CN112225576A - Preparation method of graphite electrode beneficial to reducing loss - Google Patents

Preparation method of graphite electrode beneficial to reducing loss Download PDF

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CN112225576A
CN112225576A CN202011126651.7A CN202011126651A CN112225576A CN 112225576 A CN112225576 A CN 112225576A CN 202011126651 A CN202011126651 A CN 202011126651A CN 112225576 A CN112225576 A CN 112225576A
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parts
graphite electrode
raw materials
treatment
graphene
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刘雁伟
张惠兵
辛丽芳
赤九林
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Datong Tongyang Carbon Co ltd
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Datong Tongyang Carbon Co ltd
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Abstract

The invention discloses a preparation method of a graphite electrode beneficial to reducing loss, which relates to the technical field of electrode preparation and comprises the following steps: s1, weighing the following raw materials in parts by weight: 30-32 parts of petroleum coke, 20-25 parts of needle coke, 10-12 parts of modified asphalt, 2-3 parts of graphene, 5-7 parts of polyoxyethylene fatty alcohol ether, 2-4 parts of polymethyl methacrylate, 1-3 parts of calcium oxide, 0.5-0.7 part of ferric oxide, 20-30 parts of carbon fiber and 5-8 parts of copper powder, according to the invention, the polymethyl methacrylate and the carbon fiber are added into the raw materials, so that the oxidation resistance of the graphite electrode is improved, the breakage rate of the graphite electrode in use is improved, the step of ion adsorption is added, zinc ions are attached to a dendritic structure formed between the graphene fiber in the graphite electrode and other raw materials, the conductivity of the graphite electrode is effectively improved, the graphite electrode has stable current conductivity, and the strength of the finished graphite electrode is effectively improved due to the addition of the polymethyl methacrylate and the ferric oxide.

Description

Preparation method of graphite electrode beneficial to reducing loss
Technical Field
The invention relates to the technical field of electrode preparation, in particular to a preparation method of a graphite electrode beneficial to reducing loss.
Background
The graphite electrode is made up by using petroleum coke and needle coke as raw material and modified asphalt as binding agent through the processes of calcining, proportioning, kneading, die pressing, roasting, graphitizing and machining, and is a conductor which can release electric energy in the form of electric arc in electric arc furnace to heat and melt furnace charge, and can be divided into ordinary power, high power and ultrahigh power according to its low mass index.
With the development of science and technology, the current high-capacity and ultrahigh-power arc furnace is rapidly developed, and the quality requirements on large-size and ultrahigh-power graphite electrodes are higher and higher, but the current graphite electrodes are unstable in structure and low in strength and are easily oxidized in a high-temperature environment, so that the graphite electrodes gradually become thinner from the oxidized parts, the abrasion resistance of the electrodes is reduced, the loss is high, the structure is unstable, the performance is reduced, the emission performance and the yield of the graphite electrodes are reduced to a certain degree after the graphite electrodes are subjected to anti-oxidation treatment, the production period and the energy consumption are improved, the existing graphite electrodes are low in hardness, easy to damage and low in compactness, and therefore, a preparation method of the graphite electrodes beneficial to reducing the loss is provided to solve the problems.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a graphite electrode which is beneficial to reducing loss, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a graphite electrode beneficial to reducing loss comprises the following steps:
s1, weighing the following raw materials in parts by weight: 30-32 parts of petroleum coke, 20-25 parts of needle coke, 10-12 parts of modified asphalt, 2-3 parts of graphene, 5-7 parts of polyoxyethylene fatty alcohol ether, 2-4 parts of polymethyl methacrylate, 1-3 parts of calcium oxide, 0.5-0.7 part of ferric oxide, 20-30 parts of carbon fiber and 5-8 parts of copper powder.
