CN113185307B - Rotary kiln furnace lining for roasting lithium battery anode material and preparation method thereof - Google Patents
Rotary kiln furnace lining for roasting lithium battery anode material and preparation method thereof Download PDFInfo
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- CN113185307B CN113185307B CN202110363324.1A CN202110363324A CN113185307B CN 113185307 B CN113185307 B CN 113185307B CN 202110363324 A CN202110363324 A CN 202110363324A CN 113185307 B CN113185307 B CN 113185307B
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- lithium battery
- rotary kiln
- roasting
- anode material
- battery anode
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 86
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000010405 anode material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 66
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 9
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims abstract description 7
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 claims abstract description 5
- 239000004137 magnesium phosphate Substances 0.000 claims abstract description 5
- 229960002261 magnesium phosphate Drugs 0.000 claims abstract description 5
- 229910000157 magnesium phosphate Inorganic materials 0.000 claims abstract description 5
- 235000010994 magnesium phosphates Nutrition 0.000 claims abstract description 5
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims abstract description 5
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 claims abstract description 5
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 7
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 3
- 238000000465 moulding Methods 0.000 abstract description 18
- 239000000843 powder Substances 0.000 abstract description 8
- 239000007767 bonding agent Substances 0.000 abstract description 7
- 238000004901 spalling Methods 0.000 abstract description 6
- 230000003628 erosive effect Effects 0.000 abstract description 5
- 239000007774 positive electrode material Substances 0.000 description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000008188 pellet Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000012535 impurity Substances 0.000 description 6
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000012797 qualification Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011819 refractory material Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- -1 metallurgy Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
- C04B35/043—Refractories from grain sized mixtures
-
- 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
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
- F27B7/20—Details, accessories, or equipment peculiar to rotary-drum furnaces
- F27B7/28—Arrangements of linings
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D1/00—Casings; Linings; Walls; Roofs
- F27D1/0003—Linings or walls
- F27D1/0006—Linings or walls formed from bricks or layers with a particular composition or specific characteristics
-
- 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/447—Phosphates or phosphites, e.g. orthophosphate or hypophosphite
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Abstract
The invention relates to a rotary kiln lining for roasting a lithium battery anode material and a preparation method thereof. The technical proposal is as follows: uniformly mixing 52.0-67.0 wt% of fused magnesia, 28.0-43.0 wt% of light burned magnesia, 0.5-4.5 wt% of active alumina micro powder, 0.3-3.3 wt% of ferrous oxide and 0.2-4.0 wt% of bonding agent to obtain a mixture; and then molding the mixture, and preserving heat for 3-6 hours at the temperature of 150-180 ℃ to obtain the rotary kiln furnace lining for roasting the lithium battery anode material. Wherein: the bonding agent is one of zirconium phosphate, magnesium phosphate and aluminum dihydrogen phosphate; the molding mode is one of pressure, pouring, ramming and smearing. The invention has the characteristics of simple process, high productivity, time saving and high efficiency; the prepared rotary kiln furnace lining for roasting the lithium battery anode material has good erosion resistance, good spalling resistance and long service life, and can fundamentally improve the performance of the roasted lithium battery anode material.
Description
Technical Field
The invention belongs to the technical field of rotary kiln linings for roasting. In particular to a rotary kiln lining for roasting lithium battery anode materials and a preparation method thereof.
Background
Since the safety and performance of electronic devices and electric vehicles are closely related to the capacity and efficiency of batteries, development of high-performance lithium battery materials having high stability and high energy density is a popular research project in recent years. The positive electrode material of the lithium battery is composed of Li, co, mn, ni and the like, and the preparation process is that raw materials are filled in a sagger and are sintered at 400-1000 ℃. In this process, li and Co compounds melt and permeate into the pores of the sagger, and react with constituent components to induce cracking and peeling of the sagger body. On the one hand, the reaction substance stripped by the sagger reduces the quality of the positive electrode material of the lithium battery; on the other hand, the sagger is broken due to the crack, and the broken sagger has the defect of reducing the activity of the positive electrode material of the baked lithium battery in the recycling process. In general, the erosion resistance of the sagger cannot be effectively ensured, the sagger is also easier to peel off from the baked battery powder to further cause the performance degradation of the lithium battery anode material, the whole service life of the sagger is shorter, the sagger is difficult to carry out subsequent recycling, and the great improvement of the yield of the battery powder cannot be realized.
