CN110204349A - A kind of carbon nano-tube modification enhancing graphite electrode and preparation method thereof - Google Patents
A kind of carbon nano-tube modification enhancing graphite electrode and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to graphite electrode preparation technical fields, more particularly to a kind of carbon nano-tube modification enhancing graphite electrode and preparation method thereof, including the following raw material: 100 parts of petroleum coke particles, 5-100 parts of carbon nanotube, 5-100 parts of needle coke, 5-10 parts of calcium oxide, 35-45 parts and carbon nano tube dispersion liquid 5-200 parts of pitch；Preparation method is the following steps are included: by petroleum coke particles, carbon nanotube, needle coke, calcium oxide kneading；Asphalt melting is added carbon nano tube dispersion liquid and mixes, kneading pot kneading；Material is imported in molding die and obtains graphite electrode blank to be roasted；Roasting obtains graphite electrode roasting product；Graphite electrode roasting product is heated in high-temperature electric resistance furnace, graphite electrode is prepared.By the way that carbon nano-tube material is added, product consistency is improved, graphite electrode heat-resistant knocking stability is enhanced, reduces resistivity, elasticity modulus and pressure-proof and snap-resistent intensity is improved, is obviously improved the physical property of material and electric property.
Description
Technical field
The present invention relates to graphite electrode preparation technical fields, and in particular to a kind of carbon nano-tube modification enhancing graphite electrode and
Preparation method.
Background technique
Graphite electrode be using petroleum coke, needle coke as raw material, coal tar pitch as adhesive, through raw material calcining, broken milling,
Ingredient, kneading, molding, roasting, dipping and graphitization and etc. made of a kind of high temperature resistant graphite conductive material, answer extensively
Preparation for electrical arc furnace, ladle refining furnace, ore-smelting electric furnace, resistance furnace and special-shaped graphite products.In electrical arc furnace and
In ladle refining furnace, electrode is in terminal position, and effect is high-current leading to be directed at working chamber or molten steel, in electrode and furnace charge
Between or electrode and molten steel between generate electric arc to achieve the purpose that heat furnace charge and molten steel.
Graphite electrode is electric arc furnaces and the indispensable important materials of ladle refining furnace, and consumption is very big, at present the electricity in China
Furnace graphite electrode average quantity used in unit volume blasted is 7~8kg/t steel, accounts for about the 8% of electric furnace steel making cost.Current graphite electrode is due to structure
Unstable, intensity is not high, and during transport, product often will appear breakage, influences user's use.Graphite electrode current distribution
It is universal uneven, and graphite electrode is connecting the phenomenon that electric discharge is caused there may be gap in nipple position, and graphite electricity
Pole is chronically in oxidisability hot environment and works, and is easy to produce heat in the process of work and causes to aoxidize, existing graphite
Resistance volume is larger, with high-voltage arc impact and electric current kelvin effect, keeps graphite electrode durability poor, graphite electrode is caused to connect
Head rupture, surface peel off, severe oxidation attenuates, and improve use cost.Electrode, which loosens, to be fallen into molten steel, handle too late
Shi Zaocheng production accident increases production safety hidden danger.
For above-mentioned variety of problems, CN109231987 targetedly develops oxidation resistant graphite electrode material,
CN109678516 develops a kind of antioxidative graphite electrode surface coating and preparation process, but not yet discovery is special at present
Effective method.
Summary of the invention
Lead to structural instability for the graphite electrode stability in use difference of the prior art, fast ask is lost in easy fracture, peeling
Topic, the present invention provide a kind of carbon nano-tube modification enhancing graphite electrode and preparation method thereof, by the way that carbon nano-tube material is added, mention
High product consistency enhances graphite electrode heat-resistant knocking stability, reduces resistivity, improves elasticity modulus and pressure-proof and snap-resistent intensity,
The physical property and electric property for making material are obviously improved.
