is 2.5~3.5 DEG C of min-1, 280~300 DEG C, 55~65min of constant temperature are first warming up to, so
After be warming up to 550 DEG C, and 110~130min of constant temperature, be continuously heating to different 940~950 DEG C of charing final temperatures, and constant temperature 120~
150min, finally in N2The lower cooled to room temperature of protection.
The preparation process for loading the biomass-based charcoal film catalyst of Ni-Co active components is as follows：
(1) dipper precipitation：By biomass carbon film immersion obtained in Ni (NO3)2·6H2O and Co (NO3)2·6H2O is mixed
Then CO (NH are added in 2h in solution2) 0.5h is stirred at room temperature, which is put into 95 DEG C of water bath with thermostatic control, atmospheric reverse
Start to precipitate after answering 0.5h, continues constant temperature and handle 4h, obtain gel precipitation；
(2) it dries：Gel precipitation is filtered, and successively deionized water and absolute ethyl alcohol wash with remove it is unreacted instead
Object is answered, 120 DEG C of dry 10h in drying box are subsequently placed at, water is combined to remove Free water and part, complex catalyst precursor is made
Body；
(3) it calcines：Catalyst precursor is placed in N in Muffle furnace2In atmosphere, 5h is calcined under conditions of 500 DEG C, is obtained
Load the biomass carbon membrane of Ni-Co active components；
(4) it restores：In a hydrogen atmosphere, biomass-based carbon membrane activating and reducing 1h step (3) obtained is to get load
The biomass-based charcoal film catalyst of Ni-Co active components.
A kind of experimental provision that biomass membrane type micro-wave reactor is applied to methane reforming, as shown in Fig. 2, including successively
The reactor 6 that is linked in sequence, biomass membrane type micro-wave reactor 7, three stub tuner 8, directional coupler 9, circulator 10,
The top of magnetron 11 and power supply and control device 12, reactor 6 connects methane tank 1 and carbon dioxide tank 2, nitrogen by pipeline
Gas tank 3 is accessed by pipeline in reactor 6, and the outlet at bottom pipeline of reactor 6 is also connected with steam generation facility 4, biomass membrane
Type micro-wave reactor 7 is also connected with the gas chromatograph 14 for being equipped with MS, FID, TCD detector 15, gas chromatograph 14 with
One computer 16 is connected, and microwave power meter 13 connects directional coupler 9, methane tank 1, carbon dioxide tank 2, nitrogen gas tank 3 and reacts
It is both provided with mass flow controller 5 in 6 connecting pipeline of device.
Above-mentioned biomass membrane type micro-wave reactor 7 is applied to methane reforming by a kind of experimental method of methane reforming
Experimental provision, by CH4：CO2：N2：H2O is with 1.5：1.5：3：3 ratio enters reactor 6, and the gas after reaction, which enters, to be assembled
Biomass membrane type micro-wave reactor 7 in, biomass membrane type micro-wave reactor 7 is controlled at 950 DEG C, and gas is in biomass membrane
It is detained 5s in type micro-wave reactor 7, you can obtain synthesis gas H2With CO.
Embodiment
(1) biomass carbon membrane is prepared
1. sawdust is ground to 80 mesh, sawdust presses 10 with binder, pore creating material, wetting agent and plasticizer:1:1:1:1 ratio
Example is mediated uniformly in malaxator, wherein binder is carboxymethyl cellulose, and pore creating material is polyvinyl butyral, plasticising
Agent is two fourth vinegar of phthalic acid, and wetting agent is dodecyl benzene sulfonic acid；
2. pug is put into 10T molding machine hoppers, pug is squeezed into mold under compression bar 5MPa effect, its other end just
Obtain that surface is smooth, former film of regular shape；
3. carrying out freeze-day with constant temperature to former film at 120 DEG C, obtained cellular former film is dried into 4d, drying process is necessary
Stringent control drying program, to avoid there is the problem of former film defect；
4. to keep former film natural shrinking under the conditions of thermal decomposition that smooth carbon membrane is made, the former film pre-processed is lain against
Between two panels flag, it is placed in self-made clamp and is fastened with bolt after imposing the uniform compressions of normal pressure 5MPa with powder compressing machine, so
It is fitted into quartz container, quartz container is fixed in the middle part of tubular type burner hearth flat-temperature zone, in N afterwards2With the heating of 3 DEG C/min under protection
Rate rises to 950 DEG C, and room temperature is naturally cooled to after isothermal pyrolysis.It can be obtained biomass carbon membrane.
