CN108545723A - The method of the preparation of biological alkyl graphene - Google Patents
The method of the preparation of biological alkyl graphene Download PDFInfo
- Publication number
- CN108545723A CN108545723A CN201810753573.XA CN201810753573A CN108545723A CN 108545723 A CN108545723 A CN 108545723A CN 201810753573 A CN201810753573 A CN 201810753573A CN 108545723 A CN108545723 A CN 108545723A
- Authority
- CN
- China
- Prior art keywords
- gas
- graphene
- tank
- methane
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
Abstract
The present invention relates to the methods of the preparation of technical field of graphene preparation, in particular to biological alkyl graphene, include the following steps：(1), preprocessed good waste metal copper is melted.(2), biological methane tank is sent in purification.(3), biological methane tank send molten copper liquid catalyst separator to detach.(4), cooling and solid recycling graphene is carried out.(5), after gas separate pot uses molecule sieve separation, hydrogen that waste metal copper melting furnace is sent to burn, steam is generated through being cooled to cooling water, is recycled for cooling solid recover.(6), inertia gas tank is sent to recycle the inert gas that gas separate pot detaches.(7), long-distance anti-explosion monitoring center system is opened, long-distance anti-explosion monitoring is carried out to full process stream journey and surrounding enviroment.First, be raw material with natural gas from coal or methane purification gas, and with waste metal copper it is catalyst, substantially reduces production cost.Second is that small investment, is suitble to large-scale industrialized production.
Description
Technical field
The present invention relates to the methods of the preparation of technical field of graphene preparation, in particular to biological alkyl graphene.
Background technology
Graphene oxide is generally aoxidized through strong acid by graphite and is obtained.There are mainly three types of the methods for preparing graphite oxide：
Brodie methods, Staudenmaier methods and Hummers methods.Wherein the timeliness of the preparation process of Hummers methods relatively preferably and
And it is also relatively safer in preparation process, it is current most common one kind.It is using the potassium permanganate and powdered graphite in the concentrated sulfuric acid
After oxidized reaction, obtain brown has derivative carboxylic acid group at edge and is mainly phenolic hydroxyl group and epoxy group in the plane
Graphite flake, it is graphene oxide that this graphene layers can be vigorously stirred stripping through ultrasound or high shear, and is formed in water
Stablize, the single-layer graphene oxide suspension of sundown.Since conjugate network is by serious functionalization, graphene oxide is thin
Piece has the speciality of insulation.Partial reduction can be carried out through reduction treatment, obtains the graphene platelet of chemical modification.Although last
The graphite ene product or redox graphene arrived all has more defect, its electric conductivity is caused to be not so good as original graphene,
But the processing procedure of this oxidation-stripping-reduction can effectively allow insoluble powdered graphite to become to process in water, provide system
Make the approach of redox graphene.
The major defect of graphene oxide (GO), first, oxide group content is high, wherein oxygen content is and true 10-20%
Positive simple two-dimensional graphene content is extremely low.Second is that acid big, PH4-5, inconvenient downstream industry is directly applied.Third, being not easy to store up
It deposits, easily reunites, be easy single layer, bilayer, multilayer (10 layers or less) two-dimensional graphene becomes 10 layers or more graphene wafers (is not
Graphene).
The major defect of redox graphene (RGO) is by reduction treatment, the fracture of honeycomb structure two-dimensional graphene
Seriously, while by many two-dimensional graphenes it has been reduced into graphene wafer, has lost two-dimensional graphene primary characteristic.
Graphene oxide (GO) and redox graphene (RGO) in process of production, generate a large amount of sour waters, influence
Environment.
In addition, vapour deposition process produces graphene, with carbonaceous gas (methane, second dilute, acetylene), in certain temperature and pressure
Under the conditions of power, carbon atom adheres on growth base, forms monolayer carbon structural material and is grown into.Advantage：Gained graphene knot
Structure is good, and size is not limited by raw material.Disadvantage：Preparation process is complicated, low production efficiency, it is difficult to scale of mass production.
Invention content
The technical problem to be solved by the present invention is to overcome the defects of above-mentioned technology, provide the preparation of biological alkyl graphene
Method.
