CN115093199A - Special refractory crucible for negative electrode material carbonization and manufacturing process thereof - Google Patents
Special refractory crucible for negative electrode material carbonization and manufacturing process thereof Download PDFInfo
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- CN115093199A CN115093199A CN202210763463.8A CN202210763463A CN115093199A CN 115093199 A CN115093199 A CN 115093199A CN 202210763463 A CN202210763463 A CN 202210763463A CN 115093199 A CN115093199 A CN 115093199A
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- negative electrode
- electrode material
- crucible
- blank
- refractory crucible
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- 239000007773 negative electrode material Substances 0.000 title claims abstract description 51
- 238000003763 carbonization Methods 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000004927 clay Substances 0.000 claims abstract description 41
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 39
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910001868 water Inorganic materials 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 239000005350 fused silica glass Substances 0.000 claims abstract description 24
- 238000003825 pressing Methods 0.000 claims abstract description 24
- 239000010453 quartz Substances 0.000 claims abstract description 23
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 238000007605 air drying Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims description 21
- 238000010000 carbonizing Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 239000010405 anode material Substances 0.000 claims 3
- 230000000694 effects Effects 0.000 abstract description 8
- 239000005539 carbonized material Substances 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 description 19
- 238000005260 corrosion Methods 0.000 description 19
- 239000010406 cathode material Substances 0.000 description 15
- 239000000126 substance Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 12
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 10
- 229910052863 mullite Inorganic materials 0.000 description 10
- 239000002689 soil Substances 0.000 description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 description 9
- 239000011707 mineral Substances 0.000 description 9
- 239000004576 sand Substances 0.000 description 8
- 230000035939 shock Effects 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 239000002734 clay mineral Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 230000002035 prolonged effect Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000011819 refractory material Substances 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 2
- 229910001570 bauxite Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000005495 investment casting Methods 0.000 description 1
- 239000010443 kyanite Substances 0.000 description 1
- 229910052850 kyanite Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 229910021489 α-quartz Inorganic materials 0.000 description 1
- 229910000500 β-quartz Inorganic materials 0.000 description 1
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- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/04—Clay; Kaolin
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The application provides a special refractory crucible for negative electrode material carbonization and a manufacturing process thereof, and relates to the technical field of carbonized materials. The special refractory crucible for negative electrode material carbonization comprises: clay, wrought aluminum, quartz and water. The manufacturing process comprises the following steps: crushing clay and calcined aluminum to obtain particles, adding water into the particles, mixing and grinding, and adding fused quartz for mixing to obtain a blank; and (3) mounting the core mould on an upper operating platform of a hydraulic press, mounting the outer mould on a lower operating platform of the hydraulic press, adding a blank into the outer mould during pressing, controlling the hydraulic press to press the core mould downwards until the core mould is completely sleeved in the outer mould, then maintaining pressure, relieving pressure, returning, ejecting a top cylinder, taking out a blank body, air-drying, glazing the inner wall of the blank body, and roasting. The highest use temperature of the negative electrode material can reach 1300 ℃, the use frequency of the negative electrode material can reach more than 20 times in the environment of being less than or equal to 1100 ℃, the carbonization effect of the negative electrode material can be obviously improved, the carbonization cost of the negative electrode material is greatly saved, the negative electrode material and the environment are not polluted, and the negative electrode material is more environment-friendly and safer.
Description
Technical Field
The application relates to the technical field of carbonized materials, in particular to a refractory crucible special for negative electrode material carbonization and a manufacturing process thereof.
Background
In the industrial production of the cathode material for the lithium ion battery, the powdered carbon intermediate is often subjected to heat treatment at the temperature of 900 ℃ and 1400 ℃, which is commonly referred to as carbonization treatment in the industry. The negative electrode material needs to be carbonized by a special carbonization crucible, but the prior refractory crucible has the defects of large green blank making difficulty, incapability of forming and limitation on the use temperature and the use frequency; the graphitization treatment of the graphite crucible is a process with high energy consumption and high cost. Therefore, it is desirable to provide a refractory crucible and a manufacturing process thereof, which have low energy consumption, low cost and a large number of uses.
Disclosure of Invention
The application aims to provide a special refractory crucible for negative electrode material carbonization, the highest use temperature can reach 1300 ℃, the use frequency can reach more than 20 times in the environment of being less than or equal to 1100 ℃, the carbonization effect of the negative electrode material can be obviously improved, the carbonization cost of the negative electrode material can be greatly saved, the crucible is pollution-free to the negative electrode material and the environment, and the crucible is more environment-friendly and safe.