In a first aspect, the present invention provides a kind of carbon nano-tube modification enhancing graphite electrode, the carbon nano-tube modification enhancing
Graphite electrode includes the raw material of following parts by weight:
100 parts of petroleum coke particles, 5-100 parts of carbon nanotube, 5-100 parts of needle coke, 5-10 parts of calcium oxide, pitch 35-45
Part and carbon nano tube dispersion liquid 5-200 parts.
Further, the carbon nano tube dispersion liquid includes carbon nanotube, solvent and dispersing agent,
The solvent be one or more of water, ethyl alcohol, n,N-Dimethylformamide, toluene, N-Methyl pyrrolidone,
The dispersing agent is polyvinylpyrrolidone, neopelex, cetyl trimethylammonium bromide, alkyl
One or more of phenol ethylene oxide condensates emulsifier.
Further, the weight ratio of carbon nanotube, solvent and dispersing agent is (1-10) in the carbon nano tube dispersion liquid:
(10-99): (1-10).
Further, in the carbon nano tube dispersion liquid after carbon nanotube, solvent and dispersant through nanometer sand mill
2-8h is sanded.
Further, the carbon nanotube is one or both of agglomerate shape carbon nanotube, array tube, caliber 5-
100nm, length are 1 μm of -1m, and partial size D50 is 1 μm of -2mm.
Further, for the carbon nanotube without purifying in advance, carbon nanotube is direct in graphite electrode preparation process
In-situ high temperature purification process.
Second aspect, the present invention provide a kind of carbon nano-tube modification enhancing graphite electrode preparation method, and method includes following
Step:
(1) first by 100 parts of petroleum coke particles, 5-100 parts of carbon nanotube, 5-100 parts of needle coke, 5-10 parts of calcium oxide importings
In kneading pot, it is warming up to 130-135 DEG C, kneading 65-75min；
(2) 35-45 parts of pitches are weighed, 170-180 DEG C of fusing is heated in liquid evaporation recovery system, 5-200 is added
It after part carbon nano tube dispersion liquid mixes, is added in the kneading pot of step (1), control kneading pot is warming up to 160-165 DEG C, kneading pot
Mixing speed be 1550-1650r/min, keep the temperature kneading 35-65min；
(3) after the completion of kneading, by material import molding die in, be forced into 15-25MPa, pressure maintaining 45-65min, obtain to
Roast graphite electrode blank；
(4) under the conditions of nitrogen protection atmosphere, the roasting of graphite electrode blank, 5-10 DEG C of heating rate/min, in the highest temperature
Spend 1450 DEG C keep 24 after Temperature fall, obtain graphite electrode roasting product after cooling 75h；
(5) graphite electrode roasting product is heated in high-temperature electric resistance furnace 2450-2750 DEG C, keeps the temperature 30-80h, is prepared
Graphite electrode.
Further, the blending manner of pitch and carbon nano tube dispersion liquid is high speed shear dispersion machine in the step (2)
Dispersion or forced stirrer stirring or both collaboration.
The beneficial effects of the present invention are,
(1) by the way that carbon nanotube, the refinement of graphite electrode starting material particle size gradation is added, material density is improved, graphite electricity
Pole heat-resistant knocking stability improves, and elasticity modulus is promoted；
(2) the superelevation draw ratio of carbon nano-tube material reduces the possibility of generation and the growth of micro-crack, plays nanoscale
Fiber reinforcement effect, compression strength especially flexural strength are obviously improved；
(3) carbon nanotube provides current path network bridged linkage for graphite electrode, reduces resistivity to a certain degree,
Most of all, promoting balanced current distribution；
(4) a part of carbon nanotube is received in raw material with solidapowder form and needle coke, petroleum coke kneading, another part carbon
Mitron in the form of carbon nano tube dispersion liquid first with fusing pitch mix after, then with other raw material kneadings, effectively improve carbon and receive
Dispersion degree of the mitron in graphite electrode；
(5) when graphite electrode roasts, graphitizing process not only occurs, while can be realized the in-situ purification of carbon nanotube,
Purification procedures before simplifying carbon nanotube use save the use cost of carbon nanotube；
(6) index of the carbon nano-tube modification enhancing graphite electrode prepared by the method for the invention is as follows:
5.0 μ Ω m≤ electricity Zu μ Ω of Shuai≤6.0 m, 1.65g/cm3≤ Ti accumulates Mi Du≤1.70g/cm3, 15MPa≤anti-
Roll over Qiang Du≤20MPa, 16GPa≤Dan Mo Liang≤20GPa.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention below will be implemented the present invention
Technical solution in example is clearly and completely described, it is clear that described embodiment is only that present invention a part is implemented
Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creativeness
Every other embodiment obtained, should fall within the scope of the present invention under the premise of labour.