In order to solve the above technical problems, technical solution provided by the invention is the method packet of the preparation of biological alkyl graphene
Include following steps：
(1), it after sending waste metal copper melting furnace to melt preprocessed good waste metal copper, is sent into through metallic copper flow container
In molten copper liquid catalyst separator.
(2), it opens in natural gas from coal tank or associated gas tank, gas field gas tank, methane purification gas tank, liquid gas storage tank
A kind of valve, it is purified to send biological methane tank.
(3), biological methane tank send molten copper liquid catalyst separator to detach.
(4), it opens indifferent gas tank valve the inert gas of biological degree is sent into molten copper liquid catalyst separator, by stone
Black alkene and hydrogen are blown into cooling solid recover, carry out cooling and solid and recycle graphene.Gas send gas separate pot.
(5), after gas separate pot uses molecule sieve separation, hydrogen that waste metal copper melting furnace is sent to burn, steam warp is generated
It is cooled to cooling water, is recycled for cooling solid recover.
(6), inertia gas tank is sent to recycle the inert gas that gas separate pot detaches.
(7), long-distance anti-explosion monitoring center system is opened, long-distance anti-explosion monitoring is carried out to full process stream journey and surrounding enviroment.
As an improvement, in step (1), the copper content of metal copper liquid reaches 99.99% or more.
As an improvement, in step (2), the methane content in biological methane reaches 97.0% or more, and aspirated pressure is
10—100pa。
As an improvement, in step (3),
Molten copper liquid catalyst separator complete main reaction be：
CH4 --- C (graphene)+2H2
The catalytic temperature of molten copper liquid catalyst separator is 1100-1300 DEG C.
As an improvement, in step (4), inert gas gas includes helium (He), neon (Ne), argon (Ar), krypton (Kr), xenon
(Xe), the aspirated pressure of inertia gas tank is 8-100pa.The cooling temperature of cooling solid recover is 50 DEG C or less.
As an improvement, in step (5),
Hydrogen send the burning main reaction of waste metal copper melting furnace：
2H2+O2 --- 2H2O (water vapour)
Or hydrogen is delivered coal preparing natural gas device methane.
Or send molten copper liquid catalyst separator as the gas for blowing graphene hydrogen.
The method of the preparation of biology alkyl graphene of the invention has the following advantages that：First, being carried with natural gas from coal or biogas
Pure gas is raw material, and with waste metal copper is catalyst, substantially reduces production cost.Second is that small investment, is suitble to extensive production
Industry metaplasia is produced.
Description of the drawings
Fig. 1 is the schematic diagram of the method for the preparation of biological alkyl graphene of the invention.
Fig. 2 is biomass-based graphene coproduction graphene cupro silicon preparation process and schematic device.
Fig. 3 is waste metal copper preprocessor technique and schematic device.
Fig. 4 is molten copper liquid catalyst separator technique and schematic device.
Fig. 5 is molten copper liquid catalyst pond arrangement schematic diagram.
Fig. 6 is cooling multistage solid recover technique and schematic device.
Fig. 7 is the preparation process and schematic device of biological alkyl graphene and graphene cupro silicon.
Specific implementation mode
Present invention will be described in further detail below with reference to the accompanying drawings.
In conjunction with attached drawing, include the following steps：
(1), it after sending waste metal copper melting furnace to melt preprocessed good waste metal copper, is sent into through metallic copper flow container
In molten copper liquid catalyst separator.
(2), it opens in natural gas from coal tank or associated gas tank, gas field gas tank, methane purification gas tank, liquid gas storage tank
A kind of valve, it is purified to send biological methane tank.
(3), biological methane tank send molten copper liquid catalyst separator to detach.
(4), it opens indifferent gas tank valve the inert gas of biological degree is sent into molten copper liquid catalyst separator, by stone
Black alkene and hydrogen are blown into cooling solid recover, carry out cooling and solid and recycle graphene.Gas send gas separate pot.
(5), after gas separate pot uses molecule sieve separation, hydrogen that waste metal copper melting furnace is sent to burn, steam warp is generated
It is cooled to cooling water, is recycled for cooling solid recover.
(6), inertia gas tank is sent to recycle the inert gas that gas separate pot detaches.