Another object of the present application is to provide a manufacturing process of a refractory crucible dedicated for negative electrode material carbonization, wherein a blank is obtained by crushing, mixing and grinding, a blank is obtained by pressing and correcting, and a crucible is obtained by glazing and baking, and the processes are mutually matched, so that the high temperature resistance, corrosion resistance and deformation resistance of the crucible can be significantly improved, and the service life of the crucible can be further prolonged.
The technical problem to be solved by the application is solved by adopting the following technical scheme.
The application provides a special resistant material crucible of negative pole material carbonization, by mass fraction, includes following raw materials: 30-50% of clay, 30-50% of wrought aluminum, 1-10% of quartz and 5-25% of water.
The application provides a manufacturing process of a special refractory crucible for negative electrode material carbonization, which comprises the following steps:
crushing clay and calcined aluminum to obtain particles, wherein the particle size of the particles is less than 5mm, adding water into the particles, mixing and grinding the particles, and adding fused quartz into the particles for mixing to obtain a blank; and (3) mounting the core mould on an upper operating platform of a hydraulic machine, mounting the outer mould on a lower operating platform of the hydraulic machine, adding a blank into the outer mould during pressing, controlling the hydraulic machine to press the core mould downwards until the core mould is completely sleeved in the outer mould, then maintaining pressure, relieving pressure, returning, ejecting a top cylinder, taking out a blank body, air-drying the blank body, glazing the inner wall of the blank body, and roasting.
The embodiment of the application has at least the following beneficial effects:
in this application, clay has better plasticity, associativity and contractility, and ripe aluminium has better corrosion resistance and compliance, and quartzy has better scraping resistance, chemical resistance and refractoriness, and several people collocation obtain the blank, can strengthen the refractoriness, chemical resistance and the thermal shock stability of blank for the crucible that makes has good physicochemical properties, and then improves the refractoriness, corrosion-resistant and the resistance to deformation of crucible, prolongs the life of crucible.
In the application, a blank is obtained by crushing, mixing and grinding and mixing, a blank is obtained by pressing and correcting, a crucible is obtained by glazing and roasting, the processes are mutually matched, no impurity is doped in the manufacturing process, after heating, the material in the crucible is not polluted, the service life time of the crucible can reach 20 times or more, and the crucible is high-temperature resistant, corrosion resistant, strong in acid and alkali resistance, small in high-temperature creep property and good in thermal shock resistance. The refractory crucible prepared by the process has the highest use temperature of 1300 ℃, can be used for more than 20 times in the environment of 1100 ℃ or lower, can obviously improve the carbonization effect of the cathode material, can greatly save the carbonization cost of the cathode material, has no pollution to the cathode material and the environment, and is more environment-friendly and safer.
Drawings
FIG. 1 is a schematic view of a refractory crucible for carbonizing a negative electrode material in an embodiment of the present application;
FIG. 2 is another schematic view of a refractory crucible for carbonizing a negative electrode material in an embodiment of the present application;
FIG. 3 is a cross-sectional view of an outer mold in an embodiment of the present application;
figure 4 is a cross-sectional view of a core die in an embodiment of the present application.
An icon: 100-external mold, 200-core mold, 201-exhaust hole.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. 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.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to specific examples.
A special refractory crucible for negative electrode material carbonization comprises the following raw materials in parts by mass: 30-50% of clay, 30-50% of wrought aluminum, 1-10% of quartz and 5-25% of water.
The clay is the soil with little sand and viscosity, and the water is not easy to pass through the clay, so that the clay has better plasticity. Clay is an important mineral raw material, which consists of various hydrated silicates and a certain amount of alumina, alkali metal oxides and alkaline earth metal oxides, and contains quartz, feldspar, mica, and impurities such as sulfate, sulfide and carbonate. The clay mineral is fine, usually in the size range of colloid, is in a crystal or amorphous state, most of the clay mineral is in a flake shape, and the few clay mineral is in a tubular or rod shape. The clay mineral has plasticity after being wetted by water, forms a mud cluster after being mixed with a proper amount of water, the mud cluster is deformed but not cracked under the action of external force, can still keep the original shape unchanged after the external force is dispersed, has large specific surface area, and has electronegativity on particles, so the clay mineral has good physical adsorption and surface chemical activity and has the capacity of exchanging with other cations. The clay has binding property, can be combined with non-plastic raw materials to form a good plastic clay cluster and has certain dry strength. When the dried clay pug is calcined at high temperature, the clay pug is further shrunk due to a series of physical and chemical changes such as dehydration, decomposition, mullite generation, quartz crystal transformation, transformation of fusible impurities, filling of gaps among particles by various melts and the like. The clay is Chongqing clay or Hunan clay.
