CN119241198B - Fireproof composite board based on magnesium oxysulfide and preparation method thereof - Google Patents
Fireproof composite board based on magnesium oxysulfide and preparation method thereof Download PDFInfo
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- CN119241198B CN119241198B CN202411270522.3A CN202411270522A CN119241198B CN 119241198 B CN119241198 B CN 119241198B CN 202411270522 A CN202411270522 A CN 202411270522A CN 119241198 B CN119241198 B CN 119241198B
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- 239000002131 composite material Substances 0.000 title claims abstract description 69
- OLZDXDPSDUSGIS-UHFFFAOYSA-N sulfinylmagnesium Chemical compound [Mg].S=O OLZDXDPSDUSGIS-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 48
- 239000007864 aqueous solution Substances 0.000 claims abstract description 29
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 28
- 239000004964 aerogel Substances 0.000 claims abstract description 25
- 239000004568 cement Substances 0.000 claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 14
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 14
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 239000004744 fabric Substances 0.000 claims abstract description 13
- 239000004088 foaming agent Substances 0.000 claims abstract description 13
- 239000003365 glass fiber Substances 0.000 claims abstract description 13
- 239000003607 modifier Substances 0.000 claims abstract description 13
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 11
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 43
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 39
- 229910021389 graphene Inorganic materials 0.000 claims description 28
- 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 description 25
- 239000003063 flame retardant Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 238000009210 therapy by ultrasound Methods 0.000 claims description 16
- 150000007974 melamines Chemical class 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 229920001661 Chitosan Polymers 0.000 claims description 12
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 12
- 239000000017 hydrogel Substances 0.000 claims description 12
- 239000000543 intermediate Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- TXFOLHZMICYNRM-UHFFFAOYSA-N dichlorophosphoryloxybenzene Chemical compound ClP(Cl)(=O)OC1=CC=CC=C1 TXFOLHZMICYNRM-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 229920000877 Melamine resin Polymers 0.000 claims description 10
- 229920001046 Nanocellulose Polymers 0.000 claims description 10
- 238000013329 compounding Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 9
- 239000002070 nanowire Substances 0.000 claims description 9
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 9
- YYXFJSDMOVHLMJ-UHFFFAOYSA-N (4-hydroxyphenoxy)boronic acid Chemical compound OB(O)OC1=CC=C(O)C=C1 YYXFJSDMOVHLMJ-UHFFFAOYSA-N 0.000 claims description 8
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 8
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 7
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 6
- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide Substances CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 claims description 6
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 6
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 6
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims description 6
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 claims description 6
- WPUMTJGUQUYPIV-JIZZDEOASA-L disodium (S)-malate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](O)CC([O-])=O WPUMTJGUQUYPIV-JIZZDEOASA-L 0.000 claims description 6
- 239000010881 fly ash Substances 0.000 claims description 6
- 239000000174 gluconic acid Substances 0.000 claims description 6
- 235000012208 gluconic acid Nutrition 0.000 claims description 6
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 6
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 6
- 235000019265 sodium DL-malate Nutrition 0.000 claims description 6
- 239000001394 sodium malate Substances 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- -1 modified magnesium oxysulfate Chemical class 0.000 claims description 3
- CENHPXAQKISCGD-UHFFFAOYSA-N trioxathietane 4,4-dioxide Chemical compound O=S1(=O)OOO1 CENHPXAQKISCGD-UHFFFAOYSA-N 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 230000002265 prevention Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 238000007710 freezing Methods 0.000 description 6
- 230000008014 freezing Effects 0.000 description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 4
