CN109400163B - Carbon anode and preparation method and application thereof - Google Patents
Carbon anode and preparation method and application thereof Download PDFInfo
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- CN109400163B CN109400163B CN201811644707.0A CN201811644707A CN109400163B CN 109400163 B CN109400163 B CN 109400163B CN 201811644707 A CN201811644707 A CN 201811644707A CN 109400163 B CN109400163 B CN 109400163B
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Abstract
The invention provides a carbon anode and a preparation method and application thereof, belonging to the technical field of carbon industry; the carbon anode comprises 85-95 parts of aggregate and 5-15 parts of binder. Mixing the raw materials according to a mass ratio, molding and carrying out heat treatment to obtain the carbon anode. The adhesive mainly takes liquid phenolic resin as a main body, compared with asphalt as an adhesive, the adhesive can be mixed at normal temperature, the molding process adopts compression molding, the process is simple, and the operating conditions are mild; after the phenolic resin is heated and cured, the phenolic resin has the characteristic of excellent dimensional stability, can realize rapid temperature rise in the roasting stage, shortens the roasting time and improves the production efficiency.
Description
Technical Field
The invention relates to the technical field of carbon industry, in particular to a carbon anode and a preparation method and application thereof.
Background
The prebaked anode is an anode material used in the electrolytic aluminum industry, is used for electrolyzing aluminum oxide to produce metal aluminum, and is an important raw material in the electrolytic aluminum oxide industry. At present, the main raw material of the anode is petroleum coke, which is combined by coal tar pitch and is prepared by stages of molding roasting and the like. And coal tar pitch is used as a binder, harmful substances such as sulfur dioxide and the like are released at high temperature, the environment is polluted, and the product yield is reduced.
In addition, in the process of preparing the anode by adopting the coal tar pitch, the temperature is about 145 ℃ during forming, the anode is required to be put into water after forming, the water cooling is carried out to improve the strength, and the anode is roasted for 20-30 days to obtain the finished anode product, so that the process is complex, the yield is low, and the pollution is serious.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a carbon anode, which adopts phenolic resin as a bonding agent, is bonded with a carbon material and can be formed at normal temperature, and the prepared anode carbon block has the advantages of high strength and good conductivity.
The second purpose of the invention is to provide a preparation method of the carbon anode, which adopts phenolic resin as a bonding agent, bonds carbon materials, can be formed at normal temperature, can be directly fed into a kiln for treatment after being formed, does not need high-temperature forming at about 145 ℃ and cooling in water, and has simple process, mild operation condition and environmental protection.
The third purpose of the invention is to provide an application of the carbon anode, the carbon anode has good electrochemical performance, the electrochemical reaction activity of the anode is improved, the consumption of electric energy in the electrolytic process is reduced, and the economic benefit is improved.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the carbon anode is mainly prepared by mixing aggregate and a binder, wherein the binder comprises 85-100 parts by mass of phenolic resin and 0-15 parts by mass of coal tar pitch.
In the prior art, when the anode is prepared, coal tar pitch can emit harmful substances such as sulfur dioxide and the like at high temperature, thereby polluting the environment; in addition, in the process of releasing gas from coal tar pitch, the prepared anode material has increased pores, reduced volume density, poor compactness, increased contact area of the anode to air and carbon dioxide, increased reaction activity, increased carbon loss, reduced service life of the anode and increased carbon-containing slag content in the electrolytic cell. In addition, the coal tar pitch has limited binding effect, and the prepared anode has high impurity content and affects the quality of electrolytic aluminum due to large dosage for binding aggregate.
The invention adopts phenolic resin to replace coal pitch in a large quantity or completely, improves the structural compactness of the carbon anode, improves the strength, ensures the conductivity of the carbon anode, ensures the carbon anode to have good electrochemical performance, improves the electrochemical reaction activity of the anode, reduces the consumption of electric energy in the electrolytic process, and improves the economic benefit. The phenolic resin is used as a binder, and the forming process does not need high temperature and normal temperature, so that the process is reduced, and the production cost is reduced.
In addition, because a large amount of coal tar pitch is replaced or all the coal tar pitch is replaced, the whole production process and the electrolysis process are more environment-friendly, and the method has great application prospect.
