CN106495135B - The method that graphene is prepared by stalk, forest or its byproduct - Google Patents
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Abstract
The invention discloses a kind of methods preparing graphene by stalk, forest or its byproduct, belong to stalk, forest technical field of comprehensive utilization.The present invention starts with from plant fiber extraction and purifying first, has obtained the plant fiber of high-purity；On this basis, by techniques such as gas making, charings, good graphene finished product has been obtained.Equipment is simple, technical maturity, easy to spread and implement.When extraction and purify plant fiber, using special protease and amylase, protein and starch are eliminated at normal temperatures；Normal temperature condition avoids the change of plant fiber molecular radical well, farthest maintains the complete state of plant fiber.In addition, when plant fiber extracts, using room temperature and the hyperbaric environment of inert gas offer；High pressure, which ensure that, breaks through cell wall, efficiently prepares plant fiber in steam explosion extraction process；Room temperature and inert environments avoid the change of plant fiber molecular radical, farthest maintain the complete state of plant fiber.
Description
Technical field
The present invention relates to stalk, forest technical field of comprehensive utilization, more particularly to one kind is by stalk, forest or its byproduct
The method for preparing graphene.
Background technology
Graphene（Graphene）It is the only one layer of atomic thickness for being stripped out from graphite material, being made of carbon atom
Two dimensional crystal.The strongest a kind of novel nano material of most thin, maximum intensity, electrical and thermal conductivity performance as presently found thickness
Material, graphene are referred to as " king of new material ".Ideal graphene-structured is plane hexagonal lattice, can be regarded as one layer of quilt
The graphitic molecules of stripping, each carbon atom are sp2Hydridization, and contribute the big pi bond that electronically forms on a remaining p track, π electricity
Son can move freely, and assign the good electric conductivity of graphene.At present there are mainly two types of the synthetic methods of graphene：Mechanical means
And chemical method.Mechanical means includes micromechanics partition method, epitaxy method and the method for heating SiC；Chemical method is chemistry
Reduction method and chemical dissociation method.Main raw material(s) is non-renewable graphite ore.
Stalk, forest or its byproduct are mainly made of cellulose, hemicellulose, lignin etc., and it is to plant to add up to quality
80-the 95% of object butt quality is the main source of plant fiber.Cellulose, lignin in plant fiber are natures
Middle content occupy first, organic carbon resource of deputy natural reproducible, is the main composition composition of plant cell wall.According to
It measures, the mass fraction of carbon atom is 60% or so in plant fiber.Thus plant fiber, which will likely become, prepares graphene the most
Important raw material.
The prior art not yet finds the side that graphene is directly prepared using stalk, forest or its byproduct of simple possible
Method.
Invention content
In order to make up for the deficiencies of the prior art, the present invention provides one kind preparing graphite by stalk, forest or its byproduct
The method of alkene.
The technical scheme is that：
A method of graphene, including step are prepared by stalk, forest or its byproduct：
The extraction of A plant fibers
A1）Stalk, forest or its byproduct crush after pretreatment, are placed in steam-explosion jar, are passed through into the steam-explosion jar
Inert gas seals after emptying air in tank；It is 1-5 MPa to continue to be passed through inert gas to pressure, after pressurize 20-120 minutes
It spurts, obtains steam explosion powder；
A2）The steam explosion powder is placed in steam-explosion jar, and the water of 1-20 times of quality of steam explosion powder is added, is passed through indifferent gas
Body so that steam explosion powder is uniformly distributed, and compound protease is then added, and is digested 10-80 minutes；Normal temperature type alphalise starch is then added
Enzyme digests 10-80 minutes；It then passes to steam and is warming up to 60-75 DEG C, keep the temperature 2-20 minutes, the activity of inactivator；It is described compound
Protease is formed by having the alkali protease of endopeptidase activity and having the active Proteinase K of peptide ending enzyme；The normal temperature type α-
Amylase by microwave induced gained variation bacillus licheniformis secretion gained alpha-amylase, the normal temperature type alpha-amylase it is suitable
Temperature is 22-35 DEG C；
A3）After enzyme deactivation, wait for that temperature is down to room temperature in steam-explosion jar, it is 1-5 MPa, pressurize 60- to be passed through inert gas to pressure
It is spurted after 200 minutes；
A4）Step A3）Gained spurts slurry separation of solid and liquid, obtains filter residue and filtrate；Filter residue be washed with water after through drying, powder
It is broken to obtain plant fiber；
B plant fiber gas making
By step A4）Gained plant fiber is placed in Gas-making Furnace, and set temperature is 80-300 DEG C, time 2-24 hour；Plant
Fiber is obtained after Gas-making Furnace is handled comprising the plant fiber carbonaceous gas including carbon monoxide, methane, propane；
C prepares graphene by plant fiber carbonaceous gas
C1）Metal foil is set in reaction kettle as depositing base, the depositing base is covered with reaction kettle, to reaction kettle
It is inside passed through inert gas, empties air rear enclosed；
C2）It will be passed through reaction kettle comprising the plant fiber carbonaceous gas including carbon monoxide, methane, propane obtained by step B,
It then passes to inert gas and is forced into 0.5-10 MPa, be warming up to 200-700 DEG C and carbonize 1-6 minutes, be continuously heating to 1000-
2000 DEG C carbonize 0.5-5 minutes；
C3）The gas in reaction kettle is released, the film on the depositing base is graphene.
