CN117362057B - Light anti-cracking heat-insulating refractory material and preparation method thereof - Google Patents
Light anti-cracking heat-insulating refractory material and preparation method thereof Download PDFInfo
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- CN117362057B CN117362057B CN202311670186.7A CN202311670186A CN117362057B CN 117362057 B CN117362057 B CN 117362057B CN 202311670186 A CN202311670186 A CN 202311670186A CN 117362057 B CN117362057 B CN 117362057B
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- 239000011819 refractory material Substances 0.000 title claims abstract description 57
- 238000005336 cracking Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 68
- 238000005245 sintering Methods 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 239000010881 fly ash Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000010451 perlite Substances 0.000 claims abstract description 15
- 235000019362 perlite Nutrition 0.000 claims abstract description 15
- 229920002522 Wood fibre Polymers 0.000 claims abstract description 14
- 239000010440 gypsum Substances 0.000 claims abstract description 14
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 14
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 14
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000002025 wood fiber Substances 0.000 claims abstract description 14
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 36
- 238000002156 mixing Methods 0.000 claims description 32
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 23
- 150000001263 acyl chlorides Chemical class 0.000 claims description 22
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 19
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 19
- 239000004327 boric acid Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- ZPKSAIWDCQVXSQ-UHFFFAOYSA-N (4-aminophenoxy)boronic acid Chemical compound NC1=CC=C(OB(O)O)C=C1 ZPKSAIWDCQVXSQ-UHFFFAOYSA-N 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 5
- 238000000748 compression moulding Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 230000009970 fire resistant effect Effects 0.000 claims 1
- 238000009740 moulding (composite fabrication) Methods 0.000 claims 1
- 239000008096 xylene Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 6
- 238000005452 bending Methods 0.000 abstract 1
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 12
- 238000001291 vacuum drying Methods 0.000 description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 10
- 238000009413 insulation Methods 0.000 description 10
- 238000000498 ball milling Methods 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 5
- 125000003277 amino group Chemical group 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000004113 Sepiolite Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 238000007112 amidation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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Abstract
The invention relates to the technical field of refractory materials, and particularly discloses a lightweight anti-cracking heat-insulating refractory material and a preparation method thereof, wherein 100 parts of alumina-graphene, 18-25 parts of perlite, 8-13 parts of gypsum powder, 9-12 parts of wood fiber, 14-21 parts of fly ash, 4-7 parts of silicon carbide and 2-5 parts of magnesium oxide are weighed according to parts by mass, uniformly mixed, ball-milled, pressed and molded, and sintered to obtain the lightweight anti-cracking heat-insulating refractory material, the particle size of each raw material is smaller, the sintering temperature is obviously reduced during sintering, the components of the refractory material can be uniformly dispersed, the gaps are small, the binding force is good, the volume density of a sample can be effectively reduced, the apparent porosity of the sample is improved, the material heat conductivity is reduced, the preparation process is simple, the cost is low, the prepared refractory material is light in weight and not easy to crack, the volume density is small, the compressive strength is high, and the bending strength is high, and the heat conductivity is small.
Description
Technical Field
The invention relates to the technical field of refractory materials, in particular to a light anti-cracking heat-insulating refractory material and a preparation method thereof.
Background
With the continuous development of modern industry, the energy consumption is increasingly increased, and the purposes of saving and reducing the energy consumption and improving the energy utilization rate are achieved. Energy conservation and emission reduction are more important in the fields of metallurgy, petroleum, chemical industry and the like, and industrial kilns in industrial production are main energy consumption equipment, and have huge energy consumption per year, high heat loss and low heat efficiency in the hot working process, so that high-quality heat insulation refractory materials are urgently needed. Because the heat-insulating refractory material has very light weight, is also commonly called as a light heat-insulating refractory material, the heat-insulating refractory material can be used as a working layer of a high-temperature hot tool equipment furnace lining to directly contact high-temperature solid, melt or gas-phase erosion medium, and can also be used as a heat-insulating layer of the high-temperature hot tool equipment, so that a large amount of heat loss is reduced, and the aim of saving energy is fulfilled.
