CN116639990B - Manufacturing process of composite layer graphite sagger - Google Patents
Manufacturing process of composite layer graphite sagger Download PDFInfo
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- CN116639990B CN116639990B CN202310932322.9A CN202310932322A CN116639990B CN 116639990 B CN116639990 B CN 116639990B CN 202310932322 A CN202310932322 A CN 202310932322A CN 116639990 B CN116639990 B CN 116639990B
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- sagger
- composite layer
- mixing
- layer graphite
- phenolic resin
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 23
- 239000010439 graphite Substances 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 33
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000002791 soaking Methods 0.000 claims abstract description 17
- 239000000853 adhesive Substances 0.000 claims abstract description 16
- 230000001070 adhesive effect Effects 0.000 claims abstract description 16
- 238000007598 dipping method Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 9
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 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 claims abstract description 9
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 9
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 9
- 239000011029 spinel Substances 0.000 claims abstract description 9
- 239000007774 positive electrode material Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 26
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 11
- 229910052744 lithium Inorganic materials 0.000 claims description 11
- 229920001568 phenolic resin Polymers 0.000 claims description 11
- 239000005011 phenolic resin Substances 0.000 claims description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical class OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000010405 anode material Substances 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- SXPLZNMUBFBFIA-UHFFFAOYSA-N butyl(trimethoxy)silane Chemical compound CCCC[Si](OC)(OC)OC SXPLZNMUBFBFIA-UHFFFAOYSA-N 0.000 claims description 4
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- 229910011255 B2O3 Inorganic materials 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 15
- 230000003628 erosive effect Effects 0.000 abstract description 4
- 239000011241 protective layer Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- 229910052810 boron oxide Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005470 impregnation Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 229910018068 Li 2 O Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000013065 commercial product Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- KUFFULVDNCHOFZ-UHFFFAOYSA-N 2,4-xylenol Chemical compound CC1=CC=C(O)C(C)=C1 KUFFULVDNCHOFZ-UHFFFAOYSA-N 0.000 description 1
- 229910052580 B4C Inorganic materials 0.000 description 1
- 229910010093 LiAlO Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910001038 basic metal oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 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
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- 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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- 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
- C04B41/50—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 inorganic materials
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- 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
- C04B41/85—Coating or impregnation with inorganic materials
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- 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
- F27D5/00—Supports, screens, or the like for the charge within the furnace
- F27D5/0068—Containers
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- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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- C04B2235/3427—Silicates other than clay, e.g. water glass
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Abstract
The invention discloses a process for manufacturing a composite layer graphite sagger, which belongs to the technical field of sagger production and comprises the following steps: grinding cordierite, mullite, aluminum powder, spinel and graphite powder, uniformly mixing, adding an adhesive, mixing to obtain a mixture, adding water, continuously stirring, stamping, forming, and sintering at 1350-1390 ℃ for 18-24 hours to obtain a blank; secondly, placing the green body in a vacuum drying oven for dipping treatment: vacuumizing, injecting impregnating solution, and carrying out pressure maintaining soaking and normal pressure soaking; taking out and drying at room temperature, and then putting into an oven, and drying at 110 ℃; and repeating the dipping treatment process for 2-3 times to obtain the composite layer graphite sagger. And a protective layer is formed on the surface of the green body through dipping treatment, so that the erosion resistance of the sagger is further improved in the subsequent processing and use process of the positive electrode material.
Description
Technical Field
The invention belongs to the technical field of sagger production, and particularly relates to a composite layer graphite sagger manufacturing process.
Background
The production process of the lithium battery anode material mainly comprises the steps of filling raw materials such as blended powder into a sagger, sintering the sagger at high temperature through a roller kiln, discharging the sagger containing the raw materials out of the furnace, crushing the anode material, and finally packaging the product. Wherein, the sagger discharged from the furnace is continuously filled with blended powder, and then enters a roller kiln for sintering, so that the sagger is reciprocated.
As the sagger is a carrier for the reaction of the lithium battery anode material, the sagger can be subjected to phenomena of corner falling, peeling, cracking, deformation and the like after being sintered at high temperature for tens of periods. Li with extremely strong permeability can be generated in the sintering process of the positive electrode material of the lithium battery 2 O, limited by kiln exhaust, li 2 O cannot be completely discharged during the reaction. As the sintering process of the material proceeds, the sintering temperature gradually increases, and Li is accelerated 2 O diffuses to make it enter the bottom of the sagger along the air hole to react with the material to generate Li 4 SiO 4 、β-LiAlSiO 4 And LiAlO 2 Causing erosion of the sagger. With the cyclic sintering of the sagger, the sagger is continuously eroded, so that the porosity of the sagger is increased, and Li is increased 2 The O diffusion path can pass through the bottom of the sagger to reach the contact surface with the roller rod, so that the sagger, the roller rod and Li are caused 2 The crystallization generated by the O reaction is attached to the surface of the roller and the bottom of the sagger, so that the sagger is scrapped.