- 239000004566 building material Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000007112 amidation reaction Methods 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 235000021120 animal protein Nutrition 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- FYYHWMGAXLPEAU-OUBTZVSYSA-N magnesium-25 atom Chemical group [25Mg] FYYHWMGAXLPEAU-OUBTZVSYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XMLYCEVDHLAQEL-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-phenylpropan-1-one Chemical group CC(C)(O)C(=O)C1=CC=CC=C1 XMLYCEVDHLAQEL-UHFFFAOYSA-N 0.000 description 1
- OCKGFTQIICXDQW-ZEQRLZLVSA-N 5-[(1r)-1-hydroxy-2-[4-[(2r)-2-hydroxy-2-(4-methyl-1-oxo-3h-2-benzofuran-5-yl)ethyl]piperazin-1-yl]ethyl]-4-methyl-3h-2-benzofuran-1-one Chemical compound C1=C2C(=O)OCC2=C(C)C([C@@H](O)CN2CCN(CC2)C[C@H](O)C2=CC=C3C(=O)OCC3=C2C)=C1 OCKGFTQIICXDQW-ZEQRLZLVSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000011157 hong shi Nutrition 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000003396 thiol group Chemical class [H]S* 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000004078 waterproofing 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
- C04B28/30—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 magnesium cements or similar 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
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Fireproofing Substances (AREA)
Abstract
本发明涉及复合板技术领域，具体为一种基于硫氧镁的防火复合板及其制备方法。本发明通过将轻烧氧化镁和硫酸镁水溶液混合均匀，加入改性剂、复合气凝胶、活性掺合料和发泡剂混合均匀，得到改性硫氧镁水泥浆料；在模板上依次铺设一层无纺布、一层耐碱玻璃纤维网格布，倒入改性硫氧镁水泥浆料，再依次铺设一层耐碱玻璃纤维网格布、一层无纺布；进行一次养护、二次养护，得到防火复合板。本发明制备的防火复合板不仅具有优异的防火性能，能够有效阻止火焰传播和热量传导，而且具备良好的机械强度和耐水性，满足了现代建筑对防火和安全的高要求。The present invention relates to the technical field of composite panels, and specifically to a fireproof composite panel based on magnesium oxysulfide and a preparation method thereof. The present invention obtains a modified magnesium oxysulfide cement slurry by uniformly mixing light-burned magnesium oxide and an aqueous solution of magnesium sulfate, adding a modifier, a composite aerogel, an active admixture and a foaming agent and mixing them uniformly; laying a layer of non-woven fabric and a layer of alkali-resistant glass fiber mesh cloth on the template in sequence, pouring the modified magnesium oxysulfide cement slurry, and then laying a layer of alkali-resistant glass fiber mesh cloth and a layer of non-woven fabric in sequence; performing primary curing and secondary curing to obtain a fireproof composite panel. The fireproof composite panel prepared by the present invention not only has excellent fireproof performance, can effectively prevent flame propagation and heat conduction, but also has good mechanical strength and water resistance, meeting the high requirements of modern buildings for fire prevention and safety.
Description
Technical Field
The invention relates to the technical field of composite boards, in particular to a magnesium oxysulfide-based fireproof composite board and a preparation method thereof.
Background
With the increasing demand of the building industry for fireproof materials, fireproof composite boards are becoming a significant building material and are receiving widespread attention. Magnesium Oxysulfide (MOS) cement is an air hardening cement slurry composed of MgO-MgSO 4-H2 O ternary system, and has the characteristics of light weight, high temperature resistance, easy preparation, green environmental protection and the like, thus being applied to the fields of fireproof door core boards, external wall heat insulation boards and the like.
However, magnesium oxysulfate cement is used as a brittle material, and is easy to crack under the action of external force, and the characteristics lead the magnesium oxysulfide cement to show poor durability in practical application, especially in an environment bearing impact or vibration, and meanwhile, the magnesium oxysulfide cement has poor water resistance and is easy to be influenced by a humid environment, so that the strength and the stability of the material are reduced. This limits its use in some applications where waterproofing is required.
Therefore, we propose a fire-proof composite board based on magnesium oxysulfide and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a magnesium oxysulfide-based fireproof composite board and a preparation method thereof, which are used for solving the problems in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
A preparation method of a fireproof composite board based on magnesium oxysulfide comprises the following steps:
Step S1, uniformly mixing light burned magnesia and magnesium sulfate aqueous solution, adding a modifier, composite aerogel, an active admixture and a foaming agent, and uniformly mixing to obtain modified magnesium oxysulfide cement slurry;
And S2, sequentially paving a layer of non-woven fabric and a layer of alkali-resistant glass fiber grid cloth on the template, pouring modified magnesium oxysulfide cement slurry, sequentially paving a layer of alkali-resistant glass fiber grid cloth and a layer of non-woven fabric, and performing primary curing and secondary curing to obtain the fireproof composite board.