The firing equipment of the whole lithium battery cathode material is developed towards the direction of coating the surface of a sagger with substances with smaller reactivity or improving the thermal shock resistance of the firing equipment. However, the surface coating of the sagger is complicated and difficult to mass-produce, or there is a disadvantage that peeling occurs due to the difference in thermal expansion coefficient between the coating and the sagger material. In addition, the surface of the sagger is treated only to reduce the reaction degree between the sagger body and the battery material to be baked, so that the reaction with the positive electrode active material of the lithium battery cannot be blocked basically, and the reaction is remained in the baked battery powder, thereby reducing the qualification rate of the battery. Moreover, the sagger is used for containing the lithium battery anode material, and the production efficiency is low when the sagger is matched with intermittent firing of a roller kiln, so that the yield of the lithium battery anode material cannot meet the requirement of high-speed development of the energy industry.
Rotary kilns are widely used in a plurality of production industries such as building materials, metallurgy, chemical industry, environmental protection and the like, and a plurality of rotary kiln lining designs aiming at the corresponding industries are provided. However, the existing technology for preparing the rotary kiln furnace lining is mostly used for roasting building materials such as cement, ceramic particles and the like, and a few are used for roasting refractory materials, but the rotary kiln furnace lining technology for roasting lithium battery anode materials is not reported.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a rotary kiln furnace lining for roasting lithium battery anode materials, which has the advantages of simple process, high productivity, time saving and high efficiency. The rotary kiln furnace lining for roasting the lithium battery anode material prepared by the method has the advantages of excellent erosion resistance, excellent spalling resistance, environmental friendliness and long service life, and the performance of the roasted lithium battery anode material can be fundamentally improved.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: uniformly mixing 52.0-67.0 wt% of fused magnesia, 28.0-43.0 wt% of light burned magnesia, 0.5-4.5 wt% of active alumina micro powder, 0.3-3.3 wt% of ferrous oxide and 0.2-4.0 wt% of bonding agent to obtain a mixture; and then molding the mixture, and preserving heat for 3-6 hours at the temperature of 150-180 ℃ to obtain the rotary kiln furnace lining for roasting the lithium battery anode material.
The grain size of the fused magnesia is less than 3mm and more than or equal to 1mm; the fused magnesia: mgO content is more than or equal to 96.6wt%, siO 2 The content is less than or equal to 0.79wt percent, fe 2 O 3 The content is less than or equal to 0.13 weight percent.
The grain diameter of the light burned magnesia is smaller than 1mm and larger than or equal to 0.045mm; the light burned magnesite comprises the following components: mgO content is more than or equal to 95.3wt percent, siO 2 The content is less than or equal to 0.85 weight percent, fe 2 O 3 The content is less than or equal to 0.26 weight percent.
The particle size of the activated alumina micropowder is smaller than 0.088mm; al of the activated alumina micropowder 2 O 3 The content is more than or equal to 98.8wt%.
The particle size of the ferrous oxide is smaller than 0.045mm; the FeO content of the ferrous oxide is more than or equal to 99.1wt%.
The binding agent is one of zirconium phosphate, magnesium phosphate and aluminum dihydrogen phosphate.
The molding mode is one of pressure, pouring, ramming and smearing.
