CN106744836A - A kind of method that utilization biomass material prepares Graphene - Google Patents

A kind of method that utilization biomass material prepares Graphene Download PDF

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Publication number
CN106744836A
CN106744836A CN201611083909.3A CN201611083909A CN106744836A CN 106744836 A CN106744836 A CN 106744836A CN 201611083909 A CN201611083909 A CN 201611083909A CN 106744836 A CN106744836 A CN 106744836A
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CN
China
Prior art keywords
biomass material
graphene
insulation
prepares graphene
utilization
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Pending
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CN201611083909.3A
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Chinese (zh)
Inventor
吴丽
侯银臣
安庆堂
安民
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Wenxian County Xingfa Biological Technology Co Ltd
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Wenxian County Xingfa Biological Technology Co Ltd
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Priority to CN201611083909.3A priority Critical patent/CN106744836A/en
Publication of CN106744836A publication Critical patent/CN106744836A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/32Size or surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/16Pore diameter

Abstract

A kind of method that utilization biomass material prepares Graphene.Mainly include the following steps that:Removal of impurities is carried out to biomass material, then it is crushed;Treated biomass material is mixed with chemical solvent, centre addition catalyst;Above-mentioned treated biomass material is carried out into high-temperature heating, and after obtain Graphene through ultra high pressure treatment.The preparation method of the Graphene that the present invention is provided is environmentally safe, and with biomass material as carbon source, the cost of raw material of carbon source is low and is readily available, and solves existing carbon source high cost, is unfavorable for the shortcoming of heavy industrialization.

Description

A kind of method that utilization biomass material prepares Graphene
Technical field:
The invention belongs to carbon material technical field, more particularly to a kind of method that utilization biomass material prepares Graphene.
Background technology
Graphene(Graphene)It is a kind of new material of the individual layer laminated structure being made up of carbon atom.It is a kind of former by carbon Son is with the flat film that sp2 hybridized orbits composition hexangle type is in honeycomb lattice, the two-dimensional material of only one of which carbon atom thickness.Stone Black alkene is considered as always hypothetical structure, it is impossible to independent stable existence, until, Univ Manchester UK's physics in 2004 Scholar An Delie et al. successfully isolates Graphene from graphite in an experiment, and confirms that it can be with individualism, two people Because " in the initiative experiment of two-dimensional graphene material " serves as reasons, Nobel Prize in physics in 2010 is obtained jointly
It is but also most hard nano material that Graphene is currently world most thin, and it is almost fully transparent, only absorbs 2.3% Light;Thermal conductivity factor is up to 5300W/mK, and higher than CNT and diamond, its electron mobility exceedes nano-sized carbon under normal temperature Pipe or silicon crystal, and resistivity about 10-6Ω cm, it is lower than copper or silver, it is the minimum material of current world resistivity.Because Its resistivity is extremely low, and the speed of electron transfer is exceedingly fast, therefore is expected to can be used to develop thinner, conductive speed new faster Generation electronic component or transistor.Because Graphene is substantially a kind of transparent, good conductor, it also is adapted for transparent for manufacturing Touch Screen, even tabula rasa, solar cell.
At present, grapheme material powder, such as mechanical stripping method, oxidation-reduction method, crystalline substance can be prepared using various methods External epitaxial growth, chemical vapour deposition technique, organic synthesis method and stripping CNT method etc..In these methods, machinery stripping It is very low from method and epitaxial growth method preparation efficiency, it is difficult to meet large-scale needs.Although chemical vapour deposition technique can be obtained The continuous graphene film of large scale, but suitable for micro-nano electronic device or transparent conductive film, can not but meet energy storage material And the extensive demand in functional composite material field.Oxidation-reduction method prepares grapheme material powder and is relatively easy to realize, is system The common method of standby grapheme material powder, but the method uses a large amount of strong acid and oxidation during Graphene is prepared Agent, it is serious to graphenic surface destruction, and environment is easily polluted, therefore be not suitable for the Graphene preparation of extensive industrialization.
The content of the invention
The system of the Graphene provided the invention provides a kind of method that utilization biomass material prepares Graphene, the present invention Preparation Method is with biomass material as raw material, and preparation method environmental pollution is smaller, is conducive to the industrialization development of Graphene.
The invention provides a kind of method that utilization biomass material prepares Graphene, comprise the following steps:
(1)Removal of impurities is carried out to biomass material, then it is crushed;
(2)Treated biomass material is mixed with chemical solvent, centre addition catalyst;
(3)Above-mentioned treated biomass material is carried out into high-temperature heating, and after obtain Graphene through ultra high pressure treatment.
The step(1)In biomass material be maize straw, wheat stalk, careless class, shell class and agricultural byproducts add One or more mixture in waste residue during work etc..
The step(2)In chemical solvent be any proportioning of the one or two kinds of solvent in nitric acid or sulfuric acid.
The step(2)In catalyst be silicic acid, its addition is with the mass ratio of biomass material:(0.001- 0.01):1.
The step(3)In high-temperature heating program be:100 DEG C of insulation 1h;250 DEG C of insulation 1-2h;550 DEG C of insulation 2- 4h;850 DEG C of insulation 16-20h.
The step(3)In ultra-high pressure condition be:Pressure 400-600 MPa, dwell time 25-60 min, pressurization temperature 50-85 DEG C of degree.
The present invention has advantages below:
(1)Preparing Graphene characteristic according to the preparation method described in this patent scheme is:The specific surface area of Graphene is 1800~3000cm3/g;The aperture of Graphene is 1~18nm;
(2)This patent prepares Graphene by raw material of biomass material so that biomass material is preferably processed, and significantly The added value of biomass material is improve, contributes to the fast lifting of China's rural economy.
Specific embodiment
The present embodiment is further illustrating rather than the limitation to this patent to this patent.
Embodiment 1
(1)With maize straw as biomass material, crushed after removal of impurities is carried out to it;
(2)The maize straw of crushing and chemical solvent are mixed, centre addition catalyst;
(3)Above-mentioned treated maize straw is carried out into high-temperature heating, and after obtain Graphene through ultra high pressure treatment.
The step(2)In chemical solvent be nitric acid.
The step(2)In catalyst be silicic acid, its addition is with the mass ratio of biomass material: 0.001:1.
The step(3)In high-temperature heating program be:100 DEG C of insulation 1h;250 DEG C of insulation 1h;550 DEG C of insulation 2h;850 DEG C insulation 16h.
The step(3)In ultra-high pressure condition be:The MPa of pressure 400, the min of dwell time 25,50 DEG C of pressed temperature.
Embodiment 2
(1)With wheat stalk as biomass material, crushed after removal of impurities is carried out to it;
(2)The biomass material of crushing and chemical solvent are mixed, centre addition catalyst;
(3)Above-mentioned treated biomass material is carried out into high-temperature heating, and after obtain Graphene through ultra high pressure treatment.
The step(2)In chemical solvent be sulfuric acid.
The step(2)In catalyst be silicic acid, its addition is with the mass ratio of biomass material:0.005:1.
The step(3)In high-temperature heating program be:100 DEG C of insulation 1h;250 DEG C of insulation 2h;550 DEG C of insulation 4h;850 DEG C insulation 20h.
The step(3)In ultra-high pressure condition be:The MPa of pressure 500, the min of dwell time 40,65 DEG C of pressed temperature.
Embodiment 3
(1)With rice husk and weeds mixture as biomass material, crushed after removal of impurities is carried out to it;;
(2)The biomass material of crushing and chemical solvent are mixed, centre addition catalyst;
(3)Above-mentioned treated biomass material is carried out into high-temperature heating, and after obtain Graphene through ultra high pressure treatment.
The step(2)In chemical solvent be the mixed liquor of nitric acid and sulfuric acid, its mass ratio is 1:1.
The step(2)In catalyst be silicic acid, its addition is with the mass ratio of biomass material:0.002:1.
The step(3)In high-temperature heating program be:100 DEG C of insulation 1h;250 DEG C of insulation 1.5h;550 DEG C of insulation 3h; 850 DEG C of insulation 18h.
The step(3)In ultra-high pressure condition be:The MPa of pressure 600, the min of dwell time 60,85 DEG C of pressed temperature.