Further, the modified magnesium oxysulfate cement slurry comprises, by weight, 20-45 parts of light burned magnesium oxide, 25-50 parts of a magnesium sulfate aqueous solution, 5-15 parts of composite aerogel, 15-25 parts of an active admixture, 0.1-0.5 part of a foaming agent and 0.1-3.0 parts of a modifier.
Further, the magnesium sulfate aqueous solution is a magnesium sulfate aqueous solution with a density of 1.2-1.3 g/cm 3.
Further, the preparation method of the composite aerogel comprises the following steps:
mixing graphene oxide aqueous solution, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, performing ultrasonic treatment for 30-60 min, adding a mixed solution of oleylamine, ethanol and deionized water, continuing ultrasonic treatment for 2-3 h, stirring for 22-24 h, and centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
uniformly mixing graphene oxide containing double bonds, a flame retardant and a photoinitiator, and irradiating with ultraviolet light to obtain modified graphene oxide;
And (3) uniformly mixing the carboxymethyl chitosan aqueous solution, the modified graphene oxide, the nanocellulose and the hydroxyapatite nanowire, performing ultrasonic treatment for 1-2 hours, adding glutaraldehyde, uniformly stirring, standing for 3-5 hours to obtain composite hydrogel, and performing prefreezing and freeze drying on the composite hydrogel to obtain the composite aerogel.
Further, in the step (1), the mass ratio of the graphene oxide aqueous solution to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide is 1 (0.012-0.015): (0.010-0.012), and the concentration of the graphene oxide aqueous solution is 10mg/mL.
In the step (1), the mass ratio of the oleylamine to the ethanol to the deionized water is 1 (15-20): 10-20%, and the mass of the oleylamine is 3-5% of the mass of the graphene oxide aqueous solution.
In the step (2), the mass ratio of the graphene oxide containing double bonds, the flame retardant and the photoinitiator is 1 (2-4) (0.3-0.5).
Further, the photoinitiator is 2-hydroxy-2-methyl propiophenone.
In the step (2), the ultraviolet irradiation process conditions are that the irradiation wavelength is 360-400 nm, the irradiation time is 0.5-2.0 h, and the irradiation intensity is 20-35 mW/cm 2.
Further, the preparation method of the flame retardant comprises the following steps:
Uniformly mixing melamine and pyridine, heating to 40-50 ℃, introducing nitrogen, adding thioglycollic acid and dicyclohexylcarbodiimide, uniformly mixing, heating to 60-70 ℃, reacting for 1-2 hours at a constant temperature, filtering, distilling under reduced pressure, and drying to obtain modified melamine;
Step B, uniformly mixing 4-hydroxyphenylboric acid and tetrahydrofuran, adding phenylphosphoryl dichloride, dibutyltin oxide and triethylamine under the ice bath condition, reacting for 2-4 hours, continuing to react for 8-10 hours at room temperature, precipitating, filtering, washing and drying to obtain an intermediate;
And step C, uniformly mixing the modified melamine, the intermediate, toluene and triethylamine under the protection of nitrogen, reacting for 2-4 hours at 65-75 ℃, and filtering, washing and drying to obtain the flame retardant.
According to the technical scheme, the carboxyl of thioglycollic acid and the amino of melamine are subjected to amidation reaction, the reaction can be carried out under milder conditions with the help of a dehydrating agent, only one amino group on the melamine is reacted to obtain modified melamine by controlling the slight excess of the melamine, one-Cl in the phenylphosphoryl dichloride is reacted with the hydroxyl in the 4-hydroxyphenylboric acid by controlling the slight excess of the phenylphosphoryl dichloride, the hydrogen chloride generated by the reaction is removed by triethylamine to obtain an intermediate, and finally the flame retardant containing N, P, B elements is obtained by utilizing the reaction of the rest-Cl in the phenylphosphoryl dichloride and one amino group in the modified melamine.
