CN106495652B - Ceramic nanofibers heat-insulating material and preparation method thereof - Google Patents
Ceramic nanofibers heat-insulating material and preparation method thereof Download PDFInfo
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- CN106495652B CN106495652B CN201610960579.5A CN201610960579A CN106495652B CN 106495652 B CN106495652 B CN 106495652B CN 201610960579 A CN201610960579 A CN 201610960579A CN 106495652 B CN106495652 B CN 106495652B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 53
- 239000011810 insulating material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002121 nanofiber Substances 0.000 title claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000004094 surface-active agent Substances 0.000 claims abstract description 30
- 239000000835 fiber Substances 0.000 claims abstract description 27
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 26
- 239000000853 adhesive Substances 0.000 claims abstract description 22
- 230000001070 adhesive effect Effects 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 6
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 5
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims description 5
- 235000001727 glucose Nutrition 0.000 claims description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 239000007868 Raney catalyst Substances 0.000 claims description 3
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 3
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 238000005984 hydrogenation reaction Methods 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 238000005576 amination reaction Methods 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 2
- 241000219094 Vitaceae Species 0.000 claims 1
- 235000021021 grapes Nutrition 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 9
- 125000003368 amide group Chemical group 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 5
- 125000006353 oxyethylene group Chemical group 0.000 abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract description 3
- 230000007774 longterm Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract description 3
- 239000004964 aerogel Substances 0.000 description 8
- 238000013475 authorization Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 229960001866 silicon dioxide Drugs 0.000 description 7
- 239000000725 suspension Substances 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 125000005647 linker group Chemical group 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 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 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000012774 insulation material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 239000000080 wetting agent Substances 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 229910002012 Aerosil® Inorganic materials 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- -1 dimethyl alkyl amine Chemical class 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007717 exclusion Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002103 nanocoating Substances 0.000 description 2
- 239000003605 opacifier Substances 0.000 description 2
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical compound [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 description 2
- 239000011378 shotcrete Substances 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- WSWCOQWTEOXDQX-MQQKCMAXSA-M (E,E)-sorbate Chemical compound C\C=C\C=C\C([O-])=O WSWCOQWTEOXDQX-MQQKCMAXSA-M 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 150000002169 ethanolamines Chemical class 0.000 description 1
- 238000009851 ferrous metallurgy Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229940009493 gel-one Drugs 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
- 239000007908 nanoemulsion Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229940075554 sorbate Drugs 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
-
- 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/06—Quartz; Sand
-
- 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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
-
- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/005—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing gelatineous or gel forming binders, e.g. gelatineous Al(OH)3, sol-gel binders
-
- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
-
- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
- C04B28/26—Silicates of the alkali metals
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
Abstract
The invention discloses a kind of preparation method of ceramic nanofibers heat-insulating material, comprise the following steps：（1）Ceramic nano high temperature adhesives are prepared, are 2 by weight ratio:8 hydrophobic nano silica mixes with water, adds the 10wt% organic surface active agent stirring with sulfonic group, sulfate group, amide groups, hydroxyl, the two or more groups of the hydrophilic radical of ammonium and oxyethylene group；3 5wt% inorganic dispersant is added, at room temperature ultrasonic vibration, it is stand-by after nano silicon is uniformly dispersed；（2）40 60wt% 5mm 15mm fiber is added in nano ceramics high temperature adhesives and is uniformly mixed, stands 24 hours, is 110 DEG C 350 DEG C in drying temperature, dries 24 hours.Nano-Ceramic Composites unit weight of the present invention is 0.20g/cm3± 10%, during 600 DEG C of hot-face temperature, thermal conductivity factor is less than 0.060W/mk, and materials'use is less, simple to operate, saves man-hour and cost in production, and obtained nano ceramic fibers composite is light and can be long-term use of at high temperature.
Description
Technical field
The present invention relates to heat-insulating material field, particularly a kind of ceramic nanofibers heat-insulating material and preparation method thereof.