(7), long-distance anti-explosion monitoring center system is opened, long-distance anti-explosion monitoring is carried out to full process stream journey and surrounding enviroment.
In step (1), the copper content of metal copper liquid reaches 99.99% or more.
In step (2), the methane content in biological methane reaches 97.0% or more, and aspirated pressure is 10-100pa.
In step (3),
Molten copper liquid catalyst separator complete main reaction be：
CH4 --- C (graphene)+2H2
The catalytic temperature of molten copper liquid catalyst separator is 1100-1300 DEG C.
In step (4), inert gas gas includes helium (He), neon (Ne), argon (Ar), krypton (Kr), xenon (Xe), indifferent gas
The aspirated pressure of tank is 8-100pa.The cooling temperature of cooling solid recover is 50 DEG C or less.
In step (5),
Hydrogen send the burning main reaction of waste metal copper melting furnace：
2H2+O2 --- 2H2O (water vapour)
Or hydrogen is delivered coal preparing natural gas device methane.
Or send molten copper liquid catalyst separator as the gas for blowing graphene hydrogen.
Embodiment 1：
With reference to figure 2
The first step send the silica extracted from flyash and waste and old copper material copper silicon melting furnace to be melted at 1600-1700 DEG C
Melt, send melting catalytic separation device.
Biomass straw is crushed and send the methane-generating pit methane that fermentation generates by second step, send melting catalytic separation device catalysis first
Alkane fast decoupled generates graphene dust particles and flue gas.
Third step, the dust particles of melting catalytic separation device separation and flue gas send dust collector to recycle graphite through cooling
Hydrogen gas tank is sent in alkene, flue gas purification.
The molten liquid for melting the separation of catalytic separation device is mixed with graphene and produces graphene cupro silicon by the 4th step.
It is preferred that the graphene copper content in graphene cupro silicon is 0.01-3%.
Embodiment 2：
With reference to figure 3
It send cutting machine to cut the waste metal copper of recycling, after sending clear water service sink to wash off silt and impurity, send solvent clear
Wash pool washes off greasy dirt, and waste metal copper melting furnace is sent to be melted and removed the gred after airing.
Embodiment 3：
With reference to figure 4
1, molten copper liquid delivery tube.2, molten copper liquid catalyst pond.31,32, methane gas delivery pipe.41,42, methane
The rectangular pipe dish of gas or round pipe dish.5, methane venthole.6, solid graphene.
The first step opens metallic copper tank valve by copper liquid through the feeding molten copper liquid catalyst of molten copper liquid delivery tube 1
In pond 2.
The catalytic temperature in preferred molten copper liquid catalyst pond is 1100-1300 DEG C.
Second step opens methane tank valve by methane through methane gas delivery pipe 31,32, through the rectangular pipe dish of methane gas or
Round pipe dish 41,42 is sent into molten copper liquid layer, during across molten copper liquid layer, methane is fast from methane venthole 5
Speed cracking, the main reaction of completion are：
CH4 --- C (graphene)+2H2
The thickness of preferred molten copper liquid layer is 20-120cm.
Third step opens indifferent gas tank valve, and solid graphene 6 and hydrogen are blown into solid with inert gas and cooled back
It receives in device.
It is preferred that the aspirated pressure of inertia gas tank is 8-100pa.
Embodiment 4：
With reference to figure 5
7, methane shunt conduit.81,82 ... 89,810, molten copper liquid catalyst pond.
In order to expand the scale of production, using multiple molten copper liquid catalysts pond.Methane is sent respectively through methane shunt conduit
Enter in molten copper liquid catalyst pond 81,82 ... 89,810.
Embodiment 5：
With reference to figure 6
9, bent-tube boiler cooler.101,102, air-introduced machine.11, cyclone type herringbone plate washer.121,122,123, recycling bins.
131,132,133, discharger.
The first step opens air-introduced machine 101,102 power switches.
Second step cools down the solid graphene 6 and hydrogen that are blowed from molten copper liquid catalyst separator through bend pipe
After device 9 is cooled to 50 DEG C or less, be sent into cooling multistage solid recover, solid graphene through cyclone type herringbone plate washer 11 to
Under by recycling bins 121,122,123, send graphene packing machine to be packed through discharger 131,132,133.