The content of aluminum in the cooked aluminum is more than 99.00 percent, the electric conductivity is good, the corrosion resistance is good, the welding performance is good, the strength is low, the light and thin structure is light and soft, and the vessel can be pressed.
Quartz generally refers to low temperature quartz (α -quartz), which is the most widely distributed one of the minerals in the quartz family. The quartz in the broad sense also includes high temperature quartz (beta-quartz), coesite, etc., and the main component is SiO 2 Colorless and transparent, often contains a small amount of impurity components, and becomes semitransparent or opaque crystals with hard texture. The quartz has strong hardness, the external hardness of the quartz is as high as 7.5 Mohs hardness, the density is high, the melting point can reach more than 1300 ℃, and the quartz has better scratch resistance, chemical corrosion resistance and fire resistance.
Fused silica is an amorphous (glassy) state of silicon oxide (quartz, silica). It is a typical glass whose atomic structure is disordered long-range. It provides high service temperature and low thermal expansion coefficient through three-dimensional structure cross linking, and has higher working and melting temperature. It has very high thermal shock stability, and the fused silica shell is less cracked by temperature change during roasting and casting, so that it is ideal refractory material for investment casting and may be used as facing layer or back layer paint and sand spreading material. The fused quartz has small thermal expansion coefficient, is favorable for preventing the shell from cracking and deforming in the dewaxing and roasting processes, and is favorable for ensuring the stable size of the casting. The purity of the fused quartz is high, and the prepared coating has good stability; the high temperature creep resistance of the shell is improved. The thermal conductivity of the fused quartz is poor when the temperature is low, which is beneficial to filling the thin wall casting. The crucible can be crystallized at high temperature and changed in phase at low temperature, so that the surface of the crucible is easy to clean.
The second-level fused quartz has the refractoriness of 1700 ℃, high purity, large hardness, low internal stress, low thermal expansion coefficient, high stability and good chemical corrosion resistance.
The clay has good plasticity, associativity and contractility, the wrought aluminum has good corrosion resistance and flexibility, the quartz has good scratch resistance, chemical corrosion resistance and fire resistance, and the blank is obtained by matching the clay with the quartz, so that the fire resistance, the chemical corrosion resistance and the thermal shock stability of the blank can be enhanced, the prepared crucible has good physical and chemical properties, the refractoriness, the corrosion resistance and the deformation resistance of the crucible are further improved, and the service life of the crucible is prolonged.
In this embodiment, the refractory crucible dedicated for carbonization of the negative electrode material includes, by mass, 40% of clay, 40% of wrought aluminum, 5% of quartz, and 15% of water. Under the proportion, the components are uniformly mixed, the water content is proper, the subsequent compression molding is convenient, and simultaneously, the performance of the blank can be optimal after the components are matched, so that the refractoriness, the chemical corrosion resistance and the thermal shock resistance of the blank are improved, and the service life of the crucible is effectively prolonged.
In the embodiment, the refractory crucible special for carbonizing the cathode material further comprises 10-30% of high-aluminum wrought ore in percentage by mass, and the aluminum content of the high-aluminum wrought ore is 40-50%.
The high alumina chamotte is produced in Yunnan or Guizhou, and can be a high alumina mineral raw material, chamotte ore or mullite chamotte. The high-alumina mineral material is also called as kyanite mineral (or silimanite mineral), and Al is also added 2 O 3 >50% of the materials are called high-alumina mineral materials. The high-temperature-resistant aluminum alloy material has the characteristics of high temperature resistance, acid and alkali resistance, high mechanical strength, good high-temperature resistance under heavy load, expansion at high temperature and no shrinkage after cooling. The volume shrinkage of the clay minerals at high temperature can be counteracted, the volume stability of the whole refractory material is ensured, the cold and heat impact capacities are improved, and the service life of the smelting furnace is prolonged. The fire resistance of the calcined bauxite reaches up to 1780 ℃, and the calcined bauxite has strong chemical stability and good physical properties. Preferably high alumina mineral feedstock.
Mullite refers to a series of minerals composed of aluminosilicate, and the alumina content fluctuates between 72% and 78%, so that the mullite is a high-temperature refractory material and has the advantages of high temperature resistance, high strength, small heat conductivity coefficient, obvious energy-saving effect and the like.
