CN115521145A - Process for producing negative electrode material crucible by combining phenolic resin - Google Patents
Process for producing negative electrode material crucible by combining phenolic resin Download PDFInfo
- Publication number
- CN115521145A CN115521145A CN202211308292.6A CN202211308292A CN115521145A CN 115521145 A CN115521145 A CN 115521145A CN 202211308292 A CN202211308292 A CN 202211308292A CN 115521145 A CN115521145 A CN 115521145A
- Authority
- CN
- China
- Prior art keywords
- crucible
- petroleum coke
- parts
- phenolic resin
- combining
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 38
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 34
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 34
- 239000007773 negative electrode material Substances 0.000 title claims description 22
- 239000002245 particle Substances 0.000 claims abstract description 87
- 239000000463 material Substances 0.000 claims abstract description 42
- 239000002006 petroleum coke Substances 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 239000002008 calcined petroleum coke Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 229920005989 resin Polymers 0.000 claims abstract description 17
- 239000011347 resin Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 9
- 238000007598 dipping method Methods 0.000 claims description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
- 229910002804 graphite Inorganic materials 0.000 claims description 24
- 239000010439 graphite Substances 0.000 claims description 24
- 239000000571 coke Substances 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- 238000005470 impregnation Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 5
- 239000010405 anode material Substances 0.000 claims 3
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000011230 binding agent Substances 0.000 abstract description 4
- 239000010406 cathode material Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 239000010426 asphalt Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000000465 moulding Methods 0.000 description 6
- 239000008187 granular material Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011300 coal pitch Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63472—Condensation polymers of aldehydes or ketones
- C04B35/63476—Phenol-formaldehyde condensation polymers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/48—Macromolecular compounds
- C04B41/488—Other macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/82—Coating or impregnation with organic materials
- C04B41/83—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of resin crucible production processes, and particularly relates to a process for producing a cathode material crucible by combining phenolic resin, which comprises the steps of adding auxiliary materials when a petroleum coke particle raw material is calcined, and crushing; the formula of the calcined petroleum coke particle raw material is as follows: 10-20 parts of 5-3mm, 3-1mm,10-50 parts of 1-0mm,2-20 parts of crushed calcined petroleum coke particle raw materials and auxiliary materials are added into a mixing pot to be stirred, then phenolic resin is added into the mixing pot, stirring is continued to be carried out, so that the phenolic resin infiltrates the petroleum coke particles, and a pressure forming machine is adopted for forming. According to the process, through isostatic pressing and the use of conductive resin as a binding agent, the produced product has the advantages of higher volume density, high strength, normal-temperature production, no pollution, less emission and long service life, the production cost can be reduced, the environmental protection problem is solved, and a foundation is provided for large-scale production of the cathode material.
Description
Technical Field
The invention belongs to the technical field of resin crucible production processes, and particularly relates to a process for producing a cathode material crucible by combining phenolic resin.
Background
At present, the development of new energy batteries is in vogue, lithium batteries are developed very rapidly, not only new energy automobiles but also products such as wind energy, solar energy and the like need electric energy storage, the most promising negative electrode material is artificial graphite at present, kilns for producing the artificial graphite at present mainly comprise an Acheson furnace and an inner series furnace, the two kilns both need crucibles, the mainstream production mode at present is hydraulic press production, asphalt is used as a binding agent, the pollution is serious, the high-temperature production is realized, the rejection rate is extremely high, the service life is short, and the strength is low.
Patent document CN102249237B proposes a graphite crucible, the surface of which is directly extruded and rubbed by a grinding tool, and the graphite crucible has good compactness and fewer pores; and the high-pressure impregnation is carried out twice, so that the surface of the crucible is more compact, the metal liquid is difficult to impregnate, and the service life of the crucible is greatly prolonged. However, the crucible process still uses pitch bonding, uses a hydraulic press for molding, and the like. The product combined by asphalt must be water-cooled firstly and then roasted for more than 20 days, and the roasting process must be well filled with fillers, so that the product is easy to deform, the rejection rate is high and the period is long.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a process for producing the negative electrode material crucible by combining phenolic resin, and the process has the advantages of higher product volume density, high strength, long service life and the like, solves the problem of environmental protection, and provides a basis for large-scale production of negative electrode materials.