Embodiment 1
A kind of carbon nano-tube modification enhancing graphite electrode, the raw material including following parts by weight:
100 parts of petroleum coke particles, 20 parts of carbon nanotube, 15 parts of needle coke, 5 parts of calcium oxide, 38 parts of pitch and carbon nanotube
35 parts of dispersion liquid；
Wherein carbon nanotube is agglomerate shape carbon nanotube, and caliber 10-30nm, 3-50 μm of length, partial size D50 is 1-3 μm；
Carbon nano tube dispersion liquid is by carbon nanotube, N-Methyl pyrrolidone and polyvinylpyrrolidone through nanometer sand mill sand
It grinds 5h to be made, the weight ratio of carbon nanotube, N-Methyl pyrrolidone and polyvinylpyrrolidone is 1:96:3.
The preparation method of carbon nano-tube modification enhancing graphite electrode, comprising the following steps:
(1) first by 5 parts of 100 parts of petroleum coke particles, 20 parts of carbon nanotube, 15 parts of needle coke, calcium oxide importing kneading pots,
135 DEG C are warming up to, kneading 65-75min；
(2) 38 parts of pitches are weighed, 170 DEG C of fusings are heated in liquid evaporation recovery system, 35 parts of carbon nanotubes are added
Dispersion liquid is mixed by the dispersion of high speed shear dispersion machine, is then added in the kneading pot of step (1), and control kneading pot is warming up to
160 DEG C, the mixing speed of kneading pot is 1550r/min, keeps the temperature kneading 40min；
(3) after the completion of kneading, material is imported in molding die, is forced into 15MPa, pressure maintaining 50min obtains stone to be roasted
Electrode ink blank；
(4) under the conditions of nitrogen protection atmosphere, the roasting of graphite electrode blank, 5 DEG C/min of heating rate, in maximum temperature
Temperature fall after 1450 DEG C of holdings 24 obtains graphite electrode roasting product after cooling down 75h；
(5) graphite electrode roasting product is heated in high-temperature electric resistance furnace 2500 DEG C, keeps the temperature 36h, graphite electrode is prepared.
The index that carbon nano-tube modification enhances graphite electrode is as follows:
Resistivity=5.8 μ Ω m, bulk density=1.66g/cm3, flexural strength=15.1MPa, elasticity modulus=
16.2GPa。
Embodiment 2
A kind of carbon nano-tube modification enhancing graphite electrode, the raw material including following parts by weight:
100 parts of petroleum coke particles, 80 parts of carbon nanotube, 75 parts of needle coke, 8 parts of calcium oxide, 43 parts of pitch and carbon nanotube
150 parts of dispersion liquid；
Wherein carbon nanotube is array tube, and caliber 8-20nm, length 1mm-1m, partial size D50 is 5-10 μm；
Carbon nano tube dispersion liquid is sanded 3h through nanometer sand mill by carbon nanotube, toluene and polyvinylpyrrolidone and is made,
The weight ratio of carbon nanotube, toluene and polyvinylpyrrolidone is 3:90:7.
