CN106448921B - Nitrogen mixes graphene modified graphite magma and preparation method thereof - Google Patents
Nitrogen mixes graphene modified graphite magma and preparation method thereof Download PDFInfo
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- CN106448921B CN106448921B CN201610805912.5A CN201610805912A CN106448921B CN 106448921 B CN106448921 B CN 106448921B CN 201610805912 A CN201610805912 A CN 201610805912A CN 106448921 B CN106448921 B CN 106448921B
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 56
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- -1 graphene modified graphite Chemical class 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 24
- 239000010439 graphite Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000428 dust Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 9
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 8
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 8
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 8
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims abstract description 6
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims abstract description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 8
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 229920005749 polyurethane resin Polymers 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims description 2
- 229920001807 Urea-formaldehyde Polymers 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 claims 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 238000000034 method Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/18—Conductive material dispersed in non-conductive inorganic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Conductive Materials (AREA)
Abstract
The invention discloses a kind of nitrogen to mix graphene modified graphite magma, and the preparation method that the nitrogen mixes graphene modified graphite magma includes：Nitrogen is mixed graphene, electrically conductive graphite, resin, glass dust, zinc powder, ethylene glycol ethyl ether, ethyl cellulose and PVP and is stirred to obtain the nitrogen and mixes graphene modified graphite magma.The nitrogen, which mixes graphene modified graphite magma, has very strong electric conductivity, and unit dose is few.
Description
Technical field
The present invention relates to graphite magma, in particular it relates to which nitrogen mixes graphene modified graphite magma and preparation method thereof.
Background technology
Graphite magma is the graphite magma extensive use made of allotment using electrically conductive graphite or carbon black etc. as primary raw material
In communication article, computer, portable type electronic product, the network hardware, Medical Instruments, home electronic products and aerospace electron product
Deng.And the electric conductivity of in general graphite magma needs further to be improved, the brushing thickness of graphite magma is also to cause in addition
The main reason for its electric conductivity is not high.
The content of the invention
It is an object of the invention to provide a kind of nitrogen to mix graphene modified graphite magma, and the nitrogen mixes graphene modified graphite magma
With very strong electric conductivity, and unit dose is few.
To achieve these goals, the invention provides the preparation method that a kind of nitrogen mixes graphene modified graphite magma, bag
Include：Nitrogen is mixed into graphene, electrically conductive graphite, resin, glass dust, zinc powder, ethylene glycol ethyl ether, ethyl cellulose and polyvinylpyrrolidine
Alkanone, which is stirred to obtain the nitrogen, mixes graphene modified graphite magma；
Wherein, nitrogen mix graphene preparation method it is as follows：First urea is added in graphene oxide solution and mixed,
Then it is dried to obtain mixed-powder；Finally mixed-powder is calcined to obtain the nitrogen and mix graphene；Graphene oxide
The concentration of solution is 10mg/mL, and relative to the graphene oxide solution of 100 parts by weight, the dosage of urea is 100-150 weight
Part..
Graphene modified graphite magma is mixed in order to improve obtained nitrogen preferably, relative to the electrically conductive graphite of 100 parts by weight,
The dosage that nitrogen mixes graphene is 10-20 parts by weight, and the dosage of resin is 20-25 parts by weight, and the dosage of glass dust is 1-5 weight
Part, the dosage of zinc powder is 1-5 parts by weight, and the dosage of ethylene glycol ethyl ether is 20-29 parts by weight, and the dosage of polyethylene glycol is 1-5 weights
Part is measured, the dosage of PVP is 1-5 parts by weight.
In order to improve the caking property of graphite magma, resin is added, it is preferable that resin is selected from acrylic resin, polyethylene
One or more in resin, Lauxite or polyurethane resin.
Preferably, the weight average molecular weight of acrylic resin be 10,000-2 ten thousand, the weight average molecular weight of polyvinyl resin be 20,000-4
Ten thousandth, the weight average molecular weight of Lauxite is 10,000-2 ten thousand or the weight average molecular weight of polyurethane resin is 10,000-2 ten thousand.
In order to improve each original dispersiveness in graphite magma, mixed by the way of stirring, it is preferable that state stirring
Rotating speed be 2000-3000rpm, the time of stirring is 1-2h.
In nitrogen of the present invention mixes the preparation process of graphene：In order to improve its preparation rate, it is preferable that be the step of calcining：
Started to warm up from 20 DEG C to 800 DEG C and maintain 1h at 800 DEG C, wherein heating rate is 5 DEG C/min；Then with 10 DEG C/min drop
Warm speed is cooled to 30 DEG C；Wherein, the atmosphere of calcining is N2, N2Flow be 0.001m3/h。
In the present invention, in order to improve the preparation rate that nitrogen mixes graphene, urea is fully mixed with graphene oxide
It is dried afterwards by the way of forced air drying, it is preferable that dry temperature is 40-60 DEG C, and the dry time is 6-10h.