Background technology
AND ENERGY RESOURCES CONSUMPTION IN CHINA amount ranks first in the world within 2014, and efficiency of energy utilization is low, and carbon emission amount is considerably beyond flourishing state
Family, as solving energy shortage most efficient method, it is a kind of effective measure to strengthen insulation for energy-saving and emission-reduction.
1992, American scholar Hunt A J proposed adiabatic concept first in national project conference, in 20 afterwards
Between for many years, heat-insulating material is developed rapidly, and in recent years due to the rise of nano material, especially aerogel material is as nothing
The minimum material of extremely adiabatic field thermal conductivity is widely used, wherein being showed with silica aerogel material especially excellent
It is different, but because the inherent strength of silica aerogel material is low, the shortcomings of fragility is big and easily ftractures, limit its
Use in practice, the reinforcements such as fiber are then introduced, improve the performance of material in itself.Domestic and foreign scholars are carried out in this project
Substantial amounts of research, and achieve significant achievement.
Authorization Notice No. is that CN1186298C Chinese invention patent discloses a kind of dense form ceramic fibre gunite lining
And its construction technology, it is made up of ceramics and high temperature adhesives, high temperature adhesives include Al2O3Micro mist, SiO2Micro mist, nanoscale
Al2O3The volume that powder, ammoniacal liquor and water and appropriate additive are combined to obtain dense form ceramic fibre gunite lining with ceramic fibre is close
Spend for 0.3-0.49g/cm3。
Authorization Notice No. be CN 102942332B Chinese invention patent disclose a kind of composite Nano hole heat-insulating material and
Its preparation method.Use SiO2Powder 20-40 parts, Al2O3Powder 0-20 parts, opacifier 1-10 parts, binding agent 1-5 parts, inorganic company
Continuous fiber 40-80 parts and the solvent 80-100 parts as carrier recycled, are made inorganic by inorganic continuous fiber first
Continuous fiber felts, then powder, opacifier and binding agent are added in solvent, nanoemulsions are configured to using high speed dispersor,
By the two press filtration, dry and nano heat insulating material, density 120-125kg/m is made3, normal temperature thermal conductivity factor≤0.024W/mk,
Maximum operation (service) temperature≤1000 DEG C.
Authorization Notice No. CN103058622 Chinese invention patent discloses a kind of inorganic heat insulation material and its preparation side
Method, by 15-60wt% aerosils, 15-60wt% soluble silicates, 15-40wt%（R）nN（R）3X-(1≤n≤24,
R is alkyl), 5-15wt% tin-antiomony oxides and 5-15wt% hollow glass micropearl mixing, add coupling agent modified, mixed
Thing；Mixture is mixed with water, it is hot-forming to obtain inorganic heat insulation material in obtained serous infiltration to glass mat.Often
The lower thermal conductivity factor of temperature is 0.025-0.027W/mk.
Authorization Notice No. CN103159454B Chinese invention patent discloses a kind of nanoporous aerogel/fiber composite
Super insulating material, the organic solvent tert-butyl alcohol, organic monomer acrylamide, crosslinking agent N, N '-methylene-bisacrylamide are filled
Divide to be stirred and be configured to premixed liquid, aerosil, alumina powder, Zirconium oxide fibre, screening are added into premixed liquid
Photo etching titanium dioxide, pore creating material polyethylene glycol and suspending agent sodium tripolyphosphate obtain suspension slurry, carry out froth in vacuum 15-45 minutes,
Then successively added into suspended nitride initiator ammonium persulfate, catalyst stirring de-bubble slurry is made, in-situ solidifying is coagulated
Glue complex, dry, dumping obtains the compound super insulating material that thermal conductivity factor under normal temperature is 0.045W/mk.
Authorization Notice No. discloses a kind of surface grafting of silica for CN104312215B Chinese invention patent and changed
Property method, for silica surface Atomic coordinate number deficiency, surface energy is higher, situation about easily reuniting, using epoxy radicals silicone hydride
Coupling agent, ammoniacal liquor are reacted under alkaline environment silica surface, its dispersiveness and compatibility are improved, with hindered amine antioxidant
Graft modification is carried out, obtained nano-silica surface has the antioxidant of chemical bonding, changes its surface polarity, reunites existing
As being improved.