In the step A, the mass ratio of melamine, pyridine, thioglycollic acid and dicyclohexylcarbodiimide is 1 (6.5-7.0): 0.6-0.7): 1.3-1.5.
In the step B, the mass ratio of the 4-hydroxyphenylboric acid to the tetrahydrofuran to the phenylphosphoryl dichloride to the dibutyltin oxide to the triethylamine is 1 (5-10): 1.5-1.6): 0.01-0.03): 0.8-1.0.
In the step C, the mass ratio of the modified melamine to the intermediate to the toluene to the triethylamine is 1 (1.4-1.5) (5-7) (0.8-1.0).
Further, in the step (3), the mass ratio of the carboxymethyl chitosan, the modified graphene oxide, the nano cellulose and the hydroxyapatite nanowire is 1 (0.2-0.5), 0.5-1.0 and 0.4-0.6, and the concentration of the carboxymethyl chitosan aqueous solution is 3wt%.
Further, in the step (3), the mass of glutaraldehyde is 30-50% of the mass of carboxymethyl chitosan.
Further, in the step (3), the pre-freezing process condition is that the pre-freezing is performed for 12-24 hours in a refrigerator with the temperature of minus 10 ℃ to minus 5 ℃.
Further, in the step (3), the process condition of freeze drying is that the materials are dried for 12-24 hours in a freeze dryer at the temperature of-50 to-45 ℃.
Further, the active admixture is prepared by compounding 5-10 parts of metakaolin and 10-15 parts of fly ash.
Further, the foaming agent is an animal protein foaming agent.
Further, the modifier is formed by compounding (0.3-0.5) of gluconic acid, hydroxyethylidene diphosphonic acid and sodium malate according to the mass ratio of 1 (0.3-0.5).
In the step S2, the technological conditions of primary curing and secondary curing are that the material is placed for 20-24 hours in an indoor environment with the temperature of 25-35 ℃ and the relative humidity of 60-70%, and is demoulded, and then the material is subjected to secondary curing for 7-14 days in an indoor environment with the temperature of 20-30 ℃ and the relative humidity of 70-80%, and is demoulded.
Compared with the prior art, the invention has the beneficial effects that:
1. According to the magnesium oxysulfide-based fireproof composite board and the preparation method thereof, the carboxyl of thioglycollic acid and the amino of melamine are subjected to amidation reaction to obtain modified melamine, one-Cl in phenyl phosphoryl dichloride and the hydroxyl in 4-hydroxyphenylboric acid are subjected to reaction to obtain an intermediate, and finally, the rest-Cl in phenyl phosphoryl dichloride and one amino in modified melamine are subjected to reaction to obtain a flame retardant containing N, P, B elements, and meanwhile, the flame retardant contains mercapto and amino, so that an active site is provided for subsequent reaction;
the flame retardant is used for carrying out sulfhydryl-alkene clicking reaction with double bond-containing graphene oxide, so that the flame retardant further improves the flame retardant property of the graphene oxide, and simultaneously, amino is introduced to enable the graphene oxide to carry out crosslinking reaction with aldehyde groups of glutaraldehyde, thereby realizing chemical crosslinking of graphene oxide sheets and polymer groups and improving the hydrophobic property and fireproof property of aerogel.