As in the various embodiments, the binder may include, by mass parts, 85 parts of phenolic resin, 15 parts of coal pitch, 90 parts of phenolic resin, 10 parts of coal pitch, 94 parts of phenolic resin, 6 parts of coal pitch, 98 parts of phenolic resin, 2 parts of coal pitch, 99 parts of phenolic resin, 1 part of coal pitch, 100 parts of phenolic resin, and so forth.
The binder used by the aluminum anode comprises 85-100 parts of phenolic resin and 0-15 parts of coal pitch by mass percent, wherein the phenolic resin can be quickly carbonized at the temperature of 900-1000 ℃ to form carbide, the carbide has good conductivity, and the resistivity of powder of the carbide is 30-120m omega cm.
Preferably, the phenolic resin comprises one or more of biomass modified phenolic resin, asphalt modified phenolic resin, coal tar modified phenolic resin, alkylphenol modified phenolic resin and rubber modified phenolic resin.
In the present invention, a biomass-modified phenol resin is preferably used.
Preferably, the modified phenolic resin contains one or more of sodium salt, potassium salt, molybdate, ferric salt, chromium salt, boron salt, cobalt salt, nickel salt and manganese salt.
Preferably, the modified phenolic resin contains iron salt and nickel salt.
Preferably, any one or more of sodium salt, potassium salt, molybdate, iron salt, chromium salt, boron salt, cobalt salt, nickel salt and manganese salt is/are mixed with the modified phenolic resin to obtain the modified phenolic resin containing any one or more of sodium salt, potassium salt, molybdate, iron salt, chromium salt, boron salt, cobalt salt, nickel salt and manganese salt.
Preferably, the modified phenolic resin is liquid resin, and the viscosity of the resin is 8000-16000 mpa.s.
The phenolic resin is used as a binder, so that sufficient binding performance can be provided, and the anode strength is improved; and the phenolic resin has good conductivity after being carbonized at low temperature, and can further improve the conductivity of the carbon anode. Namely, under the condition of less adding amount, enough adhesive property can be provided, the strength can meet the requirement, and further, the quality loss of the anode in the roasting process can be reduced.
Preferably, the carbon anode is mainly prepared by mixing 85-95 parts by weight of aggregate and 5-15 parts by weight of binder. More preferably, the carbon anode is mainly prepared by mixing 88-94 parts of aggregate and 6-12 parts of binder by weight.
In the carbon anode, the proportion of the aggregate to the binder is important, and the selection of the binder needs to ensure the conductivity of the carbon anode while considering the binding performance. By adjusting the use amounts of the aggregate and the binder within the above range, the binding property can be improved, the anode strength can be improved, and the electrical conductivity of the carbon anode can be ensured.
The inventor of the invention discovers through a great deal of practice that the phenolic resin is used as the binder for preparing the carbon anode, and within the dosage range, the phenolic resin can effectively improve the binding property of the carbon anode, improve the strength of the anode, simultaneously give consideration to the conductivity, avoid excessive addition, and avoid the situations of excessive loss in the roasting process and increased production cost or insufficient strength due to excessive addition in the roasting process although the strength is improved.
As in the various embodiments, the aggregate may be used in amounts of 85 parts, 86 parts, 87 parts, 88 parts, 89 parts, 90 parts, 91 parts, 92 parts, 93 parts, 94 parts, 95 parts, and the like; the binder may be used in amounts of 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, and the like.
Preferably, the aggregate comprises one or more of petroleum coke, calcined coke, needle coke, anthracite, low-rank bituminous coal, pitch coke, carbon nanotubes and crushed graphite. More preferably, the aggregate is petroleum coke, carbon nanotubes and graphite fragments.
Preferably, the aggregate comprises 80-150 parts of petroleum coke, 0-20 parts of carbon nano tubes and 5-30 parts of crushed graphite according to parts by weight.
Preferably, the petroleum coke comprises the petroleum coke with the particle size of 0-2mm, 2-4mm, 4-8mm and fine powder petroleum coke according to the particle size. More preferably, the petroleum coke comprises 30-40 parts of 0-2mm petroleum coke, 20-40 parts of 2-4mm petroleum coke, 10-30 parts of 4-8mm petroleum coke and 20-40 parts of 180-mesh fine powder petroleum coke.
The invention also provides a preparation method of the carbon anode, which comprises the following steps:
mixing the raw materials according to a mass ratio, molding and carrying out heat treatment to obtain the carbon anode.