Disclosure of Invention
The invention aims to provide a manufacturing process of a composite layer graphite sagger, which aims to solve the problem of poor corrosion resistance in the use process of the sagger.
The aim of the invention can be achieved by the following technical scheme:
the manufacturing process of the composite layer graphite sagger comprises the following steps:
grinding cordierite, mullite, aluminum powder, spinel and graphite powder, uniformly mixing, adding an adhesive, mixing to obtain a mixture, adding water, continuously stirring, stamping, forming, and sintering at 1350-1390 ℃ for 18-24 hours to obtain a blank;
secondly, placing the green body in a vacuum drying oven for dipping treatment: vacuumizing, injecting impregnating solution, and carrying out pressure maintaining soaking and normal pressure soaking; taking out and drying at room temperature, and then putting into an oven, and drying at 110 ℃; and repeating the dipping treatment process for 2-3 times to obtain the composite layer graphite sagger.
Further, 30-32% of cordierite, 15-16% of mullite, 15-16% of aluminum powder, 20-22% of spinel, 2-2.5% of graphite powder and the balance of adhesive in the mixture according to weight percentage.
Further, the water in the first step is added in an amount of 21-23% of the mass of the mixture.
Further, the pressure maintaining soaking time is 5-10min, and the normal pressure soaking time is 25-30min.
Further, in the second step, drying at room temperature until the weight is unchanged; and drying at 110 ℃ to constant weight.
Further, the adhesive is POSS modified phenolic resin and boric oxide according to the mass ratio of 7:3, mixing, ball milling and sieving with a 200-mesh sieve.
Further, the POSS modified phenolic resin is prepared by the following steps:
and (3) mixing and diluting the aqueous phenolic resin and deionized water in equal volume, adding the octaepoxycyclohexylethyl-cage-shaped POSS, and mixing to obtain the POSS modified phenolic resin. The dosage ratio of the aqueous phenolic resin to the octaepoxycyclohexylethyl-cage POSS is 20:1.
further, the impregnating solution is prepared by the following steps:
mixing aluminum sol and a silane coupling agent, stirring and reacting for 3 hours at the temperature of 60 ℃ to obtain pretreated aluminum sol, adding saturated boric acid solution into the pretreated aluminum sol, stirring and mixing, and concentrating under reduced pressure at the temperature of 35 ℃ until the volume is unchanged to obtain impregnating solution.
Further, the silane coupling agent is one of propyl trimethoxy silane and butyl trimethoxy silane.
Further, the dosage mass ratio of the aluminum sol to the silane coupling agent to the saturated boric acid is 1:0.02:0.1.
the invention has the beneficial effects that:
the invention provides a process for manufacturing a composite layer graphite sagger, which forms a protective layer on the surface of a green body through dipping treatment, and further improves the erosion resistance of the sagger in the subsequent processing and using process of a positive electrode material.
Impregnating solution permeates into the blank body in the impregnation process, forming a layer of protective film on the surface of the blank body after repeated impregnation treatment to obtain a sagger, and forming the protective film on the surface of the sagger and Li in the use process of the sagger 2 O will react and consume Li 2 O, thereby improving the permeation resistance of the sagger. Boric acid in the impregnation solution generates boron oxide at high temperature, which dissolves many basic metal oxides (e.g. Li 2 O) for Li that has permeated into the sagger 2 O can react with the impregnating solution penetrating into the sagger and is accompanied by volumeThe expansion, the reaction product blocks the pores, and the apparent porosity after molding is further reduced.
The adhesive is obtained by mixing POSS modified phenolic resin and boron oxide, the adhesive, cordierite, mullite, aluminum powder, spinel and graphite powder are used as mixture to prepare a blank, the POSS modified phenolic resin and the graphite powder are used as carbon sources to react with the boron oxide by a carbothermic reduction method, and high-temperature resistant substances such as boron carbide are generated to exist in a reaction matrix, so that gas holes can be blocked, pore channels are narrowed, and Li is reduced 2 O penetrates into the material, thereby improving the erosion resistance of the material. Compared with the water-based phenolic resin, the POSS modified phenolic resin in the adhesive can increase the number of hydrophilic groups, improve the dispersion effect, and meanwhile, epoxy groups can be copolymerized with hydroxymethyl groups in the phenolic resin, so that the crosslinking degree is properly improved, cracking caused by brittleness of the cured phenolic resin is improved, and the stability of a product is improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a POSS modified phenolic resin, which is prepared through the following steps:
mixing 10g of phenol, 1.2g of sodium hydroxide and 10mL of deionized water, adding 15g of formaldehyde at 60 ℃, stirring and reacting for 2 hours, heating to 80 ℃ after the reaction is finished, continuously stirring for 30 minutes, adding 5g of formaldehyde, keeping the temperature unchanged, continuously stirring and reacting for 30 minutes, adding 10mL of deionized water and 2, 4-xylenol, and continuously stirring for 30 minutes to obtain the water-based phenolic resin; and (3) mixing and diluting the aqueous phenolic resin and deionized water in equal volume, adding the octaepoxycyclohexylethyl-cage-shaped POSS, and mixing to obtain the POSS modified phenolic resin. The dosage ratio of the aqueous phenolic resin to the octaepoxycyclohexylethyl-cage POSS is 20:1.