In this embodiment, the raw materials of the special refractory crucible for negative electrode material carbonization still include mullite sand, and through adding mullite sand, the mechanical properties of the blank can be improved, so that the hardness of the blank is improved, the heat conductivity coefficient of the crucible can also be reduced, and when the crucible carries out carbonization treatment on the negative electrode material, the heat loss is less, so that the carbonization efficiency and the carbonization effect of the negative electrode material are improved, and the crucible is more energy-saving and environment-friendly.
In the embodiment, the outer diameter of the crucible made of the special refractory for carbonizing the cathode material is 255-260mm, the wall thickness is 19-25mm, the height is 460-570mm, and the bottom thickness is 20-30 mm. Under the specification, the crucible has wider application range and is more convenient to popularize and use.
A manufacturing process of a refractory crucible special for negative electrode material carbonization comprises the following steps:
crushing clay and calcined aluminum to obtain particles, wherein the particle size of the particles is less than 5mm, adding water into the particles, mixing and grinding the particles, and adding fused quartz into the particles for mixing to obtain a blank; and (3) mounting the core mould on an upper operating platform of a hydraulic machine, mounting the outer mould on a lower operating platform of the hydraulic machine, adding a blank into the outer mould during pressing, controlling the hydraulic machine to press the core mould downwards until the core mould is completely sleeved in the outer mould, then maintaining pressure, relieving pressure, returning, ejecting a top cylinder, taking out a blank body, air-drying the blank body, glazing the inner wall of the blank body, and roasting.
Wherein, the internal diameter of external mold is 260mm, and the height is 730mm, and the external diameter of heart mould is 220mm, and the height is 660 mm. The bottom of the core die is provided with the exhaust hole, the exhaust rod is arranged in the exhaust hole, when the core die is pressed, the blank does not enter the interior of the core die, when the core die returns, the exhaust rod falls down, and the exhaust hole exhausts, so that the green body and the core die are separated, the separation difficulty of the core die and the green body can be effectively reduced, and the production efficiency is improved.
The method comprises the steps of obtaining a blank by crushing, mixing and grinding, obtaining a blank by pressing and correcting, obtaining a crucible by glazing and roasting, matching the processes, not doping any impurity in the manufacturing process, preventing the material in the crucible from being polluted after heating, enabling the service life of the crucible to be 20 times or more, and being high-temperature resistant, corrosion resistant, acid and alkali resistant, small in high-temperature creep property and good in thermal shock resistance. The refractory crucible prepared by the process has the highest use temperature of 1300 ℃, can be used for more than 20 times in the environment of 1100 ℃ or lower, can obviously improve the carbonization effect of the cathode material, can greatly save the carbonization cost of the cathode material, has no pollution to the cathode material and the environment, and is more environment-friendly and safer. When the fused silica is added and mixed, the mixture may be mixed by milling or stirring.
When the powder is crushed, the particle size is less than 5 mm. Under the particle size, the raw materials are more convenient to compress and compact during pressing, the pores among the raw materials are reduced, the volume density of the crucible is improved, the infiltration degree of chemical reagents or other corrosive liquids to the crucible is reduced when the crucible is used, the crucible is not easy to corrode, and the service life of the crucible is prolonged.
During pressing, a primary pressing and secondary correction blank making process is adopted, and the pressure during primary pressing is 10-20 MPa. And during secondary correction, manual correction, tool correction or 5-10 ton hydraulic press correction is adopted. The pressing is normal temperature pressing, and the normal temperature is 22 +/-3 ℃.
The raw materials are pressed under the pressure, so that the combination degree of the raw materials is better, the raw materials are not easy to crack or deform, and the yield of the crucible is improved. The correction mainly comprises the control of the height and the roundness of the crucible, the manual or mechanical control of the forming condition of the crucible can be realized, the crucible can be perfected through correction under smaller errors, the yield of the crucible can be improved, the manufacturing cost of the crucible is reduced, and the defective rate is reduced.
And when glazing, adopting Shanxi glaze soil to glaze. The glaze earth, also called as clay glaze, is a ceramic glaze made of natural fusible clay or necessary flux added in it. The earth glaze has the characteristics of acid and alkali erosion resistance and higher mechanical strength than common glaze. Which can increase the mechanical strength and thermal stability of the crucible. The inner wall of the crucible is glazed, and when the negative electrode material is carbonized, the negative electrode material can be effectively prevented from entering the negative electrode material, so that the carbonization quality of the negative electrode material is poor. Through the setting of glaze layer, can effectively keep apart impurity, the glaze layer has certain mechanical strength simultaneously, can prevent the crucible fracture, further improves the mechanical properties of crucible, prevents the damage or the corruption of negative pole material or reagent to the crucible, further prolongs the life of crucible. In addition, the preparation process of the glaze soil is simple, the cost is low, and the preparation cost of the crucible can be further reduced. When the glaze soil is used for glazing, dye can be added into the glaze soil to color a glaze layer, such as yellow brown, black brown and the like, and the dye color can be specifically selected according to actual use scenes.