Preferably, the mixing and the forming are all completed at 25-70 ℃. More preferably, the mixture is mixed and molded at 40 to 60 ℃. The method can be molded at a lower temperature without molding at a high temperature of 140 ℃ and 160 ℃.
Preferably, the heat treatment comprises baking and firing.
Preferably, the baking method comprises: the temperature of the formed material is raised from room temperature to 150-200 ℃.
In the invention, the heating rate in the baking process is further optimized to improve the heat treatment effect, and the heating rate in the baking process is 2-8 ℃/h, and the more preferable heating rate is 3-5 ℃/h.
Preferably, the method of firing comprises: under the condition of carbon burying, the temperature is raised from 150-200 ℃ to 1000-1100 ℃.
Preferably, in the roasting process, at the stage of 150-400 ℃, the heating rate is 4-10 ℃/h; the temperature rise rate is 2-5 ℃/h in the 400-plus-800 ℃ stage, and the temperature rise rate is 4-10 ℃/h in the 800-plus-1100 ℃ stage.
The invention adopts the liquid phenolic resin as the binder, does not need to heat the materials in the kneading and molding processes, has very high strength and dimensional stability after the green carbon blocks are baked and cured, can quickly heat up at the temperature stage of 200-400 ℃, reduces the process time and reduces the production cost.
The invention also provides an application of the carbon anode in the electrolytic aluminum oxide. The carbon anode has good electrochemical performance, improves the electrochemical reaction activity of the anode, reduces the consumption of electric energy in the electrolytic process and improves the economic benefit.
Compared with the prior art, the invention has the beneficial effects that:
(1) the carbon anode disclosed by the invention adopts phenolic resin to replace coal pitch in a large quantity or completely, so that the structural compactness of the carbon anode is improved, the strength is improved, the electric conductivity of the carbon anode is ensured, the carbon anode has good electrochemical performance, the electrochemical reaction activity of the anode is improved, the consumption of electric energy in the electrolytic process is reduced, and the economic benefit is improved;
(2) according to the invention, phenolic resin is used as a binder, and heating treatment is not required to be carried out on materials in the kneading and forming processes, so that the process steps are reduced; after the green carbon blocks are baked and cured, the green carbon blocks have very high strength and dimensional stability, and can be quickly heated in the temperature stage of 200-400 ℃, so that the process time is shortened, the production cost is reduced, the whole production process and the electrolysis process are more environment-friendly, and the green carbon blocks have great application prospects;
(3) the carbon anode has excellent strength and conductivity, can be used for electrolyzing aluminum oxide, and improves economic benefits.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following detailed description, but those skilled in the art will understand that the following described examples are some, not all, of the examples of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. 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 examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Some material information used in the embodiments of the present invention are as follows:
petroleum coke: henan Jiangyi silver metallurgy materials, Inc.;
coal tar pitch powder: henan Jiangyi silver metallurgy materials, Inc.;
crushing graphite: zibo eight carbon plant;
the catalyst for preparing the phenolic resin is a maotan chemical reagent factory in Tianjin.
Example 1
The embodiment provides a preparation method of a carbon anode, which comprises the following steps:
(a) preparing aggregate: weighing 15 parts of petroleum coke with the diameter of 0-1mm, 20 parts of petroleum coke with the diameter of 1-2mm, 30 parts of petroleum coke with the diameter of 2-4mm, 20 parts of petroleum coke with the diameter of 4-8mm, 30 parts of petroleum coke with fine powder of 180 meshes, 7 parts of crushed graphite and 3 parts of carbon nano tubes, and putting the mixture into a mixer for uniformly mixing.
(b) Preparing asphalt modified phenolic resin: putting 200 parts of phenol, 329 parts of 37% formaldehyde and 4 parts of catalyst into a reaction bottle, heating to 73-75 ℃, uniformly mixing 10 parts of asphalt powder and 10 parts of 50% sodium hydroxide solution, and putting into the reaction bottle; and (3) keeping the temperature for 2 hours, performing reduced pressure dehydration until the viscosity is 12000cp/25 ℃, and adding 2 parts of ferric chloride and 4 parts of boric acid to obtain the required resin, wherein the resistivity of the resin carbide powder is 80m omega cm.