Preferably, step A1）Described in pretreatment include clean, rub silk, segment, drying process；Step A1）In
The crushing is that stalk, forest or its byproduct are crushed to 30-50 mesh.It is crushed to 30-50 mesh, specific surface area is larger, extraction
More fully.
Preferably, step A1）In, the addition of stalk, forest or its byproduct reaches the 5%- of tank body volume
50%.The addition of material cannot be excessive, and excessively steam explosion effect is poor.
Preferably, the obtaining step of the microwave induced gained variation bacillus licheniformis is specially：By lichens
The culture solution of bacillus is placed in microwave generator, and setting microwave power is 850-950W, pulse frequency 2300MHz, microwave
20s, cooling 20s are handled, it is 25-35 times reciprocal according to this；Culture solution after microwave treatment is coated on solid medium, 30 DEG C of items
It is cultivated 1-2 days under part, by the high bacillus licheniformis of alpha-amylase activity under four plants of room temperature of screening in the bacterium colony that survives
Dissociant.
Further, the dissociant for selecting the highest bacillus licheniformis of alpha-amylase activity under room temperature expands culture,
To obtain the normal temperature type alpha-amylase.Gained normal temperature type alpha-amylase of the invention can hydrolyze shallow lake well at normal temperatures
Powder, can go out starch impurities in a mild condition, and the starch of enzymolysis removal at normal temperatures can prevent cellulose, lignin, half fiber
The molecular structure group of dimension element etc. changes, to obtain pure plant fiber.In addition, room temperature enzymolysis can be reduced to equipment
Demand, and need not heat, greatly reduce cost.
Preferably, the addition of the normal temperature type alpha-amylase meets every kilogram of butt steam explosion powder 200-
700U。
Preferably, have the alkali protease of endopeptidase activity in the compound protease and have peptide ending enzyme work
Property Proteinase K ratio be 1:1-3；The addition of the compound protease meets every kilogram of butt steam explosion powder 300-
800U。
Preferably, for step B plant fibers when Gas-making Furnace is handled, set temperature is 130-200 DEG C, time 5-15
Hour；The Gas-making Furnace has detar, de- flue dust, dehydration vapour purification function.
Preferably, step C1）In, the metal foil is nickel foil piece or copper foil；If the depositing base by
Dry metal foil is composed, and the area of each metal foil is 1-100cm2。
Preferably, step C2）In, it is passed through inert gas and is forced into 1.5-6MPa, be warming up to 300-600 DEG C of charing
It 2-4 minutes, is continuously heating to 1200-1800 DEG C and carbonizes 1.5-3 minutes.Using two step charrings, in plant fiber carbonaceous gas
The abjections such as hydrogen, oxygen atom and carbon atom deposition is adsorbed on metal foil substrate surface, it is continuous to grow, to obtain graphene.
Beneficial effects of the present invention are：
The present invention starts with from plant fiber extraction and purifying first, has obtained the plant fiber of high-purity；On this basis,
By techniques such as gas making, charings, good graphene finished product has been obtained.Equipment is simple, technical maturity, easy to spread and implement.
