CN111362672A - Preparation process of bauxite-based ceramic filler - Google Patents
Preparation process of bauxite-based ceramic filler Download PDFInfo
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- CN111362672A CN111362672A CN202010212191.3A CN202010212191A CN111362672A CN 111362672 A CN111362672 A CN 111362672A CN 202010212191 A CN202010212191 A CN 202010212191A CN 111362672 A CN111362672 A CN 111362672A
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- bauxite
- powder
- ceramic filler
- based ceramic
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- 229910001570 bauxite Inorganic materials 0.000 title claims abstract description 71
- 239000000945 filler Substances 0.000 title claims abstract description 65
- 239000000919 ceramic Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 142
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 55
- 239000010445 mica Substances 0.000 claims abstract description 53
- 238000003756 stirring Methods 0.000 claims abstract description 50
- 238000002156 mixing Methods 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000000498 ball milling 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 19
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 18
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 18
- 239000000376 reactant Substances 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 47
- 238000001354 calcination Methods 0.000 claims description 36
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 34
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 235000012239 silicon dioxide Nutrition 0.000 claims description 19
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 16
- 239000005543 nano-size silicon particle Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 13
- 238000002390 rotary evaporation Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical class [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 abstract description 23
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 239000010459 dolomite Substances 0.000 description 13
- 229910000514 dolomite Inorganic materials 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 12
- 229910000077 silane Inorganic materials 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 10
- 239000011521 glass Substances 0.000 description 10
- 239000000377 silicon dioxide Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000010881 fly ash Substances 0.000 description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 7
- 229910052681 coesite Inorganic materials 0.000 description 7
- 229910052906 cristobalite Inorganic materials 0.000 description 7
- 238000002444 silanisation Methods 0.000 description 7
- 229910052682 stishovite Inorganic materials 0.000 description 7
- 229910052905 tridymite Inorganic materials 0.000 description 7
- 238000000280 densification Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229910052627 muscovite Inorganic materials 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- 230000003113 alkalizing effect Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 229910052845 zircon Inorganic materials 0.000 description 2
- -1 zirconium ions Chemical class 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000006884 silylation reaction Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- C04B35/01—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
- C04B35/10—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 aluminium oxide
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- 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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Abstract
The invention discloses a preparation process of a bauxite-based ceramic filler, which relates to the technical field of ceramic materials and comprises the following steps of (1) obtaining a solid reactant, (2) obtaining calcined powder, (3) mixing the calcined powder, mica powder and η -Al2O3Mixing the powder and bauxite, adding the mixture into absolute ethyl alcohol, stirring, performing ball milling treatment, pouring the mixture into a mold, and drying to obtain a filler blank; (4) adding the ball-milled material into a kiln for vacuum sintering treatment to obtain a ceramic filler; the ceramic filler prepared by the invention has higher specific surface area and compressive strength, greatly improves the comprehensive performance of the ceramic filler, and can obviously improve the ceramic fillerThe application range of the material.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a preparation process of a bauxite-based ceramic filler.
Background
The ceramic material has the advantages of large flux, low pressure drop, high mass transfer efficiency and the like, is widely applied to the industries of chemical industry, metallurgy, coal gas, oxygen generation and the like, and is a novel efficient filler with wider application. The ceramic fillers used in the prior art mainly include wollastonite, mica, glass frit, talc, bauxite, metal oxides, metal hydroxides, montmorillonite and the like.
The invention relates to a corrugated ceramic filler and a preparation method thereof in the prior art, wherein the anti-seismic temperature-resistant corrugated ceramic filler comprises the following components in percentage by weight: 50-65% of aluminum oxide, 10-15% of silicon dioxide, 10-20% of kaolin, 3-5% of zircon sand, 5-8% of calcium carbonate, 0.05-0.2% of yttrium oxide, 1.5-6.5% of zirconium oxide, 5-10% of epoxy resin and 0.1-0.3% of sodium carboxymethylcellulose. The preparation method comprises the steps of ball milling, screening, filter pressing, vacuum pugging, slicing, extruding, bonding, forming, dehydrating and calcining to obtain the finished product. The invention selects reasonable components, proportion and preparation method to improve the high temperature resistance and corrosion resistance of the regular corrugated ceramic filler, enhance the compressive strength and earthquake resistance and prolong the service life, however, the ceramic filler prepared by the combination of pure aluminum oxide, silicon dioxide, kaolin, zircon sand, calcium carbonate, yttrium oxide and zirconium oxide has the problems of small specific surface area, low compressive strength, poor earthquake resistance, easy crushing, poor high temperature resistance and corrosion resistance and short service life.