Chinese patent application CN106007754a discloses a novel refractory material consisting of the following components: 14-32% of cement, 35-45% of zirconia fiber particles, 20-24% of sepiolite, 13-23% of expanded perlite, 3-14% of citric acid and 38-40% of aluminum hydroxide or magnesium hydroxide. However, the fireproof material has poor explosion-proof performance and is easy to crack and peel, and the overall performance and the service life of the material are affected. Chinese patent CN106316426B discloses a fracture-resistant refractory material and a preparation process thereof, wherein the refractory material is prepared from alumina-silica mixed powder, calcium oxide, magnesium oxide, manganese oxide, titanium oxide, niobium pentoxide, toughened fiber modified zirconia fiber and other raw materials; the preparation method comprises the steps of mixing the raw materials, ball milling in absolute ethyl alcohol, drying the raw materials, and pressing to form to obtain a refractory material green body; and then sintering, and naturally cooling to room temperature after sintering is completed to obtain the fracture-resistant refractory material. The refractory material prepared by the invention has higher mechanical toughness and good fracture resistance, and simultaneously has excellent thermal shock resistance. But the production cost is high, and the industrial production and the use of the compound are limited.
Therefore, the development of the light refractory material with low cost, good heat insulation performance and anti-cracking effect has good development prospect and research significance.
Disclosure of Invention
In order to solve the technical problems, the invention provides the light anti-cracking heat-insulating refractory material and the preparation method thereof, which have low price and good heat-insulating effect, and simultaneously solve the problem of poor anti-cracking capability of the heat-insulating refractory material.
In order to achieve the aim, the invention discloses a light anti-cracking heat-insulating refractory material which comprises the following raw materials in parts by mass: 100 parts of aluminum oxide-graphene, 18-25 parts of perlite, 8-13 parts of gypsum powder, 9-12 parts of wood fiber, 14-21 parts of fly ash, 4-7 parts of silicon carbide and 2-5 parts of magnesium oxide;
the alumina-graphene is prepared by the following steps:
firstly, ultrasonically dispersing Graphene Oxide (GO) into thionyl chloride, reacting after uniform dispersion, performing suction filtration after the reaction, washing by using tetrahydrofuran, and vacuum drying at 60 ℃ for 12 hours to obtain acyl chloride graphene;
step two, nanometer alumina (Al 2 O 3 ) Dispersing the mixture into a mixed solution of absolute ethyl alcohol and deionized water by ultrasonic, uniformly mixing, adding gamma-aminopropyl triethoxysilane, reacting, centrifuging at 6000r/min for 10min, washing with absolute ethyl alcohol, and vacuum drying at 60 ℃ for 12h to obtain aminated alumina;
dispersing the aminated alumina into dimethylbenzene by ultrasonic, adding 4-aminophenylboric acid after uniform ultrasonic dispersion, uniformly mixing in a nitrogen atmosphere, reacting, cooling, filtering, washing by using methylbenzene, and vacuum drying for 12 hours at 60 ℃ to obtain boric acid modified alumina;
and thirdly, ultrasonically dispersing the acyl chloride graphene into N, N-dimethylformamide, adding boric acid modified alumina in a nitrogen atmosphere, uniformly mixing, reacting, filtering after the reaction, washing with ethyl acetate, and drying at 60 ℃ for 12 hours to obtain the alumina-graphene.
Preferably, in the first step, the mass ratio of the graphene oxide to the thionyl chloride is 100:24000-30000, the corresponding temperature is 70-75 ℃, and the reaction time is 18-24 hours.
Preferably, in the second step, when preparing the aminated alumina, the mass ratio of the absolute ethyl alcohol to the deionized water to the nano alumina to the gamma-aminopropyl triethoxysilane is 1800-2200:2200-2800:100:80-95, the reaction temperature is 78-82 ℃, and the reaction time is 9-12h.
Preferably, in the second step, when preparing boric acid modified alumina, the mass ratio of the dimethylbenzene to the aminated alumina to the 4-aminophenylboric acid is 1250-1600:100:14-35, the reaction temperature is 75-85 ℃, and the reaction time is 6-8h.