By adopting the technical scheme, compared with the prior art, the invention has the following positive effects:
1. the invention uses electric smelting magnesia, light burning magnesia, active alumina micropowder and ferrous oxide as main raw materials, and the preparation process is simple by carrying out pressure/pouring/ramming/smearing molding and then preserving heat for 3-6 hours at 150-180 ℃ to obtain the rotary kiln lining (hereinafter referred to as rotary kiln lining) for roasting the lithium battery anode material. The pellets of the lithium battery anode material to be roasted can be directly roasted after being filled into the prepared rotary kiln lining, so that the loading and unloading process of a sagger is omitted, and the integrated forming ensures that the roasting process of the lithium battery anode material has the advantages of simplicity, time saving and high efficiency.
2. The rotary kiln lining prepared by the method is in rolling contact with the pellets of the positive electrode material of the lithium battery, so that continuous roasting of the positive electrode material of the lithium battery is ensured, permeation and pollution of the rotary kiln lining material into the positive electrode material can be avoided to the greatest extent, the production efficiency can be greatly improved on the premise of ensuring safe production, the roasting effect and efficiency of the positive electrode material of the lithium battery are optimized to the greatest extent, and the method is suitable for roasting of powder of the positive electrode material of the lithium battery and pellets prepared by machine pressing/roll forming. Plays a key propulsion role in relieving the industrial pressure of the energy industry.
3. The rotary kiln lining material prepared by the invention is MgO-Al 2 O 3 The refractory material has the characteristics of high corrosion resistance and high spalling resistance, and the iron-rich spinel formed in the high-temperature use process has defect vacancies and can absorb impurity ions such as impurity ions escaped from the lithium battery anode material in the high-temperature reaction; li (Li) + 、Co 2+ And Ni 3+ The requirements of frequently roasting the lithium battery anode material can be met, and the service life is long; the method can fundamentally solve the problem of performance degradation of the lithium battery caused by stripping of the lining material of the rotary kiln during roasting, has small pollution to the fired product, can replace the matching of the traditional roller kiln and a sagger, and can remarkably improve the performance of the roasted lithium battery anode material.
4. The contact area between the rotary kiln lining and the anode material pellets of the lithium battery is minimized, the physical/chemical reaction between the rotary kiln lining measurement and the anode material pellets of the lithium battery can be avoided to the greatest extent, and LiCO of byproducts of the roasting reaction is avoided at the same time 3 Fe, feO and Fe 2 O 3 The residual results in the problem of degradation of the performance of the lithium battery, thereby improving the qualification rate and the performance of the positive electrode material of the lithium battery after roasting.
The rotary kiln lining prepared by the invention is used for detecting the lithium iron phosphate which is a lithium battery positive electrode material, and meanwhile, the commercial sagger is used for detecting the lithium iron phosphate which is a lithium battery positive electrode material, and the comparison result shows that the performance of the lithium iron phosphate positive electrode material roasted by the rotary kiln lining prepared by the invention is superior to that of the lithium battery positive electrode material roasted by the commercial sagger, the impurity residue rate is lower, and the apparent density is higher.
Therefore, the invention has the characteristics of simple process, high productivity, time saving and high efficiency; the prepared rotary kiln furnace lining for roasting the lithium battery anode material has good erosion resistance, good spalling resistance and long service life, and can fundamentally improve the performance of the roasted lithium battery anode material.
Drawings
FIG. 1 is a schematic diagram of a rotary kiln for using the positive electrode material of a rotary kiln baked lithium battery prepared by the invention;
fig. 2 is a schematic cross-sectional view of fig. 1.
Detailed Description
The invention is further described in connection with the following detailed description, which is not intended to limit the scope of the invention.
A rotary kiln lining for roasting lithium battery anode material and a preparation method thereof. The preparation method comprises the following steps:
uniformly mixing 52.0-67.0 wt% of fused magnesia, 28.0-43.0 wt% of light burned magnesia, 0.5-4.5 wt% of active alumina micro powder, 0.3-3.3 wt% of ferrous oxide and 0.2-4.0 wt% of bonding agent to obtain a mixture; and then molding the mixture, and preserving heat for 3-6 hours at the temperature of 150-180 ℃ to obtain the rotary kiln furnace lining for roasting the lithium battery anode material.
