CN117466658B - Corrosion-resistant mullite sagger and production process thereof - Google Patents
Corrosion-resistant mullite sagger and production process thereof Download PDFInfo
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- CN117466658B CN117466658B CN202311829381.XA CN202311829381A CN117466658B CN 117466658 B CN117466658 B CN 117466658B CN 202311829381 A CN202311829381 A CN 202311829381A CN 117466658 B CN117466658 B CN 117466658B
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- deionized water
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- sagger
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- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 58
- 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 title claims abstract description 54
- 230000007797 corrosion Effects 0.000 title claims abstract description 27
- 238000005260 corrosion Methods 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 62
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 62
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000945 filler Substances 0.000 claims abstract description 22
- 239000003822 epoxy resin Substances 0.000 claims abstract description 21
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 238000000576 coating method Methods 0.000 claims abstract description 18
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 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 10
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 8
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 8
- 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 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004375 Dextrin Substances 0.000 claims abstract description 7
- 229920001353 Dextrin Polymers 0.000 claims abstract description 7
- 235000019425 dextrin Nutrition 0.000 claims abstract description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 104
- 238000002156 mixing Methods 0.000 claims description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000000178 monomer Substances 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 30
- 239000000706 filtrate Substances 0.000 claims description 25
- 238000001914 filtration Methods 0.000 claims description 25
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 22
- BBJIPMIXTXKYLZ-UHFFFAOYSA-N isoglutamic acid Chemical compound OC(=O)CC(N)CC(O)=O BBJIPMIXTXKYLZ-UHFFFAOYSA-N 0.000 claims description 22
- -1 polysiloxane Polymers 0.000 claims description 22
- 229920001296 polysiloxane Polymers 0.000 claims description 22
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 22
- 239000003607 modifier Substances 0.000 claims description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 20
- HASCQPSFPAKVEK-UHFFFAOYSA-N dimethyl(phenyl)phosphine Chemical compound CP(C)C1=CC=CC=C1 HASCQPSFPAKVEK-UHFFFAOYSA-N 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 20
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 17
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 16
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 16
- 239000012954 diazonium Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical compound [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 claims description 16
- OSXYHAQZDCICNX-UHFFFAOYSA-N dichloro(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](Cl)(Cl)C1=CC=CC=C1 OSXYHAQZDCICNX-UHFFFAOYSA-N 0.000 claims description 16
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 16
- 230000003014 reinforcing effect Effects 0.000 claims description 16
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 15
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 15
- 239000004317 sodium nitrate Substances 0.000 claims description 15
- 235000010344 sodium nitrate Nutrition 0.000 claims description 15
- CNRYJJXBFLHSJP-UHFFFAOYSA-N 3-pyrrol-1-ylpropan-1-amine Chemical compound NCCCN1C=CC=C1 CNRYJJXBFLHSJP-UHFFFAOYSA-N 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- 229910052717 sulfur Inorganic materials 0.000 claims description 12
- 239000011593 sulfur Substances 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 229940048181 sodium sulfide nonahydrate Drugs 0.000 claims description 11
- WMDLZMCDBSJMTM-UHFFFAOYSA-M sodium;sulfanide;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[SH-] WMDLZMCDBSJMTM-UHFFFAOYSA-M 0.000 claims description 11
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 10
- UUZYBYIOAZTMGC-UHFFFAOYSA-M benzyl(trimethyl)azanium;bromide Chemical compound [Br-].C[N+](C)(C)CC1=CC=CC=C1 UUZYBYIOAZTMGC-UHFFFAOYSA-M 0.000 claims description 10
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 10
- 239000012362 glacial acetic acid Substances 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- DOKHEARVIDLSFF-UHFFFAOYSA-N prop-1-en-1-ol Chemical compound CC=CO DOKHEARVIDLSFF-UHFFFAOYSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims 1
- 230000032683 aging Effects 0.000 claims 1
- 238000001354 calcination Methods 0.000 claims 1
- 238000009740 moulding (composite fabrication) Methods 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 230000004888 barrier function Effects 0.000 abstract 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 abstract 2
- 229910001947 lithium oxide Inorganic materials 0.000 abstract 2
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 abstract 1
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- 239000003973 paint Substances 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 125000003396 thiol group Chemical group [H]S* 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- 229910003900 Li(Ni0.5Co0.2Mn0.3)O2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HYHCSLBZRBJJCH-UHFFFAOYSA-N sodium polysulfide Chemical compound [Na+].S HYHCSLBZRBJJCH-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
-
- 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
- C04B35/16—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
- C04B35/185—Mullite 3Al2O3-2SiO2
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—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
- C04B41/5001—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 with carbon or carbonisable 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
-
- 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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- 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- 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
- C04B2235/34—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
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
- C04B2235/3445—Magnesium silicates, e.g. forsterite
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- 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
- C04B2235/34—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
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a corrosion-resistant mullite sagger and a production process thereof, wherein the mullite sagger comprises the following raw materials in parts by weight: 30-40 parts of modified filler, 60-70 parts of cordierite, 25-30 parts of kaolin, 10-15 parts of alumina, 30-35 parts of deionized water and 5-10 parts of yellow dextrin are uniformly mixed, the raw materials are sealed, aged, pressed, formed and dried, and calcined at high temperature to prepare a pretreatment sagger, the surface of the pretreatment sagger is coated with a composite coating and dried, the main chain of modified epoxy resin in the composite coating contains an organosilicon structure, and the main chain is of a hyperbranched structure, so that the formed coating has better compactness and higher corrosion resistance, the modified graphene and modified epoxy resin molecules are matched through hydrolytic polymerization of siloxane groups, and the graphene has good lithium oxide corrosion barrier property and is matched with the modified epoxy resin molecules, so that the barrier to lithium oxide can be further improved, and the corrosion resistance of the sagger is further improved.
Description
Technical Field
The invention relates to the technical field of mullite sagger preparation, in particular to a corrosion-resistant mullite sagger and a production process thereof.