(c) And (b) mixing 92 parts of aggregate obtained in the step (a), 7 parts of modified phenolic resin obtained in the step (b) and 1 part of coal asphalt powder, and kneading for 60min at room temperature by using a kneader.
(d) Placing the kneaded material in the step (c) into a specific mould, and pressing and molding the material under the pressure of 630 tons by using a hydraulic machine;
(e) placing the pressed and formed carbon block in a high-temperature roasting furnace for heat treatment, heating the temperature from room temperature to 200 ℃ at the heating rate of 3 ℃/h, then carrying out carbon burying treatment on the carbon block, and heating the temperature from 200 ℃ to 400 ℃ at the heating rate of 8 ℃/h; heating from 400 to 800 ℃ at the heating rate of 4 ℃/h, heating from 800 to 1100 ℃ at the heating rate of 6 ℃/h, and roasting at 1100 ℃ for 72 h; and after the roasting is finished, slowly cooling to the temperature of 300-400 ℃, and taking out of the kiln to obtain the carbon anode.
Example 2
The embodiment provides a preparation method of a carbon anode, which comprises the following steps:
(a) preparing aggregate: weighing 20 parts of petroleum coke with the particle size of 0-1mm, 20 parts of petroleum coke with the particle size of 1-2mm, 20 parts of petroleum coke with the particle size of 2-4mm, 15 parts of petroleum coke with the particle size of 4-8mm, 30 parts of petroleum coke with fine powder with the particle size of 180 meshes, 5 parts of crushed graphite and 5 parts of carbon nano tubes, and putting the mixture into a mixer for uniformly mixing.
(b) Preparing lignin modified phenolic resin: putting 300 parts of phenol, 429 parts of formaldehyde with the concentration of 37 percent and 6 parts of catalyst into a reaction bottle, heating to 73-75 ℃, keeping the temperature for 2 hours, adding lignin, decompressing and dehydrating to 8000cp/25 ℃, and adding 5 parts of iron oxide powder and 4 parts of boric acid to obtain the required resin, wherein the resistivity of the resin carbide powder is 44m omega cm.
(c) And (b) mixing 90 parts of aggregate obtained in the step (a), 10 parts of modified phenolic resin obtained in the step (b) and 1.5 parts of asphalt powder, and kneading for 60min at room temperature by using a kneader.
(d) Placing the kneaded material in the step (c) into a specific mould, and pressing and molding the material under the pressure of 630 tons by using a hydraulic machine;
(e) placing the pressed and formed carbon block in a high-temperature roasting furnace for roasting, raising the temperature from room temperature to 200 ℃ at the temperature rise rate of 4 ℃/h, then carrying out carbon burying treatment on the carbon block, and raising the temperature from 200 ℃ to 400 ℃ at the temperature rise rate of 8 ℃/h; heating from 400 to 800 ℃ at a heating rate of 4 ℃/h, heating from 800 to 1100 ℃ at a heating rate of 6 ℃/h, and roasting at 1100 ℃ for 72 h; and after the roasting is finished, slowly cooling to the temperature of 300-400 ℃, and taking out of the kiln to obtain the carbon anode.
Example 3
The embodiment provides a preparation method of a carbon anode, which comprises the following steps:
(a) preparing aggregate: weighing 20 parts of petroleum coke with the particle size of 0-1mm, 15 parts of petroleum coke with the particle size of 1-2mm, 15 parts of petroleum coke with the particle size of 2-4mm, 15 parts of petroleum coke with the particle size of 4-8mm, 25 parts of petroleum coke with fine powder of 180 meshes, 15 parts of anthracite and 5 parts of crushed graphite, and putting the materials into a mixer to be uniformly mixed.
(b) Preparing tar modified phenolic resin: putting 200 parts of phenol, 20 parts of tar and 4 parts of catalyst into a reaction bottle, heating to 83-85 ℃, and dropwise adding 300 parts of 37% formaldehyde into the reaction bottle; after keeping the temperature for 2 hours, adding 6 parts of chromic potassium oxalate trihydrate and 4 parts of boric acid, and dehydrating under reduced pressure until the viscosity is 14000cp/25 ℃, thus obtaining the required resin, wherein the resistivity of the resin carbide powder is 62m omega cm.
(c) And (b) mixing 90 parts of aggregate obtained in the step (a), 10 parts of modified phenolic resin obtained in the step (b) and 1.5 parts of asphalt powder, and kneading for 60min at room temperature by using a kneader.