In order to realize the purpose, the invention adopts the following technical scheme:
a process for producing a negative electrode material crucible by combining phenolic resin comprises the following steps:
s1: adding auxiliary materials when calcining the petroleum coke particle raw material, and crushing;
the petroleum coke particle raw material comprises the following components in parts by weight: 10-20 parts of petroleum coke particles with the particle size of 5-3mm, 10-50 parts of petroleum coke particles with the particle size of 3-1mm, 2-20 parts of petroleum coke particles with the particle size of 1-0mm, and the balance of petroleum coke particles with the particle size of less than 0.1 mm. The formulation is selected for the petroleum coke particle feedstock for greater density.
The auxiliary materials comprise the following components in parts by weight: 1-5 parts of crushed graphite, 1-5 parts of anode scrap and 1-5 parts of shot coke. The auxiliary materials are added with shot coke, and the residual anode is the cost reduction.
S2: adding the crushed calcined petroleum coke particle raw material and auxiliary materials into a mixing pot, stirring, adding phenolic resin into the mixing pot, and continuously stirring, wherein the mixing temperature is 50-80 ℃ to enable the phenolic resin to soak the petroleum coke particles. The resin is added into the kneading pot for better mixing and film covering.
S3: and forming by using a pressure forming machine.
S4: and (3) putting the crucible green body into a crucible roasting furnace for roasting, and filling auxiliary materials during furnace charging to ensure that the crucible green body is not deformed in the roasting process, thereby obtaining the roasted crucible. The filling material is added when the crucible is baked, so that the deformation of the crucible is prevented.
S5: and dipping the roasted crucible to obtain the dipping crucible. The specific process of the impregnation comprises the following steps: and (3) putting the roasted crucible into an impregnation tank, vacuumizing the tank, adding resin, and taking out the crucible to obtain the impregnation crucible. The crucible is dipped for the purpose of filling the pores with greater density.
Preferably, the adding amount of the auxiliary materials in the S1 is 1-15% of the calcined petroleum coke particle raw material by mass percent, and the particle size of the auxiliary materials is smaller than 200 meshes.
Preferably, the pressure forming machine in S3 is an isostatic pressing machine.
Preferably, the roasting temperature in S4 is 600-1100 ℃.
Preferably, in S5, the pressure after pressurization in the dipping tank is greater than 1.5MPa, the number of times of dipping the crucible is two, and the two dipping times are for densification.
Advantageous effects
The invention discloses a process for producing a negative electrode material crucible by combining phenolic resin, which has the following beneficial effects compared with the prior art:
1. according to the process for producing the negative electrode material crucible by combining the phenolic resin, through isostatic pressing, the conductive resin is used as a binding agent, the produced product is higher in volume density, high in strength, free of pollution, less in emission and long in service life, is produced at normal temperature, can reduce the production cost, solves the problem of environmental protection, and provides a foundation for large-scale production of negative electrode materials.
2. According to the process for producing the negative electrode material crucible by combining the phenolic resin, the coal pitch is produced under the high-temperature condition, the resin is produced at the normal temperature, and heat conduction oil with great hidden danger is not needed; the process is short, the cost is low, the resin combined product is cured after heat treatment after molding and cannot deform, the roasting time is short, the product can be roasted at low temperature within three days, the product quality is good, the strength is high, the compressive strength is more than 40 MPa, the flexural strength is more than 8 MPa, the density is high, the density of asphalt combination is about 1.55, the resin can reach more than 1.7, the service life is long, the resin combined product is not easy to deform, the density is high, and the service life can be prolonged.
Drawings
FIG. 1: the negative electrode material crucible product produced by the process is photo.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
A process for producing a negative electrode material crucible by combining phenolic resin comprises the following steps:
s1: adding auxiliary materials when calcining the petroleum coke particle raw material, and crushing;
the formula of the calcined petroleum coke particle raw material is as follows: the petroleum coke particles with the particle size of 5-3mm,15 parts of petroleum coke particles with the particle size of 3-1mm,40 parts of petroleum coke particles with the particle size of 1-0mm, and 15 parts of petroleum coke particles with the particle size of less than 0.075 mm;
the formula of the auxiliary materials is as follows: 2 parts of crushed graphite, 2 parts of anode scrap and 2 parts of shot coke;
the adding amount of the auxiliary materials is 6 percent of the calcined petroleum coke particle raw material by mass percent, and the granularity of the auxiliary materials is less than 200 meshes.