The preparation method of carbon nano-tube modification enhancing graphite electrode, comprising the following steps:
(1) first by 8 parts of 100 parts of petroleum coke particles, 80 parts of carbon nanotube, 75 parts of needle coke, calcium oxide importing kneading pots,
130 DEG C are warming up to, kneading 70min；
(2) 43 parts of pitches are weighed, 175 DEG C of fusings are heated in liquid evaporation recovery system, 150 parts of carbon nanotubes are added
Dispersion liquid is stirred and evenly mixed by high forced stirrer, is then added in the kneading pot of step (1), and control kneading pot is warming up to 165
DEG C, the mixing speed of kneading pot is 1600r/min, keeps the temperature kneading 50min；
(3) after the completion of kneading, material is imported in molding die, is forced into 25MPa, pressure maintaining 60min obtains stone to be roasted
Electrode ink blank；
(4) under the conditions of nitrogen protection atmosphere, the roasting of graphite electrode blank, 10 DEG C/min of heating rate, in maximum temperature
Temperature fall after 1450 DEG C of holdings 24 obtains graphite electrode roasting product after cooling down 75h；
(5) graphite electrode roasting product is heated in high-temperature electric resistance furnace 2700 DEG C, keeps the temperature 72h, graphite electrode is prepared.
The index that carbon nano-tube modification enhances graphite electrode is as follows:
Resistivity=5.1 μ Ω m, bulk density=1.69g/cm3, flexural strength=19.5MPa, elasticity modulus=
20GPa。
Embodiment 3
A kind of carbon nano-tube modification enhancing graphite electrode, the raw material including following parts by weight:
100 parts of petroleum coke particles, 55 parts of carbon nanotube, 60 parts of needle coke, 9 parts of calcium oxide, 40 parts of pitch and carbon nanotube
90 parts of dispersion liquid；
Wherein carbon nanotube is the mixture of agglomerate shape carbon nanotube and array tube, and the caliber of agglomerate shape carbon nanotube is
10-30nm, 3-50 μm of length, partial size D50 is 1-3 μm, and the caliber of array tube is 8-20nm, and length 1mm-1m, partial size D50 are 5-
10 μm, blending mass ratio is 1:1；
Carbon nano tube dispersion liquid is sanded 7h through nanometer sand mill by carbon nanotube, toluene and polyvinylpyrrolidone and is made,
The weight ratio of carbon nanotube, toluene and polyvinylpyrrolidone is 8:70:8.
The preparation method of carbon nano-tube modification enhancing graphite electrode, comprising the following steps:
(1) first by 9 parts of 100 parts of petroleum coke particles, 55 parts of carbon nanotube, 60 parts of needle coke, calcium oxide importing kneading pots,
132 DEG C are warming up to, kneading 70min；
(2) 40 parts of pitches are weighed, 175 DEG C of fusings are heated in liquid evaporation recovery system, 90 parts of carbon nanotubes are added
Dispersion liquid is stirred and evenly mixed by high forced stirrer, is then added in the kneading pot of step (1), and control kneading pot is warming up to 163
DEG C, the mixing speed of kneading pot is 1650r/min, keeps the temperature kneading 60min；
(3) after the completion of kneading, material is imported in molding die, is forced into 20MPa, pressure maintaining 55min obtains stone to be roasted
Electrode ink blank；
(4) under the conditions of nitrogen protection atmosphere, the roasting of graphite electrode blank, 7 DEG C/min of heating rate, in maximum temperature
Temperature fall after 1450 DEG C of holdings 24 obtains graphite electrode roasting product after cooling down 75h；
(5) graphite electrode roasting product is heated in high-temperature electric resistance furnace 2600 DEG C, keeps the temperature 48h, graphite electrode is prepared.
The index that carbon nano-tube modification enhances graphite electrode is as follows:
Resistivity=5.6 μ Ω m, bulk density=1.67g/cm3, flexural strength=17MPa, elasticity modulus=
17GPa。
Comparative example 1
A kind of graphite electrode, the raw material including following parts by weight:
100 parts of petroleum coke particles, 15 parts of needle coke, 5 parts of calcium oxide, 38 parts of pitch；
A kind of preparation method of graphite electrode, comprising the following steps:
(1) 135 DEG C first are warming up to by 5 parts of 100 parts of petroleum coke particles, 15 parts of needle coke, calcium oxide importing kneading pots,
Kneading 65-75min；
(2) 38 parts of pitches are weighed, 170 DEG C of fusings are heated in liquid evaporation recovery system, are then added to step (1)
In kneading pot, control kneading pot is warming up to 160 DEG C, and the mixing speed of kneading pot is 1550r/min, keeps the temperature kneading 40min；
(3) after the completion of kneading, material is imported in molding die, is forced into 15MPa, pressure maintaining 50min obtains stone to be roasted
Electrode ink blank；
(4) under the conditions of nitrogen protection atmosphere, the roasting of graphite electrode blank, 5 DEG C/min of heating rate, in maximum temperature
Temperature fall after 1450 DEG C of holdings 24 obtains graphite electrode roasting product after cooling down 75h；
(5) graphite electrode roasting product is heated in high-temperature electric resistance furnace 2500 DEG C, keeps the temperature 36h, graphite electrode is prepared.
