CN110527542A - A kind of method of microwave radiation assist medium barrier discharge catalysis upgrading bio oil - Google Patents
A kind of method of microwave radiation assist medium barrier discharge catalysis upgrading bio oil Download PDFInfo
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- CN110527542A CN110527542A CN201910827260.9A CN201910827260A CN110527542A CN 110527542 A CN110527542 A CN 110527542A CN 201910827260 A CN201910827260 A CN 201910827260A CN 110527542 A CN110527542 A CN 110527542A
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- microwave radiation
- barrier discharge
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- pyrolysis gas
- assist medium
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2/00—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1011—Biomass
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
A kind of method that the present invention discloses microwave radiation assist medium barrier discharge catalysis upgrading bio oil includes the following steps: that carrying out vacuum pyrolysis to granular biomass generates pyrolysis gas;The pyrolysis gas of generation is passed through microwave radiation reactor, carries out microwave radiation excitation;Pyrolysis gas after microwave radiation is motivated is passed through dielectric barrier discharge catalytic reactor again;To treated, pyrolysis gas is condensed and is extracted, and obtains refining biological oil.Granular biomass is successively carried out to vacuum pyrolysis, microwave radiation excitation, dielectric barrier discharge catalysis, condensation and extraction step in the present invention, it can make full use of the moisture contained in pyrolysis gas of biomass, motivated activation, with catalytic conversion efficiency height, the characteristics of refined biological oil yield is high, fuel grade is high and catalyst low coking.
Description
Technical field
The invention belongs to biomass energy trans-utilization technical fields, are specifically related to a kind of microwave radiation assist medium resistance
The method for keeping off discharge catalytic improving quality of bio oil.
Background technique
Biomass energy is can be uniquely directly changed into the renewable energy of carbonaceous liquid fuel, develops and uses it in fossil
Today that fuel is increasingly depleted and environment deteriorates increasingly becomes more and more important.The bio-crude oil being directly pyrolyzed by biomass
With properties such as high-moisture percentage, rich oxygen content, low heat value, highly acids, it is especially interior in existing heat power equipment seriously to hinder it
Use in combustion engine.Therefore, be added catalyst in the conversion process, carry out the catalytic pyrolysis of biomass or pyrolysis gas of biomass at
For improve bio-oil fuel grade effective means, wherein to pyrolysis gas of biomass carry out catalytic pyrolysis be advantageously implemented catalyst
Recovery and reusing and recycling, while be easily achieved pyrolysis and be catalyzed two parts temperature difference regulation.It is catalyzed and mentions online in bio oil
The catalyst being widely used in matter is HZSM-5 molecular sieve, and upgrading function and effect are the most obvious, obtain the extensive pass of researchers
Infuse (Tan S, Zhang ZJ, Sun JP, et al.Recent progress of catalytic pyrolysis of
biomass by HZSM-5[J].Chinese Journal of Catalysis,2013,34(4):641-650).But it is conventional
HZSM-5 is designed for petroleum industry, during bio oil online catalysis upgrading, the easy coking and deactivation (Wang of HZSM-5
J,Zhong ZP,Song ZW,et al.Modification and regeneration of HZSM-5 catalyst in
microwave assisted catalytic fast pyrolysis of mushroom waste[J].Energy
Conversion and Management, 2016,123:29-34), and polycyclic aromatic content is higher in hydrocarbon product
(Sun LZ,Zhang XD,Chen L,et al.Comparison of catalytic fast pyrolysis of
biomass to aromatic hydrocarbons over ZSM-5 and Fe/ZSM-5 catalysts[J].Journal
of Analytical and Applied Pyrolysis,2016,121:342-346).Valence can occur in catalytic process for Ti
State variation, meanwhile, the higher valence state of Ti ion and lesser radius make it have stronger polarizability, and catalysis can be remarkably reinforced
The cracking ability of agent.Catalyst can be improved to the selectivity of light hydrocarbons in Ti modification, delays the coking and deactivation of catalyst, is respectively changing
Property molecular sieve in show preferably (Cai YX, Fan YS, Li XH, et al.Preparation of refined bio-oil