S2: adding the crushed calcined petroleum coke particle raw material and auxiliary materials into a mixing pot, stirring, adding phenolic resin into the mixing pot, and continuing stirring, wherein the mixing temperature is 65 ℃, so that the phenolic resin soaks the petroleum coke particles.
S3: the forming is carried out by a pressure forming machine which adopts an isostatic pressing forming machine.
S4: and (3) roasting the crucible green body in a crucible roasting furnace, filling auxiliary materials during furnace charging, and ensuring that the crucible green body is not deformed in the roasting process to obtain a roasted crucible, wherein the roasting temperature is 950 ℃.
S5: dipping the roasted crucible to obtain a dipping crucible, putting the roasted crucible into a dipping tank, vacuumizing the dipping tank, adding the Shengquan carbon resin, and taking out the crucible to obtain the dipping crucible, wherein the pressure in the dipping tank is more than 1.5MPa after pressurization, and the dipping crucible is dipped twice.
The photo of the produced negative electrode material crucible product is shown in fig. 1.
Example 2
A process for producing a negative electrode material crucible by combining phenolic resin comprises the following steps:
s1: adding auxiliary materials when calcining the petroleum coke particle raw material, and crushing;
the formula of the calcined petroleum coke particle raw material is as follows: 10 parts of petroleum coke particles with the particle size of 5-3mm, 50 parts of petroleum coke particles with the particle size of 3-1mm,10 parts of petroleum coke particles with the particle size of 1-0mm and the balance of petroleum coke particles with the particle size of less than 0.075 mm.
The formula of the auxiliary materials is as follows: 2 parts of crushed graphite, 2 parts of anode scrap and 2 parts of shot coke;
the adding amount of the auxiliary materials is 10 percent of the calcined petroleum coke particle raw material by mass percent, and the granularity of the auxiliary materials is less than 200 meshes.
S2: adding the crushed calcined petroleum coke particle raw material and auxiliary materials into a mixing pot, stirring, adding phenolic resin into the mixing pot, continuing stirring, and stirring paste at the temperature of 80 ℃ to enable the phenolic resin to soak the petroleum coke particles.
S3: the molding is carried out by a pressure molding machine, and the pressure molding machine adopts an isostatic pressing molding machine.
S4: and (3) placing the crucible green body into a crucible roasting furnace for roasting, and filling auxiliary materials when charging the crucible to ensure that the crucible green body does not deform in the roasting process to obtain a roasted crucible, wherein the roasting temperature is 1100 ℃.
S5: dipping the roasted crucible to obtain a dipping crucible, putting the roasted crucible into a dipping tank, vacuumizing the dipping tank, adding the Shengquan carbon resin, and taking out the crucible to obtain the dipping crucible, wherein the pressure in the dipping tank is more than 1.5MPa after pressurization, and the dipping crucible is dipped twice.
Example 3
A process for producing a negative electrode material crucible by combining phenolic resin comprises the following steps:
s1: adding auxiliary materials when calcining the petroleum coke particle raw material, and crushing;
the formula of the calcined petroleum coke particle raw material is as follows: petroleum coke particles with the particle size of 5-3mm, 20 percent of petroleum coke particles with the particle size of 3-1mm,40 parts of petroleum coke particles with the particle size of 1-0mm, and 20 parts of petroleum coke particles with the particle size of less than 0.075 mm;
the formula of the auxiliary materials is as follows: 2 parts of crushed graphite, 2 parts of anode scrap and 2 parts of shot coke;
the adding amount of the auxiliary materials is 15 percent of the calcined petroleum coke particle raw material by mass percent, and the granularity of the auxiliary materials is less than 200 meshes.
S2: adding the crushed calcined petroleum coke particle raw material and auxiliary materials into a mixing pot, stirring, adding phenolic resin into the mixing pot, continuously stirring, and enabling the phenolic resin to soak the petroleum coke particles at the mixing temperature of 50 ℃.
S3: the forming is carried out by a pressure forming machine which adopts an isostatic pressing forming machine.
S4: and (3) roasting the crucible green body in a crucible roasting furnace, filling auxiliary materials during furnace charging, and ensuring that the crucible green body is not deformed in the roasting process to obtain a roasted crucible, wherein the roasting temperature is 600 ℃.
S5: dipping the roasted crucible to obtain a dipping crucible, putting the roasted crucible into a dipping tank, vacuumizing the dipping tank, adding the Shengquan carbon resin, and taking out the crucible to obtain the dipping crucible, wherein the pressure in the dipping tank is more than 1.5MPa after pressurization, and the dipping crucible is dipped twice.