A kind of index of graphite electrode is as follows:
Resistivity=6.8 μ Ω m, bulk density=1.65g/cm3, flexural strength=11.2MPa, elasticity modulus=
13.5GPa。
Comparative example 1-3 and comparative example 1 it can be found that the addition of carbon nanotube to the physical property and electricity of graphite electrode
The improvement for learning performance has a significant effect, and can reduce graphite electrode resistivity, improve consistency, flexural strength and the bullet of graphite electrode
Property modulus.
Although the present invention is not limited thereto to the present invention have been described in detail by way of preferred embodiment.?
Under the premise of not departing from spirit and substance of the present invention, those of ordinary skill in the art can carry out the embodiment of the present invention each
Kind equivalent modifications or substitutions, and these modifications or substitutions all should in covering scope of the invention/any be familiar with this technology neck
The technical staff in domain in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all cover of the invention
Within protection scope.Therefore, protection scope of the present invention should be subject to protection scope described in claim.
Claims (10)
1. a kind of carbon nano-tube modification enhances graphite electrode, which is characterized in that the carbon nano-tube modification enhances graphite electrode packet
Include the raw material of following parts by weight:
100 parts of petroleum coke particles, 5-100 parts of carbon nanotube, 5-100 parts of needle coke, 5-10 parts of calcium oxide, 35-45 parts of pitch and
5-200 parts of carbon nano tube dispersion liquid.
2. a kind of carbon nano-tube modification as described in claim 1 enhances graphite electrode, which is characterized in that the carbon nanotube point
Dispersion liquid includes carbon nanotube, solvent and dispersing agent,
The solvent be one or more of water, ethyl alcohol, n,N-Dimethylformamide, toluene, N-Methyl pyrrolidone,
The dispersing agent is polyvinylpyrrolidone, neopelex, cetyl trimethylammonium bromide, alkyl phenol ring
One or more of oxidative ethane condensation product emulsifier.
3. a kind of carbon nano-tube modification as claimed in claim 2 enhances graphite electrode, which is characterized in that the carbon nanotube point
The weight ratio of carbon nanotube, solvent and dispersing agent is (1-10): (10-99): (1-10) in dispersion liquid.
4. a kind of carbon nano-tube modification as claimed in claim 2 enhances graphite electrode, which is characterized in that carbon nano tube dispersion liquid
2-8h is sanded through nanometer sand mill after middle carbon nanotube, solvent and dispersant.
5. a kind of carbon nano-tube modification as described in claim 1 enhances graphite electrode, which is characterized in that the carbon nanotube is
One or both of agglomerate shape carbon nanotube, array tube, caliber 5-100nm, length be 1 μm of -1m, D50 partial size be 1 μm -
2mm。
6. a kind of carbon nano-tube modification as described in claim 1 enhances graphite electrode, which is characterized in that the carbon nanotube is not
By purifying in advance.
