CN106409377B - 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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- CN106409377B CN106409377B CN201610805591.9A CN201610805591A CN106409377B CN 106409377 B CN106409377 B CN 106409377B CN 201610805591 A CN201610805591 A CN 201610805591A CN 106409377 B CN106409377 B CN 106409377B
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- 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
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- 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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- 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
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Abstract
The invention discloses the preparation methods that a kind of nitrogen mixes graphene modified graphite magma, including：Nitrogen is mixed graphene, electrically conductive graphite, resin, glass powder, zinc powder, terpinol, ethyl cellulose and polyvinylpyrrolidone and is stirred to obtain the nitrogen and mixes graphene modified graphite magma；Wherein, nitrogen mix graphene preparation method it is as follows：First urea is added in graphene oxide solution and is mixed, is then dried to obtain mixed-powder；It finally is calcined the mixed-powder to obtain the nitrogen and mixes graphene；A concentration of 10mg/mL of graphene oxide solution, relative to the graphene oxide solution of 100 parts by weight, the dosage of urea is 150 200 parts by weight.The nitrogen, which mixes graphene modified graphite magma, has electric conductivity well, and unit dose is few, painting efficiency is high.
Description
Technical field
The present invention relates to graphite magma, and in particular, to nitrogen mixes graphene modified graphite magma and preparation method thereof.
Background technology
Graphite magma is to allocate manufactured graphite magma extensive use using electrically conductive graphite or carbon black etc. as primary raw material
In communication article, computer, portable electronic product, the network hardware, Medical Instruments, home electronic products and aerospace electron product
Deng.And the electric conductivity of general graphite magma needs further to be improved, in addition the brushing thickness of graphite magma is also to cause
The main reason for its electric conductivity is not high.
Invention content
The object of the present invention is to provide a kind of nitrogen to mix graphene modified graphite magma, which mixes graphene modified graphite magma
With electric conductivity well, and unit dose is few, painting efficiency is high.
To achieve the goals above, the present invention provides the preparation method that a kind of nitrogen mixes graphene modified graphite magma, packets
It includes：Nitrogen is mixed into graphene, electrically conductive graphite, resin, glass powder, zinc powder, terpinol, ethyl cellulose and polyvinylpyrrolidone
It is stirred to obtain the nitrogen and mixes graphene modified graphite magma；
Wherein, nitrogen mix graphene preparation method it is as follows：First urea is added in graphene oxide solution and is mixed,
Then it is dried to obtain mixed-powder；It finally is calcined the mixed-powder to obtain the nitrogen and mixes graphene；Graphene oxide
A concentration of 10mg/mL of solution, relative to the graphene oxide solution of 100 parts by weight, the dosage of urea is 150-200 weight
Part.
Graphene modified graphite magma is mixed in order to improve nitrogen obtained 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 25-35 parts by weight, and the dosage of glass powder is 1-5 weight
Part, the dosage of zinc powder is 1-5 parts by weight, and the dosage of terpinol is 30-40 parts by weight, and the dosage of loose ethyl cellulose is 1-5 weights
Part is measured, the dosage of polyvinylpyrrolidone 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
It is one or more in resin, Lauxite or polyurethane resin.
Preferably, the weight average molecular weight of acrylic resin is 10,000-2 ten thousand, the weight average molecular weight of polyvinyl resin is 20,000-4
Ten thousand, 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 dispersibility in graphite magma, mixed by the way of stirring, it is preferable that state stirring
Rotating speed be 2000-3000rpm, 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 the step of calcining is：
1h is started to warm up to 800 DEG C and maintained at 800 DEG C from 20 DEG C, and wherein heating rate is 5 DEG C/min；Then with the drop of 10 DEG C/min
Warm rate 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 by the way of forced air drying afterwards, it is preferable that dry temperature is 40-60 DEG C, and the dry time is 6-10h.
The present invention also provides one kind, and the nitrogen made from above-mentioned preparation method mixes graphene modified graphite magma.