Comparative example
A process for producing a negative electrode material crucible by combining phenolic resin comprises the following steps:
s1: adding auxiliary materials when the petroleum coke particle raw material is calcined, and crushing; the formula of the calcined petroleum coke particle raw material is as follows: the granularity of the granules is 5-3mm,15%, the granularity of the granules is 3-1mm,40%, the granularity of the granules is 1-0mm,15%, the granularity of the rest granules is less than 0.075mm, and the auxiliary material formula is as follows: 2% of crushed graphite, 2% of anode scrap and 2% of shot coke; the adding amount of the auxiliary materials is 6 percent of the raw material of the calcined petroleum coke particles by mass percent, and the granularity of the auxiliary materials is less than 600 meshes.
S2: adding the crushed calcined petroleum coke particle raw material and auxiliary materials into a mixing pot, stirring, adding liquid asphalt into the mixing pot, and continuing stirring to enable the liquid asphalt to infiltrate the petroleum coke particles.
S3: the forming is carried out by a pressure forming machine which adopts an isostatic pressing forming machine.
S4: and (3) roasting the crucible green body in a crucible roasting furnace, filling auxiliary materials during furnace charging, and ensuring that the crucible green body is not deformed in the roasting process to obtain a roasted crucible, wherein the roasting temperature is 1100 ℃.
S5: dipping the roasted crucible to obtain a dipping crucible, putting the roasted crucible into a dipping tank, vacuumizing the tank, adding liquid asphalt, and taking out the tank to obtain the dipping crucible, wherein the pressure in the dipping tank is more than 1.5MPa after pressurization, and the dipping crucible is dipped twice.
Experimental example 1
The graphite crucibles prepared in examples 1 to 3 and comparative example were subjected to bulk density measurement, respectively, by the following methods: and (4) measuring the volume.
The detection results are as follows:
the bulk density of the graphite crucible in example 1 was; 1.60g/cm 3 ；
The bulk density of the graphite crucible in example 2 was 1.57g/cm 3 ；
The bulk density of the graphite crucible in example 3 was 1.61g/cm 3 ；
The graphite crucible of the comparative example had a bulk density of 1.48g/cm 3 。
As can be seen by comparing the test results of examples 1-3 and comparative example, the density of the isostatic compaction is significantly improved, the asphalt has obvious cracks, mainly caused by the after-effect of elasticity, the resin forming temperature can be all, and the roasting temperature of the asphalt combined product can not be lower than 1100 ℃.
Experimental example 2
The graphite crucibles obtained in examples 1 to 3 and comparative example were each subjected to a compressive strength test by placing a sample at the center of the working face of a testing machine at 0.5N/mm/sec 2 The load was continuously applied without impact until the sample was broken, and the load at the time of breaking the sample was recorded. The compressive strength was calculated from the load at the time of breaking the sample and the cross-sectional area of the sample by applying a pressure to a testing machine. The compressive strength is the initial load strength at which the test specimen is broken. The detection results are as follows:
the compressive strength of the graphite crucible in example 1 was 46 mpa;
the compressive strength of the graphite crucible in example 2 was 49 mpa;
the compressive strength of the graphite crucible in example 3 was 45 mpa;
the compressive strength of the graphite crucible in the comparative example was 29 MPa.
As can be seen from comparison of the test results of examples 1 to 3, example 2 is the most preferable example in the present application.
As can be seen by comparing the test results of examples 1-3 with those of comparative example, the asphalt-bonded product had significant cracking and a severe decrease in strength.
Experimental example 3
The graphite crucibles prepared in examples 1 to 3 and comparative example were subjected to the service life test, respectively, and the test results were as follows:
the service life of the graphite crucible in the embodiment 1 is 4 years;
the service life of the graphite crucible in the embodiment 2 is 4 years;
the service life of the graphite crucible in the embodiment 3 is 4 years;
the service life of the graphite crucible in the comparative example is 3 years;
as can be seen from comparison of the test results of examples 1 to 3 and the comparative example, the resin bond is a hard carbon bond, the attenuation is slow, the service life can be prolonged, the asphalt bond is loose, the strength after complete graphitization is low, and the asphalt bond is easy to damage.