by catalytic transformation of vapors derived from vacuum pyrolysis of rape
straw over modified HZSM-5[J].Energy,2016,102:95-105).Using dielectric barrier discharge mode
Low-temperature plasma synergistic catalysis is that the radical reaction for being caused electrion is reacted with the catalysis that catalyst is induced and had
A kind of new catalytic processing technique that machine combines.High voltage electric field provides big energy, anti-for decomposing, exciting and ionize
Object atom and molecule are answered, makes to change reactant rich in electronics, ion, free radical and excited state molecule in reactant and be catalyzed
The chemisorption behavior on agent surface improves selectivity (Fan YS, the Zhao WD, Shao of catalyst activity and chemical reaction
SS,et al.Promotion of the vapors from biomass vacuum pyrolysis for biofuels
under Non-thermal Plasma Synergistic Catalysis(NPSC)system[J].Energy,2018,
142:462-472)。
Although being modified to catalyst, and novel catalysis process is introduced, due to bio-crude oil or biology
Matter pyrolysis gas belongs to seriously scarce hydrogen feedstock (effective hydrogen-carbon ratio (H/C) eff is only 0.3-0.9), quite a few hydrogen in biomass
Element is present in pyrolysis gas (moisture content 25-50%) in the form of water, difficult to realize stablize to pyrolysis gas of biomass, hold
Continuous catalysis;Meanwhile the protium utilized can be shifted in aromatization become to be extremely limited, cause polycyclic aromatic hydrocarbons (PAH) etc. low
Hydrogen-carbon ratio product increases, and the dehydrogenation polymerization of polycyclic aromatic hydrocarbons (PAH) exacerbates catalyst coking.Currently, catalytic process is substantially
Sacrifice refined biological oil yield premise on promoted fuel grade, and promoted degree it is relatively limited (Castello D, He SB,
Ruiz MP,et al.Is it possible to increase the oil yield of catalytic pyrolysis
Of biomass A study using commercially-available acid and basic catalysts in
ex-situ and in-situ modus.Journal of Analytical and Applied Pyrolysis,2019,
137:77-85).In pyrolysis gas of biomass and the presence of moisture seriously affects conversion process in catalysate and product separation mentions
It is pure, if can individually dissociate the moisture in pyrolysis gas, more protiums can be not only provided for catalytic reforming reaction, improve essence
Biological oil yield and grade are made, and high energy electron generated, energetic free radical are living for activating and keeping catalyst surface
Property site play the role of it is positive, be conducive to inhibit catalyst coking.Currently, research there is no research or patent to propose to utilize moisture
The method that son participates in conversion process.
Microwave radiation is a kind of effective technology means that nonequilibrium plasma is generated using microwave, to specific gas molecule
Dissociation degree with higher generates up to 10000 DEG C of electronics and ion (Su under the premise of keeping original gas temperature
L,Kumar R,Ogungbesan B,et al.Experimental investigation of gas heating and
dissociation in a microwave plasma torch at atmospheric pressure[J].Energy
Conversion and Management,2014,78:695-703).Hydrone category polar molecule, dielectric constant is larger, is situated between
Matter loss factor is very high, has stronger absorbability to microwave, and the organic matters such as carbohydrate, methane, ethylene belong to mostly
In nonpolar molecule, dielectric constant is smaller, (Vesel A, Mozetic M, Drenik more much smaller than water to the absorbability of microwave
A,et al.Dissociation of CO2 molecules in microwave plasma[J].Chemical
Physics,2011,382(1-3):127-131).Therefore, microwave radiation is carried out to pyrolysis gas of biomass, can be more likely to dissociate
Hydrone therein, the electronics and ion energy of generation are enough to generate series of chemical, and gas temperature is then not too high,
Cause a large amount of decomposition of organic matter.Existing document report utilizes gas of the microwave radiation processing containing NO, H2O isopolarity molecule, meeting
It is allowed to part dissociation, excitation etc., generates active ion N free radical, O free radical, H free radical, OH free radical and high energy electron
Deng (Dalian research [D] of Tang Junwang conversion of NO with Microwave Irradiation: Dalian Inst of Chemicophysics, Chinese Academy of Sciences, 2001).
Currently, the technology is in the online catalysis upgrading research field of bio oil there is not yet document report.