Publication No. is that CN105038445A Chinese invention patent application discloses a kind of water containing aerosil
Property slurry, its preparation method and application, mainly have silicon dioxide aerogel powder, surfactant, binding agent and water uniformly to mix
Close the stable dispersion system formed.Water and surfactant are well mixed, form mixed liquor；Hydrophobicity is added into mixed liquor
Silicon dioxide aerogel powder, it is well mixed, forms suspension；Binding agent and auxiliary agent are added into suspension, is well mixed, shape
Into the water paste.Temperature in use is at -50 DEG C -300 DEG C, and thermal conductivity is between 0.0246-0.05W/mk.
Authorization Notice No. is to disclose a kind of aqueous solution with hydrophobic type aeroge in US7635411B2 United States Patent (USP),
The average grain diameter of aerogel powder is 0.03mm-1mm, at least contains a kind of wetting agent, wetting agent and aeroge in its aqueous solution
Mass percent be 0.05%-0.5%, wetting agent can live on surfaces such as sorbate, phosphate, dimethyl alkyl amine oxides
Property agent, the density produced is less than 0.4g/cc, and thermal conductivity is less than 0.04W/mk aerogel composite, but if gas
Gel powder, which is that nanoscale is scattered, will turn into a big problem.
It is a kind of by aerogel particle, fiber and with electrification that Authorization Notice No. has been US9399864B2 U.S. Patent Publication
Compound mixes in water, and after particle is scattered and emulsion is formed, emulsion starts to flocculate or condensed, aerogel particles, fiber, powered
Compound and de- stabilizer are gathered in sticky group, at the same formed one it is limpid, low viscosity, water-based supernatant, take off
Supernatant is removed, density is formed and is less than 0.2g/cc, thermal conductivity is 0.04W/mk aeroge composite insulation materials at 150 DEG C.So
And the operation need it is existing by nano particle with surfactant modified, then and after fiber mixes in addition charging cpd,
Then also need to add de- stabilizer, form after flocculating the step of carrying out sloughing supernatant again, process is relatively complicated, increase production
Cost.
The content of the invention
In order to solve the above-mentioned technical problem, the present invention provides a kind of preparation method of ceramic nanofibers heat-insulating material, it
Comprise the following steps：
（1）Ceramic nano high temperature adhesives are prepared, are 2 by weight ratio:8 hydrophobic nano silica mixes with water,
The hydrophilic radical with sulfonic group, sulfate group, amide groups, hydroxyl, ammonium and oxyethylene group for adding 10wt% is two or more
The organic surface active agent stirring of group；3-5wt% inorganic dispersant is added, at room temperature ultrasonic vibration, treat nanometer titanium dioxide
After silicon is uniformly dispersed, as ceramic nano high temperature adhesives are stand-by；
（2）40-60wt% 5mm-5cm fiber is added to step（1）Stirred in the nano ceramics high temperature adhesives of preparation
Well mixed, standing 24 hours is mixed, is 110 DEG C -350 DEG C in drying temperature, dries 24 hours.
Preferably, the organic surface active agent is the surface-active at least provided with hydroxyl, sulfonic group and amide group
Agent.
Preferably, the organic surface active agent is the alcoholic solution of polyhydroxy based surfactants, and the polyhydroxy primary surface is lived
Property agent be polyhydroxy unit by linking group with have 3-36 carbon atom aliphatic residue be connected.
Preferably, the linking group is one kind in sulfonate ester group and amido groups.
Preferably, the linking group of the polyhydroxy based surfactants is amide groups.
Preferably, the inorganic dispersant is sodium tripolyphosphate, calgon, calcium lignosulfonate, lignin sulfonic acid
One or more in sodium.
Preferably, the inorganic dispersant is 3wt%.
Preferably, the drying temperature is 110 DEG C.
Preferably, the average grain diameter of the nano silica powder is 30-80nm.