Preferably, in the third step, the mass ratio of the acyl chloride graphene, the N, N-dimethylformamide to the boric acid modified alumina is 24-35:1800-2200:100.
Preferably, in the third step, the reaction temperature is 20-45 ℃ and the reaction time is 5-8h.
Preferably, the preparation method of the light anti-cracking heat-insulating refractory material comprises the following steps:
the raw materials are taken according to the parts by mass: 100 parts of aluminum oxide-graphene, 18-25 parts of perlite, 8-13 parts of gypsum powder, 9-12 parts of wood fiber, 14-21 parts of fly ash, 4-7 parts of silicon carbide and 2-5 parts of magnesium oxide;
mixing the raw materials, adding absolute ethyl alcohol, mixing by using a ball mill, drying at 105-115 ℃, loading into a mould, press forming, sintering after press forming, and cooling to obtain the light anti-cracking heat-insulating refractory material.
Preferably, the mass ratio of the sum of the raw materials to the absolute ethyl alcohol is 100:220-280.
Preferably, the pressure of the compression molding is 14-18MPa.
Preferably, the sintering temperature is 1350-1450 ℃ and the sintering time is 2-4h.
Further, the ball milling time is 3-4h.
According to the method, thionyl chloride is used for modifying graphene oxide, acyl chloride groups are introduced into the surface of the graphene oxide to obtain the acyl chloride graphene, gamma-aminopropyl triethoxysilane is used for modifying nano alumina, amino groups are introduced into the surface of the nano alumina to obtain amino alumina, amino groups on the surface of the amino alumina react with boron hydroxyl groups on 4-aminophenylboric acid, boric acid is introduced into the surface of the alumina, new amino groups are introduced, and the introduced amino groups and acyl chloride on the surface of the acyl chloride graphene are subjected to amidation reaction in a nitrogen atmosphere to react to obtain the alumina-graphene. Uniformly mixing aluminum oxide-graphene, perlite, gypsum powder, wood fiber, fly ash, silicon carbide, magnesium oxide and absolute ethyl alcohol, uniformly mixing in a ball mill, and performing compression molding and sintering to obtain the light anti-cracking heat-insulating refractory material.
Fly ash is a solid waste generated when coal is burned in a thermal power plant, if the fly ash is not timely treated, the fly ash not only causes serious environmental pollution problem, but also causes serious damage to land and water resources due to long-term accumulation. Its main component is SiO 2 And Al 2 O 3 The porous refractory material can be prepared from the fly ash by a reaction sintering process, so that the problem of pollution of the fly ash to the environment is well solved.
Compared with the prior art, the invention has the beneficial effects that:
the gypsum powder used in the invention has the functions of bonding and solidifying, effectively bonds various raw materials, the added wood fibers are burnt and converted into carbon dioxide to volatilize in the sintering process, micropores are reserved, the porosity of the material is improved, the heat insulation and heat preservation performance of the material is further improved, perlite has the characteristics of being porous, light in weight, heat preservation and heat insulation and the like, good heat preservation and heat preservation effects are achieved, the fly ash is rich in source, low in cost, small in particle size of the raw materials, the sintering temperature is obviously reduced in the sintering process, meanwhile, the particle size is small, the compression is easier in the pressing forming process, so that the air in a blank is less, the air is easier to be discharged in the sintering process, the sintering process is faster, the pores are less after the sintering of the refractory material is completed, the refractory material is more compact, the components can be uniformly dispersed, the gaps are small, the binding force is good, the volume density of the sample is effectively reduced, the apparent porosity of the sample is improved, the heat conductivity of the material is reduced, and the situation that the refractory material is extremely easy to crack and peel off under a large temperature difference is avoided.
The graphene oxide used in the invention is multilayer graphene oxide, has better compressibility and rebound resilience, can absorb and release thermal stress, can improve thermal shock resistance and toughness of materials, and the aluminum oxide-graphene used introduces boron element, so that boron doping pretreatment can be realized in the ball milling process, and the heat resistance, wear resistance and mechanical strength of a machine body are improved, and has excellent oxidation resistance. The graphene oxide is introduced on the alumina, so that high-temperature sintering and alpha phase transformation of the alumina can be effectively prevented, high-temperature thermal stability of the alumina is improved, and a highly-crosslinked three-dimensional network structure can be formed at high temperature by utilizing organic groups and inorganic structures contained in a matrix, so that the high-temperature strength and the spalling resistance of the refractory material are improved. The prepared refractory material is light in weight, not easy to crack and has excellent heat insulation effect.