The binding agent is one of zirconium phosphate, magnesium phosphate and aluminum dihydrogen phosphate.
The molding mode is one of pressure, pouring, ramming and smearing.
In this embodiment:
the grain size of the fused magnesia is less than 3mm and more than or equal to 1mm; the fused magnesia: mgO content is more than or equal to 96.6wt%, siO 2 The content is less than or equal to 0.79wt percent, fe 2 O 3 The content is less than or equal to 0.13 weight percent.
The grain diameter of the light burned magnesia is smaller than 1mm and larger than or equal to 0.045mm; the light burned magnesite comprises the following components: mgO content is more than or equal to 95.3wt percent, siO 2 The content is less than or equal to 0.85 weight percent, fe 2 O 3 The content is less than or equal to 0.26 weight percent.
The particle size of the activated alumina micropowder is smaller than 0.088mm; al of the activated alumina micropowder 2 O 3 The content is more than or equal to 98.8wt%.
The particle size of the ferrous oxide is smaller than 0.045mm; the FeO content of the ferrous oxide is more than or equal to 99.1wt%.
The embodiments are not described in detail.
Example 1
A rotary kiln lining for roasting lithium battery anode material and a preparation method thereof. The preparation method comprises the following steps:
uniformly mixing 52.0wt% of fused magnesia, 43.0wt% of light burned magnesia, 1.5wt% of activated alumina micropowder, 2.3wt% of ferrous oxide and 1.2wt% of a bonding agent to obtain a mixture; and molding the mixture, and preserving heat for 6 hours at 150 ℃ to obtain the rotary kiln furnace lining for roasting the lithium battery anode material.
The binding agent is zirconium phosphate.
The shaping is pressure shaping.
Example 2
A rotary kiln lining for roasting lithium battery anode material and a preparation method thereof. The preparation method comprises the following steps:
uniformly mixing 56wt% of fused magnesia, 39wt% of light burned magnesia, 4.5wt% of activated alumina micropowder, 0.3wt% of ferrous oxide and 0.2wt% of a binding agent to obtain a mixture; and molding the mixture, and preserving heat for 5 hours at 160 ℃ to obtain the rotary kiln furnace lining for roasting the lithium battery anode material.
The binding agent is aluminum dihydrogen phosphate.
The molding is casting molding.
Example 3
A rotary kiln lining for roasting lithium battery anode material and a preparation method thereof. The preparation method comprises the following steps:
uniformly mixing 58wt% of fused magnesia, 34wt% of light burned magnesia, 2.7wt% of activated alumina micropowder, 3.3wt% of ferrous oxide and 2.0wt% of a bonding agent to obtain a mixture; and molding the mixture, and preserving heat for 4 hours at 170 ℃ to obtain the rotary kiln furnace lining for roasting the lithium battery anode material.
The binding agent is aluminum dihydrogen phosphate.
The molding is smearing molding.
Example 4
A rotary kiln lining for roasting lithium battery anode material and a preparation method thereof. The preparation method comprises the following steps:
uniformly mixing 63wt% of fused magnesia, 32wt% of light burned magnesia, 0.8wt% of activated alumina micropowder, 1.2wt% of ferrous oxide and 3.0wt% of a binding agent to obtain a mixture; and molding the mixture, and preserving heat for 3 hours at 180 ℃ to obtain the rotary kiln furnace lining for roasting the lithium battery anode material.
The binding agent is magnesium phosphate.
The shaping is ramming shaping.
Example 5
A rotary kiln lining for roasting lithium battery anode material and a preparation method thereof. The preparation method comprises the following steps:
uniformly mixing 67.0wt% of fused magnesia, 28.0wt% of light burned magnesia, 0.5wt% of activated alumina micropowder, 0.5wt% of ferrous oxide and 4.0wt% of a bonding agent to obtain a mixture; and molding the mixture, and preserving heat for 5 hours at 165 ℃ to obtain the rotary kiln furnace lining for roasting the lithium battery anode material.