example 2
The embodiment provides an impregnating solution prepared by the following steps:
mixing aluminum sol (commercial product with solid content of 20.67%) and propyl trimethoxy silane, stirring at 60deg.C for 3 hr to obtain pretreated aluminum sol, adding saturated boric acid solution into the pretreated aluminum sol, stirring, mixing, and concentrating under reduced pressure at 35deg.C until volume is unchanged to obtain soaking solution. The dosage mass ratio of the aluminum sol to the propyl trimethoxy silane to the saturated boric acid is 1:0.02:0.1.
example 3
The embodiment provides an impregnating solution prepared by the following steps:
mixing aluminum sol (commercial product with solid content of 20.67%) and butyl trimethoxy silane, stirring at 60 ℃ for 3 hours to obtain pretreated aluminum sol, adding saturated boric acid solution into the pretreated aluminum sol, stirring and mixing, and concentrating under reduced pressure at 35 ℃ until the volume is unchanged to obtain the impregnating solution. The dosage mass ratio of the aluminum sol to the butyl trimethoxy silane to the saturated boric acid is 1:0.02:0.1.
example 4
The manufacturing process of the composite layer graphite sagger comprises the following steps:
firstly, POSS modified phenolic resin prepared in example 1 and boron oxide are mixed according to a mass ratio of 7:3 mixing, ball milling, sieving with a 200-mesh sieve to obtain an adhesive, grinding 30% of cordierite, 15% of mullite, 15% of aluminum powder, 20% of spinel and 2% of graphite powder according to weight percentage, uniformly mixing, adding 18% of adhesive, mixing to obtain a mixture, adding water, continuously stirring, stamping and forming, and sintering at 1350-1390 ℃ for 18h to obtain a green body, wherein the addition amount of water is 21% of the mass of the mixture;
secondly, placing the green body in a vacuum drying oven for dipping treatment: vacuumizing, injecting the impregnating solution in the embodiment 3, and carrying out pressure maintaining soaking for 5min and normal pressure soaking for 30min; taking out, drying at room temperature until the weight is unchanged, then putting into an oven, and drying at 110 ℃ until the weight is constant; the dipping treatment process is repeated for 2 times to obtain the composite layer graphite sagger.
Comparative example 1
In this comparative example, the binder was replaced with the aqueous phenolic resin of example 1, as compared with example 4. The remaining raw materials and preparation process remain the same as in example 3. The apparent porosity was measured according to GB/T2997-2015 and the test results are shown in Table 1 below:
；
from the test results, the sagger porosity prepared by the POSS modified phenolic resin prepared by the invention is lower.
Example 5
The manufacturing process of the composite layer graphite sagger comprises the following steps:
firstly, POSS modified phenolic resin prepared in example 1 and boron oxide are mixed according to a mass ratio of 7:3 mixing, ball milling, sieving with a 200-mesh sieve to obtain an adhesive, grinding 31% of cordierite, 15% of mullite, 15% of aluminum powder, 21% of spinel and 2% of graphite powder according to weight percentage, uniformly mixing, adding 16% of adhesive, mixing to obtain a mixture, adding water, continuously stirring, stamping and forming, and sintering at 1350-1390 ℃ for 22 hours to obtain a green body, wherein the addition amount of water is 22% of the mass of the mixture;
secondly, placing the green body in a vacuum drying oven for dipping treatment: vacuumizing, injecting the impregnating solution prepared in the example 2, and carrying out pressure maintaining soaking for 10min and normal pressure soaking for 30min; taking out, drying at room temperature until the weight is unchanged, then putting into an oven, and drying at 110 ℃ until the weight is constant; the dipping treatment process is repeated for 3 times to obtain the composite layer graphite sagger.