Disclosure of Invention
The invention aims to provide a preparation process of bauxite-based ceramic filler, which aims to overcome the defects in the prior art.
The technical scheme adopted by the invention is as follows:
a preparation process of bauxite-based ceramic filler comprises the following steps:
(1) grinding zirconium oxide and yttrium oxide into powder, mixing, adding the powder into a hydrochloric acid solution, stirring to react until the powder is dissolved to obtain a mixed reaction solution, adding nano silicon dioxide into the mixed reaction solution, stirring uniformly, adding saturated ammonia water under the stirring condition, stirring to react until the reaction solution is neutral, standing for 1 hour, and performing rotary evaporation drying to obtain a solid reactant;
(2) adding the solid reactant into a calcining furnace for calcining, naturally cooling to room temperature, and then grinding to obtain calcined powder;
(3) mixing the calcined powder, mica powder and η -Al2O3Mixing the powder and bauxite, adding the mixture into absolute ethyl alcohol, uniformly stirring, performing ball milling treatment, pouring the mixture into a mold, and drying to obtain a filler blank;
before mixing the components, performing silanization treatment on mica powder to obtain silanized mica powder, wherein the preparation method of the silanized mica powder comprises the following steps:
preparing a silane gamma-APT solution, adding the silane gamma-APT into an ethanol solution with the mass fraction of 12.5%, uniformly stirring, and then mixing mica powder and the silane gamma-APT solution according to the ratio of 150 gg: uniformly mixing 400mL of the mixture in proportion, heating to 88 ℃, stirring for reaction for 1 hour, filtering, and drying at 50 ℃ to obtain the needed silanized mica powder;
alkalizing bauxite to obtain alkaline bauxite;
the preparation method of the alkaline bauxite comprises the following steps: the bauxite is subjected to heat preservation treatment at the temperature of 420 ℃ for 40min, then is cooled to room temperature by water, and then is added into a sodium hydroxide solution with the mass fraction of 6%, then is added with fly ash, the mass ratio of the fly ash to the bauxite is 1:10, the mixture is heated to 65 ℃, is stirred and reacts for 40min, stands for 1 h, and then is subjected to rotary evaporation and drying to constant weight;
(4) and adding the ball milling material into a kiln for vacuum sintering treatment to obtain the ceramic filler.
The mass ratio of the zirconium oxide to the yttrium oxide is 30: 1-1.5;
the mixing mass ratio of the zirconium oxide to the hydrochloric acid is 50 g: 350 mL.
The concentration of the hydrochloric acid solution is 0.25 mol/L.
The mass ratio of the zirconium oxide to the nano silicon dioxide is 10: 1.
The calcination temperature in the calciner is 890 ℃.
The weight part ratio of the calcined powder to the mica powder to the η -Al2O3 powder to the bauxite is 5-8:16-20:8-10: 35-39.
The mass ratio of the calcined powder to the absolute ethyl alcohol is 1: 3.
The ball milling treatment time is 1-1.5 hours.
The vacuum sintering temperature is 1350-.
The vacuum degree of vacuum sintering is 0.08-0.09 MPa.
Has the advantages that: the bauxite-based ceramic filler prepared by the process has higher specific surface area and compressive strength, greatly improves the comprehensive performance of the ceramic filler, and can remarkably improve the application range of the ceramic filler2O—Al2O3—SiO2The glass phase can be cooperated with bauxite to promote sintering, the sintering densification of the ceramic filler is improved, the bonding property between mica powder and other components can be promoted at low temperature through silanization treatment of the mica powder, the surface can be graphitized to a certain degree at high temperature, the porosity can be reduced, and meanwhile, through introducing dolomite powder, MgO in the dolomite powder can be mixed with CaO-K2O—Al2O3—SiO2The glass phase is fused, and the dolomite powder, the mica powder, the bauxite and the fly ash are tightly welded together through the generated glass phase, so that the ceramic densification is promoted, the porosity is reduced, the water absorption is reduced, and the heat temperature performance is improved.