According to the process, isostatic pressing is used, the conductive resin is used as a binding agent, the produced product is higher in volume density, high in strength, free of pollution, less in emission, long in service life, capable of reducing the production cost, capable of solving the problem of environmental protection and providing a foundation for large-scale production of the cathode material, and the production at normal temperature is carried out.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for some of the features thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (9)
1. The process for producing the negative electrode material crucible by combining phenolic resin is characterized by comprising the following steps of:
s1: adding auxiliary materials when calcining the petroleum coke particle raw material, and crushing;
s2: adding the crushed calcined petroleum coke particle raw material and auxiliary materials into a mixing pot, stirring, adding phenolic resin into the mixing pot, and continuing stirring, wherein the mixing temperature is 50-80 ℃ so that the phenolic resin infiltrates the petroleum coke particles;
s3: forming by using a pressure forming machine to obtain a crucible green body;
s4: placing the crucible green body into a crucible roasting furnace for roasting, and filling auxiliary materials during furnace charging to ensure that the crucible green body is not deformed in the roasting process to obtain a roasted crucible;
s5: and dipping the roasted crucible to obtain the dipping crucible.
2. The process for producing the crucible for the anode material by combining the phenolic resin as claimed in claim 1, wherein in the step S1, the raw material of the calcined petroleum coke particles comprises the following components in parts by weight: 10-20 parts of petroleum coke particles with the particle size of 5-3mm, 10-50 parts of petroleum coke particles with the particle size of 3-1mm, 2-20 parts of petroleum coke particles with the particle size of 1-0mm, and the balance of petroleum coke particles with the particle size of less than 0.1 mm.
3. The process for producing the negative electrode material crucible by combining the phenolic resin as claimed in claim 2, wherein in the step S1, the auxiliary material comprises the following components in parts by weight: 1-5 parts of crushed graphite, 1-5 parts of anode scrap and 1-5 parts of shot coke.
4. The process for producing the crucible with the negative electrode material by combining the phenolic resin as claimed in claim 3, wherein in the step S1, the addition amount of the auxiliary material is 1-15% of the calcined petroleum coke particle raw material by mass percent, and the particle size of the auxiliary material is less than 200 meshes.
5. The process for producing the crucible for the anode material by combining the phenolic resin as claimed in claim 3, wherein in the step S1, the raw material of the calcined petroleum coke particles comprises the following components in parts by weight: 10 parts of petroleum coke particles with the particle size of 5-3mm, 50 parts of petroleum coke particles with the particle size of 3-1mm,10 parts of petroleum coke particles with the particle size of 1-0mm, and the balance of petroleum coke particles with the particle size of less than 0.075 mm; the auxiliary materials comprise the following components in parts by weight: 2 parts of crushed graphite, 2 parts of anode scrap and 2 parts of shot coke; the adding amount of the auxiliary materials is 10 percent of the calcined petroleum coke particle raw material by mass percentage.
6. The process for producing the crucible of the negative electrode material by combining the phenolic resin according to claim 1, wherein in the step S3, the pressure forming machine is an isostatic pressing machine.
7. The process for producing the crucible for the anode material by combining the phenolic resin as claimed in claim 1, wherein the roasting temperature in the step S4 is 600-1100 ℃.
8. The process for producing the negative electrode material crucible by combining the phenolic resin as claimed in claim 1, wherein in the step S5, the specific process of impregnation is as follows: and (3) putting the roasted crucible into an impregnation tank, vacuumizing the tank, adding resin, and taking out the crucible to obtain the impregnation crucible.