Drawings
FIG. 1 is a schematic illustration of the mechanism of the present invention for preparing boric acid modified alumina;
FIG. 2 is a schematic diagram of a mechanism for preparing alumina-graphene in the present invention;
FIG. 3 is a flow chart of the preparation of alumina-graphene in the present invention;
FIG. 4 is a graph showing the flexural strength and compressive strength of the corresponding samples of examples 1 to 4 and comparative examples 1 to 2 in the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
Example 1
A preparation method of a light anti-cracking heat-insulating refractory material comprises the following steps:
100 parts of alumina-graphene, 18 parts of perlite, 8 parts of gypsum powder, 9 parts of wood fiber, 14 parts of fly ash, 4 parts of silicon carbide and 2 parts of magnesium oxide are weighed according to parts by mass to obtain a mixed raw material, absolute ethyl alcohol is added, the mixed raw material and the absolute ethyl alcohol are mixed according to a mass ratio of 100:220 by using a ball mill, the ball milling time is 3 hours, after uniform mixing, the materials are dried at 105 ℃, the materials are put into a die, the die is pressed and molded under the pressure of 14MPa, sintering is carried out after the die is pressed and molded, the sintering temperature is 1350 ℃, the sintering time is 2 hours, and after the sintering, the light anti-crack heat insulation refractory material is obtained by cooling.
Wherein the alumina-graphene is prepared by the following steps:
ultrasonically dispersing graphene oxide into thionyl chloride, wherein the mass ratio of the graphene oxide to the thionyl chloride is 100:24000, reacting at 70 ℃ for 18 hours after uniform dispersion, filtering after reaction, washing with tetrahydrofuran, and vacuum drying at 60 ℃ for 12 hours to obtain the acyl chloride graphene;
dispersing nano aluminum oxide into a mixed solution of absolute ethyl alcohol and deionized water in an ultrasonic manner, uniformly mixing, adding gamma-aminopropyl triethoxysilane, wherein the mass ratio of the absolute ethyl alcohol to the deionized water to the nano aluminum oxide to the gamma-aminopropyl triethoxysilane is 1800:2200:100:80, reacting for 9 hours at 78 ℃, centrifuging at 6000r/min for 10 minutes after reacting, washing with the absolute ethyl alcohol, and vacuum drying for 12 hours at 60 ℃ to obtain the aminated aluminum oxide;
dispersing the aminated alumina into dimethylbenzene in an ultrasonic manner, adding 4-aminophenylboric acid after uniformly dispersing, wherein the mass ratio of the dimethylbenzene to the aminated alumina to the 4-aminophenylboric acid is 1250:100:14, uniformly mixing in a nitrogen atmosphere, reacting at 75 ℃ for 6 hours, cooling, filtering, washing with methylbenzene, and vacuum drying at 60 ℃ for 12 hours to obtain boric acid modified alumina;
and fourthly, ultrasonically dispersing the acyl chloride graphene into N, N-dimethylformamide, adding boric acid modified alumina in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene to the N, N-dimethylformamide to the boric acid modified alumina is 24:1800:100, uniformly mixing, reacting at 20 ℃ for 5 hours, filtering after the reaction, washing with ethyl acetate, and drying at 60 ℃ for 12 hours to obtain the alumina-graphene.
Example 2
A preparation method of a light anti-cracking heat-insulating refractory material comprises the following steps:
100 parts of alumina-graphene, 21 parts of perlite, 10 parts of gypsum powder, 10 parts of wood fiber, 17 parts of fly ash, 5 parts of silicon carbide and 3 parts of magnesium oxide are weighed according to parts by mass to obtain a mixed raw material, absolute ethyl alcohol is added, the mixed raw material and the absolute ethyl alcohol are mixed according to a mass ratio of 100:240 by using a ball mill, the ball milling time is 3.5 hours, after uniform mixing, the materials are dried at 110 ℃, the materials are put into a die, the die is pressed and molded, the pressure of the die is 16MPa, sintering is carried out after the die is pressed and molded, the sintering temperature is 1400 ℃, the sintering time is 3 hours, and the light anti-cracking heat insulation refractory material is obtained after the sintering.