Detailed Description
A preparation process of bauxite-based ceramic filler comprises the following steps:
(1) grinding zirconium oxide and yttrium oxide into powder, mixing, adding the powder into a hydrochloric acid solution, stirring to react until the powder is dissolved to obtain a mixed reaction solution, adding nano silicon dioxide into the mixed reaction solution, stirring uniformly, adding saturated ammonia water under the stirring condition, stirring to react until the reaction solution is neutral, standing for 1 hour, and performing rotary evaporation drying to obtain a solid reactant;
(2) adding the solid reactant into a calcining furnace for calcining, naturally cooling to room temperature, and then grinding to obtain calcined powder;
(3) mixing the calcined powder, mica powder and η -Al2O3Mixing the powder and bauxite, adding the mixture into absolute ethyl alcohol, uniformly stirring, performing ball milling treatment, pouring the mixture into a mold, and drying to obtain a filler blank;
wherein, the mica powder adopts muscovite powder:
muscovite is a layered silicate mineral, belonging to the mica group and muscovite subfamily, which can be formed under different geological conditions, and is the mineral with the widest distribution in the mica group. The muscovite powder generally exists in a sheet shape, and the muscovite mainly contains elements such as silicon, potassium, sodium, aluminum and the like, K2O content 9.12%, Al2O328.13% of SiO2The content was 54.07%.
Before mixing the components, performing silanization treatment on mica powder to obtain silanized mica powder, wherein the preparation method of the silanized mica powder comprises the following steps:
preparing a silane gamma-APT solution, adding the silane gamma-APT into an ethanol solution with the mass fraction of 12.5%, uniformly stirring, and then mixing mica powder and the silane gamma-APT solution according to the ratio of 150 gg: uniformly mixing 400mL of the mixture in proportion, heating to 88 ℃, stirring for reaction for 1 hour, filtering, and drying at 50 ℃ to obtain the needed silanized mica powder;
alkalizing bauxite to obtain alkaline bauxite;
the preparation method of the alkaline bauxite comprises the following steps: the bauxite is subjected to heat preservation treatment at the temperature of 420 ℃ for 40min, cooling with water to room temperature, adding the mixture into a sodium hydroxide solution with the mass fraction of 6%, adding fly ash, wherein the mass ratio of the fly ash to the bauxite is 1:10, heating to 65 ℃, stirring for reacting for 40min, standing for 1 hour, and then performing rotary evaporation and drying to constant weight; the heat stability of the bauxite ceramic filler can be improved in a small range by further silanizing the mica powder, and the water absorption rate is further reduced, and the heat stability of the bauxite ceramic filler can be better improved by treating the bauxite2O—Al2O3—SiO2The glass phase can be cooperated with bauxite to promote sintering, the sintering densification of the ceramic filler is improved, the bonding property between mica powder and other components can be promoted at low temperature through silanization treatment of the mica powder, the surface can be graphitized to a certain degree at high temperature, the porosity can be reduced, and meanwhile, through introducing dolomite powder, MgO in the dolomite powder can be mixed with CaO-K2O—Al2O3—SiO2The glass phase is fused, and the dolomite powder and the mica powder are tightly welded with the bauxite and the fly ash through the generated glass phase, so that the ceramic densification is promoted, the porosity is reduced, the water absorption is reduced, and the heat temperature performance is improved;
bauxite comprises the following main chemical components:
silicon dioxide: 6.87 percent;
titanium dioxide: 3.32 percent;
alumina: 87.05 percent;
iron oxide: 1.42 percent;
manganese oxide: 0.01 percent;
magnesium oxide: 0.13 percent;
calcium oxide: 0.70 percent;
sodium oxide: 0.006%;
potassium oxide: 0.13 percent;
phosphorus pentoxide: 0.18 percent;
(4) the ball-milling material is added into a kiln to be subjected to vacuum sintering treatment to obtain the ceramic filler, the calcined powder prepared by the invention can promote large-angle crystal boundaries to be eliminated through crystal boundary migration in the sintering process, and particularly can promote a part of crystal grains to rotate and convert into small-angle crystal boundaries under the combined action of zirconium ions and yttrium ions, so that the crystal grains are promoted to be agglomerated.
The mass ratio of the zirconium oxide to the yttrium oxide is 30: 1-1.5;
the mixing mass ratio of the zirconium oxide to the hydrochloric acid is 50 g: 350 mL.
The concentration of the hydrochloric acid solution is 0.25 mol/L.
