CN107083252A - A kind of chemical chain pyrolysis deoxidization technique that can reduce biomass pyrolysis oil oxygen content and system - Google Patents
A kind of chemical chain pyrolysis deoxidization technique that can reduce biomass pyrolysis oil oxygen content and system Download PDFInfo
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- CN107083252A CN107083252A CN201710269727.3A CN201710269727A CN107083252A CN 107083252 A CN107083252 A CN 107083252A CN 201710269727 A CN201710269727 A CN 201710269727A CN 107083252 A CN107083252 A CN 107083252A
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- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
-
- 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
-
- 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
-
- 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
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- 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
- C10G2300/70—Catalyst aspects
Abstract
Deoxidization technique is pyrolyzed the invention discloses a kind of chemical chain that can reduce biomass pyrolysis oil oxygen content, the technology utilization metal simple-substance or lower valency metal oxide are as dehydrogenation catalyst to biomass pyrolytic deoxidation, metal simple-substance or lower valency metal oxide are oxidized to high-valence state metal oxide, the gas-phase product of biomass pyrolytic is subjected to catalytic reforming, and it is condensed after obtain biomass pyrolysis oil;High-valence state metal oxide is reduced to metal simple-substance simultaneously or lower valency metal oxide is recycled.The invention also discloses the system that above-mentioned chemical chain pyrolysis deoxidization technique is used.Chemical chain pyrolysis deoxidization technique of the present invention can effectively reduce the oxygen content of biomass pyrolysis oil, improve the quality of pyrolysis oil.
Description
Technical field
Deoxidization technique is pyrolyzed the present invention relates to a kind of chemical chain that can reduce biomass pyrolysis oil oxygen content, is also related to
The system that technique is used is stated, belongs to catalytic pyrolysis of biomass field.
Background technology
A large amount of consumption of fossil energy cause a series of environment and resource problem, and rational exploitation and utilization biomass resource is
Alleviate the important channel of the serious energy environment issues of China.The Land use systems of current biomass energy include biochemical process, chemistry
Method and thermochemical method etc..As one kind in thermochemical method, catalytic pyrolysis of biomass method for producing oil enjoys domestic and international concern, the party
Method is turned the biomass of the rich oxygen content of low energy densities by the production technology of relatively low cost and serialization by catalyst
The bio oil of the low oxygen content of high-energy-density is turned to, part is expected to and substitutes traditional petrol and diesel oil.
To realize the deoxidation of biomass pyrolysis process, research both at home and abroad focuses mostly in the research and development of catalyst, and to biology
Innovation in terms of the deoxidization technique and reactor of matter pyrolytic process but more lacks.At present, on biomass pyrolysis oil deoxidation
Research is concentrated on substantially carries out hydrogenation deoxidation (HDO) using autoclave to the bio oil that pyrolysis is obtained, however, using this kind
Mode needs to consume substantial amounts of H2, and the reaction carries out in autoclave, undoubtedly adds the consumption of energy, improves
The upgrading cost of biomass pyrolytic liquefaction.For the problem, the present invention proposes a kind of efficient deoxidation being pyrolyzed based on chemical chain
Mode, i.e., during biomass pyrolytic, using efficient dehydrogenation catalyst carrier, in fluidisation bed chemical chain pyrolysis reactor
Biomass chemical chain pyrolysis (Chemical Looping Pyrolysis, CLP) pyrolysis deoxidation is carried out, biomass is not only proposed
CLP deoxidization techniques, it is also proposed that the biomass chemical chain for being pyrolyzed deoxidization technique for the biomass chemical chain is pyrolyzed deoxygenation system.
The content of the invention
Goal of the invention:The technical problems to be solved by the invention are to provide a kind of biomass pyrolysis oil oxygen content of reducing
Chemical chain is pyrolyzed deoxidization technique, and the chemical chain pyrolysis deoxygenation system involved by the technique, can effectively reduce biomass thermal
Solve the oxygen content of oil.
In order to solve the above technical problems, the technical solution adopted in the present invention is:
It is a kind of can reduce biomass pyrolysis oil oxygen content chemical chain pyrolysis deoxidization technique, the technology utilization metal simple-substance or
Lower valency metal oxide is as dehydrogenation catalyst to biomass pyrolytic deoxidation, and metal simple-substance or lower valency metal oxide are by oxygen
Turn to high-valence state metal oxide, the pyrolysis gas-phase product of biomass be subjected to catalytic reforming, and it is condensed after obtain biomass
Pyrolysis oil;High-valence state metal oxide is reduced to metal simple-substance simultaneously or lower valency metal oxide is recycled.
