CN112537936A - Aerogel modified high-strength fireproof mortar material and preparation method thereof - Google Patents
Aerogel modified high-strength fireproof mortar material and preparation method thereof Download PDFInfo
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- CN112537936A CN112537936A CN202011579796.2A CN202011579796A CN112537936A CN 112537936 A CN112537936 A CN 112537936A CN 202011579796 A CN202011579796 A CN 202011579796A CN 112537936 A CN112537936 A CN 112537936A
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- cellulose ether
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- 239000004570 mortar (masonry) Substances 0.000 title claims abstract description 62
- 239000004964 aerogel Substances 0.000 title claims abstract description 46
- 239000000463 material Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000004576 sand Substances 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 31
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002086 nanomaterial Substances 0.000 claims abstract description 23
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000010410 layer Substances 0.000 claims abstract description 16
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 16
- 239000004568 cement Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920003086 cellulose ether Polymers 0.000 claims abstract description 13
- 239000003063 flame retardant Substances 0.000 claims abstract description 13
- 239000000835 fiber Substances 0.000 claims abstract description 12
- 239000004743 Polypropylene Substances 0.000 claims abstract description 11
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 11
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 11
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 11
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 11
- -1 polypropylene Polymers 0.000 claims abstract description 11
- 229920001155 polypropylene Polymers 0.000 claims abstract description 11
- 229920001479 Hydroxyethyl methyl cellulose Polymers 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 239000012792 core layer Substances 0.000 claims abstract description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 8
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 44
- 238000002156 mixing Methods 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 24
- 229920000877 Melamine resin Polymers 0.000 claims description 22
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 14
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 13
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 13
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 13
- 238000004321 preservation Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 10
- 239000008098 formaldehyde solution Substances 0.000 claims description 10
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 6
- 238000000352 supercritical drying Methods 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000012856 weighed raw material Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000002265 prevention Effects 0.000 claims 1
- 239000011325 microbead Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 239000012774 insulation material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 241001474374 Blennius Species 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical group [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-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
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 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
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- DGVVJWXRCWCCOD-UHFFFAOYSA-N naphthalene;hydrate Chemical compound O.C1=CC=CC2=CC=CC=C21 DGVVJWXRCWCCOD-UHFFFAOYSA-N 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention discloses an aerogel modified high-strength fireproof mortar material, which comprises cement, sand, polypropylene fibers, a composite reinforcing filler, a water reducing agent, a flame retardant and cellulose ether; the sand is a mixture of mountain sand and machine-made sand; the cellulose ether is a mixture of hydroxypropyl methyl cellulose ether and hydroxyethyl methyl cellulose ether; the composite reinforcing filler is a mixture of vitrified micro bubbles and mesoporous nano materials in a mass ratio; the mesoporous nano material is formed by using nano titanium dioxide particles as a core layer and sequentially coating a nitrogen-doped graphene aerogel layer and a zirconium oxide/silicon oxide aerogel layer on the surface of the core layer. The invention also discloses a preparation method of the high-strength fireproof mortar material. The mortar provided by the invention has good fireproof performance and good mechanical property.
Description
Technical Field
The invention relates to the field of building materials, in particular to an aerogel modified high-strength fireproof mortar material and a preparation method thereof.
Background
The energy is one of the pillars for national economic development, is an important material foundation for the development of human society, and is a precondition for economic growth and development. The energy situation in China is quite severe, and the per-capita resource occupancy is far lower than the average level in the world. Energy supply and demand in China are very tight, and building energy consumption accounts for one third of the total social energy consumption, so that building energy conservation has very important significance. The application of the heat insulation material is very effective for reducing the energy consumption of the building in long-term use, and the current heat insulation material mainly comprises a heat insulation plate and heat insulation mortar. The used heat insulation material is mainly an organic heat insulation material, has low heat conductivity coefficient, light volume weight and poor fire resistance, and seriously threatens the life and property safety of people when a fire disaster happens. The inorganic heat-insulating material has good weather resistance and fire resistance, but has higher heat conductivity coefficient, heavier volume weight and less ideal heat-insulating effect than the organic heat-insulating material.