Present invention also offers one kind nitrogen as made from above-mentioned preparation method to mix graphene modified graphite magma.
Pass through above-mentioned technical proposal, the present invention mix graphene by using electrically conductive graphite as main raw material, adding nitrogen and carried
The electric conductivity of high magma can reduce unit dose simultaneously；In addition, it with the addition of resin, glass dust, zinc powder, ethylene glycol ethyl ethers
The auxiliary agents such as ether, ethyl cellulose and PVP improve the dispersed of each raw material and further improve leading for magma
Electrical property.The preparation method raw material is simple and easy to get, and technique can simply be produced in batches.In addition, nitrogen mixes graphene in the present invention
Prepare directly using the urea of abundance as nitrogen source, it is same that graphene is directly reduced into after high-temperature process using graphite oxide
When nitrogen be made in the presence of nitrogen source mix graphene.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The present invention will be described in detail by way of examples below.
Preparation example 1
Nitrogen mixes the preparation of graphene：100g urea (analysis is pure) is added in 100mL graphene oxide solution, fully
After being stirred；Forced air drying 10h obtains mixed-powder at 40 DEG C；Then mixed-powder is calcined to obtain the nitrogen and mixed
Graphene.Wherein, the step of calcining used is：Started to warm up from 20 DEG C to 800 DEG C and maintain 1h at 800 DEG C, wherein heating up
Speed is 5 DEG C/min；Then 30 DEG C are cooled to 10 DEG C/min rate of temperature fall；Wherein, the atmosphere of the calcining is N2, N2's
Flow is 0.001m3/h。
Preparation example 2
Nitrogen mixes the preparation of graphene：150g urea (analysis is pure) is added in 100mL graphene oxide solution, fully
After being stirred；Forced air drying 6h obtains mixed-powder at 60 DEG C；Then mixed-powder is calcined to obtain the nitrogen and mixed
Graphene.Wherein, the step of calcining used is：Started to warm up from 20 DEG C to 800 DEG C and maintain 1h at 800 DEG C, wherein heating up
Speed is 5 DEG C/min；Then 30 DEG C are cooled to 10 DEG C/min rate of temperature fall；Wherein, the atmosphere of the calcining is N2, N2's
Flow is 0.001m3/h。
Embodiment 1
Nitrogen is mixed into graphene, electrically conductive graphite, acrylic resin (weight average molecular weight is 10,000), glass dust, zinc powder, ethylene glycol
Ether, ethyl cellulose and PVP are according to weight proportion：10：100：25：1：1：30：1：1 is in rotating speed
2h is stirred under 2000rpm obtains nitrogen and mix graphene modified graphite magma A1；
Wherein, added nitrogen mixes graphene as obtained by preparation example 1.
Embodiment 2
Nitrogen is mixed into graphene, electrically conductive graphite, polyvinyl resin (weight average molecular weight is 20,000), glass dust, zinc powder, ethylene glycol
Ether, ethyl cellulose and PVP are 15 according to weight proportion：100：30：3：3：30：2：3 are in rotating speed
1.5h is stirred under 2500rpm obtains nitrogen and mix graphene modified graphite magma A2；
Wherein, added nitrogen mixes graphene as obtained by preparation example 2.
Embodiment 3
Nitrogen is mixed into graphene, electrically conductive graphite, Lauxite (weight average molecular weight 1), polyurethane resin, and (weight average molecular weight is
2 ten thousand), glass dust, zinc powder, ethylene glycol ethyl ether, ethyl cellulose and PVP are 15 according to weight proportion：100：
20：15：3：3：30：2：3 are in rotating speed:1.0h is stirred under 3000rpm obtains nitrogen and mix graphene modified graphite magma A3；
Wherein, added nitrogen mixes graphene as obtained by preparation example 2.
Comparative example 1
Graphite magma B1 is prepared Following the procedure of Example 1, except that mixing graphene to add nitrogen.
Comparative example 2
Graphite magma B2 is prepared Following the procedure of Example 2, except that mixing graphene to add nitrogen.
Comparative example 3
Graphite magma B3 is prepared Following the procedure of Example 3, except that mixing graphene to add nitrogen.
Comparative example 4
Graphite magma B4 is prepared Following the procedure of Example 1, except that being zincification powder.
Detect example 1
An equal amount of insulation board is brushed with the A1-A3 and B1-B4 of phase homogenous quantities, the resistance for testing graphite linings is big
It is small.Concrete outcome is shown in Table 1.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.In addition, any group can also be carried out between a variety of embodiments of the present invention
Close, as long as it without prejudice to the thought of the present invention, it should equally be considered as content disclosed in this invention.