Wherein the alumina-graphene is prepared by the following steps:
ultrasonically dispersing graphene oxide into thionyl chloride, wherein the mass ratio of the graphene oxide to the thionyl chloride is 100:28000, reacting at 72 ℃ for 22 hours after uniform dispersion, performing suction filtration after the reaction, washing with tetrahydrofuran, and performing vacuum drying at 60 ℃ for 12 hours to obtain the acyl chloride graphene;
dispersing nano aluminum oxide into a mixed solution of absolute ethyl alcohol and deionized water in an ultrasonic manner, uniformly mixing, adding gamma-aminopropyl triethoxysilane, wherein the mass ratio of the absolute ethyl alcohol to the deionized water to the nano aluminum oxide to the gamma-aminopropyl triethoxysilane is 2000:2500:100:90, reacting for 10 hours at 80 ℃, centrifuging at 6000r/min for 10 minutes after reacting, washing with the absolute ethyl alcohol, and vacuum drying for 12 hours at 60 ℃ to obtain the aminated aluminum oxide;
dispersing the aminated alumina into dimethylbenzene in an ultrasonic manner, adding 4-aminophenylboric acid after uniformly dispersing, wherein the mass ratio of the dimethylbenzene to the aminated alumina to the 4-aminophenylboric acid is 1450:100:28, uniformly mixing in a nitrogen atmosphere, reacting at 80 ℃ for 7 hours, cooling, filtering, washing with methylbenzene, and vacuum drying at 60 ℃ for 12 hours to obtain boric acid modified alumina;
and fourthly, ultrasonically dispersing the acyl chloride graphene into N, N-dimethylformamide, adding boric acid modified alumina in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene to the N, N-dimethylformamide to the boric acid modified alumina is 30:2000:100, uniformly mixing, reacting for 7 hours at 35 ℃, filtering after the reaction, washing with ethyl acetate, and drying for 12 hours at 60 ℃ to obtain the alumina-graphene.
Example 3
A preparation method of a light anti-cracking heat-insulating refractory material comprises the following steps:
100 parts of alumina-graphene, 24 parts of perlite, 12 parts of gypsum powder, 11 parts of wood fiber, 20 parts of fly ash, 6 parts of silicon carbide and 4 parts of magnesium oxide are weighed according to parts by mass to obtain a mixed raw material, absolute ethyl alcohol is added, the mixed raw material and the absolute ethyl alcohol are mixed according to a mass ratio of 100:260 by using a ball mill, the ball milling time is 3.5 hours, after uniform mixing, the materials are dried at 110 ℃, the materials are put into a die, the die is pressed and molded, the pressure of the die is 16MPa, sintering is carried out after the die is pressed and molded, the sintering temperature is 1400 ℃, the sintering time is 3 hours, and the light anti-cracking heat insulation refractory material is obtained after the sintering.
Wherein the preparation method of alumina-graphene is the same as example 2.
Example 4
A preparation method of a light anti-cracking heat-insulating refractory material comprises the following steps:
100 parts of alumina-graphene, 25 parts of perlite, 13 parts of gypsum powder, 12 parts of wood fiber, 21 parts of fly ash, 7 parts of silicon carbide and 5 parts of magnesium oxide are weighed according to parts by mass to obtain a mixed raw material, absolute ethyl alcohol is added, the mixed raw material and the absolute ethyl alcohol are mixed according to a mass ratio of 100:280 by using a ball mill, the ball milling time is 4 hours, after uniform mixing, the materials are dried at 115 ℃, placed in a die, pressed and molded under the pressure of 18MPa, sintered after the pressing and molding, the sintering temperature is 1450 ℃, the sintering time is 4 hours, and the light anti-cracking heat-insulating refractory material is obtained after cooling.