Another technical problem to be solved by this invention is to provide a kind of ceramic nanofibers heat-insulating material, the nanometer
Ceramic composite unit weight is 0.20g/cm3± 10%, during 600 DEG C of hot-face temperature, thermal conductivity factor is less than 0.060W/m k.
By the present invention in that with a kind of Multicomponent Surfactants, electric charge is carried out to hydrophobic nano silicon-dioxide powdery and repaiied
Decorations, by stirring and ultrasonic vibration, electrical charges between particles mutual exclusion is set to reach stable suspension, the silicon-dioxide powdery with electric charge
When preparing nano ceramic fibers composite, formed and adsorbed with fiber, the Nano-Ceramic Composites unit weight after dry solidification
For 0.20g/cm3± 10%, during 600 DEG C of hot-face temperature, thermal conductivity factor is less than 0.060W/m k, and materials'use is less, operation letter
It is single, man-hour and cost are saved in production, and obtained nano ceramic fibers composite is light and can be long-term at high temperature
Use.
Embodiment
The present invention discloses a kind of ceramic nanofibers heat-insulating material, and the heat-insulating material is by a kind of ceramic nano high temperature adhesives
Mix, at ambient pressure mixing drying, prepared simply with fiber, Aero-Space, weapons equipment, Ferrous Metallurgy, stone can be used in
The fields such as oiling work, ceramic building material, naval vessel vehicle, household electrical appliance, solar energy, fire protection, information electronics, as insulating materials
Thermal conductivity factor is low under normal temperature and high temperature, and unit weight is low, long-term use of temperature is 850 DEG C, and maximum operation (service) temperature is not less than 1000 DEG C.
The preparation of ceramic nanofibers heat-insulating material of the present invention includes following steps：
1. the preparation of ceramic nano high temperature adhesives
1-1. mixes hydrophobic nano silicon-dioxide powdery with water, and the weight ratio of nano silica powder and water is 2:
8；The Multicomponent Surfactants that mass percent is aqueous silica solution gross mass 13-15% are added, are entered at 20-30 DEG C
Ultrasonic vibration again after row stirring, after nano silica powder is uniformly dispersed, that is, obtains ceramic nano high temperature adhesives.
The particle diameter of hydrophobic nano silicon-dioxide powdery is 30-80nm；Water is pure water.
Multicomponent Surfactants include at least organic surface active agent and inorganic dispersant, organic surface active agent and nothing
The mass ratio of machine dispersant is 10:3-5.Organic surface active agent is with sulfonic group, sulfate group, amide groups, hydroxyl, ammonium
And in oxyethylene group hydrophilic radical two or more groups surfactant, inorganic dispersant be sodium tripolyphosphate, six inclined phosphorus
One or more in sour sodium, calcium lignosulfonate, sodium lignin sulfonate.Wherein, organic surface active agent makes nanometer titanium dioxide
Silicon face forms the group with electric charge；Inorganic dispersant is used for electric charge being unified for single electric charge, makes to be formed between nano particle
The stable state of mutual exclusion.
Organic surface active agent preferably carries the group of hydroxyl, particular with the alcoholic solution of polyhydroxy based surfactants,
Polyhydroxy unit is connected by linking group with the aliphatic residue of 3-36 carbon atom, the linking group be sulfonate ester group and
One kind in amide group.
Preferably polyhydroxy is simultaneous with two or more the table in amide groups, sulfonic group and oxyethylene group group
Face activating agent.
The preparation of a variety of functional group's surfactants of 1-2. polyhydroxy
（1）Dissolved in etoh solvent, the mass percent of solvent by 1-6molN- alkylamines and 1mol glucose
For 40-60%, amination condensation is carried out under normal temperature.
（2）Hydrogenation reaction is carried out under Raney nickel, synthesizes N- alkyl glucose amine, reaction is filtered to remove after terminating and urged
Agent.
（3）1molN- alkyl glucoses amine and 1mol fatty acid methyl esters or 1mol fatty acid methyl ester sulfonic acid are dissolved in the third two
In alcohol, the vacuum reaction 2-5 hours at 120 DEG C -150 DEG C under base catalyst.Products therefrom does not have to desolventizing, directly as this
The surfactant of invention.