Third step opens gas separate pot air intake valve, and the gas in cooling multistage solid recover is supplied gas body separation
Tank is detached.
The present invention and its embodiments have been described above, this description is no restricted, shown in attached drawing
Only one of embodiments of the present invention.All in all if those skilled in the art are enlightened by it, this is not being departed from
In the case of innovation and creation objective, frame mode similar with the technical solution and embodiment are not inventively designed,
It should belong to the scope of protection of the present invention.
Claims (6)
1. the method for the preparation of biological alkyl graphene, it is characterised in that include the following steps：
(1), it after sending waste metal copper melting furnace to melt preprocessed good waste metal copper, is sent into and melts through metallic copper flow container
In copper liquid body catalytic separation device.
(2), one kind in natural gas from coal tank or associated gas tank, gas field gas tank, methane purification gas tank, liquid gas storage tank is opened
Valve, it is purified to send biological methane tank.
(3), biological methane tank send molten copper liquid catalyst separator to detach.
(4), it opens indifferent gas tank valve the inert gas of biological degree is sent into molten copper liquid catalyst separator, by graphene
It is blown into cooling solid recover with hydrogen, cooling and solid is carried out and recycles graphene.Gas send gas separate pot.
(5), after gas separate pot uses molecule sieve separation, hydrogen that waste metal copper melting furnace is sent to burn, steam is generated through cooling
At cooling water, recycled for cooling solid recover.
(6), inertia gas tank is sent to recycle the inert gas that gas separate pot detaches.
(7), long-distance anti-explosion monitoring center system is opened, long-distance anti-explosion monitoring is carried out to full process stream journey and surrounding enviroment.
2. the method for the preparation of biology alkyl graphene according to claim 1, it is characterised in that：In step (1), gold
The copper content for belonging to copper liquid reaches 99.99% or more.
3. the method for the preparation of biology alkyl graphene according to claim 1, it is characterised in that：It is raw in step (2)
Methane content in object methane reaches 97.0% or more, and aspirated pressure is 10-100pa.
4. the method for the preparation of biology alkyl graphene according to claim 1, it is characterised in that：In step (3),
Molten copper liquid catalyst separator complete main reaction be：
CH4 --- C (graphene)+2H2
The catalytic temperature of molten copper liquid catalyst separator is 1100-1300 DEG C.
5. the method for the preparation of biology alkyl graphene according to claim 1, it is characterised in that：It is lazy in step (4)
Property gas gas include helium (He), neon (Ne), argon (Ar), krypton (Kr), xenon (Xe), the aspirated pressure of inertia gas tank is 8-
100pa.The cooling temperature of cooling solid recover is 50 DEG C or less.
6. the method for the preparation of biology alkyl graphene according to claim 1, it is characterised in that：In step (5),
Hydrogen send the burning main reaction of waste metal copper melting furnace：
2H2+O2 --- 2H2O (water vapour)
Or hydrogen is delivered coal preparing natural gas device methane.