Summary of the invention
Goal of the invention: present invention aims in view of the deficiencies of the prior art, provide a kind of high conversion efficiency, refined biological
Oil yield and fuel grade are higher, and the online catalysis upgrading method of bio oil that catalyst coking rate is low.
Technical solution: the method for microwave radiation assist medium barrier discharge catalysis upgrading bio oil of the present invention, including
Following steps:
S1, vacuum pyrolysis generation pyrolysis gas, vacuum pyrolysis condition are as follows: vacuum pressure 5- are carried out to granular biomass
10kPa, 15-20 DEG C of heating rate/min are pyrolyzed 500-550 DEG C of final temperature;
S2, the pyrolysis gas generated in step S1 is passed through to microwave radiation reactor, carries out microwave radiation excitation, microwave frequency
2450MHz, power 1200-1800W;
S3, microwave radiation is motivated after pyrolysis gas be passed through dielectric barrier discharge catalytic reactor, discharge frequency 30- again
50kHz, power 800-1000W, discharge section length 35-45mm, and catalyst Ti/HZSM-5, is urged by 350-400 DEG C of catalytic temperature
Agent layer length 25-35mm;
S4, to through step S3, treated that pyrolysis gas is condensed and extracted, wherein condensation temperature is -5~-10 DEG C, extraction
Taking agent is CH2Cl2, evaporative removal CH after the completion of extraction2Cl2, obtain refining biological oil.
Further preferably technical solution is the present invention, and biological particles partial size is 0.1~3.0mm.
Preferably, microwave radiation reactor is quartz material, wall thickness of quartz tube degree 2-3mm, inside radius 15- in step S2
25mm, length 25-35mm.
Preferably, dielectric barrier discharge catalytic reactor described in step S3 is quartz material, outer layer covers copper mesh conduct
Low-field electrode, the coaxial stainless steel blind pipe of center arrangement is as high-field electrode, discharging gap 10-15mm, places K in stainless steel blind pipe
Type thermometric galvanic couple, for measuring catalytic temperature.
Preferably, the import of the microwave radiation reactor and the dielectric barrier discharge catalytic reactor be 45 ° gradually
Expand shape, outlet is 45 ° tapered.
Preferably, catalyst Ti/HZSM-5 is prepared using infusion process in step S3, grain diameter 1-3mm, silica alumina ratio 50,
The Ti species of load are Ti2O3Or Ti3O5, Ti element load capacity 5%.
Preferably, which is to install ceramic electric heating additional in the dielectric barrier discharge catalytic reactor outer layer
Set, heating zone length 25-35mm are Chong Die with catalyst layer.
Preferably, catalyst layer is located in dielectric barrier discharge area.
Preferably, evaporative removal CH in step S42Cl2Condition be 40 DEG C of waters bath with thermostatic control or oil bath.
The utility model has the advantages that granular biomass successively to be carried out to vacuum pyrolysis, microwave radiation excitation, medium resistance in the present invention
Discharge catalytic, condensation and extraction step are kept off, the moisture contained in pyrolysis gas of biomass is can make full use of, is motivated activation,
With catalytic conversion efficiency height, the characteristics of refined biological oil yield is high, fuel grade is high and catalyst low coking.
Detailed description of the invention
Fig. 1 is flow diagram of the invention;
Fig. 2 is the total ion current figure that refining biological oil GC-MS is analyzed in embodiment 1;
Fig. 3 is the total ion current figure that refining biological oil GC-MS is analyzed in embodiment 2.
Specific embodiment
Technical solution of the present invention is described in detail below by attached drawing, but protection scope of the present invention is not limited to
The embodiment.
Embodiment 1: using rape stalk as experimental raw, raw material particle size 0.1mm.The microwave radiation assist medium of the present embodiment
The method and step of barrier discharge catalysis upgrading bio oil are as follows: vacuum pyrolysis, vacuum pressure 5kPa, heating rate are carried out to biomass
15 DEG C/min, 500 DEG C of final temperature of pyrolysis;The pyrolysis gas that biomass vacuum pyrolysis generates is passed through into microwave radiation activated reactions device,
Middle microwave frequency 2450MHz, power 1200W;Pyrolysis gas after microwave radiation motivates is catalyzed instead by dielectric barrier discharge
Device is answered, discharge frequency 30kHz, power 800W, electric discharge section length 40mm, catalyst Ti/HZSM-5,350 DEG C of catalytic temperature, is urged
Agent layer length 30mm;Pyrolysis gas after discharge catalytic is condensed and extracted, wherein -5 DEG C of condensation temperature, extractant
CH2Cl2, after the completion of extraction in 40 DEG C of waters bath with thermostatic control evaporative removal CH2Cl2, obtain refining biological oil.