S2, first treatment of raw materials: respectively crushing the petroleum coke, the needle coke, the graphene and the carbon fiber in the step S1, and screening for later use;
s3, carrying out secondary treatment on the raw materials: grinding the calcium oxide, the ferric oxide and the copper powder in the step S1 in a ball mill, and screening the ground particles to obtain a required mixture I;
s4, mixing of raw materials: fully mixing the petroleum coke, needle coke, modified asphalt, graphene and carbon fiber which are crushed in the step S2 to prepare a required mixture II, and adding the mixture I and the mixture II prepared in the step S3 into a kneading pot for mixing for later use;
s5, wet mixing treatment: adding the modified asphalt in the step S1 into the kneading pot in the step S4, preheating the modified asphalt to 160-180 ℃, sequentially adding fatty alcohol-polyoxyethylene ether and polymethyl methacrylate into the kneading pot, and wet-mixing for 20-30min to obtain a required mixture;
s6, material molding: adding the mixture prepared in the step S5 into a mold, and carrying out extrusion molding treatment on the mold;
s7, roasting of the semi-finished product: roasting the semi-finished product extruded and shaped in the step S6, automatically heating according to a specific heating curve, namely a roasting curve, naturally cooling after heating is finished, and standing for 60-72 hours to obtain a graphite electrode roasted product;
s8, ion adsorption treatment: completely immersing the graphite electrode roasted product obtained in the step S7 into an ionic solution, standing for 48-72h, and drying after standing;
s9, graphitization treatment: placing the baked product dried in the step S8 into a graphitization furnace, and carrying out graphitization treatment on the baked product according to a power transmission curve to obtain a required graphite electrode;
s10, graphite packaging: and (4) packaging, packaging and warehousing the graphite electrode prepared in the step S9 by using a vacuum bag.
Further optimizing the technical scheme, the petroleum coke, needle coke, graphene and carbon fiber crushed in the step S2 are screened by a screen with the particle size of 30-50 nm.
Further optimizing the technical scheme, the diameter of the particle ground in the step S3 is 0.3-0.5 nm.
Further optimizing the technical scheme, the stirring of the kneading pot in the steps S4 and S5 is completed by driving the stirring shaft and the stirring blades to rotate by the stirring motor, and the rotating speed of the stirring shaft is 700 and 800 r/min.
Further optimizing the technical scheme, in the step S6, the extrusion force is 20-30KN, and the time for extrusion forming is 30-40 min.
Further optimizing the technical scheme, the roasting temperature in the step S7 is 1200-1300 ℃.
Further optimizing the technical scheme, the ionic solution in the step S8 is 5-10mol/L zinc chloride solution.
Further optimizing the technical scheme, in the step S9, the temperature of the graphitization furnace is heated to 3300-.
Further optimizing the technical solution, when the die in step S6 is extruded and shaped, the inner wall of the die needs to be brushed with lubricating oil.
Advantageous effects
Compared with the prior art, the invention provides the preparation method of the graphite electrode which is beneficial to reducing the loss, and the preparation method has the following beneficial effects:
1. according to the preparation method of the graphite electrode beneficial to reduction of loss, the polymethyl methacrylate and the carbon fiber are added into the raw materials, so that the oxidation resistance of the graphite electrode is improved, the breakage rate of the graphite electrode in use is improved, the step of ion adsorption is added, zinc ions are attached to a dendritic structure formed between the graphene fiber inside the graphite electrode and other raw materials, the conductivity of the graphite electrode is effectively improved, the graphite electrode has stable current conduction rate, the strength of the finished graphite electrode is effectively improved due to the addition of the polymethyl methacrylate and the ferric oxide, the graphite electrode has higher strength, and meanwhile, the graphite electrode has high melting point and high elasticity coefficient, good electric thermal conductivity, the anti-consumption performance of the graphite electrode is improved, and the service life and the performance of the graphite electrode are prolonged.
2. According to the preparation method of the graphite electrode beneficial to reducing the loss, after extrusion and shaping are finished, roasting is carried out, temperature rising is automatically carried out according to a specific temperature rising curve, namely a roasting curve, so that the conductivity of the graphite electrode is improved, the proportion of the graphite electrode is changed, the resistivity can be greatly reduced along with the increase of the needle coke amount, the conductivity of the graphite electrode is improved, the uniformity of a mixture can be improved by changing a material mixing process, the strength of the graphite electrode is improved, the conductivity efficiency of the graphite electrode is improved, the compactness of the graphite electrode can be greatly improved by ion adsorption, the hardness of the graphite electrode can be improved, the graphite electrode is difficult to damage, the raw materials are reasonably selected, the preparation process is scientific, and the like, and the graphite electrode with high physical and chemical properties is produced by using the method.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a graphite electrode beneficial to reducing loss according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows: referring to fig. 1, the present invention discloses a method for preparing a graphite electrode beneficial to reducing loss, comprising the following steps:
s1, weighing the following raw materials in parts by weight: 30 parts of petroleum coke, 20 parts of needle coke, 10 parts of modified asphalt, 2 parts of graphene, 5 parts of polyoxyethylene fatty alcohol ether, 2 parts of polymethyl methacrylate, 1 part of calcium oxide, 0.5 part of ferric oxide, 20 parts of carbon fiber and 5 parts of copper powder.