2. According to the magnesium oxysulfide-based fireproof composite board and the preparation method thereof, carboxymethyl chitosan is used as a natural polymer material, has excellent biocompatibility and environmental protection characteristics, modified graphene oxide is used as a flame retardant, the fireproof performance of the material can be effectively improved, nanocellulose is used as a reinforcing material, the strength and toughness of the composite material are further improved, meanwhile, hydroxyapatite nanowires with good flexibility are used as a skeleton of aerogel, the light weight characteristic and excellent heat insulation performance of the composite material are ensured, glutaraldehyde is used as a cross-linking agent, and the composite aerogel is obtained after freeze drying. The composite aerogel prepared by the invention has excellent performances of heat insulation, light weight, hydrophobicity, temperature resistance, fire resistance and the like, can be used for modifying and compositing magnesium oxysulfide materials, and can be used for obviously overcoming the defects of the existing fireproof plate in the aspects of poor water resistance, high density, high heat conductivity coefficient and the like, thereby improving the overall performance and the application value of the fireproof plate.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the embodiment, the light burned magnesia has an average grain diameter of 200 meshes and a magnesia content of 92 percent and is sourced from Hebei magnesium science and technology Co Ltd; the magnesium sulfate is more than or equal to 98%, is derived from Zhejiang Hua Xuan chemical industry Co, graphene oxide is 1-3 nm in thickness, 4-7 mu m in diameter and 2-5 layers, is derived from Zhejiang Zhi titanium nano new material Co, nanocellulose is CNF, is derived from Hubei Xinyu macro biological medicine technology Co, is 100-200 mu m in length, is 10-100 nm in diameter, is derived from Suzhou Kai New material technology Co, is metakaolin with a particle size of 1250 meshes, is derived from Shijia Yi Hongshi mineral products Co, is a first-order fly ash with a particle size of 200-300 meshes, is derived from Ji Heng novel building material Co, is a foaming agent, is an animal protein foaming agent, is of type FP-50, is a nonwoven fabric, is PP nonwoven fabric, is 25-60 g/m2, is derived from Tokyo Libant new material Co, is an alkali-resistant glass fiber cloth with a mesh size of 5 meshes, is 125g/m2, is derived from Kappy Su Kogyi Co, co.
In the following examples and comparative examples 1 part equals 10g.
Embodiment 1. The preparation method of the magnesium oxysulfide-based fireproof composite board comprises the following steps:
step S1, uniformly mixing 20 parts of light burned magnesium oxide and 25 parts of magnesium sulfate aqueous solution (density is 1.25g/cm 3), adding 0.1 part of modifier (prepared by compounding gluconic acid, hydroxyethylidene diphosphonic acid and sodium malate according to a mass ratio of 1:0.3:0.3), 5 parts of composite aerogel, 15 parts of active admixture (prepared by compounding 5 parts of metakaolin and 10 parts of fly ash) and 0.1 part of foaming agent, and uniformly mixing to obtain modified magnesium oxysulfide cement slurry;
Step S2, sequentially laying a layer of non-woven fabric and a layer of alkali-resistant glass fiber mesh cloth on a template, pouring modified magnesium oxysulfide cement slurry, sequentially laying a layer of alkali-resistant glass fiber mesh cloth and a layer of non-woven fabric, performing primary curing and secondary curing (placing for 20 hours in an indoor environment with the temperature of 25 ℃ and the relative humidity of 60%, demolding, and then performing secondary curing for 7d in an indoor environment with the temperature of 20 ℃ and the relative humidity of 70%, and demolding) to obtain a fireproof composite board;
The preparation method of the composite aerogel comprises the following steps:
mixing 100 parts of a 10mg/mL graphene oxide aqueous solution, 0.12 part of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.1 part of N-hydroxysuccinimide, performing ultrasonic treatment for 30min, adding a mixed solution of 3 parts of oleylamine, 45 parts of ethanol and 30 parts of deionized water, continuing ultrasonic treatment for 2h, stirring for 22h, centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
Uniformly mixing 1.8 parts of graphene oxide containing double bonds, 3.6 parts of flame retardant and 0.54 part of photoinitiator, and irradiating with ultraviolet light (irradiation wavelength is 360nm, irradiation time is 0.5h, and irradiation intensity is 20mW/cm 2) to obtain modified graphene oxide;
Uniformly mixing 200 parts of 3wt% carboxymethyl chitosan aqueous solution, 1.2 parts of modified graphene oxide, 3 parts of nanocellulose and 2.4 parts of hydroxyapatite nanowire, carrying out ultrasonic treatment for 1h, adding 1.8 parts of glutaraldehyde, uniformly stirring, standing for 3h to obtain composite hydrogel, pre-freezing the composite hydrogel in a refrigerator at-10 ℃ for 12h, and drying in a freeze dryer at-50 ℃ for 12h to obtain composite aerogel;
The preparation method of the flame retardant comprises the following steps:
Uniformly mixing 4 parts of melamine and 26 parts of pyridine, heating to 40 ℃, introducing nitrogen, adding 2.4 parts of thioglycollic acid and 5.2 parts of dicyclohexylcarbodiimide, uniformly mixing, heating to 60 ℃, carrying out heat preservation reaction for 1h, and obtaining modified melamine after filtering, reduced pressure distillation and drying;
step B, uniformly mixing 6 parts of 4-hydroxyphenylboric acid and 30 parts of tetrahydrofuran, adding 9 parts of phenylphosphoryl dichloride, 0.06 part of dibutyltin oxide and 4.8 parts of triethylamine under the ice bath condition, reacting for 2 hours, continuing to react for 8 hours at room temperature, and obtaining an intermediate after precipitation, filtration, washing and drying;
And step C, uniformly mixing 4 parts of modified melamine, 5.6 parts of intermediate, 20 parts of toluene and 3.2 parts of triethylamine under the protection of nitrogen, reacting for 2 hours at 65 ℃, and filtering, washing and drying to obtain the flame retardant.