Chinese patent CN201310208120.6 provides a thick plastering fireproof mortar phenolic resin plate and special fireproof mortar, wherein a plastering mortar layer with the thickness not less than 4mm is compounded on the surface of a foaming phenolic resin material, the plastering mortar layer is mainly formed by mixing and solidifying a main mortar material and a small sand material, and the main mortar material comprises 315 weight parts of portland cement 385 with the strength grade not less than 42.5, 315 weight parts of sulphoaluminate cement 385, 90-110 weight parts of 50-100 mesh sand and 90-110 weight parts of fly ash; the mixed small materials comprise the following components: 13-17 parts of redispersible latex powder, 5-7 parts of cellulose ether, 3.5-4.5 parts of chopped fiber, 90-110 parts of early strength agent, 2.5-3.5 parts of naphthalene water reducer and 0.15-0.2 part of lithium carbonate. Chinese patent CN201510591678.6 provides a fireproof heat-preservation dry powder mortar and a preparation method thereof, which comprises a composite cementing material, a lightweight aggregate, an admixture, a chemical additive and an organic polymer additive, wherein the composite cementing material comprises cement and byproduct gypsum, the lightweight aggregate is aluminum silicate vitrified micro-beads, the admixture comprises high-alumina fly ash, expanded vermiculite and blast furnace slag, the chemical additive comprises magnesium aluminum silicate, modified seaweed gel powder, vinyl acetate-vinyl versatate/acrylic acid polymer gel powder and 2-sodium naphthalenesulfonate formaldehyde polymer, and the organic polymer additive is hydroxypropyl methyl cellulose. The prior art can effectively improve the fireproof performance of the mortar. With the development of building materials, further improvement of mortar properties is required to meet the requirements.
Disclosure of Invention
One of the technical problems to be solved by the invention is as follows: aiming at the defects in the prior art, the invention provides an aerogel modified high-strength fireproof mortar material, and the self-made mesoporous nano material and vitrified micro bubbles are added into a mortar matrix to be compounded to be used as a composite reinforcing filler, so that the heat insulation performance of the mortar is effectively improved; ammonium polyphosphate, melamine and aluminum-magnesium layered hydroxide are added as a synergistic flame retardant to improve the fireproof performance of the mortar; the mortar provided by the invention has good fireproof performance and good mechanical property.
The second technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the preparation method of the aerogel modified high-strength fireproof mortar material is provided, the method is simple to operate, the requirement on equipment is low, and the prepared mortar has excellent performance.
In order to solve the first technical problem, the technical scheme of the invention is as follows:
an aerogel modified high-strength fireproof mortar material comprises cement, sand, polypropylene fibers, composite reinforcing filler, a water reducing agent, a flame retardant and cellulose ether; the sand is mountain sand, and the machine-made sand is prepared from the following raw materials in a mass ratio of (1-2): 2; the cellulose ether is hydroxypropyl methyl cellulose ether and hydroxyethyl methyl cellulose ether in a mass ratio of 1: (0.5-1.5); the composite reinforcing filler is prepared from vitrified micro bubbles and mesoporous nano materials in a mass ratio of 5: the mixture of (1-2); the mesoporous nano material is formed by using nano titanium dioxide particles as a core layer and sequentially coating a nitrogen-doped graphene aerogel layer and a zirconium oxide/silicon oxide aerogel layer on the surface of the core layer.
Preferably, the water reducing agent is sodium lignosulfonate.
Preferably, in the technical scheme, the flame retardant is a mixture of ammonium polyphosphate, aluminum-magnesium layered hydroxide and melamine, and the mass ratio of the ammonium polyphosphate to the aluminum-magnesium layered hydroxide to the melamine is 3: (0.5-1): (1-2).