(d) Putting the kneaded material in the step (b) into a vibration compaction forming machine, and pressing and forming while vibrating;
(e) placing the molded carbon block in a high-temperature roasting furnace for roasting, heating the temperature from room temperature to 150 ℃ at the heating rate of 3 ℃/h, then carrying out carbon burying treatment on the carbon block, and heating the temperature from 200 ℃ to 400 ℃ at the heating rate of 8 ℃/h; heating from 400 to 800 ℃ at a heating rate of 4 ℃/h, heating from 800 to 1100 ℃ at a heating rate of 6 ℃/h, and roasting at 1100 ℃ for 72 h; and after the roasting is finished, slowly cooling to the temperature of 300-400 ℃, and taking out of the kiln to obtain the carbon anode.
Example 4
The embodiment provides a preparation method of a carbon anode, which comprises the following steps:
(a) preparing aggregate: weighing 20 parts of petroleum coke with the particle size of 0-1mm, 15 parts of petroleum coke with the particle size of 1-2mm, 15 parts of petroleum coke with the particle size of 2-4mm, 15 parts of petroleum coke with the particle size of 4-8mm, 20 parts of petroleum coke with fine powder of 180 meshes, 15 parts of anthracite and 5 parts of crushed graphite, and putting the materials into a mixer to be uniformly mixed.
(b) Preparation of cardanol modified phenolic resin: putting 150 parts of phenol, 80 parts of cardanol, 300 parts of 37% formaldehyde and 1.5 parts of catalyst into a reaction bottle, and heating to 83-85 ℃; after keeping the temperature for 2 hours, adding 6 parts of chromic potassium oxalate trihydrate and 4 parts of boric acid, and dehydrating under reduced pressure until the viscosity is 14500cp/25 ℃, thus obtaining the required resin, wherein the resistivity of the resin carbide powder is 120m omega cm.
(c) And (b) mixing 88 parts of aggregate obtained in the step (a), 10.5 parts of modified phenolic resin obtained in the step (b) and 1.5 parts of asphalt powder, and kneading for 60min at room temperature by using a kneader.
(d) Putting the kneaded material in the step (b) into a vibration compaction forming machine, and pressing and forming while vibrating;
(e) placing the molded carbon block in a high-temperature roasting furnace for roasting, raising the temperature from room temperature to 200 ℃ at the temperature rise rate of 4 ℃/h, then carrying out carbon burying treatment on the carbon block, and raising the temperature from 200 ℃ to 400 ℃ at the temperature rise rate of 8 ℃/h; heating from 400 to 800 ℃ at a heating rate of 4 ℃/h, heating from 800 to 1100 ℃ at a heating rate of 6 ℃/h, and roasting at 1100 ℃ for 72 h; and after the roasting is finished, slowly cooling to the temperature of 300-400 ℃, and taking out of the kiln to obtain the carbon anode.
Example 5
The embodiment provides a preparation method of a carbon anode, which comprises the following steps:
(a) preparing aggregate: weighing 20 parts of petroleum coke with the particle size of 0-1mm, 15 parts of petroleum coke with the particle size of 1-2mm, 15 parts of petroleum coke with the particle size of 2-4mm, 15 parts of petroleum coke with the particle size of 4-8mm, 20 parts of petroleum coke with fine powder of 180 meshes, 15 parts of anthracite and 5 parts of crushed graphite, and putting the materials into a mixer to be uniformly mixed.
(b) Preparing butyronitrile-chlorinated polyether modified phenolic resin: putting 250 parts of phenol, 300 parts of 37% formaldehyde and 7.5 parts of catalyst into a reaction bottle, heating to 83-85 ℃, and adding 2.5 parts of ammonium molybdate; keeping the temperature for 2h, adding 10 parts of nitrile rubber and 10 parts of dibutyl ester, completely dissolving, adding 20 parts of epichlorohydrin rubber and 15 parts of xylene, and dehydrating under reduced pressure until the viscosity is 14000cp/25 ℃ to obtain the required resin, wherein the resistivity of the resin carbide powder is 85m omega cm.
(c) And (b) mixing 90 parts of aggregate obtained in the step (a), 10 parts of modified phenolic resin obtained in the step (b) and 1.5 parts of asphalt powder, and kneading for 60min at room temperature by using a kneader.