Background
With the acceleration of economic globalization pace, the demand of traditional energy is increasing, and the problems of resource shortage and environmental problems are also increasing. The new energy sources of green, low-carbon and sustainable development are not slowly found, the lithium ion power battery is used as the heart of a new energy automobile, the lithium ion power battery has the unique advantages of high energy density, long endurance time, good circularity, stable performance and the like, the application range is expanded from important fields of aviation, national defense, transportation, medical treatment and the like to mass life, the sagger is used as a common kiln furniture and is widely applied to the fields of bearing lithium ion battery materials, electronic components, magnetic materials, ceramic products and the like, the current sagger materials are mainly divided into oxide materials and non-oxide materials, the common composite sagger materials comprise Si3N4-SiC, mullite-corundum, aluminum titanate-mullite, silicon carbide-mullite and cordierite-mullite, and the cordierite-mullite is studied and used most widely.
Disclosure of Invention
The invention aims to provide a corrosion-resistant mullite sagger and a production process thereof, which solve the problem that the mullite sagger is easy to corrode and damage at the present stage.
The aim of the invention can be achieved by the following technical scheme:
the production process of the corrosion-resistant mullite sagger specifically comprises the following steps:
weighing the following raw materials in parts by weight: 30-40 parts of modified filler, 60-70 parts of cordierite, 25-30 parts of kaolin, 10-15 parts of alumina, 30-35 parts of deionized water and 5-10 parts of yellow dextrin are uniformly mixed, then sealed and aged for 24 hours, pressed, molded and dried under the condition of 150-160MPa, then insulated for 25-30 minutes under the condition of 225-250 ℃, heated to 550-600 ℃, insulated for 2-3 hours, heated to 1400-1420 ℃, insulated for 2-3 hours, and finally the pretreated sagger is prepared, the surface of the pretreated sagger is coated with composite paint, and the corrosion-resistant mullite sagger is prepared by drying.
Further, the composite coating is prepared by the following steps:
step A1: mixing diphenyl dichlorosilane and deionized water, stirring for 10-15min at the rotation speed of 200-300r/min and the temperature of 60-70 ℃, adding concentrated sulfuric acid and 1, 3-tetramethyl disiloxane, reacting for 4-6h, regulating pH to be neutral to obtain hydrogen-terminated polysiloxane, uniformly mixing pentaerythritol, acrylic acid, p-toluenesulfonic acid and DMF, and reacting for 6-8h at the rotation speed of 150-200r/min and the temperature of 110-120 ℃ to obtain a reinforced monomer;
step A2: uniformly mixing hydrogen-terminated polysiloxane, a reinforcing monomer and DMF (dimethyl formamide), stirring and adding chloroplatinic acid at the rotating speed of 150-200r/min and the temperature of 50-60 ℃, reacting for 10-15h, adding propenol, continuously reacting for 8-10h to obtain a modified monomer, uniformly mixing the modified monomer, epichlorohydrin, benzyl trimethyl ammonium bromide and DMF, stirring and adding sodium hydroxide at the rotating speed of 150-200r/min and the temperature of 30-40 ℃ for reacting for 4-6h to obtain modified epoxy resin;
step A3: dispersing graphene oxide in ethanol, adding KH570 and deionized water, reacting for 2-3h at the rotation speed of 200-300r/min and the temperature of 50-60 ℃, filtering to remove filtrate, dispersing a substrate in DMF, adding KH580 and dimethylphenylphosphine, reacting for 3-5h under the irradiation of 365nm ultraviolet light, and filtering to remove filtrate to obtain modified graphene; uniformly mixing the modified epoxy resin, KH550 and DMF, reacting for 4-6 hours at the rotating speed of 150-200r/min and the temperature of 25-30 ℃ and the pH value of 11-12, adjusting the pH value to be neutral, adding tetraethoxysilane, modified graphene, dibutyl tin dilaurate and deionized water, and stirring for 1-1.5 hours to obtain the composite coating.
Further, the dosage ratio of the diphenyldichlorosilane, the deionized water and the 1, 3-tetramethyl disiloxane in the step A1 is 2mmol to 10mL to 1mmol, the dosage of the concentrated sulfuric acid is 1-3% of the sum of the mass of the diphenyldichlorosilane, the deionized water and the 1, 3-tetramethyl disiloxane, the molar ratio of the pentaerythritol to the acrylic acid is 1:4, and the dosage of the p-toluenesulfonic acid is 3-5% of the sum of the mass of the pentaerythritol and the acrylic acid.
Further, the molar ratio of the hydrogen-terminated polysiloxane to the reinforcing monomer in the step A2 is 3n+1:n, n is a natural number larger than 0, the concentration of chloroplatinic acid in a mixed system of the hydrogen-terminated polysiloxane, the reinforcing monomer, DMF and chloroplatinic acid is 10-15ppm, the molar ratio of hydroxyl on the modified monomer to epichlorohydrin is 1:1, the dosage of benzyltrimethylammonium bromide is 3-5% of the mass of epichlorohydrin, and the dosage of sodium hydroxide is 10% of the mass of epichlorohydrin.
Further, the dosage of KH570 in the step A3 is 5-10% of the mass of graphene oxide, the molar ratio of double bond to KH580 on the substrate is 1:1, the dosage of dimethylphenylphosphine is 0.01-0.03% of the mass of KH580, and the dosage ratio of modified epoxy resin, KH550, DMF, ethyl orthosilicate, modified graphene, dibutyl tin dilaurate and deionized water is 10g:8.45g:15mL:1.25g:3g:0.02g:5mL.