Through the above technical solutions, the present invention is carried by, for main raw material, being added nitrogen with electrically conductive graphite and mixing graphene
The electric conductivity of high magma can reduce unit dose simultaneously；In addition, being added to resin, glass powder, zinc powder, terpinol, second
The auxiliary agents such as base cellulose and polyvinylpyrrolidone improve the dispersibility of each raw material and further increase the electric conductivity of magma
Energy.The preparation method raw material is simple and easy to get, simple for process to produce in batches.In addition, nitrogen mixes the preparation of graphene in the present invention
Directly using the urea of abundance as nitrogen source, graphene is directly reduced into after high-temperature process using graphite oxide and existed simultaneously
Nitrogen has been made in the presence of nitrogen source and has mixed graphene.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention will be described in detail by way of examples below.
Preparation example 1
Nitrogen mixes the preparation of graphene：150g urea (analysis is pure) is added in the graphene oxide solution of 100mL, fully
After being stirred；Forced air drying 10h obtains mixed-powder at 40 DEG C；Then it is calcined the mixed-powder to obtain the nitrogen and be mixed
Graphene.Wherein, the step of calcining used is：It is started to warm up from 20 DEG C to 800 DEG C and maintains 1h at 800 DEG C, wherein heating up
Rate is 5 DEG C/min；Then 30 DEG C are cooled to the rate of temperature fall of 10 DEG C/min；Wherein, the atmosphere of the calcining is N2, N2's
Flow is 0.001m3/h.
Preparation example 2
Nitrogen mixes the preparation of graphene：200g urea (analysis is pure) is added in the graphene oxide solution of 100mL, fully
After being stirred；Forced air drying 6h obtains mixed-powder at 60 DEG C；Then it is calcined the mixed-powder to obtain the nitrogen and be mixed
Graphene.Wherein, the step of calcining used is：It is started to warm up from 20 DEG C to 800 DEG C and maintains 1h at 800 DEG C, wherein heating up
Rate is 5 DEG C/min；Then 30 DEG C are cooled to the rate of temperature fall of 10 DEG C/min；Wherein, the atmosphere of the calcining is N2, N2's
Flow is 0.001m3/h.
Embodiment 1
By nitrogen mix graphene, electrically conductive graphite, acrylic resin (weight average molecular weight be 10,000), glass powder, zinc powder, terpinol,
Ethyl cellulose and polyvinylpyrrolidone are according to weight proportion：10：100：25：1：1：30：1：1 is in rotating speed
It it is stirred 2h under 2000rpm obtains nitrogen and mix graphene modified graphite magma A1；
Wherein, added nitrogen mixes graphene obtained by preparation example 1.
Embodiment 2
By nitrogen mix graphene, electrically conductive graphite, polyvinyl resin (weight average molecular weight be 20,000), glass powder, zinc powder, terpinol,
Ethyl cellulose and polyvinylpyrrolidone are 15 according to weight proportion：100：30：3：3：30：2：3 rotating speed be 2500rpm
Under be stirred 1.5h and obtain nitrogen and mix graphene modified graphite magma A2；
Wherein, added nitrogen mixes graphene obtained by preparation example 2.
Embodiment 3
Nitrogen is mixed graphene, electrically conductive graphite, Lauxite (weight average molecular weight 1), polyurethane resin, and (weight average molecular weight is
2 ten thousand), glass powder, zinc powder, terpinol, ethyl cellulose and polyvinylpyrrolidone are 15 according to weight proportion：100：20：
15：3：3：30：2：3 are in rotating speed:It it is stirred 1.0h under 3000rpm obtains nitrogen and mix graphene modified graphite magma A3；
Wherein, added nitrogen mixes graphene obtained by preparation example 2.
Comparative example 1
Graphite magma B1 is prepared Following the procedure of Example 1, except that mixing graphene for nitrogen is added.
Comparative example 2
Graphite magma B2 is prepared Following the procedure of Example 2, except that mixing graphene for nitrogen is added.
Comparative example 3
Graphite magma B3 is prepared Following the procedure of Example 3, except that mixing graphene for nitrogen is added.
