CN105905890A - Simple preparation method of biomass base three-dimensional multi-element co-doping graphene - Google Patents
Simple preparation method of biomass base three-dimensional multi-element co-doping graphene Download PDFInfo
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- CN105905890A CN105905890A CN201610405172.6A CN201610405172A CN105905890A CN 105905890 A CN105905890 A CN 105905890A CN 201610405172 A CN201610405172 A CN 201610405172A CN 105905890 A CN105905890 A CN 105905890A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/30—Three-dimensional structures
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
Abstract
The invention discloses a simple preparation method of biomass base three-dimensional multi-element co-doping graphene, and belongs to a simple preparation method of graphene. The method comprises the following steps that a clean quartz tube is placed into a tube furnace, and the temperature of the high temperature portion of the quartz tube is increased to the reaction temperature; the selected biomass raw material and a chemical reagent are sufficiently mixed and placed into a clean quartz boat, and after the furnace temperature is increased to the set temperature, the quartz boat is placed on an opening of the quartz tube; protective gas is introduced after a flange is fixed, and after air is exhausted, the quartz boat is pushed to the high temperature portion of the quartz tube; after a period of time, heating is stopped, the furnace temperature is cooled to the room temperature under the protection of inert gas, a sample in the quartz boat is taken out, and the three-dimensional multi-element co-doping graphene is obtained. The simple preparation method has the advantages that during preparation, no any metal catalyst is added, no catalyst pollution is caused, acid-alkali treatment is not needed, the graphene preparation cost is lowered, and the large-scale graphene preparation is promoted; the graphene yield is improved; the environmental pollution is effectively reduced; effective separation of graphene is achieved.
Description
Technical field
The present invention relates to the simple method for preparing of a kind of Graphene, be specifically related to a kind of polynary codope of biomass-based three-dimensional
The simple method for preparing of Graphene.
Background technology
Graphene be a kind of sp2 hydbridized carbon atoms formed thickness only monolayer atom be arranged in cellular hexaplanar
The nano-carbon material of crystal, the character of its uniqueness, such as electric conductivity preferable under room temperature and heat conductivity, high intensity, high light transmittance；Often
The lower chemical stability of temperature is good, acid and alkali-resistance and the corrosion etc. of organic solvent-resistant so that it is nano electron device, gas sensor,
The fields such as energy storage and composite are gathered around and are had broad application prospects, and therefore Graphene is referred to as the king of dark fund and material.Special
It not after research in recent years shows to introduce the atoms such as other atom such as nitrogen, sulfur, phosphorus, boron and silicon in the network structure of Graphene, stone
The ink characteristic electron of alkene and structure can be further improved, the Graphene after improvement ultracapacitor, fuel cell, lithium from
The fields such as sub-battery, metal-air battery, solaode, Flied emission then show more excellent performance, and have even may be used
It is directly used in fuel battery negative pole hydrogen reduction and the electro-catalysis of water decomposition anodic oxygen precipitation with replacement precious metals platinum catalyst.Relatively
In two-dimensional graphene, three-dimensional grapheme fold and mesoporous can be that reactant and product provide more transmission path and activity
Position, the most three-dimensional porous Graphene is more suitable as highly active eelctro-catalyst than two-dimensional graphene.
In view of excellent properties and the wide application prospect of doped graphene, the most a lot of researchers have been thrown oneself into and have been mixed
The exploitation preparation research of miscellaneous Graphene.Though obtaining certain progress, but really can realize method prepared by scale nothing more than having
Hummers based on natural fish scale-shaped graphite and chemical gaseous phase two kinds of methods of deposition, but there is following defect (1) in both approaches
Complex steps, (2) waste liquid are many and difficult, (3) catalyst contamination and catalyst difficulty are removed；Graphene is caused the most also to be difficult to advise
Prepared by mould, hinder the scale application of Graphene.
Utilize this renewable inexpensive substance of biomass to make raw material, use one-step synthesis can realize three-dimensional grapheme,
Prepared by the particularly scale of Heteroatom doping Graphene, there is no report at present.
Summary of the invention
Technical problem: the invention aims to provide the simple system of a kind of biomass-based three-dimensional polynary codope Graphene
Preparation Method, solve to prepare at present (1) complex steps that Graphene exists, (2) waste liquid is many and difficult, (3) catalyst contamination and
The problem that catalyst difficulty is removed, to promote the scale of Graphene to prepare and application.