Claims (6)
1. a kind of nitrogen mixes the preparation method of graphene modified graphite magma, it is characterised in that including：Nitrogen is mixed into graphene, conduction
Graphite, resin, glass dust, zinc powder, ethylene glycol ethyl ether, ethyl cellulose and PVP are stirred to obtain described
Nitrogen mixes graphene modified graphite magma；
Wherein, the nitrogen mix graphene preparation method it is as follows：First urea is added in graphene oxide solution and mixed,
Then it is dried to obtain mixed-powder；Finally the mixed-powder is calcined to obtain the nitrogen and mix graphene；The oxygen
The concentration of graphite alkene solution is 10mg/mL, and relative to the graphene oxide solution of 100 parts by weight, the dosage of the urea is
100-150 parts by weight；
Relative to the electrically conductive graphite of 100 parts by weight, dosage that the nitrogen mixes graphene is 10-20 parts by weight, the use of the resin
Measure as 20-25 parts by weight, the dosage of the glass dust is 1-5 parts by weight, and the dosage of the zinc powder is 1-5 parts by weight, the second
The dosage of glycol ether is 20-29 parts by weight, and the dosage of the ethyl cellulose is 1-5 parts by weight, the polyvinylpyrrolidine
The dosage of alkanone is 1-5 parts by weight；
The step of calcining is：Started to warm up from 20 DEG C to 800 DEG C and 800 DEG C maintain 1h, wherein heating rate be 5 DEG C/
min；Then 30 DEG C are cooled to 10 DEG C/min rate of temperature fall；Wherein, the atmosphere of the calcining is N2, N2Flow be
0.001m3/h。
2. preparation method according to claim 1, wherein, the resin is selected from acrylic resin, polyvinyl resin, ureaformaldehyde
One or more in resin or polyurethane resin.
3. preparation method according to claim 2, wherein, the weight average molecular weight of the acrylic resin is 10,000-2 ten thousand, gathered
The weight average molecular weight of vinyl is 20,000-4 ten thousand, the weight average molecular weight of Lauxite is 10,000-2 ten thousand or the weight of polyurethane resin is equal
Molecular weight is 10,000-2 ten thousand.
4. according to the preparation method described in any one in claim 1-3, wherein, the rotating speed of the stirring is 2000-
3000rpm, the time of stirring is 1-2h.
5. preparation method according to claim 4, wherein, the drying is forced air drying, and the temperature dried is 40-
60 DEG C, the dry time is 6-10h.
6. a kind of nitrogen mixes graphene modified graphite magma, it is characterised in that the nitrogen mixes graphene modified graphite magma by right
It is required that preparation method is made described in any one in 1-5.
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| CN201610805912.5A CN106448921B (en) | 2016-09-07 | 2016-09-07 | Nitrogen mixes graphene modified graphite magma and preparation method thereof |
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| CN201610805912.5A CN106448921B (en) | 2016-09-07 | 2016-09-07 | Nitrogen mixes graphene modified graphite magma and preparation method thereof |
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| Publication Number | Publication Date |
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| CN106448921A CN106448921A (en) | 2017-02-22 |
| CN106448921B true CN106448921B (en) | 2018-04-10 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102254584A (en) * | 2011-05-12 | 2011-11-23 | 中国科学院宁波材料技术与工程研究所 | General electronic paste based on graphene filler |
| CN105001716A (en) * | 2015-06-30 | 2015-10-28 | 中国科学院山西煤炭化学研究所 | Graphene-based low resistance conductive printing ink and preparation method thereof |
| CN105469858A (en) * | 2016-01-05 | 2016-04-06 | 厦门凯纳石墨烯技术股份有限公司 | Polyvinylpyrrolidone/graphene conductive slurry, preparation method and application |
| CN106448809A (en) * | 2016-09-07 | 2017-02-22 | 芜湖桑乐金电子科技有限公司 | Nitrogen-doped graphene modified graphite primary slurry and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8507797B2 (en) * | 2009-08-07 | 2013-08-13 | Guardian Industries Corp. | Large area deposition and doping of graphene, and products including the same |
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2016
- 2016-09-07 CN CN201610805912.5A patent/CN106448921B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102254584A (en) * | 2011-05-12 | 2011-11-23 | 中国科学院宁波材料技术与工程研究所 | General electronic paste based on graphene filler |
| CN105001716A (en) * | 2015-06-30 | 2015-10-28 | 中国科学院山西煤炭化学研究所 | Graphene-based low resistance conductive printing ink and preparation method thereof |
| CN105469858A (en) * | 2016-01-05 | 2016-04-06 | 厦门凯纳石墨烯技术股份有限公司 | Polyvinylpyrrolidone/graphene conductive slurry, preparation method and application |
| CN106448809A (en) * | 2016-09-07 | 2017-02-22 | 芜湖桑乐金电子科技有限公司 | Nitrogen-doped graphene modified graphite primary slurry and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| "Production of graphene from graphite oxide using urea as expansion-reduction agent";Stephen Wakeland等;《Carbon》;20100531;第48卷;第3463-3470页 * |
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