Wherein, the dehydrogenation catalyst is FeO/Fe3O4Reduction system, Zn/ZnO reduction systems, Cd/CdO reduction systems,
SnO/SnO2Reduction system and Ce2O3/CeO2One kind in reduction system.
Wherein, the dehydrogenation catalyst is preferably Zn/ZnO reduction systems, and Zn/ZnO systems are thought by thermodynamic analysis
Ideal, because Zn powder has the potentiality of form biomass pyrolysis deoxidation as a kind of excellent reducing agent, and Zn powder is oxidized
Product ZnO afterwards remains to preferable catalysis biomass hydrogenation deoxidation, test result indicates that:Gained is biological after Zn powder deoxidations
The relative amount that the oxygen content of oil have dropped acids in 23.92%, pyrolysis oil, alcohols and saccharide compound decreases, and
The relative amount of esters, carbonyl class and phenolic compound is then raised.
Wherein, the pyrolytic reaction is that temperature is 500~600 DEG C.
Wherein, the reaction temperature that the high-valence state metal oxide is reduced at high temperature is 800~1000 DEG C.
A kind of chemical chain pyrolysis deoxygenation system that can reduce biomass pyrolysis oil oxygen content, including pyrolysis reactor, reduction
Reactor, catalytic reforming reactor, condenser;Wherein, pyrolysis reactor and reduction reactor are placed in microwave heating equipment,
Pyrolysis reactor and reduction reactor are connected by pipeline with carrier gas bottle respectively, in the carrier gas of pyrolysis reactor and reduction reactor
Porch is equipped with carrier gas preheater;Biomass material is entered by first order screw feeder and second level screw feeder respectively
Enter in pyrolysis reactor;Pyrolysis reactor is by return channel and reduction reactor formation circulation loop, and pyrolysis reactor will high price
State metal oxide is sent into reduction reactor by return channel, and reduction reactor is golden by the metal simple-substance after reduction or lower valency
Belong in oxide feeding pyrolysis reactor;Pyrolysis gas-phase product in pyrolysis reactor enters catalytic reforming by cyclone separator
In reactor, the thermal decomposition product after catalytic reforming reactor catalysis upgrading, which enters in condenser, carries out fractional condensaion, after condensation
Obtain biomass pyrolysis oil.
Wherein, the pyrolysis reactor, reduction reactor and catalytic reforming reactor are connected to temperature control equipment,
Temperature control equipment detects the temperature in each reactor by thermocouple.
Wherein, the carrier gas bottle is nitrogen cylinder, and the carrier gas of pyrolytic reaction of the present invention is high pure nitrogen (99.999%).
Wherein, the catalytic reforming reactor is placed in microwave heating equipment, the reaction temperature in catalytic reforming reactor
For 550~600 DEG C;Catalyst used in catalytic reforming reactor is HZSM-5 molecular sieves, wherein, catalyst and biomass
Mass ratio be 2: 1.
Compared with prior art, technical solution of the present invention have the advantage that for:
Chemical chain pyrolysis deoxidization technique of the present invention can effectively reduce the oxygen content of biomass pyrolysis oil, improve pyrolysis oil
Quality, obtains substantial amounts of catalytic reforming predecessor;In pyrolysis reactor of the present invention and reduction reactor, using microwave radiation technology
Mode of heating, relative to traditional electric-heating technology, Microwave-assisted firing mode has homogeneous heating, saves energy consumption, without delayed
Effect, the advantage for being easy to operation and safety non-pollution, also, further to improve the heat-transfer effect of Microwave-assisted firing, this hair
Bright technique uses the carbon-based material for having superior absorbent performance to microwave to be arranged in as microwave absorption in microwave heating equipment, such as
Charcoal, activated carbon etc., so as to improve the heating rate of biomass material, realize that biomass is quick, be uniformly pyrolyzed;In addition, this hair
Bright chemical chain pyrolysis deoxidization technique carries out preliminary take off using ex situ catalytic reforming mode, i.e. biomass in pyrolysis reactor
Oxygen catalysis pyrolysis, the pyrolysis gas of the low oxygen content obtained, which enters in catalytic reforming reactor, carries out further catalytic reforming,
So as to be remarkably improved the catalytic activity of reforming catalyst, prevent caused by biomass pyrolytic carbon is covered in catalyst surface
Duct blocks coking phenomenon, improves the service efficiency of reforming catalyst;Finally, chemical chain pyrolysis deoxidization technique of the present invention has behaviour
Make the gentle advantage of easy, reaction condition, can effectively save energy consumption, reduction prepares the cost of biomass pyrolysis oil.