Preferably, in the technical scheme, the dosage of each component is as follows in parts by weight: 30-50 parts of cement, 30-50 parts of sand, 0.01-0.03 part of polypropylene fiber, 5-10 parts of composite reinforcing filler, 0.05-0.25 part of water reducing agent, 1-2 parts of flame retardant and 0.02-0.05 part of cellulose ether.
The mortar is prepared by singly using natural sand or machine-made sand or the conditions of large cement consumption, poor mortar water retention and the like occur. The natural sand and the machine-made sand are compounded, and the mountain sand and the machine-made sand are specifically adopted, wherein the mass ratio of the mountain sand to the machine-made sand is (1-2): 2, and mixing.
The addition of cellulose ether can improve the working performance of the mortar to a certain extent, for example, the good water retention performance of the mortar can be improved through thickening effect, but the type and the amount of the cellulose ether can also influence the fluidity, the air content, the setting time and various performances after hardening of the mortar. Hydroxypropyl methyl cellulose ether and hydroxyethyl methyl cellulose ether are adopted in the application in a mass ratio of 1: (0.5-1.5) in proportion.
In order to solve the second technical problem, the technical solution of the present invention is:
a preparation method of an aerogel modified high-strength fireproof mortar material comprises the following steps:
(1) uniformly mixing melamine and a graphene oxide solution, then adding a formaldehyde solution, adding nano titanium dioxide after uniform mixing, placing the prepared mixed solution into a high-pressure kettle for reaction, separating and drying solids after the reaction is finished, and then calcining to prepare the nitrogen-doped graphene aerogel modified nano titanium dioxide;
(2) mixing zirconium oxychloride, tetraethoxysilane, absolute ethyl alcohol and deionized water, uniformly stirring to prepare silicon/zirconium composite sol, adding the prepared nitrogen-doped graphene aerogel modified nano titanium dioxide, uniformly stirring, dropwise adding epoxypropane, violently stirring, standing, aging, performing replacement treatment by using ethanol as a medium, performing supercritical drying by using ethanol as a drying medium, mixing and grinding the dried solid and vitrified micro bubbles to prepare the composite reinforced filler;
(3) weighing the raw materials according to the proportion, adding the weighed raw materials into a stirrer, and uniformly stirring and mixing to obtain the high-strength fireproof mortar material.
Preferably, in the step (1), the mass concentration of the formaldehyde solution is 30-40%, the concentration of the graphene oxide is 8-15mg/ml, and the dosage ratio of the melamine, the graphene oxide solution, the formaldehyde solution and the nano titanium dioxide is (0.2-0.4) g: 15 ml: 1 ml: (0.1-0.2) g.
Preferably, in the step (1), the reaction temperature is 180 ℃, and the reaction time is 10-15 h.
Preferably, in the step (1), the conditions of the calcination treatment are as follows: introducing nitrogen in the absence of oxygen, heating to 800 ℃ at the speed of 10 ℃/min, carrying out heat preservation treatment for 3h, then cooling to 600 ℃ at the speed of 3 ℃/min, carrying out heat preservation treatment for 2h, and finally cooling to room temperature along with the furnace.
Preferably, in the step (2), the usage ratio of zirconium oxychloride, tetraethoxysilane, absolute ethyl alcohol, deionized water, nitrogen-doped graphene aerogel modified nano titanium dioxide and propylene oxide is (0.2-0.4) g: 1 ml: 15 ml: 20 ml: 10 g: (5-10) ml.