Or send molten copper liquid catalyst separator as the gas for blowing graphene hydrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810753573.XA CN108545723A (en) | 2018-07-10 | 2018-07-10 | The method of the preparation of biological alkyl graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810753573.XA CN108545723A (en) | 2018-07-10 | 2018-07-10 | The method of the preparation of biological alkyl graphene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108545723A true CN108545723A (en) | 2018-09-18 |
Family
ID=63492067
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810753573.XA Pending CN108545723A (en) | 2018-07-10 | 2018-07-10 | The method of the preparation of biological alkyl graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108545723A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109107533A (en) * | 2018-10-11 | 2019-01-01 | 中喜（宁夏）新材料有限公司 | Corn stover graphene active charcoal preparing process |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229426A (en) * | 2011-05-25 | 2011-11-02 | 中国科学院化学研究所 | Preparation method of equiangular hexagonal graphene arranged in single layer sequentially |
| CN102583359A (en) * | 2012-04-01 | 2012-07-18 | 中国科学院上海微***与信息技术研究所 | Method for preparing graphene by adopting liquid catalyst aided chemical vapor deposition |
| CN104860298A (en) * | 2015-03-25 | 2015-08-26 | 孙旭阳 | Method for preparing graphene by using molten state reaction bed |
| CN107128904A (en) * | 2017-05-11 | 2017-09-05 | 张丽慧 | A kind of method that metal catalytic prepares graphene |
| US20170267534A1 (en) * | 2016-03-18 | 2017-09-21 | Honda Motor Co., Ltd. | Method for continuous production of high quality graphene |
| CN107381555A (en) * | 2017-08-09 | 2017-11-24 | 华中科技大学 | A kind of three-dimensional grapheme of structure-controllable and its preparation method of composite |
-
2018
- 2018-07-10 CN CN201810753573.XA patent/CN108545723A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229426A (en) * | 2011-05-25 | 2011-11-02 | 中国科学院化学研究所 | Preparation method of equiangular hexagonal graphene arranged in single layer sequentially |
| CN102583359A (en) * | 2012-04-01 | 2012-07-18 | 中国科学院上海微***与信息技术研究所 | Method for preparing graphene by adopting liquid catalyst aided chemical vapor deposition |
| CN104860298A (en) * | 2015-03-25 | 2015-08-26 | 孙旭阳 | Method for preparing graphene by using molten state reaction bed |
| US20170267534A1 (en) * | 2016-03-18 | 2017-09-21 | Honda Motor Co., Ltd. | Method for continuous production of high quality graphene |
| CN107128904A (en) * | 2017-05-11 | 2017-09-05 | 张丽慧 | A kind of method that metal catalytic prepares graphene |
| CN107381555A (en) * | 2017-08-09 | 2017-11-24 | 华中科技大学 | A kind of three-dimensional grapheme of structure-controllable and its preparation method of composite |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109107533A (en) * | 2018-10-11 | 2019-01-01 | 中喜（宁夏）新材料有限公司 | Corn stover graphene active charcoal preparing process |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5751748B2 (en) | Polycrystalline silicon lump group and method for producing polycrystalline silicon lump group | |
| CN102126725B (en) | Method and equipment for purifying polycrystalline silicon by melting in electron beam shallow pool | |
| CN110217777A (en) | A kind of carbon nanotube preparing apparatus and method | |
| CN107128904A (en) | A kind of method that metal catalytic prepares graphene | |
| WO2005123583A1 (en) | Method for producing polycrystalline silicon and polycrystalline silicon for solar cell produced by the method | |
| JP4856973B2 (en) | Manufacturing method of high purity silicon | |
| CN102145894B (en) | Method and device for smelting and purifying polysilicon by using electron beams and adopting slag filtering | |
| Li et al. | Review of resource and recycling of silicon powder from diamond-wire sawing silicon waste | |
| CN110697694A (en) | Method for preparing graphene through liquid metal vapor deposition | |
| CN108557809A (en) | A kind of graphene preparation method | |
| TW201033123A (en) | Method for manufacturing a silicon material with high purity | |
| CN115092917B (en) | Method for continuously and efficiently producing graphene powder | |
| CN108545723A (en) | The method of the preparation of biological alkyl graphene | |
| CN114890410B (en) | Preparation method of high-yield high-quality graphene powder | |
| JP2006282498A (en) | Method for producing high purity silicon | |
| US10077192B2 (en) | Method for producing polycrystalline silicon | |
| TW201422524A (en) | Low-temperature manufacturing method and system for spheroidal graphite | |
| CN101413064A (en) | Vacuum decomposing apparatus for separating gallium arsenide as metal gallium and metal arsenic | |
| CN102408112A (en) | Method and equipment for purification of polysilicon by using electron beam melting under action of high purity silicon substrate | |
| JP2013256445A (en) | Method for producing single crystal silicon | |
| JP2010052960A (en) | Method for production of high-purity silicon, production apparatus, and high-purity silicon | |
| CN217780761U (en) | Production graphite alkene device | |
| CN113184854B (en) | Method for recycling solar-grade silicon diamond wire cutting waste | |
| CN101935041B (en) | Method for extracting polysilicon through electron beams and acid washing | |
| CN201358292Y (en) | Vacuum decomposer capable of decomposing gallium arsenicde into metallic gallium and metallic arsenic |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180918 |
|
| RJ01 | Rejection of invention patent application after publication |