S2, first treatment of raw materials: respectively crushing the petroleum coke, the needle coke, the graphene and the carbon fiber in the step S1, and screening, wherein the crushed petroleum coke, the needle coke, the graphene and the carbon fiber are screened by a 30nm screen for later use;
s3, carrying out secondary treatment on the raw materials: grinding the calcium oxide, the ferric oxide and the copper powder in the step S1 in a ball mill, and screening the ground particles, wherein the diameter of the ground particles is 0.3nm to obtain a required mixture I;
s4, mixing of raw materials: fully mixing the petroleum coke, needle coke, modified asphalt, graphene and carbon fiber which are crushed in the step S2 to prepare a required mixture II, and adding the mixture I and the mixture II prepared in the step S3 into a kneading pot for mixing for later use;
s5, wet mixing treatment: adding the modified asphalt obtained in the step S1 into the kneading pot obtained in the step S4, preheating the modified asphalt to 160 ℃, sequentially adding fatty alcohol-polyoxyethylene ether and polymethyl methacrylate into the kneading pot, and wet-mixing for 20min, wherein the stirring of the kneading pot is completed by driving a stirring shaft and stirring blades to rotate by a stirring motor, and the rotating speed of the stirring shaft is 700r/min, so as to obtain a required mixture;
s6, material molding: adding the mixture prepared in the step S5 into a die, and carrying out extrusion molding treatment on the die, wherein the extrusion force is 20KN, the extrusion molding time is 30min, and lubricating oil needs to be brushed on the inner wall of the die when the die is in extrusion molding;
s7, roasting of the semi-finished product: roasting the semi-finished product extruded and shaped in the step S6 at 1200 ℃, automatically heating according to a specific heating curve, namely a roasting curve, naturally cooling after heating, and standing for 60 hours to obtain a graphite electrode roasted product;
s8, ion adsorption treatment: completely immersing the graphite electrode roasted product obtained in the step S7 into an ionic solution, standing for 48 hours, and drying after the ionic solution is 5mol/L zinc chloride solution;
s9, graphitization treatment: putting the baked product dried in the step S8 into a graphitization furnace, carrying out graphitization treatment on the baked product according to a power transmission curve, heating the graphitization furnace to 3300 ℃, and controlling the cooling maintenance time to be 300h to obtain a required graphite electrode;
s10, graphite packaging: and (4) packaging, packaging and warehousing the graphite electrode prepared in the step S9 by using a vacuum bag.
Example two: referring to fig. 1, the present invention discloses a method for preparing a graphite electrode beneficial to reducing loss, comprising the following steps:
s1, weighing the following raw materials in parts by weight: 31 parts of petroleum coke, 23 parts of needle coke, 11 parts of modified asphalt, 2.5 parts of graphene, 6 parts of polyoxyethylene fatty alcohol ether, 3 parts of polymethyl methacrylate, 2 parts of calcium oxide, 0.6 part of ferric oxide, 25 parts of carbon fiber and 7 parts of copper powder.
S2, first treatment of raw materials: respectively crushing the petroleum coke, the needle coke, the graphene and the carbon fiber in the step S1, and screening, wherein the crushed petroleum coke, the needle coke, the graphene and the carbon fiber are screened by a screen with the particle size of 40nm for later use;
s3, carrying out secondary treatment on the raw materials: grinding the calcium oxide, the ferric oxide and the copper powder in the step S1 in a ball mill, and screening the ground particles, wherein the diameter of the ground particles is 0.4nm to obtain a required mixture I;
s4, mixing of raw materials: fully mixing the petroleum coke, needle coke, modified asphalt, graphene and carbon fiber which are crushed in the step S2 to prepare a required mixture II, and adding the mixture I and the mixture II prepared in the step S3 into a kneading pot for mixing for later use;
s5, wet mixing treatment: adding the modified asphalt obtained in the step S1 into the kneading pot obtained in the step S4, preheating the modified asphalt to 170 ℃, sequentially adding fatty alcohol-polyoxyethylene ether and polymethyl methacrylate into the kneading pot, and wet-mixing for 25min, wherein the stirring of the kneading pot is completed by driving a stirring shaft and stirring blades to rotate by a stirring motor, and the rotating speed of the stirring shaft is 750r/min, so as to obtain a required mixture;
s6, material molding: adding the mixture prepared in the step S5 into a die, and carrying out extrusion molding treatment on the die, wherein the extrusion force is 25KN, the extrusion molding time is 35min, and lubricating oil needs to be brushed on the inner wall of the die when the die is in extrusion molding;
s7, roasting of the semi-finished product: roasting the semi-finished product extruded and shaped in the step S6, wherein the roasting temperature is 1250 ℃, automatically heating according to a specific heating curve, namely a roasting curve, naturally cooling after heating, and standing for 65 hours to obtain a graphite electrode roasted product;
s8, ion adsorption treatment: completely immersing the graphite electrode roasted product obtained in the step S7 into an ionic solution, standing for 60 hours, and drying after the ionic solution is 8mol/L zinc chloride solution;
s9, graphitization treatment: placing the baked product dried in the step S8 into a graphitization furnace, carrying out graphitization treatment on the baked product according to a power transmission curve, heating the graphitization furnace to 3400 ℃, and controlling the cooling maintenance time to be 310h to obtain a required graphite electrode;
s10, graphite packaging: and (4) packaging, packaging and warehousing the graphite electrode prepared in the step S9 by using a vacuum bag.