The binding agent is aluminum dihydrogen phosphate.
The molding is casting molding.
Compared with the prior art, the specific embodiment has the following positive effects:
1. in the specific embodiment, the electric smelting magnesia, the light burned magnesia, the activated alumina micropowder and the ferrous oxide are taken as main raw materials, and are subjected to pressure/pouring/ramming/smearing forming and then are subjected to heat preservation for 3-6 hours at 150-180 ℃ to obtain a rotary kiln lining (hereinafter referred to as rotary kiln lining) for roasting the anode material of the lithium battery, and the preparation process is simple. When the lithium battery anode material is baked, as shown in fig. 1 and 2, fig. 1 is a schematic diagram of the use of the rotary kiln lining prepared in example 1; fig. 2 is a schematic cross-sectional view of fig. 1. As can be seen from fig. 1 and 2; the pellets of the lithium battery anode material to be roasted are put into the rotary kiln furnace lining prepared by the embodiment, so that the roasting can be directly carried out, the assembling and disassembling process of a sagger is omitted, and the integrated forming ensures that the roasting of the lithium battery anode material has the advantages of simplicity, time saving and high efficiency.
2. The rotary kiln lining prepared by the specific embodiment is in rolling contact with the pellets of the positive electrode material of the lithium battery, so that continuous roasting of the positive electrode material of the lithium battery is ensured, permeation and pollution of the rotary kiln lining material into the positive electrode material can be avoided to the greatest extent, the production efficiency can be greatly improved on the premise of ensuring safe production, and the roasting effect and efficiency of the positive electrode material of the lithium battery are greatly optimized, so that the rotary kiln lining is suitable for roasting of powder and pellets prepared by machine pressing/roll forming of the positive electrode material of the lithium battery. Plays a key propulsion role in relieving the industrial pressure of the energy industry.
3. The rotary kiln lining material prepared in the specific embodiment is MgO-Al 2 O 3 The refractory material has the characteristics of high corrosion resistance and high spalling resistance, and the iron-rich spinel formed in the high-temperature use process has defect vacancies and can absorb impurity ions such as impurity ions escaped from the lithium battery anode material in the high-temperature reaction; li (Li) + 、Co 2+ And Ni 3+ The requirements of frequently roasting the lithium battery anode material can be met, and the service life is long; the method can fundamentally solve the problem of performance degradation of the lithium battery caused by stripping of the furnace lining material during roasting, has less pollution to the fired product, can replace the matching of the traditional roller kiln and the sagger, and can remarkably improve the performance of the roasted lithium battery anode material.
4. The contact area between the rotary kiln lining and the anode material pellets of the lithium battery prepared by the specific embodiment is minimized, so that the physical/chemical reaction between the rotary kiln lining and the anode material pellets of the lithium battery for roasting the anode material of the lithium battery in the roasting process can be avoided to the greatest extent, and LiCO (LiCO) of byproducts of the roasting reaction can be avoided 3 Fe, feO and Fe 2 O 3 The residual results in the problem of degradation of the performance of the lithium battery, thereby improving the qualification rate and the performance of the positive electrode material of the lithium battery after roasting.
The rotary kiln lining prepared in the specific embodiment is used for detecting the lithium iron phosphate serving as a positive electrode material of a baked lithium battery, and meanwhile, the lithium iron phosphate serving as the positive electrode material of the same lithium battery baked by a commercially available sagger is subjected to comparative detection, and the results of the two are shown in the table 1.
Table 1 comparative results
| Commercially available sagger | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Residual Fe (ppm) | 520 | 245 | 378 | 147 | 130 | 97 |
| Residual FeO+Fe 2 O 3 (ppm) | 779 | 376 | 587 | 450 | 287 | 254 |
| Bulk density (g/cm) 3 ) | 0.66 | 0.67 | 0.68 | 0.69 | 0.68 | 0.69 |
The comparison result shows that the performance of the lithium iron phosphate anode material baked by the rotary kiln lining prepared by the specific embodiment is superior to that of the lithium battery anode material baked by a commercial sagger, the impurity residue rate is lower, and the loose packing density is higher. The chemical components of the commercial sagger are as follows: 60.0wt% of fused magnesia, 35.0wt% of light burned magnesia and 5.0wt% of activated alumina micropowder.
