CN109133959A - A kind of Carbon Fiber Rigid thermal insulation tile and preparation method thereof - Google Patents
A kind of Carbon Fiber Rigid thermal insulation tile and preparation method thereof Download PDFInfo
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- CN109133959A CN109133959A CN201811061423.9A CN201811061423A CN109133959A CN 109133959 A CN109133959 A CN 109133959A CN 201811061423 A CN201811061423 A CN 201811061423A CN 109133959 A CN109133959 A CN 109133959A
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- Prior art keywords
- carbon fiber
- thermal insulation
- insulation tile
- silicone
- rigid thermal
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 165
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 163
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 162
- 238000009413 insulation Methods 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000011521 glass Substances 0.000 claims abstract description 23
- 229920002050 silicone resin Polymers 0.000 claims abstract description 20
- 239000012298 atmosphere Substances 0.000 claims abstract description 17
- 238000005336 cracking Methods 0.000 claims abstract description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 43
- 229920001296 polysiloxane Polymers 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 26
- 239000003054 catalyst Substances 0.000 claims description 22
- 239000002243 precursor Substances 0.000 claims description 22
- 239000003431 cross linking reagent Substances 0.000 claims description 21
- 239000003960 organic solvent Substances 0.000 claims description 21
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- -1 polydimethylsiloxane Polymers 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- 238000003763 carbonization Methods 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000005470 impregnation Methods 0.000 claims description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 15
- 238000001723 curing Methods 0.000 claims description 13
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 12
- 238000007493 shaping process Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 11
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 10
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 9
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 9
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 7
- 239000004593 Epoxy Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 230000000994 depressogenic effect Effects 0.000 claims description 5
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 238000006467 substitution reaction Methods 0.000 claims description 3
- 238000009755 vacuum infusion Methods 0.000 claims description 3
- 238000004132 cross linking Methods 0.000 claims description 2
- 238000005457 optimization Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 claims 1
- 229920002472 Starch Polymers 0.000 abstract description 10
- 239000008107 starch Substances 0.000 abstract description 10
- 235000019698 starch Nutrition 0.000 abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 125000004430 oxygen atom Chemical group O* 0.000 abstract description 3
- 239000011230 binding agent Substances 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 238000007711 solidification Methods 0.000 description 7
- 230000008023 solidification Effects 0.000 description 7
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 6
- 239000003822 epoxy resin Substances 0.000 description 6
- 239000011810 insulating material Substances 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000005011 phenolic resin Substances 0.000 description 6
- 229920000647 polyepoxide Polymers 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 5
- 229920001568 phenolic resin Polymers 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 238000002679 ablation Methods 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 4
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 230000003026 anti-oxygenic effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- VKEQBMCRQDSRET-UHFFFAOYSA-N Methylone Chemical compound CNC(C)C(=O)C1=CC=C2OCOC2=C1 VKEQBMCRQDSRET-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910004012 SiCx Inorganic materials 0.000 description 1
- XCKAPGALQORDHA-UHFFFAOYSA-L [Sn+4].CCCC[Sn++]CCCC.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O Chemical compound [Sn+4].CCCC[Sn++]CCCC.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O XCKAPGALQORDHA-UHFFFAOYSA-L 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- RCHKEJKUUXXBSM-UHFFFAOYSA-N n-benzyl-2-(3-formylindol-1-yl)acetamide Chemical compound C12=CC=CC=C2C(C=O)=CN1CC(=O)NCC1=CC=CC=C1 RCHKEJKUUXXBSM-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 1
- ZMYXZXUHYAGGKG-UHFFFAOYSA-N propoxysilane Chemical compound CCCO[SiH3] ZMYXZXUHYAGGKG-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C04B32/00—Artificial stone not provided for in other groups of this subclass
- C04B32/005—Artificial stone obtained by melting at least part of the composition, e.g. metal
-
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
-
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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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
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
- C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- Chemical Kinetics & Catalysis (AREA)
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
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Abstract
The present invention relates to a kind of Carbon Fiber Rigid thermal insulation tiles, the chopped carbon fiber including constituting skeleton, and the Si/C/O glass for being bonded the chopped carbon fiber is bonded phase.The present invention also provides the preparation methods of the Carbon Fiber Rigid thermal insulation tile.The present invention prepares the bonding phase between carbon fiber using silicone resin, Si/C/O glass, which is generated, when being carbonized cracking is bonded phase, play the role of being bonded chopped carbon fiber skeleton, and after mutually being aoxidized under high temperature aerobic environment due to Si/C/O glass bonding, surface can generate layer of silicon dioxide glass-film, to prevent oxygen atom from further aoxidizing internal substance, therefore there is stronger inoxidizability, and the carbon yield that silicone resin cracks under an inert atmosphere is high, with use starch as binder compared with, mechanical strength is also higher.
Description
The application is the divisional application of entitled " a kind of Carbon Fiber Rigid thermal insulation tile and preparation method thereof ", original application
The applying date be 2016.12.2, application No. is 201611100591.5.
Technical field
The present invention relates to functional composite material technical field more particularly to a kind of Carbon Fiber Rigid thermal insulation tile and its preparation sides
Method.