9. The process for producing the crucible of the negative electrode material by combining the phenolic resin as claimed in claim 8, wherein the pressure after pressurization in the impregnation tank is more than 1.5MPa, and the number of times of impregnating the crucible is two.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211308292.6A CN115521145A (en) | 2022-10-25 | 2022-10-25 | Process for producing negative electrode material crucible by combining phenolic resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211308292.6A CN115521145A (en) | 2022-10-25 | 2022-10-25 | Process for producing negative electrode material crucible by combining phenolic resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115521145A true CN115521145A (en) | 2022-12-27 |
Family
ID=84702938
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211308292.6A Pending CN115521145A (en) | 2022-10-25 | 2022-10-25 | Process for producing negative electrode material crucible by combining phenolic resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115521145A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030367A (en) * | 1988-05-07 | 1989-01-18 | 天津市耐火器材厂 | Method for making graphite crucible |
| CN102249237A (en) * | 2010-12-20 | 2011-11-23 | 龚炳生 | Graphite crucible |
| CN106981657A (en) * | 2017-05-26 | 2017-07-25 | 成都海成远创科技有限公司 | A kind of graphite cathode material and preparation method thereof |
| WO2022056189A1 (en) * | 2020-09-11 | 2022-03-17 | Arq Ip Limited | Methods for the production of increased anisotropic coke |
| CN114572978A (en) * | 2022-03-16 | 2022-06-03 | 江西紫宸科技有限公司 | Preparation method of high-rate graphite negative electrode material, negative electrode material and lithium battery |
| CN114620707A (en) * | 2022-03-24 | 2022-06-14 | 江西正拓新能源科技股份有限公司 | Preparation method of long-cycle lithium ion battery cathode material |
-
2022
- 2022-10-25 CN CN202211308292.6A patent/CN115521145A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030367A (en) * | 1988-05-07 | 1989-01-18 | 天津市耐火器材厂 | Method for making graphite crucible |
| CN102249237A (en) * | 2010-12-20 | 2011-11-23 | 龚炳生 | Graphite crucible |
| CN106981657A (en) * | 2017-05-26 | 2017-07-25 | 成都海成远创科技有限公司 | A kind of graphite cathode material and preparation method thereof |
| WO2022056189A1 (en) * | 2020-09-11 | 2022-03-17 | Arq Ip Limited | Methods for the production of increased anisotropic coke |
| CN114572978A (en) * | 2022-03-16 | 2022-06-03 | 江西紫宸科技有限公司 | Preparation method of high-rate graphite negative electrode material, negative electrode material and lithium battery |
| CN114620707A (en) * | 2022-03-24 | 2022-06-14 | 江西正拓新能源科技股份有限公司 | Preparation method of long-cycle lithium ion battery cathode material |
Non-Patent Citations (1)
| Title |
|---|
| 宋慧平等: "《环境与资源类专业系列教材 普通高等教育十四五规划教材 粉煤灰基功能涂料》", 北京理工大学出版社, pages: 129 - 68 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106981657B (en) | A kind of graphite cathode material and preparation method thereof | |
| CN107814382B (en) | Long-life modified natural graphite negative electrode material and preparation method and application thereof | |
| CN101698945B (en) | Carbon-fiber reinforced cathode carbon block and preparation method thereof | |
| CN105967718B (en) | The graphite anode for magnesium electrolysis of resistance to high current and its preparation process | |
| CN110620236B (en) | Three-phase composite negative electrode material for lithium ion battery and preparation method thereof | |
| CN108610049B (en) | Isotropic graphite material, method for the production thereof and use thereof | |
| CN112441835A (en) | High-strength high-density carbon material and preparation method and application thereof | |
| CN110590390A (en) | Carbon fiber graphite crucible for metallurgical casting furnace and preparation method thereof | |
| CN108101042A (en) | A kind of production technology of lithium battery graphite cathode material | |
| CN101255568A (en) | Particle gradation functional gradient TiB2/C composite cathode for aluminium electrolysis and preparation method thereof | |
| KR101249647B1 (en) | Manufacturing method of graphite block | |
| CN115353391B (en) | Method for preparing special graphite material by isostatic pressing of graphite waste in short process | |
| CN108155385A (en) | A kind of lithium battery production graphite cathode material preparation method | |
| CN105529443B (en) | A kind of preparation method of negative electrode of lithium ion battery hard carbon material | |
| CN100494507C (en) | High-density semi-graphite cathode carbon block and method for producing same | |
| CN108218430B (en) | Isostatic pressing graphite product and preparation method thereof | |
| CN115521145A (en) | Process for producing negative electrode material crucible by combining phenolic resin | |
| CN113603487A (en) | Graphite with large specification and fine granularity and preparation process thereof | |
| CN107903064A (en) | A kind of preparation method of hyperfine structure graphite for electrical discharge machining | |
| CN101748441B (en) | Method and device for preparing high-density aluminium cell anode carbon block green body | |
| CN110416544B (en) | Method for preparing high-capacity artificial graphite cathode material by block semi-closed pore catalytic graphitization | |
| CN114634361A (en) | Preparation method of isotropic isostatic pressing graphite with fine structure | |
| CN114014662A (en) | Selenium-graphene composite isostatic pressing graphite material and preparation method thereof | |
| CN115626641B (en) | Preparation method of onion carbon extremely-fine particle isostatic graphite | |
| Wang et al. | Production of carbon anodes by high-temperature mould pressing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |