CN106588016A - Method for preparing graphene oxide graphite electrode - Google Patents
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Abstract
The invention relates to a method for preparing a graphene oxide graphite electrode. The method includes the steps that graphene oxide is prepared into colloidal sol to be mixed with a graphite electrode, the homogeneity and the crosslinking property of graphene oxide in the whole mixed materials are ensured through mixing and kneading, the mixed materials are mixed and kneaded and subjected to extruding forming, and finally calcination and graphitization high-temperature processing are conducted to obtain the finished graphite electrode. Compared with the prior art, on one hand, thermal reduction of graphite oxide to graphene is achieved by the method; on the other hand, due to the use of high-strength and high electron mobility properties of graphene, the method effectively improves the bending strength of the finished graphite electrode and lowers resistivity.
Description
Technical field
The present invention relates to graphite electrode preparing technical field, more particularly to a kind of preparation side of graphene oxide graphite electrode
Method.
Background technology
Graphene has its unique physical and chemical performance, is to presently, there are mankind's known strength highest material, and its is strong
Degree is up to 130GPa, also stronger than diamond, is 100 times of best iron and steel intensity in the world.Tellurian graphite resource enriches, and
Graphene can prepare Graphene by graphite, and Graphene is rated as current intensity highest, the best thing of electric conductivity, thermal conductivity
Matter, with so it will possess numerous development prospects for firing one's imagination, current graphite electrode in application process, its mechanical strength
It is not good enough with electric property.
The content of the invention
The technical problem to be solved is to provide a kind of preparation method of graphene oxide graphite electrode, the method
It is Graphene by graphene oxide thermal reduction, using Graphene high intensity, high electron mobility performance, is applied to graphite electrode
In, the rupture strength of graphite electrode articles can be improved and resistivity is reduced.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of preparation method of graphene oxide graphite electrode, it is comprised the following steps:
The preparation of A, graphene oxide colloidal sol
Under normal temperature condition, compound concentration is the graphene oxide colloidal sol of 15-30mg/ml；
B, kneading extruding
By the graphene oxide colloidal sol obtained in step A, in being added to graphite electrode thickener, the addition of graphene oxide colloidal sol
Measure as the 1-10% of graphite electrode thickener total amount, then base is squeezed into by kneading, eventually pass roasting, at graphitizable high temperature
Reason.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement.
Further, in step, the graphene oxide colloidal sol is prepared by graphene oxide with dispersant ultrasonic disperse
Obtain.
Further, the dispersant is liquid resin or alcohol.
Further, the ultrasonic disperse time control is in 5-15mi n.
Further, the liquid resin is one or more in thermosetting phenolic resin, epoxy resin, furane resins.
Further, in stepb, the graphite electrode thickener is by petroleum coke and mid temperature pitch in mass ratio 3:1 mixes
Close, heated kneading is formed.
Further, the heating-up temperature is 150-170 DEG C.
Further, the kneading time control is in 15-20mi n.
Further, in stepb, at 110-120 DEG C, squeeze pressure is controlled in 10-15MPa for the extrusion temperature control,
Dwell time is 5-10mi n, and the sintering temperature is controlled at 1000-1250 DEG C, and the graphitizable high temperature processes control and exists
2700-3400℃
Compared with prior art, the invention has the beneficial effects as follows：
The present invention provides a kind of preparation method of graphene oxide graphite electrode, the method by graphene oxide colloidal sol with
Graphite electrode thickener mixes, and ensures to make homogenieity and bridging property of the graphene oxide in overall batch mixing by kneading, through pressure
System, low-temperature bake, high-order graphitization processing, on the one hand realize that graphene oxide thermal reduction is Graphene, on the one hand using graphite
Alkene high intensity, high electron mobility performance, effectively improve the rupture strength of graphite electrode articles and reduce resistivity.
Specific embodiment
The principle and feature of the present invention are described below, example is served only for explaining the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
The preparation of A, graphene oxide colloidal sol
Under normal temperature condition, graphene oxide obtains concentration and is with thermosetting phenolic resin ultrasonic disperse 5mi n preparations
The graphene oxide colloidal sol of 30mg/ml；
B, kneading extruding
By the graphene oxide colloidal sol obtained in step A, in being added to graphite electrode thickener, the addition of graphene oxide colloidal sol
Measure as the 8% of graphite electrode thickener total amount, then base be squeezed into by kneading, extrusion temperature control at 110 DEG C, squeeze pressure control
System is 5mi n in 10MPa, dwell time, eventually passes 1250 DEG C of roastings, 2800 DEG C of graphitizable high temperatures and processes, and obtains graphite electricity
Pole product；Graphite electrode thickener is by petroleum coke and mid temperature pitch in mass ratio 3:1 mixing, 150 DEG C of heating-up temperature kneadings of Jing
15mi n are formed.