Example three: referring to fig. 1, the present invention discloses a method for preparing a graphite electrode beneficial to reducing loss, comprising the following steps:
s1, weighing the following raw materials in parts by weight: 32 parts of petroleum coke, 25 parts of needle coke, 12 parts of modified asphalt, 3 parts of graphene, 7 parts of polyoxyethylene fatty alcohol ether, 4 parts of polymethyl methacrylate, 3 parts of calcium oxide, 0.7 part of ferric oxide, 30 parts of carbon fiber and 8 parts of copper powder.
S2, first treatment of raw materials: respectively crushing the petroleum coke, the needle coke, the graphene and the carbon fiber in the step S1, and screening, wherein the crushed petroleum coke, the needle coke, the graphene and the carbon fiber are screened by a screen with the particle size of 50nm for later use;
s3, carrying out secondary treatment on the raw materials: grinding the calcium oxide, the ferric oxide and the copper powder in the step S1 in a ball mill, and screening the ground particles, wherein the diameter of the ground particles is 0.5nm to obtain a required mixture I;
s4, mixing of raw materials: fully mixing the petroleum coke, needle coke, modified asphalt, graphene and carbon fiber which are crushed in the step S2 to prepare a required mixture II, and adding the mixture I and the mixture II prepared in the step S3 into a kneading pot for mixing for later use;
s5, wet mixing treatment: adding the modified asphalt obtained in the step S1 into the kneading pot obtained in the step S4, preheating the modified asphalt to 180 ℃, sequentially adding fatty alcohol-polyoxyethylene ether and polymethyl methacrylate into the kneading pot, and wet-mixing for 30min, wherein the stirring of the kneading pot is completed by driving a stirring shaft and stirring blades to rotate by a stirring motor, and the rotating speed of the stirring shaft is 800r/min, so as to obtain a required mixture;
s6, material molding: adding the mixture prepared in the step S5 into a die, and carrying out extrusion molding treatment on the die, wherein the extrusion force is 30KN, the extrusion molding time is 40min, and lubricating oil needs to be brushed on the inner wall of the die when the die is in extrusion molding;
s7, roasting of the semi-finished product: roasting the semi-finished product extruded and shaped in the step S6, wherein the roasting temperature is 1300 ℃, automatically heating according to a specific heating curve, namely a roasting curve, naturally cooling after heating, and standing for 72 hours to obtain a graphite electrode roasted product;
s8, ion adsorption treatment: completely immersing the graphite electrode roasted product obtained in the step S7 into an ionic solution, standing for 72 hours, and drying after the ionic solution is 10mol/L zinc chloride solution;
s9, graphitization treatment: placing the baked product dried in the step S8 into a graphitization furnace, carrying out graphitization treatment on the baked product according to a power transmission curve, heating the graphitization furnace to 3500 ℃, and controlling the cooling maintenance time to be 320h to obtain a required graphite electrode;
s10, graphite packaging: and (4) packaging, packaging and warehousing the graphite electrode prepared in the step S9 by using a vacuum bag.