Brief description of the drawings
Fig. 1 is chemical chain pyrolysis concept map in biomass chemical chain of the present invention pyrolysis deoxidization technique;
Fig. 2 is the systematic schematic diagram that biomass chemical chain of the present invention is pyrolyzed deoxygenation system.
Embodiment
Technical scheme is described further below in conjunction with accompanying drawing, but the scope of protection of present invention is simultaneously
It is not limited to this.
A kind of chemical chain pyrolysis deoxidization technique that can reduce biomass pyrolysis oil oxygen content of the present invention, the technology utilization metal
Simple substance or lower valency metal oxide are as dehydrogenation catalyst to biomass pyrolytic deoxidation, metal simple-substance or the oxidation of lower valency metal
Thing is oxidized to high-valence state metal oxide, and the gas-phase product of biomass pyrolytic carried out into catalytic reforming, and it is condensed after obtain
Biomass pyrolysis oil;High-valence state metal oxide is reduced to metal simple-substance simultaneously or lower valency metal oxide carries out circulation profit
With, wherein, dehydrogenation catalyst is FeO/Fe3O4Reduction system, Zn/ZnO reduction systems, Cd/CdO reduction systems, SnO/SnO2Also
Substance system and Ce2O3/CeO2One kind in reduction system, preferably Zn/ZnO reduction systems.
The present invention can reduce biomass pyrolysis oil oxygen content chemical chain pyrolysis deoxygenation system, including pyrolysis reactor 10,
Reduction reactor 8, catalytic reforming reactor 22, condenser 23;Wherein, pyrolysis reactor 10 and reduction reactor 8 are placed in micro-
In Wave heating device 7, pyrolysis reactor 10 and reduction reactor 8 are connected by pipeline with nitrogen cylinder 1 respectively, in pyrolysis reactor
10 and reduction reactor 8 carrier gas inlet at be equipped with carrier gas preheater 11/12;N2As the carrier gas of pyrolytic reaction of the present invention,
Sent into carrier gas preheater 11/12 and preheated by the coutroi velocity of mass flowmenter 2, and then sent into pyrolysis reactor 10,
Keep the N needed for pyrolytic reaction2Atmosphere;Carrier gas preheater 11 is connected with temperature control equipment I14, and temperature control equipment I14 leads to
Thermocouple is crossed to detect and control the temperature in carrier gas preheater 11;Biomass material passes through first order screw feeder 3 respectively
Enter with second level screw feeder 4 in pyrolysis reactor 10;Pyrolysis reactor 10 passes through return channel 9 and the shape of reduction reactor 8
Into circulation loop, pyrolysis reactor 10 sends into high-valence state metal oxide in reduction reactor 8 by return channel 9, and reduction is anti-
Device 8 is answered to send into the metal simple-substance after reduction or lower valency metal oxide in pyrolysis reactor 10 by feeding pipe;Pyrolysis
Low oxygen content pyrolysis gas-phase product in reactor 10 after pyrolytic reaction enters catalytic reforming reactor by cyclone separator 21
Further catalysis upgrading is carried out in 22, wherein, the catalytic reforming reactor 22 also uses Microwave-assisted firing mode, is used
Catalyst is HZSM-5 molecular sieves, makes catalytic reforming temperature control between 550~600 DEG C by temperature control equipment II16,
Thermal decomposition product after completion catalysis upgrading, which enters in the condenser 23 being made up of mixture of ice and water, carries out fractional condensaion, passes through condensation
Obtained from liquid product be biomass pyrolysis oil;And other pyrolysis gaseous products that can not be condensed then are entered by collecting airbag 24
Row is collected, the composition of analysis product in gas chromatograph (GC).