(d) Putting the kneaded material in the step (b) into a vibration compaction forming machine, and pressing and forming while vibrating;
(e) placing the molded carbon block in a high-temperature roasting furnace for roasting, heating the temperature from room temperature to 150 ℃ at the heating rate of 3 ℃/h, then carrying out carbon burying treatment on the carbon block, and heating the temperature from 150 ℃ to 400 ℃ at the heating rate of 8 ℃/h; heating from 400 to 800 ℃ at a heating rate of 4 ℃/h, heating from 800 to 1100 ℃ at a heating rate of 6 ℃/h, and roasting at 1100 ℃ for 72 h; and after the roasting is finished, slowly cooling to the temperature of 300-400 ℃, and taking out of the kiln to obtain the carbon anode.
Example 6
The embodiment provides a preparation method of a carbon anode, which comprises the following steps:
(a) preparing aggregate: weighing 20 parts of petroleum coke with the particle size of 0-1mm, 28 parts of petroleum coke with the particle size of 1-2mm, 20 parts of petroleum coke with the particle size of 2-4mm, 15 parts of petroleum coke with the particle size of 4-8mm, 30 parts of petroleum coke with fine powder with the particle size of 180 meshes, 5 parts of crushed graphite and 5 parts of carbon nano tubes, and putting the mixture into a mixer for uniformly mixing.
(b) Preparing lignin modified phenolic resin: putting 300 parts of phenol, 429 parts of formaldehyde with the concentration of 37 percent and 6 parts of catalyst into a reaction bottle, heating to 73-75 ℃, keeping the temperature for 2 hours, adding lignin, decompressing and dehydrating to the viscosity of 11000cp/25 ℃, and adding 2 parts of ferric chloride and 6 parts of nickel chloride to obtain the required resin, wherein the resistivity of the resin carbide powder is 30m omega cm.
(c) And (b) mixing 90 parts of aggregate obtained in the step (a), 10 parts of modified phenolic resin obtained in the step (b) and 1.5 parts of asphalt powder, and kneading for 60min at room temperature by using a kneader.
(d) Placing the kneaded material in the step (c) into a specific mould, and pressing and molding the material under the pressure of 630 tons by using a hydraulic machine;
(e) placing the pressed and formed carbon block in a high-temperature roasting furnace for roasting, heating the temperature from room temperature to 160 ℃ at the heating rate of 4 ℃/h, then carrying out carbon burying treatment on the carbon block, and heating the temperature from 160 ℃ to 400 ℃ at the heating rate of 8 ℃/h; heating from 400 to 800 ℃ at a heating rate of 4 ℃/h, heating from 800 to 1100 ℃ at a heating rate of 6 ℃/h, and roasting at 1100 ℃ for 72 h; and after the roasting is finished, slowly cooling to the temperature of 300-400 ℃, and taking out of the kiln to obtain the carbon anode.
Example 7
The embodiment provides a preparation method of a carbon anode, which comprises the following steps:
(a) preparing aggregate: weighing 28 parts of petroleum coke with the diameter of 0-2mm, 20 parts of petroleum coke with the diameter of 2-4mm, 15 parts of petroleum coke with the diameter of 4-8mm, 25 parts of petroleum coke with fine powder with the diameter of 180 meshes, 5 parts of crushed graphite and 2 parts of carbon nano tubes, and putting the materials into a mixer to be uniformly mixed.
(b) Preparing lignin modified phenolic resin: putting 325 parts of phenol, 429 parts of 37% formaldehyde and 6 parts of catalyst into a reaction bottle, heating to 73-75 ℃, keeping the temperature constant for 2 hours, adding lignin, decompressing and dehydrating until the viscosity is 10000cp/25 ℃, and adding 3 parts of cobalt acetate and 9 parts of manganese oxalate to obtain the required resin, wherein the resistivity of the resin carbide powder is 57m omega cm.
(c) And (b) mixing 90 parts of aggregate obtained in the step (a), 10 parts of modified phenolic resin obtained in the step (b) and 0.8 part of asphalt powder, and kneading for 60min at room temperature by using a kneader.