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 of phase homogenous quantities and B1-B4, the resistance for testing graphite linings is big
It is small.Concrete outcome is shown in Table 1.
| A1 | A2 | A3 | B1 | B2 | B3 | B4 | |
| Resistance (Ω) | 56 | 55 | 60 | 101 | 120 | 110 | 70 |
In the present invention, in graphite magma process for preparation adding nitrogen mixes graphene, since nitrogen mixes the electric conductivity of graphene
Very well, and nitrogen mixes the loose easy dispersion of graphene-structured, so that nitrogen obtained is mixed graphene modified graphite magma resistance and is obviously reduced；
In addition, the resin, glass powder, zinc powder, terpinol, ethyl cellulose and the polyvinylpyrrolidone that are added also improve graphite original
The viscosity of slurry, and then further improve painting efficiency and using effect that nitrogen mixes graphene modified graphite magma.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, 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, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (6)
1. a kind of nitrogen mixes the preparation method of graphene modified graphite magma, which is characterized in that including：Nitrogen is mixed into graphene, conduction
Graphite, the resin in addition to ethyl cellulose, glass powder, zinc powder, terpinol, ethyl cellulose and polyvinylpyrrolidone into
Row stirs to get the nitrogen and 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 is mixed,
Then it is dried to obtain mixed-powder；It finally is calcined the mixed-powder to obtain the nitrogen and mixes graphene；The oxygen
A concentration of 10mg/mL of graphite alkene solution, relative to the graphene oxide solution of 100 parts by weight, the dosage of the urea is
150-200 parts by weight；
Relative to the electrically conductive graphite of 100 parts by weight, the dosage that the nitrogen mixes graphene is 10-20 parts by weight, described except ethyl is fine
The dosage of resin other than dimension element is 25-35 parts by weight, and the dosage of the glass powder is 1-5 parts by weight, the dosage of the zinc powder
Dosage for 1-5 parts by weight, the terpinol is 30-40 parts by weight, and the dosage of the ethyl cellulose is 1-5 parts by weight, institute
The dosage for stating polyvinylpyrrolidone is 1-5 parts by weight；
The step of calcining is：Started to warm up from 20 DEG C to 800 DEG C and at 800 DEG C maintain 1h, wherein heating rate be 5 DEG C/
min；Then 30 DEG C are cooled to the rate of temperature fall of 10 DEG C/min；Wherein, the atmosphere of the calcining is N2, N2Flow be
0.001m3/h。
2. preparation method according to claim 1, wherein the resin in addition to ethyl cellulose is selected from polypropylene tree
It is one or more in fat, polyvinyl resin, Lauxite 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, gathers
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 of claim 1-3, wherein the rotating speed of the stirring is 2000-
The time of 3000rpm, stirring are 1-2h.
5. preparation method according to claim 4, wherein the drying is forced air drying, and dry temperature is 40-
60 DEG C, the dry time is 6-10h.
6. a kind of nitrogen mixes graphene modified graphite magma, which is characterized in that the nitrogen mixes graphene modified graphite magma by right
It is required that any one of 1-5 preparation methods are made.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072702A (en) * | 1991-11-22 | 1993-06-02 | 尹维平 | A kind of admixing type inorganic conductive coatings |
| 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 |
| CN103500597A (en) * | 2013-09-30 | 2014-01-08 | 广州市尤特新材料有限公司 | Functionalized graphene-based solar back aluminum slurry and preparation method thereof |
-
2016
- 2016-09-07 CN CN201610805591.9A patent/CN106409377B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072702A (en) * | 1991-11-22 | 1993-06-02 | 尹维平 | A kind of admixing type inorganic conductive coatings |
| 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 |
| CN103500597A (en) * | 2013-09-30 | 2014-01-08 | 广州市尤特新材料有限公司 | Functionalized graphene-based solar back aluminum slurry and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Production of graphene from graphite oxide using urea as expansion-reduction agent;Stephen Wakeland,Ricardo Martinez,John K.Grey;《Carbon》;Carbon;20100531(第48期);第3463-3470页 * |
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Effective date of registration: 20201127 Address after: 246500 Susong Economic Development Zone, Anhui, Anqing Patentee after: ANHUI DASONG RESIN Co.,Ltd. Address before: No.322, building 4, Zone 8, hengtaiyun shopping mall, Nanxiang, Yongqiao District, Suzhou City, Anhui Province Patentee before: Suzhou Ziyuan Science and Technology Consulting Co.,Ltd. |