The mass ratio of the zirconium oxide to the nano silicon dioxide is 10: 1.
The calcination temperature in the calciner is 890 ℃.
The calcined powder, mica powder and η -Al2O3The weight portion ratio of the powder to the bauxite is 5-8:16-20:8-10: 35-39.
The mass ratio of the calcined powder to the absolute ethyl alcohol is 1: 3.
The ball milling treatment time is 1-1.5 hours.
The vacuum sintering temperature is 1350-.
The vacuum degree of vacuum sintering is 0.08-0.09 MPa.
The following will clearly and completely describe the technical solutions of the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation process of bauxite-based ceramic filler comprises the following steps:
(1) grinding zirconium oxide and yttrium oxide into powder, mixing, adding the powder into a hydrochloric acid solution, stirring to react until the powder is dissolved to obtain a mixed reaction solution, adding nano silicon dioxide into the mixed reaction solution, stirring uniformly, adding saturated ammonia water under the stirring condition, stirring to react until the reaction solution is neutral, standing for 1 hour, and performing rotary evaporation drying to obtain a solid reactant, wherein the mass ratio of the zirconium oxide to the yttrium oxide is 30: 1; the mixing mass ratio of the zirconium oxide to the hydrochloric acid is 50 g: 350 mL; the concentration of the hydrochloric acid solution is 0.25 mol/L; the mass ratio of the zirconium oxide to the nano silicon dioxide is 10: 1;
(2) adding the solid reactant into a calcining furnace for calcining, naturally cooling to room temperature, and then grinding to obtain calcined powder, wherein the calcining temperature in the calcining furnace is 890 ℃;
(3) mixing the calcined powder, mica powder and η -Al2O3Mixing the powder and bauxite, adding the mixture into absolute ethyl alcohol, uniformly stirring, performing ball milling treatment, pouring the mixture into a mold, drying to obtain a filler blank, calcining the powder, mica powder and η -Al2O3The weight ratio of the powder to the bauxite is 5:16:8:35, the mass ratio of the calcined powder to the absolute ethyl alcohol is 1:3, and the ball milling treatment time is 1 hour;
(4) and adding the ball-milled material into a kiln for vacuum sintering treatment to obtain the ceramic filler, wherein the vacuum sintering temperature is 1350 ℃, and the vacuum sintering degree is 0.08 MPa.
Example 2
A preparation process of bauxite-based ceramic filler comprises the following steps:
(1) grinding zirconium oxide and yttrium oxide into powder, mixing, adding the powder into a hydrochloric acid solution, stirring to react until the powder is dissolved to obtain a mixed reaction solution, adding nano silicon dioxide into the mixed reaction solution, stirring uniformly, adding saturated ammonia water under the stirring condition, stirring to react until the reaction solution is neutral, standing for 1 hour, and performing rotary evaporation drying to obtain a solid reactant, wherein the mass ratio of the zirconium oxide to the yttrium oxide is 30: 1.5; the mixing mass ratio of the zirconium oxide to the hydrochloric acid is 50 g: 350 mL; the concentration of the hydrochloric acid solution is 0.25 mol/L; the mass ratio of the zirconium oxide to the nano silicon dioxide is 10: 1;
(2) adding the solid reactant into a calcining furnace for calcining, naturally cooling to room temperature, and then grinding to obtain calcined powder, wherein the calcining temperature in the calcining furnace is 890 ℃;
(3) mixing the calcined powder, mica powder and η -Al2O3Mixing the powder and bauxite, adding the mixture into absolute ethyl alcohol, uniformly stirring, performing ball milling treatment, pouring the mixture into a mold, drying to obtain a filler blank, calcining the powder, mica powder and η -Al2O3The weight ratio of the powder to the bauxite is 8:20:10:39, the mass ratio of the calcined powder to the absolute ethyl alcohol is 1:3, and the ball milling treatment time is 1.5 hours;
(4) and adding the ball-milled material into a kiln for vacuum sintering treatment to obtain the ceramic filler, wherein the vacuum sintering temperature is 1400 ℃, and the vacuum sintering degree is 0.09 MPa.