The temperature during the calcination is 1240 ℃ and 1320 ℃. And (4) roasting in a tunnel kiln to crystallize the green body and vitrify the glaze surface. At the temperature, the earth glaze can be better adhered to the inner wall of the crucible, and the raw materials in the crucible can be contracted through high-temperature firing, so that the bonding capacity of the raw materials is enhanced, the mechanical strength of the crucible is further improved, the bonding strength of a glaze layer is improved, and the cathode material or the crucible can be protected more conveniently when the crucible is used; but also can accelerate the crystallization of the blank and the vitrification of the glaze surface and improve the manufacturing efficiency.
In the application, the hydraulic machine is a four-column hydraulic machine with the model number of YQ32-315T, and the manufacturer is Hezhou forging machine tool Co.
In the drawings, fig. 1 shows a refractory crucible dedicated to carbonization of a negative electrode material, and fig. 2 shows a schematic view of the crucible dedicated to carbonization of a negative electrode material when the crucible and a crucible cover are combined.
The features and properties of the present application are described in further detail below with reference to examples.
Example 1
A manufacturing process of a refractory crucible special for negative electrode material carbonization comprises the following steps:
1000kg of raw materials: 40% of Chongqing clay, 40% of wrought aluminum, 5% of secondary fused quartz and 15% of water;
crushing clay and calcined aluminum until the particle size is less than 5mm, adding water, mixing, grinding, adding secondary fused quartz, and mixing to obtain a blank;
mounting a core die 200 on an upper operating platform of a four-column hydraulic machine, mounting an outer die 100 on a lower operating platform of the four-column hydraulic machine, wherein the pressure is 15MPa, adding a blank into the outer die 100 during pressing, controlling the four-column hydraulic machine to press the core die 200 downwards until the core die 200 is completely sleeved in the outer die 100, then maintaining the pressure, relieving the pressure, returning, correcting through a tool to control the height and roundness of a blank, ejecting the blank out of a top cylinder, taking out the blank, and air-drying the blank;
and (3) glazing the inner wall of the air-dried green body by adopting Shanxi glaze soil, and then roasting the glazed green body by adopting a tunnel kiln at the temperature of 1300 ℃ to crystallize the green body and vitrify the glaze surface.
Wherein, the inner diameter of the outer mold 100 is 260mm, the height is 730mm, the outer diameter of the core mold 200 is 220mm, and the height is 660 mm. The bottom of the core die 200 is provided with an exhaust hole 201, and an exhaust rod is installed in the exhaust hole 201. The outer diameter of the special refractory crucible for negative electrode material carbonization is 258mm, the wall thickness is 22mm, the height is 520mm, and the bottom thickness is 25 mm.
Example 2
A manufacturing process of a refractory crucible special for negative electrode material carbonization comprises the following steps:
1000kg of raw materials: 35% of clay, 45% of wrought aluminum, 8% of secondary fused quartz and 12% of water;
crushing clay and calcined aluminum until the particle size is less than 5mm, adding water, mixing, grinding, adding secondary fused quartz, and mixing to obtain a blank;
mounting a core die 200 on an upper operating platform of a four-column hydraulic machine, mounting an outer die 100 on a lower operating platform of the four-column hydraulic machine, wherein the pressure is 10MPa, adding a blank into the outer die 100 during pressing, controlling the four-column hydraulic machine to press the core die 200 downwards until the core die 200 is completely sleeved in the outer die 100, then maintaining the pressure, relieving the pressure, returning, manually correcting to control the height and roundness of a blank, ejecting the blank out of a top cylinder, taking out the blank, and air-drying the blank;
and (3) glazing the inner wall of the air-dried green body by adopting Shanxi glaze soil, and then roasting the glazed green body by adopting a tunnel kiln at the temperature of 1240 ℃ to crystallize the green body and vitrify the glaze.
The inner diameter of the outer mold 100 is 260mm, the height thereof is 730mm, and the outer diameter of the core mold 200 is 220mm, and the height thereof is 660 mm. The bottom of the core die 200 is provided with an exhaust hole 201, and an exhaust rod is installed in the exhaust hole 201. The outer diameter of the special refractory crucible for carbonizing the cathode material is 255mm, the wall thickness is 19mm, the height is 460mm, and the bottom thickness is 20 mm.