Technical scheme: the simple method for preparing of a kind of biomass-based three-dimensional polynary codope Graphene of the present invention, including
Following step:
A, putting in tube furnace by a clean quartz ampoule, heating makes the temperature in the middle part of quartz ampoule be increased to reaction temperature；
B, the tubular biomass chosen in the ratio addition of the mass ratio of 1:5～1:100 in mortar and chemical reagent, fill
Dividing mixing and be put in quartz boat, quartz boat is positioned at quartz ampoule inner spout, is passed through inertia protection gas 30min after flange is fixing；
C, after air in tube drains until quartz, quartz boat is shifted onto the high-temperature region heating 1～5h in the middle part of quartz ampoule, makes raw material
Fully stop heating after reaction, under inert gas shielding, quartz boat is cooled to room temperature, take out sample in quartz boat；
D, by after sample in a solvent ultrasonic disperse 1～5h, separated by centrifuge, i.e. obtain the distribution of the different number of plies
Three-dimensional grapheme.
Described tubular biomass comprises tubular biomass fruit, tubulose agricultural crop straw and tubular biomass grass；Described
Tubular biomass fruit be tubulose oriental plane tree fruit；Described tubulose agricultural crop straw is Caulis et Folium Oryzae, Wheat Straw；Described pipe
Shape biomass grass is phragmites communis.
Described chemical reagent is labile inorganic matter and Organic substance；Described inorganic matter be ammonium hydrogen carbonate, ammonium carbonate,
One or more combination in ammonium sulfate, ammonium hydrogen sulfate, ammonium phosphate salt；Described Organic substance be dicyanodiamine, tripolycyanamide and
One or more combination in carbamide.
The ratio of described reaction mixing quality ratio is 1:5～1:100；Pyrolysis temperature is 600～1100 DEG C；Pyrolysis time is
1～5h.
Described noble gas is the one in nitrogen and argon, and flow velocity is 0.03～0.6L/min.
Described dispersion solvent is the one in water and ethanol.
Described dispersing mode is ultrasonic disperse, and the time is 1～5h.
Described separate mode is centrifugation.
Beneficial effect and advantage: the present invention prepares three-dimensional grapheme with Rapid Thermal solution, solve and prepare graphite at present
(1) complex steps that alkene exists, the problem that (2) waste liquid is many and difficult, (3) catalyst contamination and catalyst difficulty are removed, have:
(1) using tubular biomass is raw material, can effectively reduce the preparation cost of Graphene, thus effectively promote graphite
Prepared by the scale of alkene；
(2) use the labile inorganic ammonium salt of hetero atom and organic reagent, the productivity of Graphene can be effectively improved.
(3) use the green solvent dispersed sample such as water and ethanol, can effectively reduce environmental pollution.
(4) use ultrasonic disperse and centrifugal collection, can effectively realize efficiently separating of Graphene.
(5) owing to using a step quickly to prepare, any metallic catalyst is not used, without catalyst contamination, it is not necessary at soda acid
Reason, environmental friendliness, thus simple and strong operability.
Accompanying drawing explanation
Fig. 1 (a) for the 200nm three-dimensional grapheme scanning nuclear microprobe figure obtained by the embodiment of the present invention 1.
Fig. 1 (b) for the 20nm three-dimensional grapheme scanning nuclear microprobe figure obtained by the embodiment of the present invention 1.
Fig. 2 (a) is the atomic force microscopy Electronic Speculum figure of the three-dimensional grapheme obtained by the embodiment of the present invention 1.
Fig. 2 (b) is the Thickness Analysis figure of the three-dimensional grapheme obtained by the embodiment of the present invention 1.
Fig. 2 (c) is the distribution diagram of element of the three-dimensional grapheme obtained by the embodiment of the present invention 1.
Detailed description of the invention
The simple method for preparing of Graphene, comprises the steps:
A, putting in tube furnace by a clean quartz ampoule, heating makes the temperature in the middle part of quartz ampoule be increased to reaction temperature；
B, the tubular biomass chosen in the ratio addition of the mass ratio of 1:5～1:100 in mortar and chemical reagent, fill
Dividing mixing and be put in quartz boat, quartz boat is positioned at quartz ampoule inner spout, is passed through inertia protection gas 30min after flange is fixing；
C, after air in tube drains until quartz, quartz boat is shifted onto the high-temperature region heating 1～5h in the middle part of quartz ampoule, makes raw material
Fully stop heating after reaction, under inert gas shielding, quartz boat is cooled to room temperature, take out sample in quartz boat；
D, by after sample in a solvent ultrasonic disperse 1～5h, separated by centrifuge, i.e. obtain the distribution of the different number of plies
Three-dimensional grapheme.