Example 3
A preparation process of bauxite-based ceramic filler comprises the following steps:
(1) grinding zirconium oxide and yttrium oxide into powder, mixing, adding the powder into a hydrochloric acid solution, stirring to react until the powder is dissolved to obtain a mixed reaction solution, adding nano silicon dioxide into the mixed reaction solution, stirring uniformly, adding saturated ammonia water under the stirring condition, stirring to react until the reaction solution is neutral, standing for 1 hour, and performing rotary evaporation drying to obtain a solid reactant, wherein the mass ratio of the zirconium oxide to the yttrium oxide is 30: 1.2; the mixing mass ratio of the zirconium oxide to the hydrochloric acid is 50 g: 350 mL; the concentration of the hydrochloric acid solution is 0.25 mol/L; the mass ratio of the zirconium oxide to the nano silicon dioxide is 10: 1;
(2) adding the solid reactant into a calcining furnace for calcining, naturally cooling to room temperature, and then grinding to obtain calcined powder, wherein the calcining temperature in the calcining furnace is 890 ℃;
(3) mixing the calcined powder, mica powder and η -Al2O3Mixing the powder and bauxite, adding the mixture into absolute ethyl alcohol, uniformly stirring, performing ball milling treatment, pouring the mixture into a mold, performing drying treatment to obtain a filler blank, calcining the powder and mica powder、η-Al2O3The weight ratio of the powder to the bauxite is 7:17:9:38, the mass ratio of the calcined powder to the absolute ethyl alcohol is 1:3, and the ball milling treatment time is 1.2 hours;
(4) and adding the ball-milled material into a kiln for vacuum sintering treatment to obtain the ceramic filler, wherein the vacuum sintering temperature is 1380 ℃, and the vacuum sintering degree is 0.082 MPa.
And (3) detecting thermal stability and water absorption:
thermal stability (No damage for several times of normal temperature-500 ℃ cycle)
TABLE 1
Control group: application No. 201210405305.1, a corrugated ceramic packing and a method of making the same;
it can be seen from table 1 that the thermal stability of the bauxite-based ceramic filler prepared by the process of the present invention is greatly improved, and at the same time, the water absorption is reduced in a small range.
Example 4
A preparation process of bauxite-based ceramic filler comprises the following steps:
(1) grinding zirconium oxide and yttrium oxide into powder, mixing, adding the powder into a hydrochloric acid solution, stirring to react until the powder is dissolved to obtain a mixed reaction solution, adding nano silicon dioxide into the mixed reaction solution, stirring uniformly, adding saturated ammonia water under the stirring condition, stirring to react until the reaction solution is neutral, standing for 1 hour, and performing rotary evaporation drying to obtain a solid reactant, wherein the mass ratio of the zirconium oxide to the yttrium oxide is 30: 1.2; the mixing mass ratio of the zirconium oxide to the hydrochloric acid is 50 g: 350 mL; the concentration of the hydrochloric acid solution is 0.25 mol/L; the mass ratio of the zirconium oxide to the nano silicon dioxide is 10: 1;
(2) adding the solid reactant into a calcining furnace for calcining, naturally cooling to room temperature, and then grinding to obtain calcined powder, wherein the calcining temperature in the calcining furnace is 890 ℃;
(3) subjecting the calcination toPowder, mica powder, η -Al2O3Mixing the powder and bauxite, adding the mixture into absolute ethyl alcohol, uniformly stirring, performing ball milling treatment, pouring the mixture into a mold, drying to obtain a filler blank, calcining the powder, mica powder and η -Al2O3The weight ratio of the powder to the bauxite is 7:17:9:38, the mass ratio of the calcined powder to the absolute ethyl alcohol is 1:3, and the ball milling treatment time is 1.2 hours;
before mixing the components, performing silanization treatment on mica powder to obtain silanized mica powder, wherein the preparation method of the silanized mica powder comprises the following steps:
preparing a silane gamma-APT solution, adding the silane gamma-APT into an ethanol solution with the mass fraction of 12.5%, uniformly stirring, and then mixing mica powder and the silane gamma-APT solution according to the ratio of 150 gg: uniformly mixing 400mL of the mixture in a ratio, adding dolomite powder, wherein the mass ratio of the dolomite powder to the mica powder is 1:5, heating to 88 ℃, stirring for reaction for 1 hour, filtering, and drying at 50 ℃ to obtain the needed silanized mica powder;
(4) and adding the ball-milled material into a kiln for vacuum sintering treatment to obtain the ceramic filler, wherein the vacuum sintering temperature is 1380 ℃, and the vacuum sintering degree is 0.082 MPa.