Preferably, in the step (2), the standing and aging treatment time is 20 to 40 hours, and the replacement treatment condition is that the replacement is performed 3 times for 20 to 30 hours each time.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
the aerogel modified high-strength fireproof mortar material comprises cement, sand, polypropylene fibers, a composite reinforcing filler, a water reducing agent, a flame retardant and cellulose ether, wherein the sand is a mixture of mountain sand and machine-made sand, the cellulose ether is a mixture of hydroxypropyl methyl cellulose ether and hydroxyethyl methyl cellulose ether, the composite reinforcing filler is a mixture of vitrified micro bubbles and a mesoporous nano material, and the mesoporous nano material is prepared by taking nano titanium dioxide particles as a core layer and sequentially coating a nitrogen-doped graphene aerogel layer and a zirconium oxide/silicon oxide aerogel layer on the surface of the nano titanium dioxide particles. The mesoporous nano material has a layered multi-level pore structure, has a large specific surface area, and can well obstruct the heat transfer in the mortar, thereby reducing the heat conduction performance of the mortar material and further improving the fireproof performance of the mortar. The invention adopts the mutual cooperation of the composite reinforced filler and the flame retardant to further improve the fireproof performance of the mortar. The added flame retardant is a compound of ammonium polyphosphate, aluminum-magnesium layered hydroxide and melamine, and when a fire disaster occurs, the ammonium polyphosphate is heated and dehydrated to generate polyphosphoric acid, so that a carbonized film is generated on the surface of a coating by dehydration, and a large amount of non-combustible gas is generated to form a foam heat-insulating layer, thereby achieving the purpose of flame retardance; the melamine can burn at high temperature to release nitrogen and carbon dioxide, so that the concentration of combustible gas is diluted, and the purpose of flame retardance is achieved; the aluminum-magnesium layered hydroxide is dehydrated and absorbs heat at high temperature, and is decomposed to generate steam, so that the concentration of combustible gas is diluted, and a metal oxide passivation layer is generated on the surface of the combustible, thereby effectively preventing further combustion.
The mesoporous nano material prepared by the invention takes nano titanium dioxide as a core layer, and a nitrogen-doped graphene aerogel layer and a zirconium oxide/silicon oxide aerogel layer are sequentially coated on the surface of the nano titanium dioxide, so that in the preparation process, the dosage ratio of each component is effectively adjusted, the dosage of propylene oxide is controlled, and the forming speed of a zirconium oxide gel framework is effectively adjusted, so that the silicon oxide gel and the zirconium oxide gel have sufficient time to grow, a through network structure is formed, and the zirconium oxide/silicon oxide gel layer with a stable porous structure is prepared. According to the invention, the graphene aerogel is doped by taking melamine as a nitrogen source, the dosage of the melamine is effectively controlled, nitrogen doping is completed on the premise of not damaging the graphene aerogel structure, and the nitrogen doping causes new defects of the material, so that the hierarchical porous nitrogen-doped/graphene aerogel layer is obtained. The mesoporous nano material prepared by the invention is compounded with the vitrified micro bubbles to be used as a composite reinforcing filler to be added into mortar, so that the heat transfer in the mortar is effectively blocked, and the fireproof performance of the mortar is further improved. The fireproof mortar material prepared by the invention is simple to prepare and low in cost, and the prepared fireproof mortar material has good fireproof performance and excellent mechanical performance.
Detailed Description
The invention is further illustrated by the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
The following raw materials have the following performance parameters and sources:
the nano titanium dioxide is purchased from Nanjing Xiancheng nano material science and technology Limited company, the particle diameter is 5-10nm, the purity is 99.3wt percent, and the nano titanium dioxide is anatase type.
Cement: taiwan mud P.O42.5R; the specific surface area is 356m2Per kg, standard consistency of 26.8%, initial setting time of 155min, final setting time of 222 min.
Mountain sand: adopting mountain sand of Guizhou, the bulk density is 1480kg/m3The average particle size is 1-2 mm.
And (3) machining sand: the machine-made sand produced by brother mining industry is adopted: the fineness modulus is 3.4, and the content of mud powder is 5.0%.