Wherein the alumina-graphene is prepared by the following steps:
ultrasonically dispersing graphene oxide into thionyl chloride, wherein the mass ratio of the graphene oxide to the thionyl chloride is 100:30000, reacting for 24 hours at 75 ℃ after uniform dispersion, filtering after reaction, washing with tetrahydrofuran, and drying in vacuum for 12 hours at 60 ℃ to obtain the acyl chloride graphene;
dispersing nano alumina into a mixed solution of absolute ethyl alcohol and deionized water in an ultrasonic manner, uniformly mixing, adding gamma-aminopropyl triethoxysilane, wherein the mass ratio of the absolute ethyl alcohol to the deionized water to the nano alumina to the gamma-aminopropyl triethoxysilane is 2200:2800:100:95, reacting for 12 hours at 82 ℃, centrifuging at 6000r/min for 10 minutes after reacting, washing with the absolute ethyl alcohol, and vacuum drying for 12 hours at 60 ℃ to obtain the aminated alumina;
dispersing the aminated alumina into dimethylbenzene in an ultrasonic manner, adding 4-aminophenylboric acid after uniformly dispersing, wherein the mass ratio of the dimethylbenzene to the aminated alumina to the 4-aminophenylboric acid is 1600:100:35, uniformly mixing in a nitrogen atmosphere, reacting at 85 ℃ for 8 hours, cooling, filtering, washing with methylbenzene, and vacuum drying at 60 ℃ for 12 hours to obtain boric acid modified alumina;
and fourthly, ultrasonically dispersing the acyl chloride graphene into N, N-dimethylformamide, adding boric acid modified alumina in a nitrogen atmosphere, wherein the mass ratio of the acyl chloride graphene to the N, N-dimethylformamide to the boric acid modified alumina is 35:2200:100, uniformly mixing, reacting at 45 ℃ for 8 hours, filtering after the reaction, washing with ethyl acetate, and drying at 60 ℃ for 12 hours to obtain the alumina-graphene.
Comparative example 1
A preparation method of a light anti-cracking heat-insulating refractory material comprises the following steps:
100 parts of alumina-graphene, 25 parts of perlite, 13 parts of gypsum powder, 12 parts of wood fiber, 21 parts of fly ash, 7 parts of silicon carbide and 5 parts of magnesium oxide are weighed according to parts by mass to obtain a mixed raw material, absolute ethyl alcohol is added, the mixed raw material and the absolute ethyl alcohol are mixed according to a mass ratio of 100:280 by using a ball mill, the ball milling time is 4 hours, after uniform mixing, the materials are dried at 115 ℃, placed in a die, pressed and molded under the pressure of 18MPa, sintered after the pressing and molding, the sintering temperature is 1450 ℃, the sintering time is 4 hours, and the light anti-cracking heat-insulating refractory material is obtained after cooling.
Wherein the alumina-graphene is prepared by the following steps:
ultrasonically dispersing graphene oxide into thionyl chloride, wherein the mass ratio of the graphene oxide to the thionyl chloride is 100:30000, reacting for 24 hours at 75 ℃ after uniform dispersion, filtering after reaction, washing with tetrahydrofuran, and drying in vacuum for 12 hours at 60 ℃ to obtain the acyl chloride graphene;
dispersing nano alumina into a mixed solution of absolute ethyl alcohol and deionized water in an ultrasonic manner, uniformly mixing, adding gamma-aminopropyl triethoxysilane, wherein the mass ratio of the absolute ethyl alcohol to the deionized water to the nano alumina to the gamma-aminopropyl triethoxysilane is 2200:2800:100:95, reacting for 12 hours at 82 ℃, centrifuging at 6000r/min for 10 minutes after reacting, washing with the absolute ethyl alcohol, and vacuum drying for 12 hours at 60 ℃ to obtain the aminated alumina;
dispersing the acyl chloride graphene into N, N-dimethylformamide by ultrasonic, adding the aminated alumina and the triethylamine, wherein the mass ratio of the acyl chloride graphene to the N, N-dimethylformamide to the aminated alumina to the triethylamine is 35:2200:100:5, uniformly mixing, reacting at 80 ℃ for 18 hours, filtering after the reaction, washing with absolute ethyl alcohol, and drying at 60 ℃ for 12 hours to obtain the alumina-graphene.