(2) catalyst of the biomass-based carbon membrane of load Ni-Co active components is prepared
1. by Ni (NO3)2·6H2O and Co (NO3)2·6H2O is with 1:3 molar ratio, which is dissolved in deionized water, is made mixing
Solution takes solution dipping gained biomass basement membrane, room temperature immersion 2h that 0.5h is stirred at room temperature, which is put into 95 DEG C
Water bath with thermostatic control in, start to precipitate after synthesis under normal pressure 0.5h, continue constant temperature handle 4h, obtain gel precipitation；
2. precipitation is filtered, and successively deionized water and absolute ethyl alcohol are washed to remove unreacted reactant, then
110 DEG C of dry 12h in drying box are placed it in, water is combined to remove Free water and part, catalyst precursor is made；
3. catalyst precursor is placed in Muffle furnace, N2Calcination temperature roasts 5h under conditions of being 500 DEG C in atmosphere；
4. by the catalyst after calcining, after restoring 1h in a hydrogen atmosphere, you can obtain the biomass-based charcoal of load Ni-Co
Film catalyst.
(3) biomass membrane type micro-wave reactor is assembled
There are the microwave source of the microwave heating equipment used 10 power-adjustables (0~1000W), this experiment microwave to use
1000W will fill the internal diameter 40mm high 200mm's of biomass-based charcoal film catalyst with the flange and screw rod of polytetrafluoroethylene (PTFE) material
Quartz ampoule is fixed on microwave heating equipment central area, completes the assembling of biomass falling film reactor.
(4) methane reforming is tested
The assembled biomass membrane type micro-wave reactor of above-mentioned steps 7 is installed on to methane reforming experiment as shown in Figure 2
In.
(5) experimentation
By CH4/CO2/N2/H2O is with 1:1:3:3 ratios are passed through reactor, and the gas after reaction enters the new-type biology of assembling
Plasma membrane type micro-wave reactor 7, for biomass membrane type micro-wave reactor 7 controlled at 950 DEG C, gas is anti-in biomass membrane type micro-wave
It answers in device 7 and is detained 5s, you can obtain synthesis gas H2With CO.
(6) test result
The gas composition H obtained after determination experiment2/ CO=1.10, H2It is improved with CO productivity ratio conventional equipments
32%；Its reaction speed also improves 25% than conventional equipment；CH4And CO2Conversion ratio about 95%；Compound reforming reaction energy utilization
Efficiency is 97%；And without there is apparent carbon distribution during preparing synthesis gas.
Certainly, above description is not limitation of the present invention, and the present invention is also not limited to the example above, this technology neck
The variations, modifications, additions or substitutions that the technical staff in domain is made in the essential scope of the present invention should also belong to the present invention's
Protection domain.
Claims (9)
1. a kind of biomass membrane type micro-wave reactor, which is characterized in that including microwave heating equipment, biomass-based charcoal film catalyst
And quartz ampoule, the quartz ampoule that inside is filled to biomass-based charcoal film catalyst with the flange and screw rod of polytetrafluoroethylene (PTFE) material are fixed
A cell quartz plate, biomass-based charcoal are set at microwave heating equipment central area, 28~32mm of the quartzy bottom of the tube of distance
It is separated with silica wool between film catalyst and quartz plate.
2. a kind of biomass membrane type micro-wave reactor as described in claim 1, which is characterized in that with biomass carbon membrane be to carry
Body, Ni and Co are the catalyst of active component, and the biomass-based carbon membrane that load Ni-Co active components are made by co-impregnation is urged
Agent.