Polypropylene fiber: the tensile strength is 380MPa, the diameter is 1mm, the elastic modulus is more than or equal to 5GPa, and the density is 0.91g/cm3。
Ammonium polyphosphate: solubility (25 ℃) is less than or equal to 0.50g/100ml, viscosity (25 ℃) is less than or equal to 80 Mpa.s, average grain diameter is 12 mu m, and thermal decomposition temperature is more than or equal to 280 ℃.
Aluminum magnesium layered hydroxide: the average particle size was 200 nm.
Hydroxypropyl methylcellulose ether: the viscosity was 100 pas.
Hydroxyethyl methyl cellulose ether: the viscosity was 15 ten thousand mPas.
Vitrification of the micro-beads: bulk density of kg/m3The standard penetration density is 202kg/m3The water content is 1%, and the thermal conductivity is 0.071W/mk.
Example 1
(1) Uniformly mixing 0.2g of melamine and 15ml of graphene oxide solution with the concentration of 8mg/ml, then adding 1ml of formaldehyde solution with the mass concentration of 37%, uniformly mixing, then adding 0.1g of nano titanium dioxide, placing the prepared mixed solution in an autoclave for reaction at 180 ℃, separating and drying the solid after the reaction is finished, then placing the solid in a muffle furnace, firstly heating to 800 ℃ at the speed of 10 ℃/min under the atmosphere of oxygen-free nitrogen gas, carrying out heat preservation treatment for 3 hours, then cooling to 600 ℃ at the speed of 3 ℃/min, carrying out heat preservation treatment for 2 hours, and finally cooling to room temperature along with the furnace to prepare the nitrogen-doped graphene aerogel modified nano titanium dioxide;
(2) mixing and stirring 0.2g of zirconium oxychloride, 1ml of tetraethoxysilane, 15ml of absolute ethyl alcohol and 20ml of deionized water uniformly to prepare silicon/zirconium composite sol, adding the 10g of prepared nitrogen-doped graphene aerogel modified nano titanium dioxide, stirring uniformly, dropwise adding 5ml of epoxypropane, stirring vigorously, standing, aging for 20 hours, performing replacement treatment by using ethanol as a medium for 3 times, performing 20 hours each time, performing supercritical drying by using ethanol as a drying medium to obtain a mesoporous nano material, and mixing the mesoporous nano material and the vitrified micro beads in a mass ratio of 1: 5, mixing and grinding the mixture according to the proportion to prepare the composite reinforced filler;
(3) adding 30 parts of cement, 20 parts of mountain sand, 20 parts of machine-made sand, 0.01 part of polypropylene fiber, 5 parts of composite reinforcing filler, 0.05 part of sodium lignosulfonate, 1 part of ammonium polyphosphate, 0.35 part of aluminum-magnesium layered hydroxide, 0.65 part of melamine, 0.02 part of hydroxypropyl methyl cellulose ether and 0.02 part of hydroxyethyl methyl cellulose ether into a stirrer, and stirring and mixing uniformly to prepare the high-strength fireproof mortar material.