And (3) detecting thermal stability and water absorption:
thermal stability (No damage for many times of normal temperature-550 ℃ cycle)
TABLE 2
From table 2, it can be seen that the thermal stability of the bauxite-based ceramic filler prepared by the process of the present invention is greatly improved, and meanwhile, the thermal stability of the bauxite-based ceramic filler can be improved to a small extent by further silylation treatment of the mica powder, and the water absorption rate is further reduced.
Example 5
A preparation process of bauxite-based ceramic filler comprises the following steps:
(1) grinding zirconium oxide and yttrium oxide into powder, mixing, adding the powder into a hydrochloric acid solution, stirring to react until the powder is dissolved to obtain a mixed reaction solution, adding nano silicon dioxide into the mixed reaction solution, stirring uniformly, adding saturated ammonia water under the stirring condition, stirring to react until the reaction solution is neutral, standing for 1 hour, and performing rotary evaporation drying to obtain a solid reactant, wherein the mass ratio of the zirconium oxide to the yttrium oxide is 30: 1.2; the mixing mass ratio of the zirconium oxide to the hydrochloric acid is 50 g: 350 mL; the concentration of the hydrochloric acid solution is 0.25 mol/L; the mass ratio of the zirconium oxide to the nano silicon dioxide is 10: 1;
(2) adding the solid reactant into a calcining furnace for calcining, naturally cooling to room temperature, and then grinding to obtain calcined powder, wherein the calcining temperature in the calcining furnace is 890 ℃;
(3) mixing the calcined powder, mica powder and η -Al2O3Mixing the powder and bauxite, adding the mixture into absolute ethyl alcohol, uniformly stirring, performing ball milling treatment, pouring the mixture into a mold, drying to obtain a filler blank, calcining the powder, mica powder and η -Al2O3The weight ratio of the powder to the bauxite is 7:17:9:38, the mass ratio of the calcined powder to the absolute ethyl alcohol is 1:3, and the ball milling treatment time is 1.2 hours;
before mixing the components, performing silanization treatment on mica powder to obtain silanized mica powder, wherein the preparation method of the silanized mica powder comprises the following steps:
preparing a silane gamma-APT solution, adding the silane gamma-APT into an ethanol solution with the mass fraction of 12.5%, uniformly stirring, and then mixing mica powder and the silane gamma-APT solution according to the ratio of 150 gg: uniformly mixing 400mL of the mixture in a ratio, adding dolomite powder, wherein the mass ratio of the dolomite powder to the mica powder is 1:5, heating to 88 ℃, stirring for reaction for 1 hour, filtering, and drying at 50 ℃ to obtain the needed silanized mica powder;
alkalizing bauxite to obtain alkaline bauxite;
the preparation method of the alkaline bauxite comprises the following steps: the bauxite is subjected to heat preservation treatment at the temperature of 420 ℃ for 40min, then is cooled to room temperature by water, and then is added into a sodium hydroxide solution with the mass fraction of 6%, then is added with fly ash, the mass ratio of the fly ash to the bauxite is 1:10, the mixture is heated to 65 ℃, is stirred and reacts for 40min, stands for 1 h, and then is subjected to rotary evaporation and drying to constant weight;
(4) and adding the ball-milled material into a kiln for vacuum sintering treatment to obtain the ceramic filler, wherein the vacuum sintering temperature is 1380 ℃, and the vacuum sintering degree is 0.082 MPa.
And (3) detecting thermal stability and water absorption:
thermal stability (No damage for many times of normal temperature-550 ℃ cycle)
TABLE 3
It can be seen from table 3 that the thermal stability of the bauxite-based ceramic filler prepared by the process of the present invention is greatly improved, and meanwhile, the thermal stability of the bauxite ceramic filler can be improved to a small extent by further silanizing the mica powder, and the water absorption is further reduced, and the thermal stability of the bauxite ceramic filler can be improved better by treating the bauxite2O—Al2O3—SiO2The glass phase can be cooperated with bauxite to promote sintering, the sintering densification of the ceramic filler is improved, the bonding property between mica powder and other components can be promoted at low temperature through silanization treatment of the mica powder, the surface can be graphitized to a certain degree at high temperature, the porosity can be reduced, and meanwhile, through introducing dolomite powder, MgO in the dolomite powder can be mixed with CaO-K2O—Al2O3—SiO2The glass phase is fused, and the dolomite powder, the mica powder, the bauxite and the fly ash are tightly welded together through the generated glass phase, so that the ceramic densification is promoted, the porosity is reduced, the water absorption is reduced, and the heat temperature performance is improved.