When the present invention is extracted with purify plant fiber, using special protease and special amylase, in room temperature item
Protein and starch are eliminated under part；Under room temperature condition avoid well lignin in plant fiber, hemicellulose and
The change of cellulosic molecule group farthest maintains the complete state of plant fiber.In addition, when plant fiber extracts, adopt
The hyperbaric environment provided with room temperature and inert gas；Condition of high voltage, which ensure that, generates rushing from inside to outside in steam explosion extraction process
Power is hit to break through cell wall, high efficiency extraction plant fiber；Room temperature and inert gas environment equally well avoid plant fibre
The change of lignin, hemicellulose and cellulosic molecule group in dimension farthest maintains the complete state of plant fiber.
Above 2 points are that gas making below and carbonization prepare high-quality graphene and lay a good foundation.
Specific implementation mode
Embodiment 1
A method of graphene, including step are prepared by stalk：
The extraction of A plant fibers
A1）Maize straw is placed in through cleaning, rubbing silk, segment, crushed after being dried to 40 mesh in steam-explosion jar（Maize straw
Addition reaches the 20% of tank body volume）, it is passed through after nitrogen empties air in tank and seals into steam-explosion jar；Continue to be passed through nitrogen
It is 2 MPa to pressure, pressurize is spurted after 80 minutes, obtains steam explosion powder.
Step A1）Cell wall is broken through spurting the impact force from inside to outside generated in the process using high pressure gas, is made thin
The tolerant whole of intracellular " broken wall and go out " is conducive to the enzymolysis removing of the impurity compositions such as protein, the starch of next step；Protein, shallow lake
The compositions such as powder exist only in into the cell, thus must broken wall.Room temperature explosion and inert gas environment can effectively avoid plant fibre
Dimension（Lignin, hemicellulose, cellulose）The variation of molecular radical, to ensure the complete state of plant fiber.
A2）Steam explosion powder is placed in steam-explosion jar, and the water of 10 times of quality of steam explosion powder is added, is passed through nitrogen so that vapour
Quick-fried powder is uniformly distributed, and compound protease is then added（500U/Kg butt steam explosion powder）, digest 40 minutes；It is then added normal
Warm type alpha-amylase（400U/Kg butt steam explosion powder）, digest 30 minutes；It then passes to steam and is warming up to 65 DEG C, keep the temperature 10 points
Clock, the activity of inactivator.
Wherein, compound protease is by having the alkali protease of endopeptidase activity and having the active Proteinase K of peptide ending enzyme
It forms, the alkali protease for having endopeptidase activity in compound protease is with the ratio for having the active Proteinase K of peptide ending enzyme
1: 1；The compound protease can effectively hydrolyzing protein at normal temperatures.
Normal temperature type alpha-amylase is by microwave induced gained variation bacillus licheniformis secretion gained alpha-amylase；It is microwave induced
Gained variation bacillus licheniformis obtaining step be specially：The culture solution of bacillus licheniformis is placed in microwave generator, if
It is 900W, pulse frequency 2300MHz, microwave treatment 20s to set microwave power, cooling 20s, reciprocal 30 times according to this；At microwave
Culture solution after reason is coated on solid medium, is cultivated 1-2 days under the conditions of 30 DEG C, by screening four plants in the bacterium colony that survives
The dissociant of the high bacillus licheniformis of alpha-amylase activity under room temperature.Select the highest lichens of alpha-amylase activity under room temperature
The dissociant of bacillus expands culture, to obtain normal temperature type alpha-amylase；Normal temperature type alpha-amylase is in 22-35 DEG C of temperature
Under expeditiously hydrolyze starch, it is not necessary to as the thermal-stable α-amylase mostly used greatly at present needs high temperature（80-90℃）Condition, because
And reduce energy consumption and also reduce requirement to equipment, while greatly reducing the generation of side reaction.
It herein can be mildly by protein, Starch Hydrolysis at the peptides of small molecule, amino acid, maltose, Portugal with enzyme process
Grape sugar etc. enters in filtrate, to success deproteination matter and starch, to ensure the purity of plant fiber.
Steam explosion under room temperature, high pressure, referred to as " empty quick-fried ".The empty quick-fried method of high pressure is used herein, it is therefore intended that both really
Protect composition in plant fiber（Cellulose, hemicellulose, lignin）Between separation, and avoid the degradation of composition in plant fiber
With loss, high yield pulp1, the high activity of plant fiber are fully ensured that.
A3）After enzyme deactivation, wait for that temperature is down to room temperature in steam-explosion jar, it is 2 MPa to be passed through nitrogen to pressure, after pressurize 100 minutes
It spurts.