Background technique
Carbon Fiber Rigid thermal insulation tile has many advantages, such as that heatproof is high, light porous, good heat-insulation effect, can be directly as superhigh temperature
Heat-barrier material uses, and is also used as raw material, prepares light ablative material by compound resin or anti-oxidant carbon base ceramics are multiple
Condensation material.
United States Atomic Energy Commission discloses a kind of preparation side of fibrous insulating material in United States Patent (USP) 3577344
Method.The patent uses the oxide ceramic fibres such as chopped carbon fiber, quartz fibre or alumina silicate to be raw material, solubility is used to form sediment
Powder is bonding agent, prepares corresponding fibrous insulating material green body by wet therapy forming process, and then makes the starch after gelatinization polymerization
Cracking forms bonding charcoal phase in high temperature furnace.The fibrous insulating material is used for nuclear power field high-temperature hot protection.Due to the fiber
Heat-barrier material is bonding agent using soluble starch, and the carbon yield after the starch after polymerization cracks in high temperature furnace is lower, causes
The Carbon Fiber Rigid thermal insulation tile mechanical strength of preparation is inadequate.
No. 3577344 lightweight fibres of above-mentioned United States Patent (USP) are disclosed disclosed in U.S. Department of Energy in United States Patent (USP) 4152482
Tie up the preparation process amelioration of heat-barrier material.United States Patent (USP) 4152482, by layered filtration, multi-shell curing technique, eliminate viscous
The stress accumulation generated in fibrous matrix when connecing phase resin solidification.In addition, layered filtration technique makes the light fibre heat-insulated
The structure of material is more controllable, and different fibrous matrixes, high emissivity filler etc. can be used to realize product in different layers
It can change of gradient.Fibrous material partnership of the U.S. (Fiber Materials Incorporation, FMI) produces one kind
The trade mark isCarbon fiber light rigidity thermal insulation tile.The carbon fiber that diameter is 14-16 microns is chopped to 1.6mm
It is long, rear wet forming is mixed with beating with water soluble phenol resin and solvent, after phenolic resin curing under 1440 ℉ (782.2 DEG C)
Carbonization, and then be made after 3240 ℉ (1782.2 DEG C) high-temperature heat treatmentCarbon Fiber Rigid thermal insulation tile.The density of Carbon Fiber Rigid thermal insulation tile is 0.15-0.23g/cm3, thickness direction compressive strength is 0.2-
0.6MPa.Changqing Hong etc. is prepared for a kind of carbon fiber-based ablator PICA (phenolic impregnated 3-
D fine-woven pierced carbon fabric ablator), density is 0.352~0.701g/cm3,
4.5MW/m2Oxygen/acetylene torch ablation test in, linear ablative rate is 0.019~0.036mm/s, and mass ablative rate is
0.045~0.061g/s.This kind of PICA material is carefully compiled by 3D and punctures the preparation of carbon fiber precast body composite phenolic resin.But this
A little materials using phenolic resin residue carbon of biomass pyrolysis as bonding phase, can burn under 1200 DEG C of high temperature air atmosphere, lead to it
Inoxidizability is not high, and temperature tolerance is insufficient.
Summary of the invention
The purpose of the present invention is overcoming the disadvantage that existing Carbon Fiber Rigid thermal insulation tile mechanical strength is inadequate, temperature tolerance is insufficient,
Finally provide that a kind of temperature tolerance is higher, carbon fiber light rigidity lightweight, that intensity is bigger using different technical solutions
Thermal insulation tile and preparation method thereof can be used as oxygen-free atmosphere super high sintering temperature furnace, nuclear power station high-temperature service, chemical reactor etc.
Thermally protective materials use.
For this purpose, the present invention achieves the object of the present invention by following technical solution:
1, a kind of Carbon Fiber Rigid thermal insulation tile, wherein the chopped carbon fiber including constituting skeleton, and it is described for being bonded
The Si/C/O glass of chopped carbon fiber is bonded phase.
2, Carbon Fiber Rigid thermal insulation tile according to technical solution 1, wherein the Si/C/O glass bonding is mutually by silicon tree
Rouge prepolymer, crosslinking agent, catalyst and organic solvent are according to 10:(0.1~10): (0.1~10): the mass ratio of (10~100)
It is sucked in carbon fiber dry body after being configured to silicone precursor mixed liquor by Vacuum infusion techniques, using room temperature curing, carbon
Change and is obtained after high-temperature heat treatment.
3, the Carbon Fiber Rigid thermal insulation tile according to technical solution 2, in which:
The silicone prepolymer be selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane,
Dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and the epoxy radicals end-blocking poly dimethyl silicon that hydroxy-end capped phenyl replaces
One of group of oxygen alkane composition or several mixtures；The viscosity of the silicone prepolymer is 200~100000cst；With/
Or
The crosslinking agent is selected from by ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxy silane
One of group of alkane and dimethyl diethoxysilane composition or several mixtures；And/or
The catalyst is dibutyl tin dilaurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from one of group being made of benzene, dimethylbenzene, styrene and acetone or several mixing
Object.