Example 3
A manufacturing process of a refractory crucible special for negative electrode material carbonization comprises the following steps:
1000kg of raw materials: 50% of clay, 30% of wrought aluminum, 4% of secondary fused quartz and 16% of water;
crushing clay and calcined aluminum until the particle size is less than 5mm, adding water, mixing, grinding, adding secondary fused quartz, and mixing to obtain a blank;
mounting a core die 200 on an upper operating platform of a four-column hydraulic machine, mounting an outer die 100 on a lower operating platform of the four-column hydraulic machine, wherein the pressure is 20MPa, adding a blank into the outer die 100 during pressing, controlling the four-column hydraulic machine to press the core die 200 downwards until the core die 200 is completely sleeved in the outer die 100, then maintaining the pressure, relieving the pressure, returning, correcting by using a 5-ton four-column hydraulic machine to control the height and roundness of a blank, ejecting a cylinder, taking out the blank, and air-drying the blank;
and (3) glazing the inner wall of the air-dried green body by adopting Shanxi glaze soil, and then roasting the glazed green body by adopting a tunnel kiln at the temperature of 1320 ℃ to crystallize the green body and vitrify the glaze.
The inner diameter of the outer mold 100 is 260mm, the height thereof is 730mm, and the outer diameter of the core mold 200 is 220mm, and the height thereof is 660 mm. The bottom of the core mold 200 is provided with an exhaust hole 201, and an exhaust rod is installed in the exhaust hole 201. The outer diameter of the special refractory crucible for negative electrode material carbonization is 260mm, the wall thickness is 25mm, the height is 500mm, and the bottom thickness is 30 mm.
Example 4
A manufacturing process of a refractory crucible special for negative electrode material carbonization comprises the following steps:
1000kg of raw materials: 30% of clay, 50% of wrought aluminum, 2% of secondary fused quartz, 6% of water and 12% of high-aluminum wrought ore, wherein the aluminum content of the high-aluminum wrought ore is 50%;
crushing clay, calcined aluminum and high-aluminum calcined ore to a particle size of less than 5mm, adding water, mixing and grinding, and then adding secondary fused quartz, and mixing to obtain a blank;
mounting a core die 200 on an upper operating platform of a four-column hydraulic machine, mounting an outer die 100 on a lower operating platform of the four-column hydraulic machine, wherein the pressure is 12MPa, adding a blank into the outer die 100 during pressing, controlling the four-column hydraulic machine to press the core die 200 downwards until the core die 200 is completely sleeved in the outer die 100, then maintaining the pressure, relieving the pressure, returning, correcting by using a 10-ton four-column hydraulic machine to control the height and roundness of a blank, ejecting a cylinder, taking out the blank, and air-drying the blank;
and (3) glazing the inner wall of the air-dried green body by adopting Shanxi glaze, and then roasting the glazed green body by adopting a tunnel kiln at the temperature of 1280 ℃ to crystallize the green body and vitrify the glaze.
The inner diameter of the outer mold 100 is 260mm, the height thereof is 730mm, and the outer diameter of the core mold 200 is 220mm, and the height thereof is 660 mm. The bottom of the core die 200 is provided with an exhaust hole 201, and an exhaust rod is installed in the exhaust hole 201. The outer diameter of the special refractory crucible for carbonizing the cathode material is 257mm, the wall thickness is 20mm, the height is 530mm, and the bottom thickness is 22 mm.
Example 5
A manufacturing process of a special refractory crucible for negative electrode material carbonization comprises the following steps:
1000kg of raw materials: 40% of clay, 30% of wrought aluminum, 2% of secondary fused quartz, 15% of water, 10% of high-aluminum wrought ore and 3% of mullite sand, wherein the aluminum content of the high-aluminum wrought ore is 40%;
crushing clay, calcined alumina and high-alumina calcined ore to a particle size of less than 5mm, adding water, mixing and grinding, and then adding secondary fused quartz and mullite sand, and mixing to obtain a blank;
installing the core mould 200 on an upper operation table of a four-column hydraulic press, installing the outer mould 100 on a lower operation table of the four-column hydraulic press, wherein the pressure is 18MPa, adding a blank into the outer mould 100 during pressing, controlling the four-column hydraulic press to press the core mould 200 downwards until the core mould 200 is completely sleeved in the outer mould 100, then maintaining the pressure, relieving the pressure, returning, correcting through a tool to control the height and roundness of a blank body, ejecting the blank body out of a top cylinder, taking out the blank body, and air-drying the blank body;
and (3) glazing the inner wall of the air-dried green body by adopting Shanxi glaze soil, and then roasting the glazed green body by adopting a tunnel kiln at the temperature of 1310 ℃ to crystallize the green body and vitrify the glaze surface.