Further, the modified filler is prepared by the following steps:
step B1: uniformly mixing 3-aminopentanedioic acid, deionized water and concentrated hydrochloric acid, stirring and adding a sodium nitrate solution at the rotating speed of 150-200r/min and the temperature of 3-5 ℃ for reaction for 3-5 hours to obtain a diazonium solution, heating deionized water to boiling, adding sodium sulfide nonahydrate and sulfur for uniform mixing, adding a hydroxide solution for neutralization, stirring and adding the diazonium solution at the rotating speed of 120-150r/min, standing for 2-3 hours at the temperature of 20-25 ℃, regulating the pH value to be acidic, and filtering to remove filtrate to obtain an intermediate 1;
step B2: uniformly mixing the intermediate 1, zinc powder and glacial acetic acid, reacting for 4-6 hours at the rotation speed of 60-80r/min and the temperature of 100-105 ℃ to obtain an intermediate 2, mixing the intermediate 2, N- (3-aminopropyl) pyrrole, DCC and DMF, and reacting for 6-8 hours at the rotation speed of 150-200r/min and the temperature of 20-25 ℃ to obtain a modifier;
step B3: dispersing mullite in ethanol, adding KH570 and deionized water, reacting for 2-3h at the rotation speed of 200-300r/min and the temperature of 50-60 ℃, preparing pretreated mullite, dispersing pretreated mullite in DMF, adding modifier and dimethyl phenyl phosphine, reacting for 3-5h under the irradiation of 365nm ultraviolet light, filtering to remove filtrate, dispersing substrate in ferric chloride ethanol solution, adding pyrrole, standing for 15-20h at the temperature of 5-10 ℃, filtering to remove filtrate, roasting the filter cake at the temperature of 800-850 ℃ for 6-8h, and preparing modified filler.
Further, the dosage ratio of the 3-aminopentanedioic acid, deionized water, concentrated hydrochloric acid and sodium nitrate solution in the step B1 is 10mmol:100mL:4mL:7mL, the mass fraction of the concentrated hydrochloric acid is 36%, the mass fraction of the sodium nitrate solution is 25%, the dosage ratio of deionized water, sodium sulfide nonahydrate, sulfur and diazonium solution is 30mL:25mmol:10.6mmol:500mL, and the mass fraction of the sodium hydroxide solution is 36%.
Further, the dosage ratio of the intermediate 1, zinc powder and glacial acetic acid in the step B2 is 8g to 5mmol to 30mL, and the molar ratio of the intermediate 2, N- (3-aminopropyl) pyrrole and DCC is 1 to 2 to 2.1.
Further, the dosage of KH570 in the step B3 is 3-5% of the mass of mullite, the molar ratio of double bonds on pretreated mullite to modifier is 1:1, the dosage of dimethylphenylphosphine is 1-3% of the mass of modifier, the dosage ratio of substrate, ferric chloride ethanol solution and pyrrole is 30mg:0.5mL:3mL, and the mass fraction of ferric chloride ethanol solution is 15%.
The invention has the beneficial effects that: the corrosion-resistant mullite sagger prepared by the invention comprises the following raw materials: the modified filler, cordierite, kaolin, alumina, deionized water and yellow dextrin are uniformly mixed, the raw materials are sealed, aged, pressed, molded and dried, and then calcined at high temperature to prepare a pretreatment sagger, the surface of the pretreatment sagger is smeared with a composite coating and dried to prepare the modified filler, 3-aminopentanedioic acid is taken as a raw material for diazotizing treatment, sodium sulfide nonahydrate and sulfur react to form sodium polysulfide to react with diazonium liquid to form disulfide, intermediate 1 is prepared, zinc powder is used for reducing the intermediate 1 to form sulfhydryl, intermediate 2 is prepared, carboxyl on the intermediate 2 and amino on N- (3-aminopropyl) pyrrole react with amino on N- (3-aminopropyl) pyrrole under the action of DCC to prepare a modifier, KH570 is used for treating the mullite to graft double bonds on the surface, then the modified agent is used for processing under the illumination condition to lead double bonds on the surface of pretreated mullite and mercapto grafting on the modified agent, pyrrole is added to form polypyrrole cladding on the surface, finally carbonization is carried out to prepare modified filler, the surface of the modified filler is doped with carbon of nitrogen and sulfur, and the modified filler is compounded with cordierite, kaolin and alumina to prevent the erosion of carbon dioxide and carbon monoxide, thereby prolonging the service life of the sagger, diphenyl dichlorosilane is hydrolyzed and polymerized with 1, 3-tetramethyl disiloxane to form hydrogen-terminated polysiloxane, pentaerythritol and acrylic acid are esterified under the action of p-toluenesulfonic acid to prepare reinforced monomer, the hydrogen-terminated polysiloxane and the reinforced monomer react with the double bonds on the reinforced monomer under the action of chloroplatinic acid to form Si-H terminated hyperbranched structure, then reacting with allyl alcohol to form hydroxyl end-capping, preparing modified monomer, reacting the modified monomer with epoxy chloropropane to enable epoxy groups on the epoxy chloropropane to react with hydroxyl groups on the modified monomer, closing a loop under alkaline conditions to form new epoxy groups, preparing modified epoxy resin, treating graphene oxide with KH570 to enable a surface to be grafted with double bonds, reacting with KH580 under illumination conditions to enable the double bonds to react with sulfhydryl groups, further enabling the surface of the graphene oxide to be grafted with siloxane to prepare modified graphene, reacting modified epoxy resin with KH550 to enable hydroxyl groups on the KH550 to react with epoxy groups on the modified epoxy resin to form siloxane end-capping, and then hydrolyzing and polymerizing with modified graphene and tetraethoxysilane to prepare composite coating.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but 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 production process of the corrosion-resistant mullite sagger specifically comprises the following steps:
weighing the following raw materials in parts by weight: 30 parts of modified filler, 60 parts of cordierite, 25 parts of kaolin, 10 parts of alumina, 30 parts of deionized water and 5 parts of yellow dextrin are uniformly mixed, sealed and aged for 24 hours, pressed, molded and dried under the condition of 150MPa, then heat-preserved for 25 minutes under the condition of 225 ℃, heated to 550 ℃, heat-preserved for 2 hours, heated to 1400 ℃ and heat-preserved for 2 hours, so that a pretreatment sagger is prepared, composite paint is smeared on the surface of the pretreatment sagger, and the corrosion-resistant mullite sagger is prepared by drying.