Example 2
(1) Uniformly mixing 0.4g of melamine and 15ml of graphene oxide solution with the concentration of 15mg/ml, then adding 1ml of formaldehyde solution with the mass concentration of 37%, uniformly mixing, then adding 0.2g of nano titanium dioxide, placing the prepared mixed solution in an autoclave for reaction at 180 ℃, separating and drying the solid after the reaction is finished, then placing the solid in a muffle furnace, firstly heating to 800 ℃ at the speed of 10 ℃/min under the atmosphere of oxygen-free nitrogen gas, carrying out heat preservation treatment for 3 hours, then cooling to 600 ℃ at the speed of 3 ℃/min, carrying out heat preservation treatment for 2 hours, and finally cooling to room temperature along with the furnace to prepare the nitrogen-doped graphene aerogel modified nano titanium dioxide;
(2) mixing and stirring 0.4g of zirconium oxychloride, 1ml of tetraethoxysilane, 15ml of absolute ethyl alcohol and 20ml of deionized water uniformly to prepare silicon/zirconium composite sol, adding the 10g of prepared nitrogen-doped graphene aerogel modified nano titanium dioxide, stirring uniformly, dropwise adding 10ml of epoxypropane, stirring vigorously, standing, aging for 40 hours, performing replacement treatment by using ethanol as a medium for 3 times, performing 30 hours each time, performing supercritical drying by using ethanol as a drying medium to obtain a mesoporous nano material, and mixing the mesoporous nano material and the vitrified microbeads in a mass ratio of 2: 5, mixing and grinding the mixture according to the proportion to prepare the composite reinforced filler;
(3) adding 50 parts of cement, 20 parts of mountain sand, 20 parts of machine-made sand, 0.03 part of polypropylene fiber, 10 parts of composite reinforcing filler, 0.25 part of sodium lignosulfonate, 1 part of ammonium polyphosphate, 0.35 part of aluminum-magnesium layered hydroxide, 0.65 part of melamine, 0.02 part of hydroxypropyl methyl cellulose ether and 0.02 part of hydroxyethyl methyl cellulose ether into a stirrer, and stirring and mixing uniformly to prepare the high-strength fireproof mortar material.
Example 3
(1) Uniformly mixing 0.3g of melamine and 15ml of graphene oxide solution with the concentration of 10mg/ml, then adding 1ml of formaldehyde solution with the mass concentration of 37%, uniformly mixing, then adding 0.15g of nano titanium dioxide, placing the prepared mixed solution in an autoclave for reaction at 180 ℃, separating and drying the solid after the reaction is finished, then placing the solid in a muffle furnace, firstly heating to 800 ℃ at the speed of 10 ℃/min under the atmosphere of oxygen-free nitrogen gas, carrying out heat preservation treatment for 3 hours, then cooling to 600 ℃ at the speed of 3 ℃/min, carrying out heat preservation treatment for 2 hours, and finally cooling to room temperature along with the furnace to prepare the nitrogen-doped graphene aerogel modified nano titanium dioxide;
(2) mixing and stirring 0.3g of zirconium oxychloride, 1ml of tetraethoxysilane, 15ml of absolute ethyl alcohol and 20ml of deionized water uniformly to prepare silicon/zirconium composite sol, adding the 10g of prepared nitrogen-doped graphene aerogel modified nano titanium dioxide, stirring uniformly, dropwise adding 7ml of epoxypropane, stirring vigorously, standing and aging for 30 hours, performing replacement treatment by using ethanol as a medium for 3 times, performing 25 hours each time, performing supercritical drying by using ethanol as a drying medium to obtain a mesoporous nano material, and mixing the mesoporous nano material and the vitrified micro beads in a mass ratio of 1: 5, mixing and grinding the mixture according to the proportion to prepare the composite reinforced filler;
(3) adding 35 parts of cement, 20 parts of mountain sand, 20 parts of machine-made sand, 0.02 part of polypropylene fiber, 7 parts of composite reinforcing filler, 0.1 part of sodium lignosulfonate, 1 part of ammonium polyphosphate, 0.35 part of aluminum-magnesium layered hydroxide, 0.65 part of melamine, 0.02 part of hydroxypropyl methyl cellulose ether and 0.02 part of hydroxyethyl methyl cellulose ether into a stirrer, and stirring and mixing uniformly to prepare the high-strength fireproof mortar material.