Embodiment 2
The preparation of A, graphene oxide colloidal sol
Under normal temperature condition, graphene oxide prepares the oxidation for obtaining that concentration is 15mg/ml with alcohol ultrasonic disperse 7mi n
Graphene sol；
B, kneading extruding
By the graphene oxide colloidal sol obtained in step A, in being added to graphite electrode thickener, the addition of graphene oxide colloidal sol
Measure as the 5% of graphite electrode thickener total amount, then base be squeezed into by kneading, extrusion temperature control at 112 DEG C, squeeze pressure control
System is 6mi n in 11MPa, dwell time, eventually passes 1250 DEG C of roastings, 2800 DEG C of graphitizable high temperatures and processes, and obtains graphite electricity
Pole product；Graphite electrode thickener is by petroleum coke and mid temperature pitch in mass ratio 3:1 mixing, 152 DEG C of heating kneadings 16mi of Jing
N is formed.
Embodiment 3
The preparation of A, graphene oxide colloidal sol
Under normal temperature condition, graphene oxide is prepared with liquid thermosetting epoxy resin ultrasonic disperse 10mi n and obtains concentration
For the graphene oxide colloidal sol of 18mg/ml；
B, kneading extruding
By the graphene oxide colloidal sol obtained in step A, in being added to graphite electrode thickener, the addition of graphene oxide colloidal sol
Measure as the 6% of graphite electrode thickener total amount, then base be squeezed into by kneading, extrusion temperature control at 115 DEG C, squeeze pressure control
System is 8mi n in 13MPa, dwell time, eventually passes 1000 DEG C of roastings, 2700 DEG C of graphitizable high temperatures and processes, and obtains graphite electricity
Pole product；Graphite electrode thickener is by petroleum coke and mid temperature pitch in mass ratio 3:1 mixing, 155 DEG C of heating kneadings 18mi of Jing
N is formed.
Embodiment 4
The preparation of A, graphene oxide colloidal sol
Under normal temperature condition, graphene oxide is prepared with liquid thermoset furane resins ultrasonic disperse 12mi n and obtains concentration
For the graphene oxide colloidal sol of 20mg/ml；
B, kneading extruding
By the graphene oxide colloidal sol obtained in step A, in being added to graphite electrode thickener, the addition of graphene oxide colloidal sol
Measure as the 1% of graphite electrode thickener total amount, then base be squeezed into by kneading, extrusion temperature control at 120 DEG C, squeeze pressure control
System is 10mi n in 15MPa, dwell time, eventually passes 1150 DEG C of roastings, 3000 DEG C of graphitizable high temperatures and processes, and obtains graphite electricity
Pole product；Graphite electrode thickener is by petroleum coke and mid temperature pitch in mass ratio 3:1 mixing, 160 DEG C of heating kneadings 18mi of Jing
N is formed.
Embodiment 5
The preparation of A, graphene oxide colloidal sol
Under normal temperature condition, graphene oxide obtains concentration and is with liquid epoxies ultrasonic disperse 15mi n preparations
The graphene oxide colloidal sol of 25mg/ml；
B, kneading extruding
By the graphene oxide colloidal sol obtained in step A, in being added to graphite electrode thickener, the addition of graphene oxide colloidal sol
Measure as the 5% of graphite electrode thickener total amount, then base is squeezed into by kneading, the extrusion temperature is controlled at 118 DEG C, extruding pressure
Power control is 9mi n in 14MPa, dwell time, eventually passes 1200 DEG C of roastings, 3400 DEG C of graphitizable high temperatures and processes and obtain graphite
Electrode product；Graphite electrode thickener is by petroleum coke and mid temperature pitch in mass ratio 3:1 mixes, and heated heating-up temperature is
170 DEG C of kneading 20mi n are formed.
Graphene oxide graphite electrode performance in the inspection present invention, is to have carried out performance evaluation to graphitization sample.Uniformly
Kneading, extrusion molding green compact test the physical properties of sample after roasting, graphitization process.
Blank, embodiment 1 and the performance parameter of embodiment 2 are as shown in the table：
Can be learnt by upper table, its rupture strength of graphene oxide graphite electrode of the present invention is improved, and resistivity is obtained
Reduce.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
The foregoing is only presently preferred embodiments of the present invention, not to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene oxide graphite electrode, it is characterised in that it is comprised the following steps:
The preparation of A, graphene oxide colloidal sol
Under normal temperature condition, compound concentration is the graphene oxide colloidal sol of 15-30mg/ml；
B, kneading extruding
By the graphene oxide colloidal sol obtained in step A, in being added to graphite electrode thickener, graphene oxide colloidal sol addition is
The 1-10% of graphite electrode thickener total amount, is then squeezed into base by kneading, eventually passes roasting, graphitizable high temperature process, i.e.,
.
2. the preparation method of a kind of graphene oxide graphite electrode according to claim 1, it is characterised in that in step A
In, the graphene oxide colloidal sol is prepared with dispersant ultrasonic disperse by graphene oxide and obtained.