A4）Step A3）Gained spurts slurry and is separated by solid-liquid separation through press master shove, obtains filter residue and filtrate；Filter residue is washed with water
After washing 3 times through drying, crush to obtain plant fiber.
B plant fiber gas making
By step A4）Gained plant fiber is placed in Gas-making Furnace（There is Gas-making Furnace detar, de- flue dust, dehydration vapour to purify work(
Energy）, set temperature is 180 DEG C, 10 hours time；Plant fiber obtained after Gas-making Furnace is handled purification comprising carbon monoxide,
Plant fiber carbonaceous gas including methane, propane.
C prepares graphene by plant fiber carbonaceous gas
C1）Nickel foil piece is set in reaction kettle by way of holder paste, and the area of each nickel foil piece is 10cm2, nickel foil
Piece is covered with reaction kettle as depositing base, and nitrogen is passed through into reaction kettle, empties air rear enclosed.
C2）It will be passed through reaction kettle comprising the plant fiber carbonaceous gas including carbon monoxide, methane, propane obtained by step B,
It then passes to nitrogen and is forced into 4MPa, be warming up to 360 DEG C and carbonize 3 minutes, be continuously heating to 1200 DEG C and carbonize 2 minutes.Using two
Walk charring, the abjections such as hydrogen, oxygen atom in plant fiber carbonaceous gas and carbon atom deposition is adsorbed on nickel foil matrix surface, even
Continuous growth, to obtain graphene.
C3）The gas in reaction kettle is released rapidly, and the film on depositing base is graphene.After testing, the present embodiment
The graphene film layer thickness being prepared is 0.51nm.
Embodiment 2
A method of graphene, including step are prepared by Eucalyptus：
The extraction of A plant fibers
A1）Eucalyptus through cleaning, chipping, crushed after being dried to 40 mesh, be placed in steam-explosion jar（The addition of Eucalyptus reaches tank body
The 30% of volume）, it is passed through after nitrogen empties air in tank and seals into steam-explosion jar；Continue to be passed through nitrogen to pressure to be 3MPa, protect
Pressure is spurted after 100 minutes, obtains steam explosion powder.
Step A1）Cell wall is broken through spurting the impact force from inside to outside generated in the process using high pressure gas, is made thin
The tolerant whole of intracellular " broken wall and go out " is conducive to the enzymolysis removing of the impurity compositions such as protein, the starch of next step；Protein, shallow lake
The compositions such as powder exist only in into the cell, thus must broken wall.Room temperature explosion and inert gas environment can effectively avoid plant fibre
Dimension（Lignin, hemicellulose, cellulose）The variation of molecular radical, to ensure the complete state of plant fiber.
A2）Steam explosion powder is placed in steam-explosion jar, and the water of 12 times of quality of steam explosion powder is added, is passed through nitrogen so that vapour
Quick-fried powder is uniformly distributed, and compound protease is then added（600U/Kg butt steam explosion powder）, digest 30 minutes；It is then added normal
Warm type alpha-amylase（500U/Kg butt steam explosion powder）, digest 20 minutes；It then passes to steam and is warming up to 70 DEG C, keep the temperature 8 points
Clock, the activity of inactivator.
Wherein, compound protease is by having the alkali protease of endopeptidase activity and having the active Proteinase K of peptide ending enzyme
It forms, the alkali protease for having endopeptidase activity in compound protease is with the ratio for having the active Proteinase K of peptide ending enzyme
1: 2；The compound protease can effectively hydrolyzing protein at normal temperatures.
Normal temperature type alpha-amylase is by microwave induced gained variation bacillus licheniformis secretion gained alpha-amylase；It is microwave induced
Gained variation bacillus licheniformis obtaining step be specially：The culture solution of bacillus licheniformis is placed in microwave generator, if
It is 900W, pulse frequency 2300MHz, microwave treatment 20s to set microwave power, cooling 20s, reciprocal 30 times according to this；At microwave
Culture solution after reason is coated on solid medium, is cultivated 1-2 days under the conditions of 30 DEG C, by screening four plants in the bacterium colony that survives
The dissociant of the high bacillus licheniformis of alpha-amylase activity under room temperature.Select the highest lichens of alpha-amylase activity under room temperature
The dissociant of bacillus expands culture, to obtain normal temperature type alpha-amylase；Normal temperature type alpha-amylase is in 22-35 DEG C of temperature
Under expeditiously hydrolyze starch, it is not necessary to as the thermal-stable α-amylase mostly used greatly at present needs high temperature（80-90℃）Condition, because
And reduce energy consumption and also reduce requirement to equipment, while greatly reducing the generation of side reaction.