Described tubular biomass comprises tubular biomass fruit, tubulose agricultural crop straw and tubular biomass grass；Described
Tubular biomass fruit be tubulose oriental plane tree fruit；Described tubulose agricultural crop straw is Caulis et Folium Oryzae, Wheat Straw；Described pipe
Shape biomass grass is phragmites communis.
Described chemical reagent is easily to decompose inorganic matter and Organic substance；Described inorganic matter is ammonium hydrogen carbonate, ammonium carbonate, sulfur
One or more combination in acid ammonium, ammonium hydrogen sulfate, ammonium phosphate salt；Described Organic substance is dicyanodiamine, tripolycyanamide and urine
One or more combination in element.
The ratio of described reaction mixing quality ratio is 1:5～1:100；Pyrolysis temperature is 600～1100 DEG C；Pyrolysis time is
1～5h.
Described noble gas is the one in nitrogen and argon, and flow velocity is 0.03～0.6L/min.
Described dispersion solvent is the one in water and ethanol.
Described dispersing mode is ultrasonic disperse, and the time is 1～5h.
Described separate mode is centrifugation.
It is further described to embodiments of the invention below in conjunction with the accompanying drawings:
Embodiment 1: a clean quartz ampoule is put in tube furnace, in atmosphere, the temperature of tube furnace is increased to 700
℃；
The tubular biomass oriental plane tree fruit of selection and ammonium sulfate are sufficiently mixed by 1:5 in mortar and to put into one clean
In clean quartz boat；When tube furnace temperature reaches 700 DEG C, quartz boat is placed on one end of quartz ampoule, logical after mounting flange
Entering nitrogen 30min, flow velocity is 0.06L/min, after air drains, quartz boat is shifted the high-temperature region of quartz ampoule onto, heats 2h, stop
Only heating, under the nitrogen protection that flow velocity is 0.05L/min, is cooled to room temperature by reacting furnace, takes out material from quartz boat；
Material is put in a beaker, add deionized water and carry out ultrasonic disperse 1h, by dispersion liquid by centrifuge not
Separate with rotating speed, dried in vacuum drying oven, i.e. obtain different number of plies three-dimensional grapheme.
Embodiment 2: a clean quartz ampoule is put in tube furnace, in atmosphere, the temperature of tube furnace is increased to 900
℃；
The tubular biomass Wheat Straw of selection and dicyanodiamine are sufficiently mixed by 1:20 in mortar and to put into one clean
In quartz boat；When tube furnace temperature reaches 900 DEG C, quartz boat is placed on one end of quartz ampoule, is passed through after mounting flange
Argon 20 min, flow velocity is 0.2L/min, after air drains, quartz boat is shifted the high-temperature region of quartz ampoule onto, heats 2h, stops
Heating, under the argon shield that flow velocity is 0.05L/min, is cooled to room temperature by reacting furnace, takes out material from quartz boat；
Material is put in a beaker, add and go dehydrated alcohol to carry out ultrasonic disperse 2h, by dispersion liquid by centrifuge
Different rotating speeds separates, dried in vacuum drying oven, i.e. obtains different number of plies three-dimensional grapheme.
Embodiment 3: a clean quartz ampoule is put in tube furnace, in atmosphere, the temperature of tube furnace is increased to 1000
℃；
The tubular biomass Caulis et Folium Oryzae of selection and ammonium hydrogen carbonate are sufficiently mixed in mortar by 1:50 and put into a clean stone
Ying Zhouzhong；When tube furnace temperature reaches 1000 DEG C, quartz boat is placed on one end of quartz ampoule, after mounting flange, is passed through nitrogen
Gas 30min, flow velocity is 0.1L/min, after air drains, quartz boat is shifted the high-temperature region of quartz ampoule onto, heats 2h, stop adding
Heat, under the nitrogen protection that flow velocity is 0.05L/min, is cooled to room temperature by reacting furnace, takes out material from quartz boat；
Material is put in a beaker, add deionized water and carry out ultrasonic disperse 3h, by dispersion liquid by centrifuge not
Separate with rotating speed, dried in vacuum drying oven, i.e. obtain different number of plies three-dimensional grapheme.