Example 4
(1) Uniformly mixing 0.35g of melamine and 15ml of graphene oxide solution with the concentration of 12mg/ml, then adding 1ml of formaldehyde solution with the mass concentration of 37%, uniformly mixing, then adding 0.15g of nano titanium dioxide, placing the prepared mixed solution in an autoclave for reaction at 180 ℃, separating and drying the solid after the reaction is finished, then placing the solid in a muffle furnace, firstly heating to 800 ℃ at the speed of 10 ℃/min under the atmosphere of oxygen-free nitrogen gas, carrying out heat preservation treatment for 3 hours, then cooling to 600 ℃ at the speed of 3 ℃/min, carrying out heat preservation treatment for 2 hours, and finally cooling to room temperature along with the furnace to prepare the nitrogen-doped graphene aerogel modified nano titanium dioxide;
(2) mixing and stirring 0.3g of zirconium oxychloride, 1ml of tetraethoxysilane, 15ml of absolute ethyl alcohol and 20ml of deionized water uniformly to prepare silicon/zirconium composite sol, adding the 10g of prepared nitrogen-doped graphene aerogel modified nano titanium dioxide, stirring uniformly, dropwise adding 8ml of epoxypropane, stirring vigorously, standing and aging for 30 hours, performing replacement treatment by using ethanol as a medium for 3 times, performing 20 hours each time, performing supercritical drying by using ethanol as a drying medium to obtain a mesoporous nano material, and mixing the mesoporous nano material and the vitrified microbeads in a mass ratio of 2: 5, mixing and grinding the mixture according to the proportion to prepare the composite reinforced filler;
(3) adding 40 parts of cement, 20 parts of mountain sand, 20 parts of machine-made sand, 0.01 part of polypropylene fiber, 5-10 parts of composite reinforcing filler, 0.15 part of sodium lignosulfonate, 1 part of ammonium polyphosphate, 0.35 part of aluminum-magnesium layered hydroxide, 0.65 part of melamine, 0.02 part of hydroxypropyl methyl cellulose ether and 0.02 part of hydroxyethyl methyl cellulose ether into a stirrer, and stirring and mixing uniformly to prepare the high-strength fireproof mortar material.
Comparative example 1
The conditions for adding no aluminum magnesium layered hydroxide to the flame retardant were the same as in example 4.
Comparative example 2
The mesoporous nanomaterial was not added, and the other conditions were the same as in example 4.
The mortar materials prepared in the examples and the comparative examples are mixed with water according to GB/T20473-:
1. mechanical properties
The compression strength was tested using an Instron 5567 universal material tester.
2. Coefficient of thermal conductivity
And breaking the test block, clamping a heat probe for measuring the heat conductivity coefficient by using the test block, covering the test block by using a vacuum cover, adjusting the scanning frequency of an instrument, and measuring the heat conductivity coefficient of the fireproof mortar, wherein the adopted experimental instrument is a TPS2500Hot Disk heat conductivity coefficient instrument.
The test results are shown in table 1:
TABLE 1
From the test results, compared with the comparative example, the mortar prepared by the invention has more excellent fireproof performance and mechanical performance. Therefore, the ammonium polyphosphate, the melamine and the aluminum-magnesium layered hydroxide are compounded to have better flame-retardant and fireproof performances. After the mesoporous nano material and the vitrified micro bubbles are compounded, the fireproof performance of the mortar can be improved, and the mechanical property of the mortar is also obviously improved.
Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Claims (10)
1. The utility model provides an aerogel modified fire prevention mortar material that excels in which characterized in that: the high-strength fireproof mortar material comprises cement, sand, polypropylene fibers, composite reinforcing filler, a water reducing agent, a flame retardant and cellulose ether; the sand is mountain sand, and the machine-made sand is prepared from the following raw materials in a mass ratio of (1-2): 2; the cellulose ether is hydroxypropyl methyl cellulose ether and hydroxyethyl methyl cellulose ether in a mass ratio of 1: (0.5-1.5); the composite reinforcing filler is prepared from vitrified micro bubbles and mesoporous nano materials in a mass ratio of 5: the mixture of (1-2); the mesoporous nano material is formed by using nano titanium dioxide particles as a core layer and sequentially coating a nitrogen-doped graphene aerogel layer and a zirconium oxide/silicon oxide aerogel layer on the surface of the core layer.
2. The aerogel modified high-strength fire-proof mortar material as claimed in claim 1, wherein: the water reducing agent is sodium lignosulphonate.