Wherein, pyrolysis reactor 10 is also connected with temperature control equipment III13, temperature control equipment III13 control pyrolysis
Pyrolysis temperature in reactor 10 is maintained between 500~600 DEG C;Reduction reactor 8 is also connected with temperature control equipment IV15,
Reduction temperature in temperature control equipment IV15 control reduction reactors 8 is between 800~1000 DEG C.
Chemical chain of the present invention is pyrolyzed deoxidization technique, and pyrolysis reactor 10 is heated by microwave heating equipment 7, using temperature
Control device III13 adjustment pyrolysis temperatures are spent, make its control within 500~600 DEG C, meanwhile, dehydrogenation catalyst passes through conveying
Pipeline enters in pyrolysis reactor 10, after after abundant fluidisation, and biomass material is passed through into first order screw feeder 3 and the respectively
Deuterostrophies feeder 4 enters in pyrolysis reactor 10, chemical chain pyrolysis is carried out after being sufficiently mixed with catalyst carrier de-
Oxygen, the low oxygen content pyrolysis gas-phase product for completing to obtain after pyrolytic reaction enters catalytic reforming reactor by cyclone separator 21
22 carry out further catalysis upgrading, wherein, catalytic reforming reactor 22 also uses Microwave-assisted firing mode, and what is used urges
Agent is HZSM-5 molecular sieves, makes catalytic reforming temperature control between 550~600 DEG C by temperature control equipment II16, complete
Enter into the thermal decomposition product after catalysis upgrading in the condenser 23 being made up of mixture of ice and water and carry out fractional condensaion;Meanwhile, in heat
Solve and the dehydrogenation catalyst after biomass pyrolytic deoxygenation is completed in reactor 10, reduction reactor 8 is entered by material returning device 9
In, the reduction reactor 8 uses Microwave-assisted firing mode, and the temperature control of reduction reaction is made by temperature control equipment IV15
It is next by being carried out in feeding pipe feeding pyrolysis reactor 10 after treating that dehydrogenation catalyst is fully reduced at 800~1000 DEG C
The biomass pyrolytic deoxygenation of individual circulation, realizes the circulation of chemical chain.
Chemical chain pyrolysis deoxidization technique catalytic reforming reactor 22 of the present invention can be had using the catalytic reforming mode of ex situ
The anti-coking performance of effect enhancing catalytic reforming catalyst, the production for improving hydrocarbons in catalytic reforming effect, increase thermal decomposition product
Rate.
Obviously, above-described embodiment is only intended to clearly illustrate example of the present invention, and is not to the present invention
The restriction of embodiment.For those of ordinary skill in the field, it can also be made on the basis of the above description
Its various forms of changes or variation.There is no necessity and possibility to exhaust all the enbodiments.And these belong to this hair
Among the obvious changes or variations that bright spirit is extended out is still in protection scope of the present invention.
Claims (9)
1. a kind of chemical chain pyrolysis deoxidization technique that can reduce biomass pyrolysis oil oxygen content, it is characterised in that:The technology utilization
Metal simple-substance or lower valency metal oxide are as dehydrogenation catalyst to biomass pyrolytic deoxidation, metal simple-substance or lower valency metal
Oxide is oxidized to high-valence state metal oxide, and the gas-phase product of biomass pyrolytic carried out into catalytic reforming, and it is condensed after
Obtain biomass pyrolysis oil;High-valence state metal oxide is reduced to metal simple-substance simultaneously or lower valency metal oxide is followed
Ring is utilized.
2. the chemical chain pyrolysis deoxidization technique according to claim 1 that biomass pyrolysis oil oxygen content can be reduced, its feature
It is:The dehydrogenation catalyst is FeO/Fe3O4Reduction system, Zn/ZnO reduction systems, Cd/CdO reduction systems, SnO/SnO2
Reduction system and Ce2O3/CeO2One kind in reduction system.
3. the chemical chain pyrolysis deoxidization technique according to claim 1 that biomass pyrolysis oil oxygen content can be reduced, its feature
It is:The dehydrogenation catalyst is preferably Zn/ZnO reduction systems.
4. the chemical chain pyrolysis deoxidization technique according to claim 1 that biomass pyrolysis oil oxygen content can be reduced, its feature
It is:The pyrolysis reaction temperature is 500~600 DEG C.