Embodiment 4: a clean quartz ampoule is put in tube furnace, in atmosphere, the temperature of tube furnace is increased to 1100
℃；
The tubular biomass phragmites communis of selection and ammonium phosphate are sufficiently mixed in mortar by 1:100 and put into a clean quartz
In boat；When tube furnace temperature reaches 1100 DEG C, quartz boat is placed on one end of quartz ampoule, after mounting flange, is passed through argon
30min, flow velocity is 0.3L/min, after air drains, quartz boat is shifted the high-temperature region of quartz ampoule onto, heats 2h, stops heating,
Under the argon shield that flow velocity is 0.05L/min, reacting furnace is cooled to room temperature, from quartz boat, takes out material；
Material is put in a beaker, add and go dehydrated alcohol to carry out ultrasonic disperse 5h, by dispersion liquid by centrifuge
Different rotating speeds separates, dried in vacuum drying oven, i.e. obtains different number of plies three-dimensional grapheme.
By Fig. 1 (a), Fig. 1 (b) it can be seen that the prepared Graphene that material is accessory pinna shape.
Three-dimensional nitrogen (N), sulfur (S), phosphorus within prepared Graphene is 10 layers is understood by 2 (a), Fig. 2 (b) and Fig. 2 (c)
And silicon (Si) polynary codope Graphene (P).
Claims (8)
1. the simple method for preparing of a biomass-based three-dimensional polynary codope Graphene, it is characterised in that: Graphene simple
Preparation method, comprises the steps:
A, putting in tube furnace by a clean quartz ampoule, heating makes the temperature in the middle part of quartz ampoule be increased to reaction temperature；
B, the tubular biomass chosen in the ratio addition of the mass ratio of 1:5～1:100 in mortar and chemical reagent, the most mixed
Merging and be put in quartz boat, quartz boat is positioned at quartz ampoule inner spout, is passed through inertia protection gas 30min after flange is fixing；
C, after air in tube drains until quartz, quartz boat is shifted onto the high-temperature region heating 1～5h in the middle part of quartz ampoule, makes raw material abundant
Stop heating after reaction, under inert gas shielding, quartz boat is cooled to room temperature, take out sample in quartz boat；
D, by after sample in a solvent ultrasonic disperse 1～5h, separated by centrifuge, i.e. obtain the three of the distribution of the different number of plies
Dimension Graphene.
The simple method for preparing of biomass-based three-dimensional the most according to claim 1 polynary codope Graphene, its feature exists
In: described tubular biomass comprises tubular biomass fruit, tubulose agricultural crop straw and tubular biomass grass；Described tubulose
Biomass fruit is tubulose oriental plane tree fruit；Described tubulose agricultural crop straw is Caulis et Folium Oryzae, Wheat Straw；Described tubulose is biological
Matter grass is phragmites communis.
The simple method for preparing of biomass-based three-dimensional the most according to claim 1 polynary codope Graphene, its feature exists
In: described chemical reagent is labile inorganic matter and Organic substance；Described inorganic matter is ammonium hydrogen carbonate, ammonium carbonate, sulphuric acid
One or more combination in ammonium, ammonium hydrogen sulfate and ammonium phosphate salt；Described Organic substance is dicyanodiamine, tripolycyanamide and carbamide
In one or more combination.
The simple method for preparing of biomass-based three-dimensional the most according to claim 1 polynary codope Graphene, its feature exists
In: the ratio of described reaction mixing quality ratio is 1:5～1:100；Temperature be pyrolysis temperature be 600～1100 DEG C；Time is heat
The solution time is 1～5h.
The simple method for preparing of biomass-based three-dimensional the most according to claim 1 polynary codope Graphene, its feature exists
In: described noble gas is in nitrogen and argon and one, and flow velocity is 0.03～0.6L/min.
The simple method for preparing of biomass-based three-dimensional the most according to claim 1 polynary codope Graphene, its feature exists
In: described dispersion solvent is the one in water and ethanol.
The simple method for preparing of biomass-based three-dimensional the most according to claim 1 polynary codope Graphene, its feature exists
In: described dispersing mode is ultrasonic disperse, and the time is 1～5h.