2. the preparation of ceramic nano heat-insulating material
The preparation of 2-1. ceramic nanofibers heat-insulating materials
（1）The fiber that length is 5mm-5cm is stirred by mixing with ceramic nano high temperature adhesives in step 1,
The mass percent of fiber and ceramic nano high temperature adhesives is 4:6-6:4.
（2）Dried at 110 DEG C -350 DEG C, after 24 hours, that is, obtain ceramic nanofibers heat-insulating material.
Fiber surface carries the electric charge different from nano silica powder surface charge in theory, and the two is attracting, is formed
Combine closely, make heat-insulating property more excellent.By testing, the ceramic nanofibers heat-insulating material prepared according to the method described above
Unit weight is 0.2g/cm3± 10%, during 600 DEG C of hot-face temperature, thermal conductivity factor is less than or equal to 0.06W/mk.
It is thermal conductivity factor when hot-face temperature is 600 DEG C that thermal conductivity factor is surveyed in the present invention.
The preparation of 2-2. ceramic nanofibers heat-insulating shields
（1）The fiber that length is 5mm-5cm is well mixed with ceramic nano high temperature adhesives in step 1, fiber and pottery
The mass percent of porcelain nanometer high temperature adhesives is 6:4-9:1, add in 3-5wt% sodium metasilicate powder, Ludox and Alumina gel
One or more, be uniformly mixed, import mould in.
（2）The mixing material imported after mould is shaken under forcing press with 20MPa intervals paddle type mill pressurizes, then 110
Dried at DEG C -350 DEG C, after 24 hours, produce ceramic nanofibers heat-insulating shield.
Gained ceramic nanofibers heat-insulating shield unit weight is 0.2-0.25g/cm3, during 600 DEG C of hot-face temperature, thermal conductivity factor is small
In equal to 0.06W/mk.
2-3. ceramic nano coatings
（1）Added in the ceramic nano high temperature adhesives obtained in step 1 3-5wt% sodium metasilicate powder, Ludox and
One or more in Alumina gel, 3wt% clay is added, be well mixed.
（2）By step 2-3-（1）In ceramic nano coating be applied to and needed such as on wall or pipeline in heat guard,
Smearing thickness is 1-10mm, is completely dried after being dried 8 hours at 110 DEG C, or is entered using the method for adding normal temperature cure agent
Row solidification, the coating intensity prepared according to the method described above is more than or equal to 0.5MPa, for a long time using not caving in.
Embodiment 1
1. the preparation of surfactant
3mol monoethanolamines are mixed with 1mol glucose and are dissolved in ethanol, the mass percent of solvent is 40-60%, normal temperature
Under reacted；Hydrogenation reaction is carried out under Raney nickel, is theoretically synthesized 1mol product A, reaction is filtered to remove after terminating and urged
Agent, above-mentioned product A and 1mol fatty acid methyl ester sulfonic acid are dissolved in 10-30wt% propane diols, under base catalyst, 150
DEG C vacuum reaction 5 hours.Products therefrom does not have to desolventizing, and directly as the surfactant B of the present invention, surfactant B is
Polyhydroxy is with sulfonic group, the alcoholic solution of amide group compound.
2. the preparation of high-temperature nano bonding agent
It is 2 to take hydrophobic type silicon dioxide nano powder to be dispersed in the mass ratio of silica nanometer powder and water in pure water:
8, add 10wt% surfactant B, 5min stirred at 20 DEG C, add 3wt% inorganic dispersants, be sodium tripolyphosphate,
One or more in calgon, calcium lignosulfonate, sodium lignin sulfonate, the ultrasonic vibration at 20 DEG C, treat titanium dioxide
Silicon nano power body is gradually uniformly dispersed to form stable suspension, and ceramic nano high temperature adhesives are made.