Example 6
The manufacturing process of the composite layer graphite sagger comprises the following steps:
firstly, POSS modified phenolic resin prepared in example 1 and boron oxide are mixed according to a mass ratio of 7:3 mixing, ball milling, sieving with a 200-mesh sieve to obtain an adhesive, grinding 32% of cordierite, 16% of mullite, 16% of aluminum powder, 20% of spinel and 2% of graphite powder according to weight percentage, uniformly mixing, adding 14% of adhesive, mixing to obtain a mixture, adding water, continuously stirring, stamping and forming, and sintering at 1350-1390 ℃ for 24 hours to obtain a green body, wherein the addition amount of water is 23% of the mass of the mixture;
secondly, placing the green body in a vacuum drying oven for dipping treatment: vacuumizing, injecting the impregnating solution prepared in the example 3, and carrying out pressure maintaining soaking for 10min and normal pressure soaking for 25min; taking out, drying at room temperature until the weight is unchanged, then putting into an oven, and drying at 110 ℃ until the weight is constant; the dipping treatment process is repeated for 3 times to obtain the composite layer graphite sagger.
Comparative example 2
In this comparative example, compared with example 6, the impregnation liquid was changed to an alumina sol (commercially available, solid content of 20.67%), and the remaining raw materials and the preparation process were the same as in example 6.
Comparative example 3
In this comparative example, compared with comparative example 1, the impregnation liquid was changed to an alumina sol (commercially available, solid content of 20.67%), and the remaining raw materials and the preparation process were kept the same as in comparative example 1.
Examples 5 to 6 and comparative examples 2 to 3 were tested and the apparent porosity was measured according to GB/T2997-2015. When lithium cobalt oxide, a positive electrode material of a lithium battery, was synthesized at 1050 ℃, the number of cycles of a plurality of sets of saggers (the end of the cycle with the occurrence of flaking of the saggers) was recorded, and the results are shown in table 2:
；
as can be seen from Table 2, the sagger prepared by the invention has good recycling effect and better corrosion resistance.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The manufacturing process of the composite layer graphite sagger for the lithium battery anode material is characterized by comprising the following steps of:
grinding cordierite, mullite, aluminum powder, spinel and graphite powder, uniformly mixing, adding an adhesive, mixing to obtain a mixture, adding water, continuously stirring, stamping, forming, and sintering at 1350-1390 ℃ for 18-24 hours to obtain a blank; 30-32% of cordierite, 15-16% of mullite, 15-16% of aluminum powder, 20-22% of spinel, 2-2.5% of graphite powder and the balance of adhesive in the mixture according to weight percentage; the adhesive is POSS modified phenolic resin and boric oxide according to the mass ratio of 7:3, mixing, ball milling and sieving with a 200-mesh sieve to obtain the product;
secondly, mixing aluminum sol and a silane coupling agent, stirring and reacting for 3 hours at the temperature of 60 ℃ to obtain pretreated aluminum sol, adding saturated boric acid solution into the pretreated aluminum sol, stirring and mixing, and concentrating under reduced pressure at the temperature of 35 ℃ until the volume is unchanged to obtain impregnating solution; the dosage mass ratio of the aluminum sol to the silane coupling agent to the saturated boric acid is 1:0.02:0.1;
placing the green body in a vacuum drying oven for dipping treatment: vacuumizing, injecting impregnating solution, and carrying out pressure maintaining soaking and normal pressure soaking; taking out and drying at room temperature, and then putting into a baking oven for baking; and repeating the dipping treatment process for 2-3 times to obtain the composite layer graphite sagger for the lithium battery anode material.
2. The process for manufacturing the composite layer graphite sagger for the positive electrode material of the lithium battery, which is disclosed in claim 1, is characterized in that the water addition amount in the first step is 21-23% of the mass of the mixture.
3. The process for manufacturing the composite layer graphite sagger for the positive electrode material of the lithium battery, which is disclosed in claim 1, is characterized in that the pressure maintaining soaking time is 5-10min and the normal pressure soaking time is 25-30min.
4. The process for manufacturing a composite layer graphite sagger for a positive electrode material of a lithium battery according to claim 1, wherein in the second step, the composite layer graphite sagger is dried at room temperature until the weight is unchanged; the temperature is set in the oven and is 110 ℃ to be dried to constant weight.
5. The process for manufacturing a composite layer graphite sagger for a lithium battery anode material according to claim 1, wherein the POSS modified phenolic resin is prepared by the following steps:
mixing and diluting the water-based phenolic resin and deionized water in equal volume, adding octaepoxycyclohexylethyl-cage-shaped POSS, and mixing to obtain POSS modified phenolic resin; the dosage ratio of the aqueous phenolic resin to the octaepoxycyclohexylethyl-cage POSS is 20:1.
6. the process for manufacturing a composite layer graphite sagger for a lithium battery anode material according to claim 1, wherein the silane coupling agent is one of propyl trimethoxysilane and butyl trimethoxysilane.
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