Being computed refined biological oil yield is 19.41%, 13.67% when not assisted using microwave radiation, it increases
5.74%.It is 38.19MJ/kg using ZDHW-5G type oxygen bomb type calorimeter instrument measurement refining biological oil higher calorific value, more not using micro-
34.03MJ/kg when wave radiation assists, increases 4.16MJ/kg;Refined biological oleic acid is measured using PHS-3 type digital pH meter
Property be 6.2, more using microwave radiation auxiliary when 5.25, increase 0.95;Refined raw is measured using capillary viscosimetry
Object oil kinematic viscosity is 4.70mm2/ s, 5.18mm when not assisted using microwave radiation2/ s, reduces 0.48mm2/s.It utilizes
The catalyst coking rate of 1 type synchronous solving of Thermo TGA/DSC measurement continuous use 2h is 2.10%, more not using micro-
8.85% when wave radiation assists, have dropped 6.75%.
Utilize the chemistry of refining biological oil obtained by Agilent 7890A/5975 type gas chromatography mass spectrometry (GC/MS) analysis-e/or determining
It is as shown in Figure 2 to test and analyze result for composition.The chemical composition of bio oil is listed in table 1, detects 20 kinds of main chemical combination altogether
Object, wherein oxygen-bearing organic matter only has 3 kinds, total content 6.53%;Remaining 17 kinds of compound belongs to hydro carbons, and total content is
93.47%.Testing result further illustrates the higher fuel grade of refining biological oil.
The primary chemical composition of refining biological oil is made in 1 embodiment 1 of table
Embodiment 2: using rape stalk as experimental raw, raw material particle size 3.0mm, the microwave radiation assist medium of the present embodiment
The method and step of barrier discharge catalysis upgrading bio oil are as follows: vacuum pyrolysis, vacuum pressure 10kPa, heating speed are carried out to biomass
20 DEG C/min of rate, 550 DEG C of final temperature of pyrolysis;The pyrolysis gas that biomass vacuum pyrolysis generates is passed through into microwave radiation activated reactions device,
Wherein microwave frequency 2450MHz, power 1800W;Pyrolysis gas after microwave radiation motivates is catalyzed by dielectric barrier discharge
Reactor, discharge frequency 50kHz, power 1000W, electric discharge section length 40mm, catalyst Ti/HZSM-5, catalytic temperature 400
DEG C, catalyst layer length 30mm;Pyrolysis gas after discharge catalytic is condensed and extracted, wherein -10 DEG C of condensation temperature, is extracted
Take agent CH2Cl2, after the completion of extraction in 40 DEG C of waters bath with thermostatic control evaporative removal CH2Cl2, obtain refining biological oil.
Being computed refined biological oil yield is 20.09%, 13.67% when not assisted using microwave radiation, it increases
6.42%.It is 38.66MJ/kg using ZDHW-5G type oxygen bomb type calorimeter instrument measurement refining biological oil higher calorific value, more not using micro-
34.03MJ/kg when wave radiation assists, increases 4.63MJ/kg;Refined biological oleic acid is measured using PHS-3 type digital pH meter
Property be 6.12, more using microwave radiation auxiliary when 5.25, increase 0.87;Refined raw is measured using capillary viscosimetry
Object oil kinematic viscosity is 4.68mm2/ s, 5.18mm when not assisted using microwave radiation2/ s, reduces 0.50mm2/s.It utilizes
The catalyst coking rate of 1 type synchronous solving of Thermo TGA/DSC measurement continuous use 2h is 1.98%, more not using micro-
8.44% when wave radiation assists, have dropped 6.46%.