4, the Carbon Fiber Rigid thermal insulation tile according to technical solution 1 or 2, wherein the length of the carbon fiber be 1~
5mm, diameter are 8~12 μm.
5, a kind of preparation method of Carbon Fiber Rigid thermal insulation tile, wherein the following steps are included:
(1) the wet base of chopped carbon fiber is obtained by wet forming, carbon fiber dry body is obtained after drying；
(2) silicone precursor is made after mixing silicone prepolymer, crosslinking agent, catalyst and organic solvent to mix
Liquid；
(3) the carbon fiber dry body is impregnated using silicone precursor mixed liquor, using room temperature curing, carbonization and high temperature
Carbon Fiber Rigid thermal insulation tile is obtained after heat treatment.
6, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 5, wherein in the step (2):
According to 10:(0.1~10): (0.1~10): the mass ratio of (10~100) by silicone prepolymer, crosslinking agent, urge
Silicone precursor mixed liquor is made after agent and organic solvent mixing.
7, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 5 or 6, wherein the step (2)
In:
The silicone prepolymer be selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane,
Dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and the epoxy radicals end-blocking poly dimethyl silicon that hydroxy-end capped phenyl replaces
One of group of oxygen alkane composition or several mixtures；The viscosity of the silicone prepolymer is 200~100000cst；With/
Or
The crosslinking agent is selected from by ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxy silane
One of group of alkane and dimethyl diethoxysilane composition or several mixtures；And/or
The catalyst is dibutyl tin dilaurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from one of group being made of benzene, dimethylbenzene, styrene and acetone or several mixing
Object.
8, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 5, wherein in the step (1):
Chopped carbon fiber is mixed with water according to the mass ratio of 1:150~250, wet base is obtained by filtration after stirring to pulp, then
Wet base is packed into shaping mould, wet base is depressed by preset height according to the target density of material, dry 4 at 60~150 DEG C~
36 hours, obtain carbon fiber dry body.
9, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 5, wherein in the step (1) also
Including removing glue step:
Carbon fiber is prescinded to 1~5mm, chopped carbon fiber is obtained, chopped carbon fiber is mixed with acetone, is stirring mixing water
Under conditions of cold reflux, acetone is heated to 55~60 DEG C and is flowed back 24~72 hours, cleaning is attached to chopped carbon fiber surface
Epoxy resin surface treating agent, obtain chopped carbon fiber then by strainer filtering, then after making acetone volatilize.
10, the preparation method of the Carbon Fiber Rigid thermal insulation tile according to technical solution 5, wherein in the step (3):
Vacuum impregnation and room temperature curing specifically: be first placed in the carbon fiber dry body that step (1) obtains together with shaping mould
In vacuum impregnation tank, the vacuum impregnation tank is sealed and is evacuated to 10-2~10-4atm；By silicone resin made from step (2)
Presoma mixed liquor injects in the vacuum impregnation tank, and liquid level is made not have the shaping mould upper surface, and opening blow valve makes tank
Internal air pressure balance stands 24~100 hours, so that silicone resin crosslinking curing to 1atm；And/or
The carbonization is heated to 600~1000 DEG C in argon gas atmosphere stove and keeps the temperature 1~10 hour；And/or
The high-temperature heat treatment is heated to 1500~2200 DEG C in argon gas atmosphere stove and keeps the temperature 1~10 hour.
Implement Carbon Fiber Rigid thermal insulation tile and preparation method thereof of the invention, has the advantages that
1, the present invention prepares the bonding phase between carbon fiber using silicone resin, and it is viscous to generate Si/C/O glass when being carbonized cracking
Phase is connect, which is bonded the point of intersection for being mutually covered on carbon fiber surface and carbon fiber and carbon fiber, plays bonding and is chopped
The effect of carbon fiber skeleton, and since Si/C/O glass bonding is mutually under high temperature aerobic environment after oxidation, surface can generate one
Layer silica glass film has inoxidizability so that oxygen atom be prevented further to aoxidize internal substance.Therefore, with use
Phenolic resinoid residue carbon of biomass pyrolysis is compared as the material of bonding phase, the inoxidizability of Carbon Fiber Rigid thermal insulation tile produced by the present invention
It is stronger.On the other hand, with use starch as binder compared with, carbon yield that silicone resin of the invention cracks under an inert atmosphere
Higher than the starch of gelatinization, therefore mechanical strength is also higher by 20%~50%.
2, the present invention makes silicone precursor mixed liquor sufficiently in conjunction with carbon fiber dry body by vacuum impregnation technique, is formed
Carbon Fiber Rigid thermal insulation tile it is uniform in material, overall performance stablize, be more advantageous to Si/C/O glass bonding mutually play its bonding make
With.
3, present invention optimizes the proportions of each raw material in the silicone precursor mixed liquor used, when silicone resin pre-polymerization
Object, crosslinking agent, catalyst and organic solvent are according to 10:(0.1~10): (0.1~10): the mass ratio of (10~100) is prepared
When, enable to the Si/C/O glass bonding of cracking mutually to more uniformly spread, mechanical strength is higher, and antioxygenic property is more preferable.