It herein can be mildly by protein, Starch Hydrolysis at the peptides of small molecule, amino acid, maltose, Portugal with enzyme process
Grape sugar etc. enters in filtrate, to success deproteination matter and starch, to ensure the purity of plant fiber.
Steam explosion under room temperature, high pressure, referred to as " empty quick-fried ".The empty quick-fried method of high pressure is used herein, it is therefore intended that both really
Protect composition in plant fiber（Cellulose, hemicellulose, lignin）Between separation, and avoid the degradation of composition in plant fiber
With loss, high yield pulp1, the high activity of plant fiber are fully ensured that.
A3）After enzyme deactivation, wait for that temperature is down to room temperature in steam-explosion jar, it is 3 MPa to be passed through nitrogen to pressure, and pressurize is sprayed after 90 minutes
It puts.
A4）Step A3）Gained spurts slurry and is separated by solid-liquid separation through filter press press filtration, obtains filter residue and filtrate；Filter residue is washed with water
After washing 4 times through drying, crush to obtain plant fiber.
B plant fiber gas making
By step A4）Gained plant fiber is placed in Gas-making Furnace（There is Gas-making Furnace detar, de- flue dust, dehydration vapour to purify work(
Energy）, set temperature is 200 DEG C, 15 hours time；Plant fiber obtained after Gas-making Furnace is handled purification comprising carbon monoxide,
Plant fiber carbonaceous gas including methane, propane.
C prepares graphene by plant fiber carbonaceous gas
C1）Copper foil is set in reaction kettle by way of holder paste, and the area of each copper foil is 15cm2, copper foil
Piece is covered with reaction kettle as depositing base, and nitrogen is passed through into reaction kettle, empties air rear enclosed.
C2）It will be passed through reaction kettle comprising the plant fiber carbonaceous gas including carbon monoxide, methane, propane obtained by step B,
It then passes to nitrogen and is forced into 5 MPa, be warming up to 400 DEG C and carbonize 4 minutes, be continuously heating to 1500 DEG C and carbonize 3 minutes.Using two
Walk charring, the abjections such as hydrogen, oxygen atom in plant fiber carbonaceous gas and carbon atom deposition is adsorbed on copper foil matrix surface, even
Continuous growth, to obtain graphene.
C3）The gas in reaction kettle is released rapidly, and the film on depositing base is graphene.After testing, the present embodiment
The graphene film layer thickness being prepared is 0.48nm.
Claims (9)
1. a kind of method preparing graphene by stalk, forest or its byproduct, which is characterized in that including step：
The extraction of A plant fibers
A1）Stalk, forest or its byproduct crush after pretreatment, are placed in steam-explosion jar, and inertia is passed through into the steam-explosion jar
Gas seals after emptying air in tank；Continue to be passed through inert gas to pressure to be 1-5 MPa, pressurize is sprayed after 20-120 minutes
It puts, obtains steam explosion powder；
A2）The steam explosion powder is placed in steam-explosion jar, and the water of 1-20 times of quality of steam explosion powder is added, is passed through inert gas,
So that steam explosion powder is uniformly distributed, compound protease is then added, digests 10-80 minutes；Normal temperature type alpha-amylase is then added,
Enzymolysis 10-80 minutes；It then passes to steam and is warming up to 60-75 DEG C, keep the temperature 2-20 minutes, the activity of inactivator；The compound egg
White enzyme is formed by having the alkali protease of endopeptidase activity and having the active Proteinase K of peptide ending enzyme；Normal temperature type α-the shallow lake
Powder enzyme is by microwave induced gained variation bacillus licheniformis secretion gained alpha-amylase, the suitable temperature of the normal temperature type alpha-amylase
Degree is 22-35 DEG C；
The obtaining step of the microwave induced gained variation bacillus licheniformis is specially：The culture solution of bacillus licheniformis is set
In microwave generator, setting microwave power is 850-950W, pulse frequency 2300MHz, microwave treatment 20s, cools down 20s, according to
This is 25-35 times reciprocal；Culture solution after microwave treatment is coated on solid medium, is cultivated 1-2 days under the conditions of 30 DEG C, by depositing
The dissociant of the high bacillus licheniformis of alpha-amylase activity under four plants of room temperature is screened in the bacterium colony survived；