The specific surface area (BET method) and the compressive strength (GB-T4740-:
TABLE 4
Control group: application No. 201210405305.1, a corrugated ceramic packing and a method of making the same;
as can be seen from Table 4, the ceramic filler prepared by the method has higher specific surface area and compressive strength, greatly improves the comprehensive performance of the ceramic filler, and can remarkably improve the application range of the ceramic filler.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the present invention is not limited to the illustrated embodiments, and all the modifications and equivalents of the embodiments may be made without departing from the spirit of the present invention.
Claims (10)
1. A preparation process of bauxite-based ceramic filler is characterized by comprising the following steps: the method comprises the following steps:
(1) grinding zirconium oxide and yttrium oxide into powder, mixing, adding the powder into a hydrochloric acid solution, stirring to react until the powder is dissolved to obtain a mixed reaction solution, adding nano silicon dioxide into the mixed reaction solution, stirring uniformly, adding saturated ammonia water under the stirring condition, stirring to react until the reaction solution is neutral, standing for 1 hour, and performing rotary evaporation drying to obtain a solid reactant;
(2) adding the solid reactant into a calcining furnace for calcining, naturally cooling to room temperature, and then grinding to obtain calcined powder;
(3) mixing the calcined powder, mica powder, η -Al2O3 powder and bauxite, adding into absolute ethyl alcohol, uniformly stirring, performing ball milling treatment, pouring into a mold, and drying to obtain a filler blank;
(4) and adding the ball milling material into a kiln for vacuum sintering treatment to obtain the ceramic filler.
2. The process of claim 1, wherein the bauxite-based ceramic filler is prepared by: the mass ratio of the zirconium oxide to the yttrium oxide is 30: 1-1.5;
the mixing mass ratio of the zirconium oxide to the hydrochloric acid is 50 g: 350 mL.
3. The process according to claim 1 or 2, wherein the bauxite-based ceramic filler is prepared by: the concentration of the hydrochloric acid solution is 0.25 mol/L.
4. The process of claim 1, wherein the bauxite-based ceramic filler is prepared by: the mass ratio of the zirconium oxide to the nano silicon dioxide is 10: 1.
5. The process of claim 1, wherein the bauxite-based ceramic filler is prepared by: the calcination temperature in the calciner is 890 ℃.
6. The process for preparing bauxite-based ceramic filler according to claim 1, wherein the weight ratio of the calcined powder, the mica powder, the η -Al2O3 powder and the bauxite is 5-8:16-20:8-10: 35-39.
7. The process of claim 1, wherein the bauxite-based ceramic filler is prepared by: the mass ratio of the calcined powder to the absolute ethyl alcohol is 1: 3.
8. The process of claim 1, wherein the bauxite-based ceramic filler is prepared by: the ball milling treatment time is 1-1.5 hours.
9. The process of claim 1, wherein the bauxite-based ceramic filler is prepared by: the vacuum sintering temperature is 1350-.
10. The process according to claim 1 or 9, wherein the bauxite-based ceramic filler is prepared by: the vacuum degree of vacuum sintering is 0.08-0.09 MPa.
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| CN112479686A (en) * | 2020-11-30 | 2021-03-12 | 江苏明江机械制造有限公司 | Hard zirconium heat-insulating material and preparation method thereof |
| CN116731458A (en) * | 2023-08-16 | 2023-09-12 | 山东森荣新材料股份有限公司 | Polytetrafluoroethylene sealing gasket and preparation method thereof |
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2020
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112479686A (en) * | 2020-11-30 | 2021-03-12 | 江苏明江机械制造有限公司 | Hard zirconium heat-insulating material and preparation method thereof |
| CN116731458A (en) * | 2023-08-16 | 2023-09-12 | 山东森荣新材料股份有限公司 | Polytetrafluoroethylene sealing gasket and preparation method thereof |
| CN116731458B (en) * | 2023-08-16 | 2023-10-24 | 山东森荣新材料股份有限公司 | Polytetrafluoroethylene sealing gasket and preparation method thereof |
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