3. a kind of preparation method of graphene oxide graphite electrode according to claim 2, it is characterised in that the dispersion
Agent is liquid resin or alcohol.
4. a kind of preparation method of graphene oxide graphite electrode according to claim 2, it is characterised in that the ultrasound
Jitter time is controlled in 5-15min.
5. a kind of preparation method of graphene oxide graphite electrode according to claim 3, it is characterised in that the liquid
Resin is one or more in thermosetting phenolic resin, epoxy resin, furane resins.
6. the preparation method of a kind of graphene oxide graphite electrode according to claim 1, it is characterised in that in step B
In, the graphite electrode thickener is by petroleum coke and mid temperature pitch in mass ratio 3:1 mixing, heated kneading is formed.
7. a kind of preparation method of graphene oxide graphite electrode according to claim 6, it is characterised in that the heating
Temperature is 150-170 DEG C.
8. a kind of preparation method of graphene oxide graphite electrode according to claim 6, it is characterised in that the kneading
Time control is in 15-20min.
9. the preparation method of a kind of graphene oxide graphite electrode according to claim 1, it is characterised in that in step B
In, at 110-120 DEG C, squeeze pressure is controlled in 10-15MPa, and the dwell time is 5-10min, described for the extrusion temperature control
Sintering temperature is controlled at 1000-1250 DEG C, and the graphitizable high temperature processes control at 2700-3400 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107277960A (en) * | 2017-05-24 | 2017-10-20 | 方大炭素新材料科技股份有限公司 | A kind of method for reducing graphite electrode/connection resistance rate |
| CN108516813A (en) * | 2018-06-27 | 2018-09-11 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene ceramic tile |
| CN108585861A (en) * | 2018-03-22 | 2018-09-28 | 合肥炭素有限责任公司 | A kind of electrode contact and preparation method thereof |
| CN109020547A (en) * | 2018-09-03 | 2018-12-18 | 大同宇林德石墨设备股份有限公司 | A kind of preparation method of the graphite electrode nipple containing graphene |
| CN109768277A (en) * | 2019-01-11 | 2019-05-17 | 北京科技大学 | A kind of graphene oxide modified coal pitch binder and preparation method thereof |
| CN110590363A (en) * | 2019-09-29 | 2019-12-20 | 西姆信息技术服务(大连)有限公司 | Ultrahigh-power graphite electrode and manufacturing method thereof |
| CN111620333A (en) * | 2020-06-23 | 2020-09-04 | 柯良节 | Composite graphite electrode and preparation method thereof |
| CN113979751A (en) * | 2021-09-28 | 2022-01-28 | 大同新成新材料股份有限公司 | Graphene-carbon graphite composite isostatic pressing material and preparation method thereof |
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| CN102158999A (en) * | 2011-05-16 | 2011-08-17 | 方大炭素新材料科技股份有限公司 | Phi 800mm general power graphite electrode and production method thereof |
| CN105885906A (en) * | 2016-04-12 | 2016-08-24 | 方大炭素新材料科技股份有限公司 | Preparation method of oxidized graphene modified medium-temperature coal tar pitch |
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| CN102158999A (en) * | 2011-05-16 | 2011-08-17 | 方大炭素新材料科技股份有限公司 | Phi 800mm general power graphite electrode and production method thereof |
| CN105885906A (en) * | 2016-04-12 | 2016-08-24 | 方大炭素新材料科技股份有限公司 | Preparation method of oxidized graphene modified medium-temperature coal tar pitch |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107277960A (en) * | 2017-05-24 | 2017-10-20 | 方大炭素新材料科技股份有限公司 | A kind of method for reducing graphite electrode/connection resistance rate |
| CN108585861A (en) * | 2018-03-22 | 2018-09-28 | 合肥炭素有限责任公司 | A kind of electrode contact and preparation method thereof |
| CN108516813A (en) * | 2018-06-27 | 2018-09-11 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene ceramic tile |
| CN109020547A (en) * | 2018-09-03 | 2018-12-18 | 大同宇林德石墨设备股份有限公司 | A kind of preparation method of the graphite electrode nipple containing graphene |
| CN109768277A (en) * | 2019-01-11 | 2019-05-17 | 北京科技大学 | A kind of graphene oxide modified coal pitch binder and preparation method thereof |
| CN109768277B (en) * | 2019-01-11 | 2020-11-06 | 北京科技大学 | Graphene oxide modified coal tar pitch binder and preparation method thereof |
| CN110590363A (en) * | 2019-09-29 | 2019-12-20 | 西姆信息技术服务(大连)有限公司 | Ultrahigh-power graphite electrode and manufacturing method thereof |
| CN111620333A (en) * | 2020-06-23 | 2020-09-04 | 柯良节 | Composite graphite electrode and preparation method thereof |
| CN113979751A (en) * | 2021-09-28 | 2022-01-28 | 大同新成新材料股份有限公司 | Graphene-carbon graphite composite isostatic pressing material and preparation method thereof |
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Application publication date: 20170426 |