Detailed description of the invention
Fig. 1 is the Carbon Fiber Rigid thermal insulation tile preparation technology flow chart according to the preferred embodiment of the present invention；
Fig. 2 is the shooting picture in kind of the Carbon Fiber Rigid thermal insulation tile according to made from the preferred embodiment of the present invention；
Fig. 3 is the Carbon Fiber Rigid thermal insulation tile stereoscan photograph according to made from the preferred embodiment of the present invention.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
Member's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
As described above, the present invention provides a kind of Carbon Fiber Rigid thermal insulation tile in first aspect, wherein the Carbon Fiber Rigid
Thermal insulation tile includes the chopped carbon fiber for constituting skeleton, and the Si/C/O glass for being bonded the chopped carbon fiber is bonded phase.
In some preferred embodiments, the length of chopped carbon fiber is 1~5mm, and diameter is 8~12 μm.Further
Preferably, the length of chopped carbon fiber is 2mm, and diameter is 10 μm.Carbon fiber used in the present invention can be but not limited to
The carbon fiber of the trades mark such as T-300, T-700, T-800, T-1000.
In some preferred embodiments, Si/C/O glass bonding mutually by silicone prepolymer A, crosslinking agent B,
Catalyst C and organic solvent D is sucked in carbon fiber dry body after being configured to silicone precursor mixed liquor by Vacuum infusion techniques,
Using being obtained after room temperature curing, carbonization and high-temperature heat treatment.Preferably, silicone prepolymer in silicone precursor mixed liquor
A, the mass ratio of crosslinking agent B, catalyst C and organic solvent D is 10:(0.1~10): (0.1~10): (10~100).Such as it can
Think 10:(0.1,0.5,2,5 or 10): (0.1,0.5,2,5 or 10): (10,20,50 or 100).
The present invention prepares the bonding phase between carbon fiber using silicone resin.Silicone resin disperse phase is after hardening in carbon fiber surface
Face and carbon fiber and carbon fiber point of intersection are evenly dispersed.When 800 DEG C of carbonizations crack, it is viscous that silicone resin is cracked to form Si/C/O glass
Connect phase, i.e. SiCxOyGlass phase, the glass phase are covered on the point of intersection of carbon fiber surface and carbon fiber and carbon fiber, play bonding
The effect of chopped carbon fiber skeleton.After mutually being aoxidized under high temperature aerobic environment due to Si/C/O glass bonding, surface can generate one
Layer silica glass film, to prevent oxygen atom from further aoxidizing internal substance, therefore Si/C/O glass bonding mutually has
Inoxidizability, when undergoing high temperature, ablation shrinkage is smaller, high reliablity；If replacing silicon using epoxy resin or phenolic aldehyde
If resin, oxygen abundance under conditions of ablation after basic noresidue, ablation shrinkage is big, thus reliability obviously compared with
It is low.
In some preferred embodiments, the silicone prepolymer A is selected from by hydroxy-end capped polydimethylsiloxanes
Dimethyl silicone polymer, the amino-terminated poly dimethyl silicon that alkane, hydroxy-end capped polydiphenylsiloxane, hydroxy-end capped phenyl replace
One of group of oxygen alkane and epoxy radicals end-blocking dimethyl silicone polymer composition or several mixtures.Wherein hydroxy-end capped phenyl
Substituted dimethyl silicone polymer can replace for part phenyl, and degree of substitution can be 30% to 70%.It may further be preferable that
The viscosity of the silicone prepolymer is 200~100000cst；Further preferably 10000~20000CSt；In addition further excellent
It is selected as 2000~4000CSt.
In some preferred embodiments, the crosslinking agent B is selected from by ethyl orthosilicate, methyl orthosilicate, methyl
One of group of trimethoxy silane, methyltriethoxysilane and dimethyl diethoxysilane composition or several mixing
Object；It may further be preferable that the crosslinking agent B is ethyl orthosilicate.
In some preferred embodiments, the catalyst C is dibutyl tin dilaurate or γ-three second of amine propyl
Oxysilane.The inventors discovered that using dibutyl tin dilaurate as catalyst in system of the invention, capable of making
It obtains curing reaction speed faster, the time is fully cured no more than 24 hours；If using other catalyst such as γ-amine propyl
For triethoxysilane as catalyst, being fully cured the time then needs 48 hours or more.Therefore in some preferred embodiments
In, the catalyst C is dibutyl tin dilaurate.
In some preferred embodiments, the organic solvent D is selected from and is made of benzene, dimethylbenzene, styrene and acetone
One of group or several mixtures；It may further be preferable that organic solvent D is dimethylbenzene.It is more highly preferred at one
Embodiment in, silicone prepolymer A be hydroxyl endblocked polydimethylsiloxane, crosslinking agent B is ethyl orthosilicate, catalyst C
For dibutyl tin dilaurate, organic solvent D is dimethylbenzene, obtains silicon after mixing according to the mass ratio of 10:1:0.1:50
Resin precursor mixed liquor.