Comparative example 2
A preparation method of a light anti-cracking heat-insulating refractory material comprises the following steps:
weighing 26 parts of graphene oxide, 74 parts of nano aluminum oxide, 25 parts of perlite, 13 parts of gypsum powder, 12 parts of wood fiber, 21 parts of fly ash, 7 parts of silicon carbide and 5 parts of magnesium oxide according to parts by mass to obtain a mixed raw material, adding absolute ethyl alcohol, mixing the mixed raw material and the absolute ethyl alcohol according to a mass ratio of 100:280 by using a ball mill, ball milling for 4 hours, drying at 115 ℃ after mixing uniformly, loading into a mould, press forming at 18MPa, sintering after press forming at 1450 ℃ for 4 hours, and cooling to obtain the light anti-cracking heat-insulating refractory material.
The nano alumina used in the embodiment of the invention is purchased from Nanjing Baacket New Material Co., ltd, the model is PAT-G05A, and the average grain diameter is 50nm; the graphene oxide is multilayer graphene oxide, and is purchased from Suzhou Hengzhu technology Co., ltd (purity > 95wt%, thickness is 3.4-8nm, and sheet diameter is 10-50 μm); silicon carbide is purchased from Ningxia Hui carbon Limited under the model DH-06 with the average grain diameter of 38 mu m; magnesium oxide was purchased from Shandong Xiangshaozhao new materials Co., ltd, and had a particle size of 48 μm; the fly ash is purchased from a second power plant of the saddle mountain and is a first grade product; perlite is purchased from the Lingshou county Lingze mineral product processing plant and has an average particle size of 150 μm; gypsum powder is purchased from mineral processing factories of Yan nationality in the Ming county of life, and the product number is SG-2022; wood fiber was purchased from stone house, tenbang mineral products limited, under the number 1023; other materials and reagents are commercially available.
The light anti-cracking heat insulation refractory materials in examples 1-4 and comparative examples 1-2 are used as samples for performance test, and the volume density of the samples is detected by GB/T2997-2015 'test method for volume density, apparent porosity and true porosity of compact shaped refractory products'; the flexural strength and the compressive strength of the sample at room temperature are respectively tested by adopting the standards of GB/T3001-2017 refractory material normal temperature flexural strength test method and GB/T5072-2008 refractory material normal temperature compressive strength test method; the thermal conductivity of the sample at 800 ℃ is detected by adopting YB/T4130-2005 (water flow flat plate method); the results of each test are shown in the table:
TABLE 1
| Project testing | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 |
| Bulk Density (g/cm) 3 ） | 2.37 | 2.33 | 2.34 | 2.31 | 2.32 | 2.34 |
| Flexural strength (MPa) | 67.1 | 68.5 | 68.9 | 69.1 | 57.2 | 54.0 |
| Compressive Strength (MPa) | 129.8 | 130.7 | 132.4 | 132.9 | 124.7 | 121.5 |
| Coefficient of thermal conductivity (W/m) -1 ·k -1 ） | 0.35 | 0.33 | 0.32 | 0.30 | 0.42 | 0.48 |
As can be seen from the test results of Table 1, the refractory material prepared in the present invention has the characteristics of light cracking resistance, heat insulation and heat preservation, wherein the volume density can be as low as 2.31g/cm 3 The flexural strength is 69.1MPa, the compressive strength is 132.9MPa, and the heat conductivity coefficient is 0.30W/m -1 ·k -1 。
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made hereto without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The light anti-cracking heat-insulating refractory material is characterized by comprising the following raw materials in parts by mass: 100 parts of aluminum oxide-graphene, 18-25 parts of perlite, 8-13 parts of gypsum powder, 9-12 parts of wood fiber, 14-21 parts of fly ash, 4-7 parts of silicon carbide and 2-5 parts of magnesium oxide;
the alumina-graphene is prepared by the following steps:
the method comprises the steps of firstly, ultrasonically dispersing graphene oxide into thionyl chloride, reacting after uniform dispersion, carrying out suction filtration, washing and drying to obtain acyl chloride graphene;
wherein the reaction temperature is 70-75 ℃ and the reaction time is 18-24 hours;
dispersing nano alumina into a mixed solution of absolute ethyl alcohol and deionized water in an ultrasonic manner, uniformly mixing, adding gamma-aminopropyl triethoxysilane, reacting, centrifuging, washing and drying to obtain aminated alumina;
wherein the reaction temperature is 78-82 ℃ and the reaction time is 9-12h;
dispersing the aminated alumina into dimethylbenzene by ultrasonic, adding 4-aminophenylboric acid after uniform ultrasonic dispersion, uniformly mixing in a nitrogen atmosphere, reacting, cooling, filtering, washing and drying to obtain boric acid modified alumina;
wherein the reaction temperature is 75-85 ℃ and the reaction time is 6-8h;
step three, ultrasonically dispersing acyl chloride graphene into N, N-dimethylformamide, adding boric acid modified alumina in a nitrogen atmosphere, uniformly mixing, reacting, filtering, washing and drying to obtain alumina-graphene;
wherein the reaction temperature is 20-45 ℃ and the reaction time is 5-8h.