A3）After enzyme deactivation, wait for that temperature is down to room temperature in steam-explosion jar, it is 1-5 MPa, 60-200 points of pressurize to be passed through inert gas to pressure
It is spurted after clock；
A4）Step A3）Gained spurts slurry separation of solid and liquid, obtains filter residue and filtrate；Filter residue be washed with water after through drying, crush
Plant fiber；
B plant fiber gas making
By step A4）Gained plant fiber is placed in Gas-making Furnace, and set temperature is 80-300 DEG C, time 2-24 hour；Plant fiber
It is obtained comprising the plant fiber carbonaceous gas including carbon monoxide, methane, propane after Gas-making Furnace is handled；
C prepares graphene by plant fiber carbonaceous gas
C1）Metal foil is set in reaction kettle as depositing base, the depositing base is covered with reaction kettle, leads into reaction kettle
Enter inert gas, empties air rear enclosed；
C2）It will be passed through reaction kettle comprising the plant fiber carbonaceous gas including carbon monoxide, methane, propane obtained by step B, then
It is passed through inert gas and is forced into 0.5-10 MPa, be warming up to 200-700 DEG C and carbonize 1-6 minutes, be continuously heating to 1000-2000 DEG C
Charing 0.5-5 minutes；
C3）The gas in reaction kettle is released, the film on the depositing base is graphene.
2. the method for preparing graphene by stalk, forest or its byproduct as described in claim 1, it is characterised in that：Step A1）
Described in pretreatment include clean, rub silk, segment, drying process；Step A1）Described in crush be by stalk, forest or it is secondary
Product is crushed to 30-50 mesh.
3. the method for preparing graphene by stalk, forest or its byproduct as described in claim 1, it is characterised in that：Step A1）
In, the addition of stalk, forest or its byproduct reaches the 5%-50% of tank body volume.
4. the method for preparing graphene by stalk, forest or its byproduct as described in claim 1, it is characterised in that：It selects often
The dissociant of the lower highest bacillus licheniformis of alpha-amylase activity of temperature expands culture, to obtain the normal temperature type alphalise starch
Enzyme.
5. the method for preparing graphene by stalk, forest or its byproduct as described in claim 1 or 4, it is characterised in that：It is described
The addition of normal temperature type alpha-amylase meets every kilogram of butt steam explosion powder 200-700U.
6. the method for preparing graphene by stalk, forest or its byproduct as described in claim 1, it is characterised in that：It is described multiple
It is 1 to have the alkali protease of endopeptidase activity in hop protein enzyme and have the ratio of the active Proteinase K of peptide ending enzyme:1-3；Institute
The addition for stating compound protease meets every kilogram of butt steam explosion powder 300-800U.
7. the method for preparing graphene by stalk, forest or its byproduct as described in claim 1, it is characterised in that：Step B plants
For fibres when Gas-making Furnace is handled, set temperature is 130-200 DEG C, time 5-15 hour；The Gas-making Furnace has detar, takes off
Flue dust, dehydration vapour purification function.
8. the method for preparing graphene by stalk, forest or its byproduct as described in claim 1, it is characterised in that：Step C1）
In, the metal foil is nickel foil piece or copper foil；The depositing base is composed of several metal foils, each metal foil
Area be 1-100cm2。
9. the method for preparing graphene by stalk, forest or its byproduct as described in claim 1, it is characterised in that：Step C2）
In, it is passed through inert gas and is forced into 1.5-6MPa, be warming up to 300-600 DEG C and carbonize 2-4 minutes, be continuously heating to 1200-1800
DEG C charing 1.5-3 minutes.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1896252A (en) * | 2006-06-24 | 2007-01-17 | 中国科学技术大学 | Production of marsh-gas by organic efficient anaerobic fermentation |
| CN102220566A (en) * | 2011-06-09 | 2011-10-19 | 无锡第六元素高科技发展有限公司 | Method for preparing single-layer or multi-layer graphene through chemical vapor deposition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1896252A (en) * | 2006-06-24 | 2007-01-17 | 中国科学技术大学 | Production of marsh-gas by organic efficient anaerobic fermentation |
| CN102220566A (en) * | 2011-06-09 | 2011-10-19 | 无锡第六元素高科技发展有限公司 | Method for preparing single-layer or multi-layer graphene through chemical vapor deposition |
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