3. The aerogel modified high-strength fire-proof mortar material as claimed in claim 1, wherein: the flame retardant is a mixture of ammonium polyphosphate, aluminum-magnesium layered hydroxide and melamine, and the mass ratio of the ammonium polyphosphate to the aluminum-magnesium layered hydroxide to the melamine is 3: (0.5-1): (1-2).
4. The aerogel modified high-strength fire-proof mortar material as claimed in claim 1, wherein: the weight portions of the components are as follows: 30-50 parts of cement, 30-50 parts of sand, 0.01-0.03 part of polypropylene fiber, 5-10 parts of composite reinforcing filler, 0.05-0.25 part of water reducing agent, 1-2 parts of flame retardant and 0.02-0.05 part of cellulose ether.
5. The preparation method of the aerogel modified high-strength fire-proof mortar material according to any one of claims 1 to 4, characterized by comprising the following steps:
(1) uniformly mixing melamine and a graphene oxide solution, then adding a formaldehyde solution, adding nano titanium dioxide after uniform mixing, placing the prepared mixed solution into a high-pressure kettle for reaction, separating and drying solids after the reaction is finished, and then calcining to prepare the nitrogen-doped graphene aerogel modified nano titanium dioxide;
(2) mixing zirconium oxychloride, tetraethoxysilane, absolute ethyl alcohol and deionized water, uniformly stirring to prepare silicon/zirconium composite sol, adding the prepared nitrogen-doped graphene aerogel modified nano titanium dioxide, uniformly stirring, dropwise adding epoxypropane, violently stirring, standing, aging, performing replacement treatment by using ethanol as a medium, performing supercritical drying by using ethanol as a drying medium, mixing and grinding the dried solid and vitrified micro bubbles to prepare the composite reinforced filler;
(3) weighing the raw materials according to the proportion, adding the weighed raw materials into a stirrer, and uniformly stirring and mixing to obtain the high-strength fireproof mortar material.
6. The preparation method of the aerogel modified high-strength fireproof mortar material according to claim 5, wherein the preparation method comprises the following steps: in the step (1), the mass concentration of the formaldehyde solution is 30-40%, the concentration of the graphene oxide is 8-15mg/ml, and the dosage ratio of the melamine, the graphene oxide solution, the formaldehyde solution and the nano titanium dioxide is (0.2-0.4) g: 15 ml: 1 ml: (0.1-0.2) g.
7. The preparation method of the aerogel modified high-strength fireproof mortar material according to claim 5, wherein the preparation method comprises the following steps: in the step (1), the reaction temperature is 180 ℃, and the reaction time is 10-15 h.
8. The preparation method of the aerogel modified high-strength fireproof mortar material according to claim 5, wherein the preparation method comprises the following steps: in the step (1), the calcination treatment conditions are as follows: introducing nitrogen in the absence of oxygen, heating to 800 ℃ at the speed of 10 ℃/min, carrying out heat preservation treatment for 3h, then cooling to 600 ℃ at the speed of 3 ℃/min, carrying out heat preservation treatment for 2h, and finally cooling to room temperature along with the furnace.
9. The preparation method of the aerogel modified high-strength fireproof mortar material according to claim 5, wherein the preparation method comprises the following steps: in the step (2), the usage ratio of the zirconium oxychloride, the tetraethoxysilane, the absolute ethyl alcohol, the deionized water, the nitrogen-doped graphene aerogel modified nano titanium dioxide and the propylene oxide is (0.2-0.4) g: 1 ml: 15 ml: 20 ml: 10 g: (5-10) ml.
10. The preparation method of the aerogel modified high-strength fireproof mortar material according to claim 5, wherein the preparation method comprises the following steps: in the step (2), the standing aging treatment time is 20-40h, and the replacement treatment condition is that the replacement is carried out for 3 times, and each time lasts for 20-30 h.
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