The inner diameter of the outer mold 100 is 260mm, the height thereof is 730mm, and the outer diameter of the core mold 200 is 220mm, and the height thereof is 660 mm. The bottom of the core die 200 is provided with an exhaust hole 201, and an exhaust rod is installed in the exhaust hole 201. The outer diameter of the special refractory crucible for negative electrode material carbonization is 259mm, the wall thickness is 24mm, the height is 540mm, and the bottom thickness is 28 mm.
Example 6
A manufacturing process of a refractory crucible special for negative electrode material carbonization comprises the following steps:
1000kg of raw materials: 40% of clay, 40% of wrought aluminum, 1% of secondary fused quartz, 15% of water and 4% of mullite sand;
crushing clay and calcined aluminum until the particle size is smaller than 5mm, adding water, mixing, grinding, adding secondary fused quartz and mullite sand, and mixing to obtain a blank;
mounting a core die 200 on an upper operating platform of a four-column hydraulic machine, mounting an outer die 100 on a lower operating platform of the four-column hydraulic machine, wherein the pressure is 15MPa, adding a blank into the outer die 100 during pressing, controlling the four-column hydraulic machine to press the core die 200 downwards until the core die 200 is completely sleeved in the outer die 100, then maintaining the pressure, relieving the pressure, returning, correcting through a tool to control the height and roundness of a blank, ejecting the blank out of a top cylinder, taking out the blank, and air-drying the blank;
and (3) glazing the inner wall of the air-dried green body by adopting Shanxi glaze, and then roasting the glazed green body by adopting a tunnel kiln at 1300 ℃ to crystallize the green body and vitrify the glaze.
Wherein, the inner diameter of the outer die 100 is 260mm, the height is 730mm, the outer diameter of the core die 200 is 220mm, and the height is 660 mm. The bottom of the core die 200 is provided with an exhaust hole 201, and an exhaust rod is installed in the exhaust hole 201. The outer diameter of the special refractory crucible for negative electrode material carbonization is 258mm, the wall thickness is 22mm, the height is 520mm, and the bottom thickness is 25 mm.
Example 7
A manufacturing process of a refractory crucible special for negative electrode material carbonization comprises the following steps:
1000kg of raw materials: 40% of Hunan clay, 40% of wrought aluminum, 5% of quartz and 15% of water;
crushing clay and calcined aluminum until the particle size is less than 5mm, adding water, mixing, grinding, adding quartz, and mixing to obtain a blank;
installing the core mould 200 on an upper operation table of a four-column hydraulic press, installing the outer mould 100 on a lower operation table of the four-column hydraulic press, wherein the pressure is 15MPa, adding a blank into the outer mould 100 during pressing, controlling the four-column hydraulic press to press the core mould 200 downwards until the core mould 200 is completely sleeved in the outer mould 100, then maintaining the pressure, relieving the pressure and returning, correcting through a tool to control the height and roundness of a blank body, ejecting the blank body out of a top cylinder, taking out the blank body, and air-drying the blank body;
and (3) glazing the inner wall of the air-dried green body by adopting Shanxi glaze soil, and then roasting the glazed green body by adopting a tunnel kiln at the temperature of 1300 ℃ to crystallize the green body and vitrify the glaze surface.
Wherein, the inner diameter of the outer die 100 is 260mm, the height is 730mm, the outer diameter of the core die 200 is 220mm, and the height is 660 mm. The bottom of the core mold 200 is provided with an exhaust hole 201, and an exhaust rod is installed in the exhaust hole 201. The outer diameter of the special refractory crucible for negative electrode material carbonization is 258mm, the wall thickness is 22mm, the height is 520mm, and the bottom thickness is 25 mm.
Test results
The refractory crucible of example 1 of the present application and a commercially available graphite crucible were selected for experiments to test the crucible performance, and the results were as follows:
TABLE 1 crucible Performance index
As can be seen from Table 1, the performance index of the refractory crucible prepared in example 1 of the present application is slightly different from that of the graphite crucible. The refractory crucible has better refractoriness and chemical corrosion resistance, and can improve the use times of the refractory crucible.