The invention has the beneficial effects that: according to the invention, the polymethyl methacrylate and the carbon fiber are added into the raw materials, so that the oxidation resistance of the graphite electrode is improved, and the breakage rate of the graphite electrode in use is improved; after the extrusion and shaping are finished, roasting is carried out, the temperature rise is automatically carried out according to a specific temperature rise curve, namely a roasting curve, the conductivity of the graphite electrode is improved, the proportion of the graphite electrode is changed, the resistivity can be greatly reduced along with the increase of the amount of needle coke, the conductivity of the graphite electrode is improved, the uniformity of a mixture can be improved by changing a material mixing process, the strength of the graphite electrode is improved, the conductivity efficiency of the graphite electrode is improved, the compactness of the graphite electrode can be greatly improved through ion adsorption, the hardness of the graphite electrode can be improved, the graphite electrode is not easy to damage, the raw materials are reasonably selected, the preparation process is scientific and the like, and the graphite electrode with high physical and chemical properties is produced by using the method and the.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A preparation method of a graphite electrode beneficial to reducing loss is characterized by comprising the following steps:
s1, weighing the following raw materials in parts by weight: 30-32 parts of petroleum coke, 20-25 parts of needle coke, 10-12 parts of modified asphalt, 2-3 parts of graphene, 5-7 parts of polyoxyethylene fatty alcohol ether, 2-4 parts of polymethyl methacrylate, 1-3 parts of calcium oxide, 0.5-0.7 part of ferric oxide, 20-30 parts of carbon fiber and 5-8 parts of copper powder;
s2, first treatment of raw materials: respectively crushing the petroleum coke, the needle coke, the graphene and the carbon fiber in the step S1, and screening for later use;
s3, carrying out secondary treatment on the raw materials: grinding the calcium oxide, the ferric oxide and the copper powder in the step S1 in a ball mill, and screening the ground particles to obtain a required mixture I;
s4, mixing of raw materials: fully mixing the petroleum coke, needle coke, modified asphalt, graphene and carbon fiber which are crushed in the step S2 to prepare a required mixture II, and adding the mixture I and the mixture II prepared in the step S3 into a kneading pot for mixing for later use;
s5, wet mixing treatment: adding the modified asphalt in the step S1 into the kneading pot in the step S4, preheating the modified asphalt to 160-180 ℃, sequentially adding fatty alcohol-polyoxyethylene ether and polymethyl methacrylate into the kneading pot, and wet-mixing for 20-30min to obtain a required mixture;
s6, material molding: adding the mixture prepared in the step S5 into a mold, and carrying out extrusion molding treatment on the mold;
s7, roasting of the semi-finished product: roasting the semi-finished product extruded and shaped in the step S6, automatically heating according to a specific heating curve, namely a roasting curve, naturally cooling after heating is finished, and standing for 60-72 hours to obtain a graphite electrode roasted product;
s8, ion adsorption treatment: completely immersing the graphite electrode roasted product obtained in the step S7 into an ionic solution, standing for 48-72h, and drying after standing;
s9, graphitization treatment: placing the baked product dried in the step S8 into a graphitization furnace, and carrying out graphitization treatment on the baked product according to a power transmission curve to obtain a required graphite electrode;
s10, graphite packaging: and (4) packaging, packaging and warehousing the graphite electrode prepared in the step S9 by using a vacuum bag.
2. The method as claimed in claim 1, wherein the petroleum coke, needle coke, graphene and carbon fiber in step S2 are sieved through a 30-50nm sieve.
3. The method as claimed in claim 1, wherein the particle diameter of the graphite electrode ground in step S3 is 0.3-0.5 nm.
4. The method as claimed in claim 1, wherein the stirring of the kneading pot in steps S4 and S5 is accomplished by a stirring motor driving a stirring shaft and stirring blades to rotate, and the rotation speed of the stirring shaft is 800 r/min.
5. The method for preparing a graphite electrode beneficial to reducing loss according to claim 1, wherein the method comprises the following steps: in the step S6, the extrusion force is 20-30KN, and the time for extrusion shaping is 30-40 min.
6. The method as claimed in claim 1, wherein the temperature of the step S7 is 1200-1300 ℃.
7. A method as claimed in claim 1, wherein the ionic solution in step S8 is 5-10mol/L zinc chloride solution.
8. The method as claimed in claim 1, wherein the step S9 is performed by heating the graphite furnace to 3300-.
9. The method as claimed in claim 1, wherein in step S6, when the mold is shaped by extrusion, a lubricant is applied to the inner wall of the mold.
CN202011126651.7A 2020-10-20 2020-10-20 Preparation method of graphite electrode beneficial to reducing loss Pending CN112225576A (en)

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