The composite coating is prepared by the following steps:
step A1: mixing diphenyl dichlorosilane and deionized water, stirring for 10min at the rotation speed of 200r/min and the temperature of 60 ℃, adding concentrated sulfuric acid and 1, 3-tetramethyl disiloxane, reacting for 4h, adjusting pH to be neutral to obtain hydrogen-terminated polysiloxane, uniformly mixing pentaerythritol, acrylic acid, p-toluenesulfonic acid and DMF, and reacting for 6h at the rotation speed of 150r/min and the temperature of 110 ℃ to obtain a reinforced monomer;
step A2: uniformly mixing hydrogen-terminated polysiloxane, a reinforcing monomer and DMF (dimethyl formamide), stirring and adding chloroplatinic acid at the rotating speed of 150r/min and the temperature of 50 ℃, reacting for 10 hours, adding propenol, continuously reacting for 8 hours to obtain a modified monomer, uniformly mixing the modified monomer, epoxy chloropropane, benzyl trimethyl ammonium bromide and DMF, stirring and adding sodium hydroxide at the rotating speed of 150r/min and the temperature of 30 ℃, and reacting for 4 hours to obtain a modified epoxy resin;
step A3: dispersing graphene oxide in ethanol, adding KH570 and deionized water, reacting for 2 hours at the rotation speed of 200r/min and the temperature of 50 ℃, filtering to remove filtrate, dispersing a substrate in DMF, adding KH580 and dimethylphenylphosphine, reacting for 3 hours under the irradiation of 365nm ultraviolet light, and filtering to remove filtrate to obtain modified graphene; uniformly mixing the modified epoxy resin, KH550 and DMF, reacting for 4 hours at the rotation speed of 150r/min and the temperature of 25 ℃ and the pH value of 11, adjusting the pH value to be neutral, adding the ethyl orthosilicate, the modified graphene, the dibutyl tin dilaurate and deionized water, and stirring for 1 hour to prepare the composite coating.
The dosage ratio of the diphenyldichlorosilane, the deionized water and the 1, 3-tetramethyl disiloxane in the step A1 is 2mmol to 10mL to 1mmol, the dosage of the concentrated sulfuric acid is 1% of the sum of the mass of the diphenyldichlorosilane, the deionized water and the 1, 3-tetramethyl disiloxane, the molar ratio of the pentaerythritol to the acrylic acid is 1:4, and the dosage of the p-toluenesulfonic acid is 3% of the sum of the mass of the pentaerythritol and the acrylic acid.
The molar ratio of the hydrogen-terminated polysiloxane to the reinforcing monomer in the step A2 is 4:1, the concentration of chloroplatinic acid in a mixed system of the hydrogen-terminated polysiloxane, the reinforcing monomer, DMF and chloroplatinic acid is 10ppm, the molar ratio of hydroxyl on the modified monomer to epoxy chloropropane is 1:1, the dosage of benzyl trimethyl ammonium bromide is 3% of the mass of epoxy chloropropane, and the dosage of sodium hydroxide is 10% of the mass of epoxy chloropropane.
The dosage of KH570 in the step A3 is 5% of the mass of graphene oxide, the molar ratio of double bond to KH580 on a substrate is 1:1, the dosage of dimethylphenylphosphine is 0.01% of the mass of KH580, and the dosage ratio of modified epoxy resin, KH550, DMF, ethyl orthosilicate, modified graphene, dibutyl tin dilaurate and deionized water is 10g:8.45g:15mL:1.25g:3g:0.02g:5mL.
The modified filler is prepared by the following steps:
step B1: uniformly mixing 3-aminopentanedioic acid, deionized water and concentrated hydrochloric acid, stirring at a rotating speed of 150r/min and a temperature of 3 ℃, adding sodium nitrate solution, reacting for 3 hours to obtain diazonium solution, heating deionized water to boiling, adding sodium sulfide nonahydrate and sulfur, uniformly mixing, adding hydrogen sulfide solution for neutralization, stirring at a rotating speed of 120r/min, adding diazonium solution, standing at a temperature of 20 ℃ for 2 hours, regulating pH to be acidic, and filtering to remove filtrate to obtain an intermediate 1;
step B2: uniformly mixing the intermediate 1, zinc powder and glacial acetic acid, reacting for 4 hours at the rotation speed of 60r/min and the temperature of 100 ℃ to obtain an intermediate 2, mixing the intermediate 2, N- (3-aminopropyl) pyrrole, DCC and DMF, and reacting for 6 hours at the rotation speed of 150r/min and the temperature of 20 ℃ to obtain a modifier;
step B3: dispersing mullite in ethanol, adding KH570 and deionized water, reacting for 2 hours at the rotation speed of 200r/min and the temperature of 50 ℃, preparing pretreated mullite, dispersing pretreated mullite in DMF, adding a modifier and dimethylphenylphosphine, reacting for 3 hours under the irradiation of 365nm ultraviolet light, filtering to remove filtrate, dispersing a substrate in ferric chloride ethanol solution, adding pyrrole, standing for 15 hours at the temperature of 5 ℃, filtering to remove filtrate, and roasting a filter cake for 6 hours at the temperature of 800 ℃ to prepare the modified filler.
The dosage ratio of the 3-aminopentanedioic acid to deionized water to the concentrated hydrochloric acid to the sodium nitrate solution in the step B1 is 10mmol to 100mL to 4mL to 7mL, the mass fraction of the concentrated hydrochloric acid is 36%, the mass fraction of the sodium nitrate solution is 25%, the dosage ratio of the deionized water to the sodium sulfide nonahydrate to the sulfur to the diazonium solution is 30mL to 25mmol to 10.6mmol to 500mL, and the mass fraction of the sodium hydroxide solution is 36%.