To sum up, the special resistant material crucible of negative pole material carbonization of this application embodiment, clay have better plasticity, associativity and contractility, and ripe aluminium has better corrosion resistance and compliance, and quartz has better resistance to scratching, chemical corrosion resistance and refractoriness, and several collocation obtain the blank, can strengthen the fire resistance, the chemical corrosion resistance and the thermal shock stability of blank for the crucible that makes has good physicochemical property, and then improves the refractoriness, corrosion-resistant and the resistance to deformation of crucible, prolongs the life of crucible.
According to the manufacturing process of the special refractory crucible for negative electrode material carbonization, the blank is obtained through crushing, mixed grinding and mixing, the blank is obtained through pressing and correcting, the crucible is obtained through glazing and roasting, all the processes are mutually matched, no impurity is doped in the manufacturing process, after heating, the material in the crucible is not polluted, the service life of the crucible can reach 20 times or more, and the crucible is high-temperature resistant, corrosion resistant, high in acid and alkali resistance, small in high-temperature creep property and good in thermal shock resistance. The refractory crucible prepared by the process has the highest use temperature of 1300 ℃, can be used for more than 20 times in the environment of 1100 ℃ or lower, can obviously improve the carbonization effect of the cathode material, can greatly save the carbonization cost of the cathode material, has no pollution to the cathode material and the environment, and is more environment-friendly and safer.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments in the present application without making any creative effort belong to the protection scope of the present application.
Claims (10)
1. The special refractory crucible for carbonizing the negative electrode material is characterized by comprising the following raw materials in parts by mass: 30-50% of clay, 30-50% of wrought aluminum, 1-10% of quartz and 5-25% of water.
2. The special refractory crucible for carbonizing a negative electrode material according to claim 1, comprising 40% of clay, 40% of calcined aluminum, 5% of quartz and 15% of water by mass fraction.
3. The refractory crucible special for carbonizing a negative electrode material according to claim 2, further comprising 10 to 30% by mass of a high-alumina ripe ore having an aluminum content of 40 to 50%.
4. The special refractory crucible for carbonizing an anode material according to claim 3, wherein the quartz is secondary fused quartz.
5. The crucible as claimed in claim 1, wherein the crucible has an outer diameter of 255-260mm, a wall thickness of 19-25mm, a height of 460-570mm, and a bottom thickness of 20-30 mm.
6. The manufacturing process of the special refractory crucible for carbonizing the negative electrode material according to any one of claims 1 to 5, characterized by comprising the following steps: crushing clay and calcined aluminum to obtain particles with the particle size of less than 5mm, adding water into the particles, mixing and grinding, and adding fused quartz for mixing to obtain a blank; and (3) mounting the core mould on an upper operating platform of a hydraulic press, mounting the outer mould on a lower operating platform of the hydraulic press, adding a blank into the outer mould during pressing, controlling the hydraulic press to press the core mould downwards until the core mould is completely sleeved in the outer mould, maintaining pressure, relieving pressure, returning, ejecting a top cylinder, taking out a blank body, air-drying the blank body, glazing the inner wall of the blank body, and roasting.
7. The manufacturing process of the special refractory crucible for carbonizing the negative electrode material as claimed in claim 6, wherein an exhaust hole is formed in the bottom of the core mold, and an exhaust rod is installed in the exhaust hole.
8. The process for manufacturing a refractory crucible for carbonization of an anode material according to claim 6, wherein a primary pressing and secondary correction blank making process is used during pressing, and the pressure during primary pressing is 10 to 20 MPa.
9. The manufacturing process of the special refractory crucible for carbonizing the negative electrode material according to claim 6, wherein during secondary correction, manual correction, tool correction or 5-10 ton hydraulic press correction is adopted.
10. The process for manufacturing the special refractory crucible for carbonizing an anode material as claimed in claim 6, wherein the temperature is 1240-1320 ℃ during the baking.
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| CN107875027A (en) * | 2017-11-27 | 2018-04-06 | 东莞市爱嘉义齿有限公司 | A kind of artificial tooth material and preparation method thereof |
| CN107986769A (en) * | 2017-12-13 | 2018-05-04 | 苏州浩焱精密模具有限公司 | A kind of preparation method of quartz pincers pot mould |
| CN109574640A (en) * | 2019-01-25 | 2019-04-05 | 山东铭特陶瓷材料有限公司 | The preparation method of high-temperature corundum mullite crucible |
| CN114603146A (en) * | 2022-01-31 | 2022-06-10 | 北京科技大学 | Preparation method of homogenized large-size tungsten crucible |
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