Claims (6)

1. a kind of method that utilization biomass material prepares Graphene, comprises the following steps:
(1)Removal of impurities is carried out to biomass material, then it is crushed;
(2)Treated biomass material is mixed with chemical solvent, centre addition catalyst;
(3)Above-mentioned treated biomass material is carried out into high-temperature heating, and after obtain Graphene through ultra high pressure treatment.
2. the method that a kind of utilization biomass material according to claim 1 prepares Graphene, it is characterised in that the step Suddenly(1)In biomass material be maize straw, the waste residue during wheat stalk, careless class, shell class and agricultural byproducts processing One or more mixture in.
3. the method that a kind of utilization biomass material according to claim 1 prepares Graphene, it is characterised in that the step Suddenly(2)In chemical solvent be any proportioning of the one or two kinds of solvent in nitric acid or sulfuric acid.
4. the method that a kind of utilization biomass material according to claim 1 prepares Graphene, it is characterised in that the step Suddenly(2)In catalyst be silicic acid, its addition is with the mass ratio of biomass material:(0.001-0.01):1.
5. the method that a kind of utilization biomass material according to claim 1 prepares Graphene, it is characterised in that the step Suddenly(3)In high-temperature heating program be:100 DEG C of insulation 1h;250 DEG C of insulation 1-2h;550 DEG C of insulation 2-4h;850 DEG C of insulation 16- 20h。
6. the method that a kind of utilization biomass material according to claim 1 prepares Graphene, it is characterised in that the step Suddenly(3)In ultra-high pressure condition be:Pressure 400-600 MPa, dwell time 25-60 min, 50-85 DEG C of pressed temperature.
CN201611083909.3A 2016-11-30 2016-11-30 A kind of method that utilization biomass material prepares Graphene Pending CN106744836A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107758644A (en) * 2017-10-13 2018-03-06 杭州高烯科技有限公司 A kind of method that super-pressure thermal reduction prepares graphene film
CN110668430A (en) * 2019-11-12 2020-01-10 沈阳中科腐蚀控制工程技术中心 Method for preparing graphene by fermenting graphene with graphene

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104016341A (en) * 2014-07-01 2014-09-03 济南圣泉集团股份有限公司 Preparation method of porous graphene
CN104386684A (en) * 2014-12-16 2015-03-04 中国科学院宁波材料技术与工程研究所 Preparation method of graphene and graphene

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104016341A (en) * 2014-07-01 2014-09-03 济南圣泉集团股份有限公司 Preparation method of porous graphene
CN104386684A (en) * 2014-12-16 2015-03-04 中国科学院宁波材料技术与工程研究所 Preparation method of graphene and graphene

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107758644A (en) * 2017-10-13 2018-03-06 杭州高烯科技有限公司 A kind of method that super-pressure thermal reduction prepares graphene film
CN110668430A (en) * 2019-11-12 2020-01-10 沈阳中科腐蚀控制工程技术中心 Method for preparing graphene by fermenting graphene with graphene

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