The dosage ratio of the intermediate 1 to the zinc powder to the glacial acetic acid in the step B2 is 8g to 5mmol to 30mL, and the molar ratio of the intermediate 2 to the N- (3-aminopropyl) pyrrole to the DCC is 1 to 2 to 2.1.
The dosage of KH570 in the step B3 is 3-5% of the mass of mullite, the molar ratio of double bonds on pretreated mullite to modifier is 1:1, the dosage of dimethylphenylphosphine is 1% of the mass of modifier, the dosage ratio of substrate, ferric chloride ethanol solution and pyrrole is 30mg:0.5mL:3mL, and the mass fraction of ferric chloride ethanol solution is 15%.
Example 2
The production process of the corrosion-resistant mullite sagger specifically comprises the following steps:
weighing the following raw materials in parts by weight: 35 parts of modified filler, 65 parts of cordierite, 28 parts of kaolin, 13 parts of alumina, 33 parts of deionized water and 8 parts of yellow dextrin are uniformly mixed, then the mixture is sealed and aged for 24 hours, the mixture is pressed, molded and dried under the condition of 155MPa, then the mixture is subjected to heat preservation for 25 minutes under the condition of 235 ℃, the temperature is increased to 580 ℃, the temperature is kept for 3 hours, the temperature is increased to 1410 ℃ and the temperature is kept for 3 hours, so that a pretreatment sagger is prepared, composite paint is smeared on the surface of the pretreatment sagger, and the corrosion-resistant mullite sagger is prepared by drying.
The composite coating is prepared by the following steps:
step A1: mixing diphenyl dichlorosilane and deionized water, stirring for 15min at the rotation speed of 200r/min and the temperature of 65 ℃, adding concentrated sulfuric acid and 1, 3-tetramethyl disiloxane, reacting for 5h, adjusting pH to be neutral to obtain hydrogen-terminated polysiloxane, uniformly mixing pentaerythritol, acrylic acid, p-toluenesulfonic acid and DMF, and reacting for 7h at the rotation speed of 150r/min and the temperature of 115 ℃ to obtain a reinforced monomer;
step A2: uniformly mixing hydrogen-terminated polysiloxane, a reinforcing monomer and DMF (dimethyl formamide), stirring and adding chloroplatinic acid at the rotating speed of 150r/min and the temperature of 55 ℃, reacting for 15 hours, adding propenol, continuously reacting for 9 hours to obtain a modified monomer, uniformly mixing the modified monomer, epoxy chloropropane, benzyl trimethyl ammonium bromide and DMF, stirring and adding sodium hydroxide at the rotating speed of 150r/min and the temperature of 35 ℃, and reacting for 5 hours to obtain a modified epoxy resin;
step A3: dispersing graphene oxide in ethanol, adding KH570 and deionized water, reacting for 3 hours at the rotation speed of 200r/min and the temperature of 55 ℃, filtering to remove filtrate, dispersing a substrate in DMF, adding KH580 and dimethylphenylphosphine, reacting for 4 hours under the irradiation of 365nm ultraviolet light, and filtering to remove filtrate to obtain modified graphene; uniformly mixing the modified epoxy resin, KH550 and DMF, reacting for 5 hours at the rotating speed of 150r/min and the temperature of 28 ℃ and the pH value of 12, adjusting the pH value to be neutral, adding the ethyl orthosilicate, the modified graphene, the dibutyl tin dilaurate and deionized water, and stirring for 1.5 hours to obtain the composite coating.
The dosage ratio of the diphenyldichlorosilane, the deionized water and the 1, 3-tetramethyl disiloxane in the step A1 is 2mmol:10mL:1mmol, the dosage of the concentrated sulfuric acid is 2% of the sum of the mass of the diphenyldichlorosilane, the deionized water and the mass of the 1, 3-tetramethyl disiloxane, the molar ratio of the pentaerythritol to the acrylic acid is 1:4, and the dosage of the p-toluenesulfonic acid is 4% of the sum of the mass of the pentaerythritol and the acrylic acid.
The molar ratio of the hydrogen-terminated polysiloxane to the reinforcing monomer in the step A2 is 7:2, the concentration of chloroplatinic acid in a mixed system of the hydrogen-terminated polysiloxane, the reinforcing monomer, DMF and chloroplatinic acid is 13ppm, the molar ratio of hydroxyl on the modified monomer to epoxy chloropropane is 1:1, the dosage of benzyl trimethyl ammonium bromide is 4% of the mass of epoxy chloropropane, and the dosage of sodium hydroxide is 10% of the mass of epoxy chloropropane.
The dosage of KH570 in the step A3 is 8% of the mass of graphene oxide, the molar ratio of double bond to KH580 on a substrate is 1:1, the dosage of dimethylphenylphosphine is 0.02% of the mass of KH580, and the dosage ratio of modified epoxy resin, KH550, DMF, ethyl orthosilicate, modified graphene, dibutyl tin dilaurate and deionized water is 10g:8.45g:15mL:1.25g:3g:0.02g:5mL.
The modified filler is prepared by the following steps:
step B1: uniformly mixing 3-aminopentanedioic acid, deionized water and concentrated hydrochloric acid, stirring at a rotating speed of 150r/min and a temperature of 4 ℃, adding sodium nitrate solution, reacting for 4 hours to obtain diazonium solution, heating deionized water to boiling, adding sodium sulfide nonahydrate and sulfur, uniformly mixing, adding hydrogen sulfide solution for neutralization, stirring at a rotating speed of 120r/min, adding diazonium solution, standing at a temperature of 23 ℃ for 3 hours, regulating pH to be acidic, and filtering to remove filtrate to obtain an intermediate 1;
step B2: uniformly mixing the intermediate 1, zinc powder and glacial acetic acid, reacting for 5 hours at the rotation speed of 60r/min and the temperature of 105 ℃ to obtain an intermediate 2, mixing the intermediate 2, N- (3-aminopropyl) pyrrole, DCC and DMF, and reacting for 7 hours at the rotation speed of 150r/min and the temperature of 25 ℃ to obtain a modifier;
step B3: dispersing mullite in ethanol, adding KH570 and deionized water, reacting for 3 hours at the rotation speed of 200r/min and the temperature of 55 ℃, preparing pretreated mullite, dispersing pretreated mullite in DMF, adding a modifier and dimethylphenylphosphine, reacting for 4 hours under the irradiation of 365nm ultraviolet light, filtering to remove filtrate, dispersing a substrate in ferric chloride ethanol solution, adding pyrrole, standing for 18 hours at the temperature of 8 ℃, filtering to remove filtrate, and roasting a filter cake for 7 hours at the temperature of 830 ℃ to prepare the modified filler.