(d) Placing the kneaded material in the step (c) into a specific mould, and pressing and molding the material under the pressure of 630 tons by using a hydraulic machine;
(e) placing the pressed and formed carbon block in a high-temperature roasting furnace for roasting, heating the temperature from room temperature to 150 ℃ at the heating rate of 3 ℃/h, then carrying out carbon burying treatment on the carbon block, and heating the temperature from 150 ℃ to 400 ℃ at the heating rate of 6 ℃/h; heating from 400 to 800 ℃ at a heating rate of 4 ℃/h, heating from 800 to 1100 ℃ at a heating rate of 6 ℃/h, and roasting at 1100 ℃ for 72 h; and after the roasting is finished, slowly cooling to the temperature of 300-400 ℃, and taking out of the kiln to obtain the carbon anode.
Example 8
This example refers to the preparation of example 2, with the only difference that: in step (a): preparing aggregate: weighing 50 parts of petroleum coke with the particle size of 2-4mm, 35 parts of petroleum coke with the particle size of 4-8mm, 30 parts of petroleum coke with fine powder of 180 meshes, 7 parts of crushed graphite and 5 parts of carbon nano tubes, and uniformly mixing in a mixer.
Example 9
This example refers to the preparation of example 2, with the only difference that: in step (a): preparing aggregate: weighing 15 parts of petroleum coke with the particle size of 0-1mm, 20 parts of petroleum coke with the particle size of 1-2mm, 30 parts of petroleum coke with the particle size of 2-4mm, 20 parts of petroleum coke with the particle size of 4-8mm and 30 parts of petroleum coke with fine powder with the particle size of 180 meshes, and uniformly mixing in a mixer.
Example 10
This example refers to the preparation of example 2, with the only difference that: in step (a): preparing aggregate: weighing 15 parts of petroleum coke with the diameter of 0-1mm, 20 parts of petroleum coke with the diameter of 1-2mm, 30 parts of petroleum coke with the diameter of 2-4mm, 20 parts of petroleum coke with the diameter of 4-8mm, 30 parts of petroleum coke with fine powder of 180 meshes, 30 parts of crushed graphite and 20 parts of carbon nano tubes, and putting the mixture into a mixer for uniformly mixing.
Example 11
This example refers to the preparation of example 2, with the only difference that: in the step (c), 92 parts of aggregate obtained in the step (a), 7 parts of modified phenolic resin obtained in the step (b) and 1 part of coal tar pitch powder are mixed, and kneaded for 60min at the temperature of 50 ℃ by using a kneader.
Example 12
This example refers to the preparation of example 2, with the only difference that: in the step (c), 94 parts of the aggregate obtained in the step (a), 5.5 parts of the modified phenolic resin obtained in the step (b) and 0.5 part of coal tar pitch powder are mixed, and kneaded for 60min at room temperature by using a kneader.
Example 13
This example refers to the preparation of example 2, with the only difference that: in the step (c), 92 parts of the aggregate obtained in the step (a) and 8 parts of the modified phenolic resin obtained in the step (b) are mixed, and kneaded for 60min at room temperature by using a kneader.
Example 14
This example refers to the preparation of example 2, with the only difference that: in the step (c), 92 parts of aggregate obtained in the step (a), 4 parts of modified phenolic resin obtained in the step (b) and 4 parts of coal tar pitch powder are mixed, and kneaded for 60min at room temperature by using a kneader.
Comparative example 1
The preparation method of the carbon anode in the comparative example 1 comprises the following steps:
(a) preparing raw materials: weighing 15 parts of petroleum coke with the particle size of 0-1mm, 20 parts of petroleum coke with the particle size of 1-2mm, 30 parts of petroleum coke with the particle size of 2-4mm, 20 parts of petroleum coke with the particle size of 4-8mm and 30 parts of petroleum coke with fine powder with the particle size of 180 meshes, and putting the mixture into a mixer to be uniformly mixed;
(b) heating the petroleum coke obtained in the step (a) to 160 ℃, and mixing for 30 min; heating 16 parts of coal tar pitch powder to 145 ℃, adding the coal tar pitch powder into preheated petroleum coke after the coal tar pitch powder is completely dissolved, and kneading the mixture for 40min at the temperature of 140 ℃ and 160 ℃;
(c) putting the kneaded material in the step (b) into a vibration compaction forming machine, preheating the vibration forming machine to 140 ℃ in advance, and pressing and forming while vibrating;
(d) putting the pressed and molded carbon block into water for cooling;
(e) placing the cooled carbon block in a high-temperature roasting furnace for roasting, heating the temperature from room temperature to 800 ℃ at the heating rate of 3 ℃/h, then carrying out carbon burying treatment on the carbon block, heating the carbon block from 800 ℃ to 1100 ℃ at the heating rate of 6 ℃/h, and roasting the carbon block for 72h at 1100 ℃; and after the roasting is finished, slowly cooling to the temperature of 300-400 ℃, and taking out of the kiln to obtain the carbon anode.