The present invention provides a kind of preparation method of Carbon Fiber Rigid thermal insulation tile in second aspect.Fig. 1 is please referred to, is
Carbon Fiber Rigid thermal insulation tile preparation technology flow chart according to the preferred embodiment of the invention.Wherein, the preparation method includes such as
Lower step:
(1) the wet base of chopped carbon fiber is obtained by wet forming, carbon fiber dry body is obtained after drying；
(2) silicone precursor is made after mixing silicone prepolymer, crosslinking agent, catalyst and organic solvent to mix
Liquid；
(3) silicone precursor mixed liquor impregnation of carbon fibers dry body is used, such as carbon fiber is impregnated by vacuum impregnation technique
Dry body is tieed up, to make carbon fiber dry body absorb the silicone precursor mixed liquor, using room temperature curing, carbonization and high warm
Carbon Fiber Rigid thermal insulation tile is obtained after processing.
In some preferred embodiments, in the step (1): by chopped carbon fiber and water according to 1:150~250
Mass ratio mixes, and wet base is obtained by filtration after stirring to pulp, then wet base is packed into shaping mould, will be wet according to the target density of material
Base is depressed into preset height, 4~36 hours dry at 60~150 DEG C, obtains carbon fiber dry body.It specifically, will be except short after glue
It cuts carbon fiber to mix with deionized water, mashing is sufficiently stirred in agitator, slurry is transferred in filtering tooling, filter off big absolutely
Then wet base is packed into shaping mould, wet base is depressed into scheduled height according to the target density of material by partial water, 60~
Dry 4~36 hours (4,10,20,30 or 36), it is dry to obtain carbon fiber under 150 DEG C (such as 60 DEG C, 80 DEG C, 100 DEG C or 150 DEG C)
Base；Chopped carbon fiber and the mass ratio of deionized water are 1:150~250 (such as 1:150,1:200 or 1:250), further excellent
It is selected as 1:200.
Further include except glue step in some preferred embodiments, in the step (1): i.e. by diameter for 8~
12 μm of carbon fiber obtains chopped carbon fiber after prescinding to 1~5mm long.Chopped carbon fiber is mixed with acetone then, is being stirred
Under conditions of water cooled reflux, acetone is heated to 55~60 DEG C and is flowed back 24~72 hours, cleaning is attached to chopped carbon fiber
The epoxy resin surface treating agent on surface obtains chopped carbon fiber then by strainer filtering, then after making acetone volatilize.Tool
Body, chopped carbon fiber is placed in the kettle for filling acetone, kettle top is equipped with stirring and water cooled reflux device.Opening stirs mixing water
Acetone is heated to 55~60 DEG C (such as 55 DEG C, 58 DEG C or 60 DEG C) and flowed back 24~72 hours (24,36,48 by cold reflux device
Or 72 hours), the epoxy resin adhesive for being attached to carbon fiber surface is thoroughly washed.A kind of optimization except glue program is perseverance
60 DEG C of temperature are flowed back 48 hours, which is enough thoroughly to clean up the epoxy resin adhesive for being attached to carbon fiber surface.With
Afterwards, the carbon fiber cleaned in kettle is come out by strainer filtering, is dried in draught cupboard, so that acetone sufficiently volatilizees.
In some preferred embodiments, in step (2): according to 10:(0.1~10): (0.1~10): (10~100)
Mass ratio will silicone prepolymer A, crosslinking agent B, catalyst C and organic solvent D mix after be made silicone precursor mix
Liquid.It such as can be 10:(0.1,0.5,2,5 or 10): (0.1,0.5,2,5 or 10): (10,20,50 or 100).Wherein silicon tree
Rouge prepolymer A, crosslinking agent B, catalyst C and organic solvent D are as described in the first aspect of the invention.
In some preferred embodiments, vacuum impregnation and room temperature curing in the step (3) specifically: first by step
(1) the carbon fiber dry body obtained is placed in vacuum impregnation tank together with shaping mould, and the vacuum impregnation tank is sealed and is locked, and is taken out
Vacuum is to 10-2~10-4Atm, more preferably 10-4atm；It again will be described in the injection of silicone precursor mixed liquor made from step (2)
In vacuum impregnation tank, liquid level is made not have the shaping mould upper surface, opening blow valve keeps air pressure balance in tank body quiet to 1atm
It sets 24~100 hours, so that silicone resin full cross-linked solidification at room temperature.
In some preferred embodiments, carbonization treatment in the step (3) specifically: the carbon fiber after solidification is rigid
Property thermal insulation tile blank is put into carbide furnace, is warming up to 600~1000 DEG C (such as 600 DEG C, 800 DEG C or 1000 under an argon atmosphere
DEG C), 1~10 hour (such as 1,2,5 or 10 hour) is kept the temperature, so that silicone resin carbonization, generates Si/C/O glass and be bonded phase.
In one more preferably embodiment, it is heated to 800 DEG C in argon gas atmosphere stove, keeps the temperature 2 hours, obtains Carbon Fiber Rigid
The ripe base of thermal insulation tile.