The dosage ratio of the 3-aminopentanedioic acid to deionized water to the concentrated hydrochloric acid to the sodium nitrate solution in the step B1 is 10mmol to 100mL to 4mL to 7mL, the mass fraction of the concentrated hydrochloric acid is 36%, the mass fraction of the sodium nitrate solution is 25%, the dosage ratio of the deionized water to the sodium sulfide nonahydrate to the sulfur to the diazonium solution is 30mL to 25mmol to 10.6mmol to 500mL, and the mass fraction of the sodium hydroxide solution is 36%.
The dosage ratio of the intermediate 1 to the zinc powder to the glacial acetic acid in the step B2 is 8g to 5mmol to 30mL, and the molar ratio of the intermediate 2 to the N- (3-aminopropyl) pyrrole to the DCC is 1 to 2 to 2.1.
The dosage of KH570 in the step B3 is 3-5% of the mass of mullite, the molar ratio of double bonds on pretreated mullite to modifier is 1:1, the dosage of dimethylphenylphosphine is 2% of the mass of modifier, the dosage ratio of substrate, ferric chloride ethanol solution and pyrrole is 30mg:0.5mL:3mL, and the mass fraction of ferric chloride ethanol solution is 15%.
Example 3
The production process of the corrosion-resistant mullite sagger specifically comprises the following steps:
weighing the following raw materials in parts by weight: 40 parts of modified filler, 70 parts of cordierite, 30 parts of kaolin, 15 parts of alumina, 35 parts of deionized water and 10 parts of yellow dextrin are uniformly mixed, then the mixture is sealed and aged for 24 hours, the mixture is pressed, molded and dried under the condition of the pressure of 1160MPa, then the mixture is subjected to heat preservation for 30 minutes under the condition of the temperature of 250 ℃, the temperature is raised to 600 ℃, the heat preservation is carried out for 3 hours, the temperature is raised to 1420 ℃, the heat preservation is carried out for 3 hours, the pretreatment sagger is prepared, the surface of the pretreatment sagger is coated with the composite coating, and the corrosion-resistant mullite sagger is prepared by drying.
The composite coating is prepared by the following steps:
step A1: mixing diphenyl dichlorosilane and deionized water, stirring for 15min at the rotation speed of 300r/min and the temperature of 70 ℃, adding concentrated sulfuric acid and 1, 3-tetramethyl disiloxane, reacting for 6h, adjusting pH to be neutral to obtain hydrogen-terminated polysiloxane, uniformly mixing pentaerythritol, acrylic acid, p-toluenesulfonic acid and DMF, and reacting for 8h at the rotation speed of 200r/min and the temperature of 120 ℃ to obtain a reinforced monomer;
step A2: uniformly mixing hydrogen-terminated polysiloxane, a reinforcing monomer and DMF (dimethyl formamide), stirring and adding chloroplatinic acid at the rotating speed of 200r/min and the temperature of 60 ℃, reacting for 15 hours, adding propenol, continuously reacting for 10 hours to obtain a modified monomer, uniformly mixing the modified monomer, epoxy chloropropane, benzyl trimethyl ammonium bromide and DMF, stirring and adding sodium hydroxide at the rotating speed of 200r/min and the temperature of 40 ℃, and reacting for 6 hours to obtain the modified epoxy resin;
step A3: dispersing graphene oxide in ethanol, adding KH570 and deionized water, reacting for 3 hours at the rotation speed of 300r/min and the temperature of 60 ℃, filtering to remove filtrate, dispersing a substrate in DMF, adding KH580 and dimethylphenylphosphine, reacting for 5 hours under the irradiation of 365nm ultraviolet light, and filtering to remove filtrate to obtain modified graphene; uniformly mixing the modified epoxy resin, KH550 and DMF, reacting for 4-6 hours at the rotating speed of 200r/min and the temperature of 30 ℃ and the pH value of 12, adjusting the pH value to be neutral, adding tetraethoxysilane, modified graphene, dibutyl tin dilaurate and deionized water, and stirring for 1.5 hours to obtain the composite coating.
The dosage ratio of the diphenyldichlorosilane, the deionized water and the 1, 3-tetramethyl disiloxane in the step A1 is 2mmol:10mL:1mmol, the dosage of the concentrated sulfuric acid is 3% of the sum of the mass of the diphenyldichlorosilane, the deionized water and the 1, 3-tetramethyl disiloxane, the molar ratio of the pentaerythritol to the acrylic acid is 1:4, and the dosage of the p-toluenesulfonic acid is 5% of the sum of the mass of the pentaerythritol and the acrylic acid.
The molar ratio of the hydrogen-terminated polysiloxane to the reinforcing monomer in the step A2 is 10:3, the concentration of chloroplatinic acid in a mixed system of the hydrogen-terminated polysiloxane, the reinforcing monomer, DMF and chloroplatinic acid is 15ppm, the molar ratio of hydroxyl on the modified monomer to epoxy chloropropane is 1:1, the dosage of benzyl trimethyl ammonium bromide is 5% of the mass of epoxy chloropropane, and the dosage of sodium hydroxide is 10% of the mass of epoxy chloropropane.