7. a kind of carbon nano-tube modification as claimed in any one of claims 1 to 6 enhances graphite electrode preparation method, feature exists
In, method the following steps are included:
(1) first by 5-10 parts of 100 parts of petroleum coke particles, 5-100 parts of carbon nanotube, 5-100 parts of needle coke, calcium oxide importing kneadings
Pot kneading；
(2) 35-45 parts of pitches are weighed, fusing is heated in liquid evaporation recovery system, 5-200 parts of carbon nano tube dispersion liquids are added
After mixing, kneading in the kneading pot of step (1) is added；
(3) after the completion of kneading, material is imported in molding die, graphite electrode blank to be roasted is obtained；
(4) under the conditions of nitrogen protection atmosphere, the roasting of graphite electrode blank obtains graphite electrode roasting product after cooling；
(5) graphite electrode roasting product is heated in high-temperature electric resistance furnace, graphite electrode is prepared.
8. a kind of carbon nano-tube modification as claimed in claim 7 enhances graphite electrode preparation method, which is characterized in that method packet
Include following steps:
(1) first by 5-10 parts of 100 parts of petroleum coke particles, 5-100 parts of carbon nanotube, 5-100 parts of needle coke, calcium oxide importing kneadings
In pot, it is warming up to 130-135 DEG C, kneading 65-75min；
(2) 35-45 parts of pitches are weighed, 170-180 DEG C of fusing is heated in liquid evaporation recovery system, 5-200 parts of carbon are added
It after nanotube dispersion liquid mixes, is added in the kneading pot of step (1), control kneading pot is warming up to 160-165 DEG C, and kneading pot stirs
Mixing speed is 1550-1650r/min, keeps the temperature kneading 35-65min；
(3) after the completion of kneading, material is imported in molding die, is forced into 15-25MPa, pressure maintaining 45-65min is obtained wait roast
Graphite electrode blank；
(4) under the conditions of nitrogen protection atmosphere, the roasting of graphite electrode blank, 5-10 DEG C of heating rate/min, in maximum temperature
Temperature fall after 1450 DEG C of holdings 24 obtains graphite electrode roasting product after cooling down 75h；
(5) graphite electrode roasting product is heated in high-temperature electric resistance furnace 2450-2750 DEG C, keeps the temperature 30-80h, graphite electrode is made.
9. a kind of carbon nano-tube modification as claimed in claim 7 enhances graphite electrode preparation method, which is characterized in that the carbon
Without purifying in advance, carbon nanotube is purified nanotube in the roasting of step (4) and the heating process of step (5).
10. a kind of carbon nano-tube modification as claimed in claim 7 enhances graphite electrode preparation method, which is characterized in that described
In step (2) blending manner of pitch and carbon nano tube dispersion liquid be high speed shear dispersion machine disperse or forced stirrer stirring or
The two collaboration.
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| CN112225576A (en) * | 2020-10-20 | 2021-01-15 | 大同通扬碳素有限公司 | Preparation method of graphite electrode beneficial to reducing loss |
| CN113735605A (en) * | 2021-10-12 | 2021-12-03 | 上海仁朋实业有限公司 | Ultrahigh-power graphite electrode and preparation method thereof |
| CN117486612A (en) * | 2024-01-02 | 2024-02-02 | 唐山金湾特碳石墨有限公司 | Preparation method of purified carbon rod and purified carbon rod prepared by preparation method |
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2019
- 2019-06-26 CN CN201910562399.5A patent/CN110204349A/en not_active Withdrawn
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| CN112225576A (en) * | 2020-10-20 | 2021-01-15 | 大同通扬碳素有限公司 | Preparation method of graphite electrode beneficial to reducing loss |
| CN113735605A (en) * | 2021-10-12 | 2021-12-03 | 上海仁朋实业有限公司 | Ultrahigh-power graphite electrode and preparation method thereof |
| CN113735605B (en) * | 2021-10-12 | 2022-10-11 | 上海仁朋实业有限公司 | Ultrahigh-power graphite electrode and preparation method thereof |
| CN117486612A (en) * | 2024-01-02 | 2024-02-02 | 唐山金湾特碳石墨有限公司 | Preparation method of purified carbon rod and purified carbon rod prepared by preparation method |
| CN117486612B (en) * | 2024-01-02 | 2024-03-26 | 唐山金湾特碳石墨有限公司 | Preparation method of purified carbon rod and purified carbon rod prepared by preparation method |
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Application publication date: 20190906 |