In some preferred embodiments, step (3) the high temperature heat treatment specifically: add in argon gas atmosphere stove
Heat is to 1500~2200 DEG C (such as 1500 DEG C, 1800 DEG C or 2200 DEG C) and keeps the temperature 1~10 hour (such as 1,2,5 or 10 are small
When).For example, the ripe base of Carbon Fiber Rigid thermal insulation tile is put into the pyrolysis furnace of argon atmosphere, 1800 DEG C are warming up to, keeps the temperature 1 hour,
With the thermal stress for eliminating resin solidification, carbonisation accumulates in thermal insulation tile green body, the production of Carbon Fiber Rigid thermal insulation tile is finally obtained
Product.
Fig. 2 and Fig. 3 are please referred to, is the Carbon Fiber Rigid thermal insulation tile according to made from the preferred embodiment of the present invention
Material object shooting picture and stereoscan photograph.From fig. 2 it can be seen that the Carbon Fiber Rigid thermal insulation tile includes chopped carbon fiber bone
Frame, and the Si/C/O glass bonding phase of the cracking that is distributed between chopped carbon fiber, Si/C/O glass bonding are mutually covered on carbon
The point of intersection of fiber surface and carbon fiber and carbon fiber plays the role of being bonded chopped carbon fiber skeleton.
The present invention will be hereafter further detailed in the form of embodiment, but since the present inventor can not
Present inventive concept all technical solutions obtained are based on It is not necessary to exhaustively show, protection scope of the present invention should not necessarily be limited by
Following examples, and should include being based on present inventive concept all technical solutions obtained.
Embodiment 1
1. prescinding the carbon fiber that diameter is 10 μm to 2mm long, chopped carbon fiber is placed in the kettle for filling acetone, kettle top
Stirring and water cooled reflux device are installed.Stirring and water cooled reflux device are opened, acetone is heated to 55 DEG C and is flowed back 48 hours,
The epoxy resin adhesive for being attached to carbon fiber surface is thoroughly washed.The carbon fiber cleaned in kettle is gone out by strainer filtering
Come, is dried in draught cupboard, so that acetone sufficiently volatilizees.
2. abundant in agitator by according to mass ratio being that 1:150 is mixed with deionized water except the chopped carbon fiber after glue
Slurry is transferred in filtering tooling, filters off the water of the overwhelming majority, wet base is then packed into shaping mould by stirring to pulp, according to
Wet base is depressed into preset height by the target density of material, 24 hours dry at 120 DEG C, obtains carbon fiber dry body.
3. the carbon fiber dry body with shaping mould is placed in vacuum impregnation tank, impregnating autoclave is sealed and locked, then
Impregnating autoclave is evacuated to 10-2atm。
4. preparing silicone resin precursor mixed liquor: by hydroxyl endblocked polydimethylsiloxane, ethyl orthosilicate, tin dilaurate
Dibutyl tin and dimethylbenzene are spare after mixing according to the mass ratio of 10:1:0.1:50.Wherein, hydroxy-end capped poly dimethyl silicon
The viscosity of oxygen alkane is 4000cst.
5. making liquid level not have the setting in step 4. silicone precursor mixed liquor injection vacuum impregnation tank obtained
Mould upper surface, opening blow valve makes air pressure balance in tank body 24 hours be stood, so that silicone resin is full cross-linked solid to 1atm
Change.
6. the Carbon Fiber Rigid thermal insulation tile blank after solidification is put into carbide furnace, it is warming up to 800 DEG C under an argon atmosphere,
Heat preservation 2 hours, so that silicone resin carbonization, generates Si/C/O glass and be bonded phase.
7. the 6. ripe base of Carbon Fiber Rigid thermal insulation tile that step is prepared is put into the pyrolysis furnace of argon atmosphere, it is warming up to 1800
DEG C, 2 hours are kept the temperature, with the thermal stress for eliminating resin solidification, carbonisation accumulates in thermal insulation tile green body, finally obtains carbon fiber
Rigid thermal insulation tile product.
Embodiment 2 to 22
Other than the content shown in the lower table 1 and table 2, carry out in the same manner as example 1 embodiment 2 to
22.The mechanical strength of the obtained Carbon Fiber Rigid thermal insulation tile of test, as a result referring to table 2.
Comparative example 1~2
The present invention also use United States Patent (USP) 3577344 disclosed in fibrous insulating material as a comparison case 1.Specifically prepared
Journey is as follows: it is 0.25 inch long to be that 0.5~0.7 μm of carbon fiber is cut into for average diameter, then will be after carbon fiber, starch and water mixes
It is beaten, the mass ratio of starch and carbon fiber is 0.75:1 in slurry obtained, and the ratio of carbon fiber and water is every 1kg carbon fiber
Tie up corresponding 380L water.Slurry is filtered by 0.25 inch of strainer, and continues stirring 30 minutes, is then poured into mold
In.It is dehydrated 7 minutes by vacuum tank in communication, and the temperature of mold increases to 95 degrees Celsius.In the atmosphere of saturated steam
Lower persistently standing 4 hours are enclosed, starch gelatinization is made.It is later, compound obtained is 24 hours dry in the environment of compared with low humidity,
Then at 1000 degrees Centigrade 16 hours to realize carbonization.Through detecting, the thickness direction pressure of the fibrous insulating material of comparative example 1
Contracting intensity is specially 0.1~0.2MPa.Therefore compressive strength of the Carbon Fiber Rigid thermal insulation tile prepared by the present invention in thickness direction
The fibrous insulating material prepared than comparative example 1 is generally higher by 20%~50%, and some is even higher by 100% or more.This is because
The carbon yield that silicone resin cracks under an inert atmosphere in Carbon Fiber Rigid thermal insulation tile produced by the present invention is higher than the starch of gelatinization.