The dosage of KH570 in the step A3 is 10% of the mass of graphene oxide, the molar ratio of double bond to KH580 on a substrate is 1:1, the dosage of dimethylphenylphosphine is 0.03% of the mass of KH580, and the dosage ratio of modified epoxy resin, KH550, DMF, ethyl orthosilicate, modified graphene, dibutyl tin dilaurate and deionized water is 10g:8.45g:15mL:1.25g:3g:0.02g:5mL.
The modified filler is prepared by the following steps:
step B1: uniformly mixing 3-aminopentanedioic acid, deionized water and concentrated hydrochloric acid, stirring at the rotating speed of 200r/min and the temperature of 5 ℃, adding sodium nitrate solution, reacting for 5 hours to obtain diazonium solution, heating deionized water to boiling, adding sodium sulfide nonahydrate and sulfur, uniformly mixing, adding hydrogen sulfide solution for neutralization, stirring at the rotating speed of 150r/min, adding diazonium solution, standing at the temperature of 25 ℃ for 3 hours, regulating pH to be acidic, and filtering to remove filtrate to obtain an intermediate 1;
step B2: uniformly mixing the intermediate 1, zinc powder and glacial acetic acid, reacting for 6 hours at the temperature of 105 ℃ at the rotating speed of 80r/min to obtain an intermediate 2, mixing the intermediate 2, N- (3-aminopropyl) pyrrole, DCC and DMF, and reacting for 8 hours at the temperature of 25 ℃ at the rotating speed of 200r/min to obtain a modifier;
step B3: dispersing mullite in ethanol, adding KH570 and deionized water, reacting for 3 hours at the rotation speed of 300r/min and the temperature of 60 ℃, preparing pretreated mullite, dispersing pretreated mullite in DMF, adding a modifier and dimethylphenylphosphine, reacting for 5 hours under the irradiation of 365nm ultraviolet light, filtering to remove filtrate, dispersing a substrate in ferric chloride ethanol solution, adding pyrrole, standing for 20 hours at the temperature of 10 ℃, filtering to remove filtrate, and roasting a filter cake for 8 hours at the temperature of 850 ℃ to prepare the modified filler.
The dosage ratio of the 3-aminopentanedioic acid to deionized water to the concentrated hydrochloric acid to the sodium nitrate solution in the step B1 is 10mmol to 100mL to 4mL to 7mL, the mass fraction of the concentrated hydrochloric acid is 36%, the mass fraction of the sodium nitrate solution is 25%, the dosage ratio of the deionized water to the sodium sulfide nonahydrate to the sulfur to the diazonium solution is 30mL to 25mmol to 10.6mmol to 500mL, and the mass fraction of the sodium hydroxide solution is 36%.
The dosage ratio of the intermediate 1 to the zinc powder to the glacial acetic acid in the step B2 is 8g to 5mmol to 30mL, and the molar ratio of the intermediate 2 to the N- (3-aminopropyl) pyrrole to the DCC is 1 to 2 to 2.1.
The dosage of KH570 in the step B3 is 5% of the mass of mullite, the molar ratio of double bonds on pretreated mullite to modifier is 1:1, the dosage of dimethylphenylphosphine is 3% of the mass of modifier, the dosage ratio of substrate, ferric chloride ethanol solution and pyrrole is 30mg:0.5mL:3mL, and the mass fraction of ferric chloride ethanol solution is 15%.
Comparative example 1
This comparative example uses graphene oxide instead of modified graphene as compared to example 1, with the rest of the steps being identical.
Comparative example 2
This comparative example was compared to example 1 without the addition of reinforcing monomer, and the rest of the procedure was the same.
Comparative example 3
This comparative example uses mullite instead of modified filler as compared to example 1, the rest of the procedure being the same.
The sagger samples prepared in examples 1 to 3 and comparative examples 1 to 3 were aligned and placed in an alumina crucible, and Li (Ni 0.5 Co 0.2 Mn 0.3 ）O 2 The ternary positive electrode material precursors are paved on the surfaces of the samples, the mass of the precursors on each sample surface is 3, an alumina crucible is kept at the temperature of 1000 ℃ for 4 hours, the materials are naturally cooled and taken out, the processes of charging, heat preservation and cooling are repeated, the erosion phenomenon is observed, and the detection results are shown in the following table.
The table shows that the paint has good corrosion resistance.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (8)
1. A production process of a corrosion-resistant mullite sagger is characterized by comprising the following steps of: the method specifically comprises the following steps:
weighing the following raw materials in parts by weight: 30-40 parts of modified filler, 60-70 parts of cordierite, 25-30 parts of kaolin, 10-15 parts of alumina, 30-35 parts of deionized water and 5-10 parts of yellow dextrin, uniformly mixing the raw materials, sealing, ageing, compacting, forming, drying, calcining at a high temperature to obtain a pretreatment sagger, coating a composite coating on the surface of the pretreatment sagger, and drying to obtain the corrosion-resistant mullite sagger;
the composite coating is prepared by the following steps:
step A1: after mixing and stirring diphenyl dichlorosilane and deionized water, adding concentrated sulfuric acid and 1, 3-tetramethyl disiloxane, reacting, adjusting pH to be neutral to obtain hydrogen-terminated polysiloxane, and mixing pentaerythritol, acrylic acid, p-toluenesulfonic acid and DMF for reacting to obtain a reinforced monomer;
step A2: mixing and stirring hydrogen-terminated polysiloxane, a reinforcing monomer and DMF, adding chloroplatinic acid, reacting, adding propenol, continuing to react to obtain a modified monomer, mixing and stirring the modified monomer, epichlorohydrin, benzyl trimethyl ammonium bromide and DMF, adding sodium hydroxide, and reacting to obtain modified epoxy resin;
step A3: dispersing graphene oxide in ethanol, adding KH570 and deionized water for reaction, filtering to remove filtrate, dispersing a substrate in DMF, adding KH580 and dimethylphenylphosphine, reacting under irradiation of 365nm ultraviolet light, and filtering to remove filtrate to obtain modified graphene; mixing modified epoxy resin, KH550 and DMF for reaction, adjusting pH to be neutral, adding tetraethoxysilane, modified graphene, dibutyl tin dilaurate and deionized water, and stirring to obtain a composite coating;
the modified filler is prepared by the following steps:
step B1: mixing and stirring 3-aminopentanedioic acid, deionized water and concentrated hydrochloric acid, adding a sodium nitrate solution, reacting to obtain a diazonium solution, heating deionized water to boiling, adding sodium sulfide nonahydrate and sulfur, mixing uniformly, adding a hydrogen oxide solution for neutralization, stirring, adding the diazonium solution, standing, regulating pH to be acidic, and filtering to remove filtrate to obtain an intermediate 1;
step B2: mixing intermediate 1, zinc powder and glacial acetic acid for reaction to obtain intermediate 2, and mixing intermediate 2, N- (3-aminopropyl) pyrrole, DCC and DMF for reaction to obtain a modifier;
step B3: dispersing mullite in ethanol, adding KH570 and deionized water for reaction to obtain pretreated mullite, dispersing pretreated mullite in DMF, adding modifier and dimethyl phenyl phosphine, reacting under 365nm ultraviolet irradiation, filtering to remove filtrate, dispersing substrate in ferric chloride ethanol solution, adding pyrrole, standing, filtering to remove filtrate, and roasting filter cake to obtain modified filler.