Therefore, the specific implementation mode has the characteristics of simple process, high productivity, time saving and high efficiency; the prepared rotary kiln furnace lining for roasting the lithium battery anode material has excellent erosion resistance, excellent spalling resistance and long service life, and the performance of the roasted lithium battery anode material is fundamentally improved.
Claims (6)
1. A preparation method of a rotary kiln furnace lining for roasting a lithium battery anode material is characterized by uniformly mixing 52.0-67.0 wt% of fused magnesia, 28.0-43.0 wt% of light burned magnesia, 0.5-4.5 wt% of active alumina micropowder, 0.3-3.3 wt% of ferrous oxide and 0.2-4.0 wt% of binding agent to obtain a mixture; then the mixture is molded, and the temperature is kept for 3 to 6 hours at the temperature of 150 to 180 ℃ to prepare a rotary kiln furnace lining for roasting the anode material of the lithium battery;
the particle size of the ferrous oxide is smaller than 0.045mm; the FeO content of the ferrous oxide is more than or equal to 99.1wt%;
the binding agent is one of zirconium phosphate, magnesium phosphate and aluminum dihydrogen phosphate.
2. The rotary kiln lining for roasting lithium battery anode material according to claim 1The preparation method is characterized in that the grain size of the fused magnesia is less than 3mm and more than or equal to 1mm; the fused magnesia: mgO content is more than or equal to 96.6wt%, siO 2 The content is less than or equal to 0.79wt percent, fe 2 O 3 The content is less than or equal to 0.13 weight percent.
3. The method for preparing the rotary kiln lining for roasting the lithium battery anode material, which is characterized in that the grain size of the light burned magnesia is less than 1mm and more than or equal to 0.045mm; the light burned magnesite comprises the following components: mgO content is more than or equal to 95.3wt percent, siO 2 The content is less than or equal to 0.85 weight percent, fe 2 O 3 The content is less than or equal to 0.26 weight percent.
4. The method for preparing a rotary kiln lining for roasting a lithium battery anode material according to claim 1, wherein the particle size of the activated alumina micropowder is less than 0.088mm; al of the activated alumina micropowder 2 O 3 The content is more than or equal to 98.8wt%.
5. The method for preparing a rotary kiln lining for roasting lithium battery anode materials according to claim 1, wherein the forming mode is one of pressure, pouring, ramming and smearing.
6. A rotary kiln lining for roasting lithium battery anode material, characterized in that the rotary kiln lining for roasting lithium battery anode material is prepared by the method for preparing the rotary kiln lining for roasting lithium battery anode material according to any one of claims 1-5.
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| CN108373324A (en) * | 2018-03-28 | 2018-08-07 | 广东山摩新材料科技有限公司 | A kind of lightweight saggar and preparation method thereof for anode material of lithium battery roasting |
| CN108610024A (en) * | 2018-05-07 | 2018-10-02 | 武汉科技大学 | A kind of saggar and preparation method thereof for anode material for lithium-ion batteries roasting |
| CN112279662A (en) * | 2020-11-06 | 2021-01-29 | 湘潭海泡石科技有限公司 | Sagger for magnesium aluminate spinel-cordierite calcined lithium battery positive electrode material and preparation method thereof |
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| CN108610024A (en) * | 2018-05-07 | 2018-10-02 | 武汉科技大学 | A kind of saggar and preparation method thereof for anode material for lithium-ion batteries roasting |
| CN112279662A (en) * | 2020-11-06 | 2021-01-29 | 湘潭海泡石科技有限公司 | Sagger for magnesium aluminate spinel-cordierite calcined lithium battery positive electrode material and preparation method thereof |
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