2. The lightweight anti-cracking heat-insulating refractory material according to claim 1, wherein in the first step, the mass ratio of graphene oxide to thionyl chloride is 100:24000-30000.
3. The lightweight anti-cracking heat-insulating refractory material according to claim 1, wherein in the second step, when preparing the aminated alumina, the mass ratio of absolute ethyl alcohol, deionized water, nano alumina and gamma-aminopropyl triethoxysilane is 1800-2200:2200-2800:100:80-95.
4. The light anti-cracking heat-insulating refractory material according to claim 1, wherein in the second step, when boric acid modified alumina is prepared, the mass ratio of xylene, aminated alumina and 4-aminophenylboric acid is 1250-1600:100:14-35.
5. The lightweight, anti-cracking, heat-insulating and fire-resistant material according to claim 1, wherein in the third step, the mass ratio of the acyl chloride graphene, the N, N-dimethylformamide to the boric acid modified alumina is 24-35:1800-2200:100.
6. A method for preparing the lightweight anti-cracking heat-insulating refractory material according to any one of claims 1 to 5, comprising the following steps:
the raw materials are taken according to the parts by mass: 100 parts of aluminum oxide-graphene, 18-25 parts of perlite, 8-13 parts of gypsum powder, 9-12 parts of wood fiber, 14-21 parts of fly ash, 4-7 parts of silicon carbide and 2-5 parts of magnesium oxide;
mixing the raw materials, adding absolute ethyl alcohol, mixing by using a ball mill, drying at 105-115 ℃ after uniform mixing, pressing, forming and sintering to obtain the light anti-cracking heat-insulating refractory material.
7. The method for preparing the light anti-cracking heat-insulating refractory material according to claim 6, wherein the mass ratio of the total mass of the raw materials to the absolute ethyl alcohol is 100:220-280.
8. The method for preparing the lightweight anti-cracking heat-insulating refractory material according to claim 6, wherein the pressure of the compression molding is 14-18MPa.
9. The method for preparing the light anti-cracking heat-insulating refractory material according to claim 6, wherein the sintering temperature is 1350-1450 ℃ and the sintering time is 2-4h.
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| CN105482511A (en) * | 2015-11-10 | 2016-04-13 | 西南石油大学 | Aluminium oxide/graphene oxide sheet-shaped hybrid and preparation method thereof |
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| CN108975950A (en) * | 2018-09-18 | 2018-12-11 | 明光瑞尔非金属材料有限公司 | A kind of refractory brick of high temperature resistance and high strength and preparation method thereof |
| CN115650707A (en) * | 2022-11-03 | 2023-01-31 | 中国人民解放军陆军装甲兵学院 | Preparation method of magnesia-alumina transparent ceramic |
| CN117082718A (en) * | 2023-08-11 | 2023-11-17 | 上海贺鸿电子科技股份有限公司 | Antistatic multilayer circuit board and preparation method thereof |
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