Utilize the chemistry of refining biological oil obtained by Agilent 7890A/5975 type gas chromatography mass spectrometry (GC/MS) analysis-e/or determining
It is as shown in Figure 3 to test and analyze result for composition.The chemical composition of bio oil is listed in table 2, detects 21 kinds of main chemical combination altogether
Object, wherein oxygen-bearing organic matter only has 2 kinds, total content 6.00%;Remaining 19 kinds of compound belongs to hydro carbons, and total content is
94.00%.Testing result further illustrates the higher fuel grade of refining biological oil.
The primary chemical composition of refining biological oil is made in 2 embodiment 2 of table
As described above, must not be explained although the present invention has been indicated and described referring to specific preferred embodiment
For the limitation to invention itself.It without prejudice to the spirit and scope of the invention as defined in the appended claims, can be right
Various changes can be made in the form and details for it.
Claims (9)
1. a kind of method of microwave radiation assist medium barrier discharge catalysis upgrading bio oil, which is characterized in that including walking as follows
It is rapid:
S1, vacuum pyrolysis generation pyrolysis gas, vacuum pyrolysis condition are carried out to granular biomass are as follows: vacuum pressure 5-10kPa,
15-20 DEG C of heating rate/min is pyrolyzed 500-550 DEG C of final temperature;
S2, the pyrolysis gas generated in step S1 is passed through to microwave radiation reactor, carries out microwave radiation excitation, microwave frequency
2450MHz, power 1200-1800W;
S3, microwave radiation is motivated after pyrolysis gas be passed through dielectric barrier discharge catalytic reactor again, discharge frequency 30-50kHz,
Power 800-1000W, discharge section length 35-45mm, catalyst Ti/HZSM-5, and 350-400 DEG C of catalytic temperature, catalyst layer
Length 25-35mm;
S4, to through step S3, treated that pyrolysis gas is condensed and extracted, wherein condensation temperature is -5~-10 DEG C, extractant
For CH2Cl2, evaporative removal CH after the completion of extraction2Cl2, obtain refining biological oil.
2. the method for microwave radiation assist medium barrier discharge catalysis upgrading bio oil according to claim 1, feature
It is, biological particles partial size is 0.1~3.0mm.
3. the method for microwave radiation assist medium barrier discharge catalysis upgrading bio oil according to claim 1, feature
It is, microwave radiation reactor is quartz material, wall thickness of quartz tube degree 2-3mm, inside radius 15-25mm, length in step S2
For 25-35mm.
4. the method for microwave radiation assist medium barrier discharge catalysis upgrading bio oil according to claim 1, feature
Be, dielectric barrier discharge catalytic reactor described in step S3 is quartz material, outer layer covers copper mesh as low-field electrode, in
The heart arranges that coaxial stainless steel blind pipe is used as high-field electrode, discharging gap 10-15mm, placement K-type thermometric galvanic couple in stainless steel blind pipe,
For measuring catalytic temperature.
5. the method for microwave radiation assist medium barrier discharge catalysis upgrading bio oil according to claim 1, feature
It is, the import of the microwave radiation reactor and the dielectric barrier discharge catalytic reactor is 45 ° of gradually expanded forms, and outlet is equal
It is tapered for 45 °.
6. the method for microwave radiation assist medium barrier discharge catalysis upgrading bio oil according to claim 1, feature
It is, catalyst Ti/HZSM-5 is prepared using infusion process in step S3, grain diameter 1-3mm, silica alumina ratio 50, the Ti object of load
Kind is Ti2O3Or Ti3O5, Ti element load capacity 5%.
7. the method for microwave radiation assist medium barrier discharge catalysis upgrading bio oil according to claim 6, feature
It is, which is to install ceramic electrical hot jacket, heating zone additional in the dielectric barrier discharge catalytic reactor outer layer
Length 25-35mm, it is Chong Die with catalyst layer.
8. the method for microwave radiation assist medium barrier discharge catalysis upgrading bio oil according to claim 7, feature
It is, catalyst layer is located in dielectric barrier discharge area.
9. the method for microwave radiation assist medium barrier discharge catalysis upgrading bio oil according to claim 1, feature
It is, evaporative removal CH in step S42Cl2Condition be 40 DEG C of waters bath with thermostatic control or oil bath.
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