2. The process for producing the corrosion-resistant mullite sagger according to claim 1, which is characterized in that: the dosage ratio of the diphenyldichlorosilane, the deionized water and the 1, 3-tetramethyl disiloxane in the step A1 is 2mmol:10mL:1mmol, the dosage of the concentrated sulfuric acid is 1-3% of the mass sum of the diphenyldichlorosilane, the deionized water and the 1, 3-tetramethyl disiloxane, the molar ratio of the pentaerythritol to the acrylic acid is 1:4, and the dosage of the p-toluenesulfonic acid is 3-5% of the mass sum of the pentaerythritol and the acrylic acid.
3. The process for producing the corrosion-resistant mullite sagger according to claim 1, which is characterized in that: the molar ratio of the hydrogen-terminated polysiloxane to the reinforcing monomer in the step A2 is 3n+1:n, n is a natural number larger than 0, the concentration of chloroplatinic acid in a mixed system of the hydrogen-terminated polysiloxane, the reinforcing monomer, DMF and chloroplatinic acid is 10-15ppm, the molar ratio of hydroxyl on the modified monomer to epoxy chloropropane is 1:1, the dosage of benzyl trimethyl ammonium bromide is 3-5% of the mass of epoxy chloropropane, and the dosage of sodium hydroxide is 10% of the mass of epoxy chloropropane.
4. The process for producing the corrosion-resistant mullite sagger according to claim 1, which is characterized in that: the dosage of KH570 in the step A3 is 5-10% of the mass of graphene oxide, the molar ratio of double bond to KH580 on a substrate is 1:1, the dosage of dimethyl phenyl phosphine is 0.01-0.03% of the mass of KH580, and the dosage ratio of modified epoxy resin, KH550, DMF, ethyl orthosilicate, modified graphene, dibutyl tin dilaurate and deionized water is 10g:8.45g:15mL:1.25g:3g:0.02g:5mL.
5. The process for producing the corrosion-resistant mullite sagger according to claim 1, which is characterized in that: the dosage ratio of the 3-aminopentanedioic acid to deionized water to the concentrated hydrochloric acid to the sodium nitrate solution in the step B1 is 10mmol to 100mL to 4mL to 7mL, the mass fraction of the concentrated hydrochloric acid is 36%, the mass fraction of the sodium nitrate solution is 25%, the dosage ratio of the deionized water to the sodium sulfide nonahydrate to the sulfur to the diazonium solution is 30mL to 25mmol to 10.6mmol to 500mL, and the mass fraction of the sodium hydroxide solution is 36%.
6. The process for producing the corrosion-resistant mullite sagger according to claim 1, which is characterized in that: the dosage ratio of the intermediate 1 to the zinc powder to the glacial acetic acid in the step B2 is 8g to 5mmol to 30mL, and the molar ratio of the intermediate 2 to the N- (3-aminopropyl) pyrrole to the DCC is 1 to 2 to 2.1.
7. The process for producing the corrosion-resistant mullite sagger according to claim 1, which is characterized in that: the dosage of KH570 in the step B3 is 3-5% of the mass of mullite, the molar ratio of double bonds on pretreated mullite to modifier is 1:1, the dosage of dimethylphenylphosphine is 1-3% of the mass of modifier, the dosage ratio of substrate, ferric chloride ethanol solution and pyrrole is 30mg:0.5mL:3mL, and the mass fraction of ferric chloride ethanol solution is 15%.
8. The utility model provides a corrosion-resistant mullite sagger which characterized in that: the method according to any one of claims 1-7.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103820788A (en) * | 2014-02-20 | 2014-05-28 | 铜陵祥云消防科技有限责任公司 | Antirust agent containing modified mullite powder |
| CN109467422A (en) * | 2018-04-20 | 2019-03-15 | 湖南德景源科技有限公司 | Dedicated high circulation special cermacis crucible of a kind of lithium electricity and preparation method thereof |
| CN116875169A (en) * | 2023-09-08 | 2023-10-13 | 江苏新历科技有限公司 | Waterproof corrosion-resistant water paint and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820788A (en) * | 2014-02-20 | 2014-05-28 | 铜陵祥云消防科技有限责任公司 | Antirust agent containing modified mullite powder |
| CN109467422A (en) * | 2018-04-20 | 2019-03-15 | 湖南德景源科技有限公司 | Dedicated high circulation special cermacis crucible of a kind of lithium electricity and preparation method thereof |
| CN116875169A (en) * | 2023-09-08 | 2023-10-13 | 江苏新历科技有限公司 | Waterproof corrosion-resistant water paint and preparation method thereof |
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