3. a kind of biomass membrane type micro-wave reactor as claimed in claim 2, which is characterized in that the system of the biomass carbon membrane
It is standby that steps are as follows：
(1) pug mixes：Sawdust, reagent are mixed according to a certain percentage, mediated in malaxator uniformly；
(2) extrusion forming：Pug is put into molding machine hopper, adjusts technological parameter, it is smooth, regular shape intact to obtain surface
Fall into original film；
(3) dry：Freeze-day with constant temperature at a certain temperature strictly controls drying program, and former film shrink defects are generated when avoiding dry；
(4) it carbonizes：Former film after drying is put into retort, is warming up to 940~960 DEG C, after constant temperature under nitrogen protection, from
So it is cooled to room temperature, you can obtain biomass carbon membrane.
4. a kind of biomass membrane type micro-wave reactor as claimed in claim 3, which is characterized in that the reagent in step (1) is
The intermixture of binder, pore creating material, wetting agent and plasticizer, wherein binder is carboxymethyl cellulose, and pore creating material is polyethylene
Butyral, plasticizer are two fourth vinegar of phthalic acid, and wetting agent is dodecyl benzene sulfonic acid.
5. a kind of biomass membrane type micro-wave reactor as claimed in claim 3, which is characterized in that sawdust in step (1) with
Binder, pore creating material, wetting agent and plasticizer proportioning be 8~10:1:1:1:1.
6. a kind of biomass membrane type micro-wave reactor as described in claim 1, which is characterized in that wherein, the charing of step (4)
Process is：N2Gas velocity control is 320~350mLmin-1, heating rate is 2.5~3.5 DEG C of min-1, first it is warming up to 280
~300 DEG C, 55~65min of constant temperature, 550 DEG C, and 110~130min of constant temperature are then heated to, is continuously heating to different charings eventually
940~950 DEG C of temperature, and 120~150min of constant temperature, finally in N2The lower cooled to room temperature of protection.
7. a kind of biomass membrane type micro-wave reactor as described in claim 1, which is characterized in that load Ni-Co active components
Biomass-based charcoal film catalyst preparation process it is as follows：
(1) dipper precipitation：By biomass carbon film immersion obtained in Ni (NO3)2·6H2O and Co (NO3)2·6H2O mixed solutions
In 1.5~2.5h, CO (NH are then added2) 0.4~0.6h is stirred at room temperature, which is put into 92~96 DEG C of thermostatted water
In bath, start to precipitate after 0.4~0.6h of synthesis under normal pressure, continues constant temperature and handle 3~5h, obtain gel precipitation；
(2) it dries：Gel precipitation is filtered, and successively deionized water and absolute ethyl alcohol are washed to remove unreacted reaction
Object is subsequently placed at 110~130 DEG C of dry 10~12h in drying box, combines water to remove Free water and part, is made and urges
Agent presoma；
(3) it calcines：Catalyst precursor is placed in N in Muffle furnace2In atmosphere, 4~6h is calcined under conditions of 500~550 DEG C,
Obtain the biomass carbon membrane of load Ni-Co active components；
(4) it restores：In a hydrogen atmosphere, biomass-based carbon membrane step (3) obtained carries out activating and reducing to get load Ni-
The biomass-based charcoal film catalyst of Co active components.
8. a kind of experiment that any biomass membrane type micro-wave reactor in claim 1~7 is applied to methane reforming
Device, which is characterized in that including be linked in sequence successively reactor, biomass membrane type micro-wave reactor, three stub tuner,
The top of directional coupler, circulator, magnetron and power supply and control device, the reactor connects methane tank by pipeline
And carbon dioxide tank, nitrogen gas tank are accessed by pipeline in the reactor, the outlet at bottom pipeline of the reactor is also connected with steaming
Vapour generating means, the biomass membrane type micro-wave reactor are also connected with gas chromatograph.
9. a kind of experimental method of methane reforming, using the methane reforming experimental provision described in claim 8, feature exists
In by CH4：CO2：N2：H2O is with 1:1:3:3~1.5:1.5:3:3 ratios enter reactor, and gas enters assembled after reaction
In biomass membrane type micro-wave reactor, controlled at 950 DEG C, gas declines biomass membrane type micro-wave reactor in biomass membrane
Wave reactor is detained 5s, you can obtains synthesis gas H2With CO.
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Application publication date: 20181102 |