3. the preparation of nano ceramic fibers composite
It is that 5mm fibers are put into high temperature adhesives by 50wt% length, uniformly mixes, 24 hours are stood, at 110 DEG C
Lower drying 24 hours, that is, obtain ceramic nanofibers composite, unit weight 0.18g/cm3, during 600 DEG C of hot-face temperature, heat conduction
Coefficient 0.056W/m k.
It is the embodiment of manufactured ceramic nanofibers composite at different conditions in table 1.
Table 1
Stirring is stirred in table 1, is surpassed for ultrasonic vibration；
Stable state is that nano particle is in dispersed state in suspension for long；
Metastable condition is that nanometer produces through having to reunite after a while, or just has a small amount of group during the course of the reaction
It is poly- to produce；Unstable state has reunion to produce to be obvious.
Comparative example
It is classified as in table 2 by listed organic surface active agent processing nano-silicon dioxide particle, then pass through in the prior art
Cross nanometer high temperature adhesives made of inorganic dispersant modification.
It is 2 to take hydrophobic type silicon dioxide nano powder to be dispersed in the mass ratio of silica nanometer powder and water in pure water:
8,10wt% organic surface active agent is added, 5min is stirred at 20 DEG C, adds 3wt% inorganic dispersants, is tripolyphosphate
One or more in sodium, calgon, calcium lignosulfonate, sodium lignin sulfonate, the ultrasonic vibration at 20 DEG C, treat dioxy
SiClx nano-powder is gradually scattered to form suspension, and ceramic nano high temperature adhesives are made.
Table 2
Simply presently preferred embodiments of the present invention described above, not it is used for limiting the practical range of the present invention；It is i.e. all
It is that the scope of the present invention is covered according to the equivalent changes and modifications made in the scope of the invention.
Claims (5)
- A kind of 1. preparation method of ceramic nanofibers heat-insulating material, it is characterised in that：It comprises the following steps：（1）Organic table The preparation of face activating agent：Dissolved in etoh solvent, the quality hundred of solvent by 1-6molN- alkylamines and 1mol glucose It is 40-60% to divide ratio, and amination condensation is carried out under normal temperature, hydrogenation reaction is carried out under Raney nickel, synthesizes N- alkyl grapes Osamine, reaction terminates rear Filtration of catalyst, by 1molN- alkyl glucoses amine and 1mol fatty acid methyl esters or 1mol fat Fatty acid methyl esters sulfonic acid is dissolved in propane diols, and vacuum reaction 2-5 hours at 120 DEG C -150 DEG C, obtain polyhydroxy under base catalyst The alcoholic solution of based surfactants, its organic surface active agent as the present invention；（2）Ceramic nano high temperature adhesives are prepared, It is 2 by weight ratio:8 hydrophobic nano silica mixes with water, adds the organic of aqueous silica solution gross mass 10wt% Surfactant is stirred, and adds aqueous silica solution gross mass 3-5wt% inorganic dispersant, at room temperature ultrasound shake Swing, after nano silicon is uniformly dispersed, as ceramic nano high temperature adhesives are stand-by；（3）Raw material gross mass 40- will be accounted for 60wt% 5mm-5cm fiber is added to step（2）It is uniformly mixed in the ceramic nano high temperature adhesives of middle preparation, it is quiet Put 24 hours, be 110 DEG C -350 DEG C in drying temperature, dry 24 hours.
- 2. the preparation method of ceramic nanofibers heat-insulating material according to claim 1, it is characterised in that：Described inorganic point Powder is the one or more in sodium tripolyphosphate, calgon, calcium lignosulfonate, sodium lignin sulfonate.
- 3. the preparation method of ceramic nanofibers heat-insulating material according to claim 1, it is characterised in that：Described inorganic point Powder is the 3% of aqueous silica solution gross mass.
- 4. the preparation method of ceramic nanofibers heat-insulating material according to claim 1, it is characterised in that：The drying temperature Spend for 110 DEG C.
- 5. the preparation method of ceramic nanofibers heat-insulating material according to claim 1, it is characterised in that：The nanometer two The average grain diameter of silica powder is 30-80nm.
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