Comparative example 2
Comparative example 2 the preparation process of example 2 was referenced, with the following differences: in the step (c), 80 parts of aggregate obtained in the step (a), 14.5 parts of modified phenolic resin obtained in the step (b) and 2.5 parts of coal asphalt powder are mixed, and kneaded for 60min at room temperature by using a kneader.
Experimental example 1
In order to comparatively illustrate the performance of the carbon anodes prepared in the examples and comparative examples of the present invention, the following tests were performed on the carbon anodes prepared in the examples and comparative examples, and the test results are shown in table 1.
TABLE 1 Performance test results for different carbon anodes
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (13)
1. The carbon anode is prepared by mixing aggregate and a binder, and is characterized in that 85-95 parts by weight of aggregate and 5-15 parts by weight of binder are counted; the binder comprises 85-100% of phenolic resin and 0-15% of coal tar pitch by mass percent;
the phenolic resin comprises one or more of biomass modified phenolic resin, asphalt modified phenolic resin, coal tar modified phenolic resin, alkylphenol modified phenolic resin and rubber modified phenolic resin; the modified phenolic resin is liquid resin, and the viscosity of the resin is 8000-16000 mpa.s;
carbonizing the phenolic resin at the temperature of 900-1000 ℃ to form a carbide, wherein the resistivity of the carbide powder is 30-120m omega cm;
the preparation method of the carbon anode comprises the following steps:
mixing the raw materials according to a mass ratio, molding and carrying out heat treatment to obtain the carbon anode;
the mixing and molding are finished at 25-70 ℃.
2. The carbon anode according to claim 1, wherein the modified phenolic resin contains one or more of sodium salt, potassium salt, molybdate, iron salt, chromium salt, boron salt, cobalt salt, nickel salt and manganese salt.
3. The carbon anode of claim 1, wherein the aggregate comprises one or more of petroleum coke, calcined coke, needle coke, anthracite, lean bituminous coal, pitch coke, carbon nanotubes, and crushed graphite.
4. The carbon anode of claim 3, wherein the aggregate comprises petroleum coke, carbon nanotubes, and graphite fines.
5. The carbon anode according to claim 3, wherein the aggregate comprises 80-150 parts by weight of petroleum coke, 0-20 parts by weight of carbon nanotubes and 5-30 parts by weight of crushed graphite.
6. The carbon anode according to any one of claims 3 to 5, wherein the petroleum coke comprises, by particle size, 0-2mm petroleum coke, 2-4mm petroleum coke, 4-8mm petroleum coke, and fine petroleum coke.
7. The carbon anode according to claim 6, wherein the petroleum coke comprises, by weight, 0-2mm petroleum coke 30-40 parts, 2-4mm petroleum coke 20-40 parts, 4-8mm petroleum coke 10-30 parts, and 180 mesh fine powder petroleum coke 20-40 parts.
8. The carbon anode according to claim 1, wherein the heat treatment comprises baking and roasting.
9. The carbon anode of claim 8, wherein the baking method comprises: the temperature of the formed material is raised from room temperature to 150-200 ℃.
10. The carbon anode according to claim 9, wherein the baking process is carried out at a temperature increase rate of 2-8 ℃/h.
11. The carbon anode according to claim 10, wherein the temperature rise rate of the baking process is 3-5 ℃/h.
12. The carbon anode of claim 8, wherein the firing method comprises: under the condition of carbon burying, the temperature is raised from 150-200 ℃ to 1000-1100 ℃.
13. The carbon anode according to claim 12, wherein in the roasting process, the temperature rise rate is 4-10 ℃/h in the stage of 150-400 ℃; the temperature rise rate is 2-5 ℃/h in the 400-plus-800 ℃ stage, and the temperature rise rate is 4-10 ℃/h in the 800-plus-1100 ℃ stage.
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