The present invention also use United States Patent (USP) 4152482 disclosed in Carbon Fiber Rigid thermal insulation tile as a comparison case 2.Specific system
Standby process is as follows: the carbon fiber that average diameter is 5~7 μm is cut into it is 250 μm long, then by carbon fiber and phenolic resin according to 1:
0.35 mass ratio is mixed, and wherein the partial size of phenolic resin is 10 μm or so, and by the strainer of 0.5mm to carbon fiber
It is filtered.It is beaten after water then is added in the mixture, wherein 300L water is added in every 1kg mixture, slurry is continued to stir
It 20 minutes, is then poured into mold.It is dehydrated 15 minutes by vacuum tank in communication, and carbon fiber and phenolic resin are constituted
Compound tiles molding under the action of vacuum.Mold temperature is heated to 130 DEG C.Standing 24 hours under air atmosphere makes phenolic aldehyde
Resin solidification, and remove extra moisture.Material obtained is heated to 1000 DEG C under nitrogen atmosphere, and continuous heating 30 divides
Carbonization is realized after clock, and the Carbon Fiber Rigid thermal insulation tile of comparative example 2 is made.5min detection pair is heated at 1200 DEG C, under air atmosphere
The antioxygenic property of the Carbon Fiber Rigid thermal insulation tile of ratio 2.The experimental results showed that Carbon Fiber Rigid prepared by comparative example 2 is heat-insulated
Watt in 1200 DEG C of generation combustion phenomena, final residual quality is 0.5%.And the present invention is cracked under an inert atmosphere due to silicone resin
Product Si/C/O glass bonding mutually there is inoxidizability, therefore Carbon Fiber Rigid thermal insulation tile made from embodiment 1-11 is 1200
DEG C heating 5min after structure do not collapse, quality increase be 10%~20%.
Claims (10)
1. a kind of Carbon Fiber Rigid thermal insulation tile, which is characterized in that the chopped carbon fiber including constituting skeleton, and for being bonded
State the Si/C/O glass bonding phase of chopped carbon fiber.
2. Carbon Fiber Rigid thermal insulation tile according to claim 1, which is characterized in that Si/C/O glass is bonded mutually using silicon tree
Rouge prepares the bonding phase between carbon fiber, generates when being carbonized cracking.
3. Carbon Fiber Rigid thermal insulation tile according to claim 1 or 2, which is characterized in that the Si/C/O glass is bonded phase
By silicone prepolymer, crosslinking agent, catalyst and organic solvent according to 10:(0.1~10): (0.1~10): (10~100)
Mass ratio is sucked in carbon fiber dry body after being configured to silicone precursor mixed liquor by Vacuum infusion techniques, solid using room temperature
Change, obtained after carbonization and high-temperature heat treatment.
4. Carbon Fiber Rigid thermal insulation tile according to claim 3, it is characterised in that:
The silicone prepolymer is selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane, hydroxyl
Block dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and epoxy radicals end-blocking dimethyl silicone polymer that phenyl replaces
One of group of composition or several mixtures；The dimethyl silicone polymer that wherein hydroxy-end capped phenyl replaces is part phenyl
Replace, degree of substitution is 30% to 70%；The viscosity of the silicone prepolymer be 200~100000cst, preferably 10000~
20000CSt；Further preferably 2000~4000CSt；And/or
The crosslinking agent be selected from by ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane and
One of group of dimethyl diethoxysilane composition or several mixtures；And/or
The catalyst is dibutyl tin dilaurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from one of group being made of benzene, dimethylbenzene, styrene and acetone or several mixtures.
5. Carbon Fiber Rigid thermal insulation tile according to claim 3, it is characterised in that:
The silicone prepolymer is hydroxyl endblocked polydimethylsiloxane, and the crosslinking agent is ethyl orthosilicate, the catalysis
Agent is dibutyl tin dilaurate, and the organic solvent is dimethylbenzene, is obtained after mixing according to the mass ratio of 10:1:0.1:50
To silicone precursor mixed liquor；And/or
The length of the carbon fiber is 1~5mm, and diameter is 8~12 μm；Preferably, the length of chopped carbon fiber is 2mm, diameter
It is 10 μm.
6. a kind of preparation method of Carbon Fiber Rigid thermal insulation tile, which comprises the following steps:
(1) the wet base of chopped carbon fiber is obtained by wet forming, carbon fiber dry body is obtained after drying；
(2) silicone precursor mixed liquor is made after mixing silicone prepolymer, crosslinking agent, catalyst and organic solvent；
(3) the carbon fiber dry body is impregnated using silicone precursor mixed liquor, at room temperature curing, carbonization and high warm
Carbon Fiber Rigid thermal insulation tile is obtained after reason；
In the step (2):
According to 10:(0.1~10): (0.1~10): the mass ratio of (10~100) is by silicone prepolymer, crosslinking agent, catalyst
Silicone precursor mixed liquor is made with after organic solvent mixing.
7. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 6, which is characterized in that in the step (2):
The silicone prepolymer is selected from by hydroxyl endblocked polydimethylsiloxane, hydroxy-end capped polydiphenylsiloxane, hydroxyl
Block dimethyl silicone polymer, amino-terminated dimethyl silicone polymer and epoxy radicals end-blocking dimethyl silicone polymer that phenyl replaces
One of group of composition or several mixtures；The dimethyl silicone polymer that wherein hydroxy-end capped phenyl replaces is part phenyl
Replace, degree of substitution is 30% to 70%；The viscosity of the silicone prepolymer be 200~100000cst, preferably 10000~
20000CSt；Further preferably 2000~4000CSt；And/or
The crosslinking agent be selected from by ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane and
One of group of dimethyl diethoxysilane composition or several mixtures；And/or
The catalyst is dibutyl tin dilaurate or γ-amine propyl-triethoxysilicane；And/or
The organic solvent is selected from one of group being made of benzene, dimethylbenzene, styrene and acetone or several mixtures.
8. the preparation method of Carbon Fiber Rigid thermal insulation tile according to claim 6, which is characterized in that the silicone resin pre-polymerization
Object is hydroxyl endblocked polydimethylsiloxane, and the crosslinking agent is ethyl orthosilicate, and the catalyst is di lauric dibutyl
Tin, the organic solvent are dimethylbenzene, obtain silicone precursor mixing after mixing according to the mass ratio of 10:1:0.1:50
Liquid.
9. the preparation method of Carbon Fiber Rigid thermal insulation tile according to any one of claim 6~8, it is characterised in that:
In the step (1): chopped carbon fiber is mixed with water according to the mass ratio of 1:150~250, further preferably 1:
200, wet base is obtained by filtration after stirring to pulp, then wet base is packed into shaping mould, is depressed into wet base according to the target density of material
Preset height, it is 4~36 hours dry at 60~150 DEG C, obtain carbon fiber dry body；
Preferably, further include except glue step in the step (1): carbon fiber being prescinded to 1~5mm, chopped carbon fiber is obtained, it is excellent
Selection of land, the length of chopped carbon fiber are 2mm, and diameter is 10 μm, chopped carbon fiber are mixed with acetone, in stirring and water cooled reflux
Under conditions of, acetone is heated to 55~60 DEG C and is flowed back 24~72 hours, cleaning is attached to the epoxy on chopped carbon fiber surface
Resinae surface treating agent obtains chopped carbon fiber then by strainer filtering, then after so that acetone is volatilized；A kind of optimization removes glue
Program is 60 DEG C of constant temperature and flows back 48 hours.
10. the preparation method of Carbon Fiber Rigid thermal insulation tile according to any one of claim 6~8, which is characterized in that institute
It states in step (3):
Vacuum impregnation and room temperature curing specifically: the carbon fiber dry body that step (1) obtains first is placed in vacuum together with shaping mould
In impregnating autoclave, the vacuum impregnation tank is sealed and is evacuated to 10-2~10-4atm；By silicone resin forerunner made from step (2)
Body mixed liquor injects in the vacuum impregnation tank, and liquid level is made not have the shaping mould upper surface, and opening blow valve makes in tank body
Air pressure balance stands 24~100 hours, so that silicone resin crosslinking curing to 1atm；And/or
The carbonization is heated to 600~1000 DEG C in argon gas atmosphere stove and keeps the temperature 1~10 hour；Preferably, the carbonization exists
It is heated to 800 DEG C in argon gas atmosphere stove, keeps the temperature 2 hours, obtains the ripe base of Carbon Fiber Rigid thermal insulation tile；And/or
The high-temperature heat treatment is heated to 1500~2200 DEG C in argon gas atmosphere stove and keeps the temperature 1~10 hour；Preferably, described
High-temperature heat treatment is warming up to 1800 DEG C in argon gas atmosphere stove, keeps the temperature 1 hour.
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| CN201811061423.9A CN109133959B (en) | 2016-12-02 | 2016-12-02 | Carbon fiber rigid heat insulation tile and preparation method thereof |
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| CN110981487A (en) * | 2019-11-22 | 2020-04-10 | 航天特种材料及工艺技术研究所 | Preparation method of ceramic-based modified carbon fiber heat insulation material |
| CN114014685A (en) * | 2021-11-26 | 2022-02-08 | 航天特种材料及工艺技术研究所 | Antioxidant porous carbon-ceramic composite material and preparation method thereof |
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| CN114213156B (en) * | 2021-12-28 | 2023-06-16 | 山东工业陶瓷研究设计院有限公司 | Preparation method of ceramic heat-insulating tile surface coating |
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Also Published As
| Publication number | Publication date |
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| CN109133959B (en) | 2021-05-07 |
| CN106747267A (en) | 2017-05-31 |
| CN106747267B (en) | 2019-01-08 |
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