5. the chemical chain pyrolysis deoxidization technique according to claim 1 that biomass pyrolysis oil oxygen content can be reduced, its feature
It is:The reaction temperature that the high-valence state metal oxide is reduced at high temperature is 800~1000 DEG C.
6. a kind of chemical chain pyrolysis deoxygenation system that can reduce biomass pyrolysis oil oxygen content, it is characterised in that:It is anti-including pyrolysis
Answer device, reduction reactor, catalytic reforming reactor, condenser;Wherein, pyrolysis reactor and reduction reactor are placed in microwave and added
In thermal, pyrolysis reactor and reduction reactor are connected by pipeline with carrier gas bottle respectively, anti-in pyrolysis reactor and reduction
Answer and carrier gas preheater is equipped with the carrier gas inlet of device;Biomass material passes through first order screw feeder and second level spiral shell respectively
Feeder is revolved to enter in pyrolysis reactor;Pyrolysis reactor is by return channel and reduction reactor formation circulation loop, and pyrolysis is anti-
Device is answered to send into high-valence state metal oxide in reduction reactor by return channel, reduction reactor is by the metal simple-substance after reduction
Or in lower valency metal oxide feeding pyrolysis reactor;Pyrolysis gas-phase product in pyrolysis reactor is entered by cyclone separator
Enter in catalytic reforming reactor, it is cold that the thermal decomposition product after catalytic reforming reactor catalysis upgrading enters progress classification in condenser
It is solidifying, biomass pyrolysis oil is obtained after condensation.
7. the chemical chain pyrolysis deoxygenation system according to claim 6 that biomass pyrolysis oil oxygen content can be reduced, its feature
It is:The pyrolysis reactor, reduction reactor and catalytic reforming reactor are connected to temperature control equipment, temperature control
Device detects the temperature in each reactor by thermocouple.
8. the chemical chain pyrolysis deoxygenation system according to claim 6 that biomass pyrolysis oil oxygen content can be reduced, its feature
It is:The catalytic reforming reactor is placed in microwave heating equipment, the reaction temperature in catalytic reforming reactor be 550~
600℃。
9. the chemical chain pyrolysis deoxygenation system according to claim 8 that biomass pyrolysis oil oxygen content can be reduced, its feature
It is:Catalyst used in the catalytic reforming reactor includes but is not limited to HZSM-5 molecular sieves, wherein, catalyst with
The mass ratio of biomass is 2: 1.
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CN107629815A (en) * | 2017-11-06 | 2018-01-26 | 南昌大学 | A kind of non-method for eating woody oil soap higher value application |
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CN107723008A (en) * | 2017-11-06 | 2018-02-23 | 南昌大学 | A kind of method of stalk discarded object Quick-gasifying |
CN107828439A (en) * | 2017-11-06 | 2018-03-23 | 南昌大学 | A kind of method for preparing biomass-based Aviation Fuel using stalk and waste plastic food bag |
CN107858169A (en) * | 2017-11-06 | 2018-03-30 | 南昌大学 | A kind of microwave radiation technology dual bed is catalyzed the method that fast pyrogenation stalk prepares biomass-based motor petrol with discarded soap stock altogether |
CN107652998A (en) * | 2017-11-06 | 2018-02-02 | 南昌大学 | A kind of method using biomass controlled syntheses aviation kerosine aromatic component |
CN107903932A (en) * | 2017-11-06 | 2018-04-13 | 南昌大学 | A kind of method using discarded LDPE: Low-density polyethylene plastics controlled syntheses aviation kerosine aromatic component |
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CN107903933A (en) * | 2017-11-06 | 2018-04-13 | 南昌大学 | A kind of method for preparing hydrocarbon-rich fuel oil using maize straw and rubbish from cooking |
CN107629815B (en) * | 2017-11-06 | 2019-10-01 | 南昌大学 | A kind of non-method for eating woody oil soap higher value application |
CN108728143A (en) * | 2018-05-28 | 2018-11-02 | 山东理工大学 | Biomass ex situ catalysis pyrolysis liquefaction system |
CN108840337A (en) * | 2018-07-27 | 2018-11-20 | 昆明理工大学 | A kind of integrated conduct method of low purity oxygen zinc and Peel of Navel Orange |
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Application publication date: 20170822 |