The simple method for preparing of biomass-based three-dimensional the most according to claim 1 polynary codope Graphene, its feature exists
In: described separate mode is centrifugation.
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| CN201610405172.6A CN105905890A (en) | 2016-06-08 | 2016-06-08 | Simple preparation method of biomass base three-dimensional multi-element co-doping graphene |
| CN201610832047.3A CN106365153B (en) | 2016-06-08 | 2016-09-19 | A kind of simple preparation method of the polynary codope graphene of biomass-based three-dimensional |
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| CN201610405172.6A CN105905890A (en) | 2016-06-08 | 2016-06-08 | Simple preparation method of biomass base three-dimensional multi-element co-doping graphene |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106564874A (en) * | 2016-10-18 | 2017-04-19 | 宁波工程学院 | Lignin-based two-dimensional carbon nano-material as well as preparing method and application thereof |
| CN109626370A (en) * | 2019-01-21 | 2019-04-16 | 青岛科技大学 | The preparation and its application of biomass-based porous carbon materials based on sycamore seed |
| CN111029530A (en) * | 2019-11-21 | 2020-04-17 | 合肥国轩高科动力能源有限公司 | Nitrogen and sulfur co-doped hollow biomass carbon material, preparation method thereof, and lithium-sulfur battery positive pole piece and battery prepared from same |
| CN112366316A (en) * | 2020-09-27 | 2021-02-12 | 泰山学院 | Preparation method and application of nitrogen and phosphorus co-doped graphene |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109110749A (en) * | 2018-09-09 | 2019-01-01 | 宁波诺丁汉新材料研究院有限公司 | A kind of edge carboxylated graphene and the method for preparing it is sheared based on supercritical fluid |
| CN111410186A (en) * | 2020-03-16 | 2020-07-14 | 华中科技大学 | Preparation method and application of two-dimensional carbon nanosheet |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103466613A (en) * | 2013-10-11 | 2013-12-25 | 中南林业科技大学 | Method for preparing graphene from lignin |
| CN104045077B (en) * | 2014-05-27 | 2015-09-23 | 海南大学 | The three-dimensional classifying porous Carbon Materials of a kind of Graphene and preparation method |
| CN105314629B (en) * | 2015-11-27 | 2017-08-11 | 燕山大学 | A kind of method that biomass carbon source directly prepares codope three-dimensional graphene electrode material |
| CN105502366A (en) * | 2015-12-30 | 2016-04-20 | 成都新柯力化工科技有限公司 | Method for preparing graphene by using biomass as raw materials |
-
2016
- 2016-06-08 CN CN201610405172.6A patent/CN105905890A/en not_active Withdrawn
- 2016-09-19 CN CN201610832047.3A patent/CN106365153B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106564874A (en) * | 2016-10-18 | 2017-04-19 | 宁波工程学院 | Lignin-based two-dimensional carbon nano-material as well as preparing method and application thereof |
| CN106564874B (en) * | 2016-10-18 | 2018-12-21 | 宁波工程学院 | A kind of lignin-base two dimension carbon nanomaterial and its preparation method and application |
| CN109626370A (en) * | 2019-01-21 | 2019-04-16 | 青岛科技大学 | The preparation and its application of biomass-based porous carbon materials based on sycamore seed |
| CN111029530A (en) * | 2019-11-21 | 2020-04-17 | 合肥国轩高科动力能源有限公司 | Nitrogen and sulfur co-doped hollow biomass carbon material, preparation method thereof, and lithium-sulfur battery positive pole piece and battery prepared from same |
| CN111029530B (en) * | 2019-11-21 | 2022-04-12 | 合肥国轩高科动力能源有限公司 | Nitrogen and sulfur co-doped hollow biomass carbon material, preparation method thereof, and lithium-sulfur battery positive pole piece and battery prepared from same |
| CN112366316A (en) * | 2020-09-27 | 2021-02-12 | 泰山学院 | Preparation method and application of nitrogen and phosphorus co-doped graphene |
| CN112366316B (en) * | 2020-09-27 | 2022-03-01 | 泰山学院 | Preparation method and application of nitrogen and phosphorus co-doped graphene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106365153B (en) | 2018-12-28 |
| CN106365153A (en) | 2017-02-01 |
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Application publication date: 20160831 |