Embodiment 2a preparation method of a fire-proof composite board based on magnesium oxysulfide comprises the following processes:
Step S1, uniformly mixing 35 parts of light burned magnesium oxide and 40 parts of magnesium sulfate aqueous solution (density is 1.25g/cm 3), adding 1.8 parts of modifier (which is formed by compounding gluconic acid, hydroxyethylidene diphosphonic acid and sodium malate according to a mass ratio of 1:0.4:0.4), 10 parts of composite aerogel, 20 parts of active admixture (which is formed by compounding 7 parts of metakaolin and 13 parts of fly ash) and 0.3 part of foaming agent, and uniformly mixing to obtain modified magnesium oxysulfide cement slurry;
Step S2, sequentially laying a layer of non-woven fabric and a layer of alkali-resistant glass fiber mesh cloth on a template, pouring modified magnesium oxysulfide cement slurry, sequentially laying a layer of alkali-resistant glass fiber mesh cloth and a layer of non-woven fabric, performing primary curing and secondary curing (placing for 22 hours in an indoor environment with the temperature of 30 ℃ and the relative humidity of 65%, demolding, and then performing secondary curing for 10 days in an indoor environment with the temperature of 25 ℃ and the relative humidity of 75%, and demolding) to obtain a fireproof composite board;
The preparation method of the composite aerogel comprises the following steps:
Mixing 100 parts of a 10mg/mL graphene oxide aqueous solution, 0.14 part of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.12 part of N-hydroxysuccinimide, performing ultrasonic treatment for 50min, adding a mixed solution of 4 parts of oleylamine, 7.2 parts of ethanol and 6 parts of deionized water, continuing ultrasonic treatment for 2.5h, stirring for 23h, and centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
uniformly mixing 3 parts of graphene oxide containing double bonds, 9 parts of flame retardant and 1.2 parts of photoinitiator, and irradiating with ultraviolet light (the technical condition of ultraviolet light irradiation is that the irradiation wavelength is 380nm, the irradiation time is 1h, and the irradiation intensity is 30mW/cm 2) to obtain modified graphene oxide;
Uniformly mixing 300 parts of 3wt% carboxymethyl chitosan aqueous solution, 2.7 parts of modified graphene oxide, 6 parts of nanocellulose and 4.5 parts of hydroxyapatite nanowire, carrying out ultrasonic treatment for 1.5 hours, adding 3.6 parts of glutaraldehyde, uniformly stirring, standing for 4 hours to obtain composite hydrogel, pre-freezing the composite hydrogel in a refrigerator at-6 ℃ for 18 hours, and drying in a freeze dryer at-48 ℃ for 18 hours to obtain composite aerogel;
The preparation method of the flame retardant comprises the following steps:
Uniformly mixing 10 parts of melamine and 660 parts of pyridine, heating to 45 ℃, introducing nitrogen, adding 6.5 parts of thioglycollic acid and 14 parts of dicyclohexylcarbodiimide, uniformly mixing, heating to 65 ℃, carrying out heat preservation reaction for 1.5 hours, and obtaining modified melamine after filtering, reduced pressure distillation and drying;
Step B, uniformly mixing 14.5 parts of 4-hydroxyphenylboric acid and 110 parts of tetrahydrofuran, adding 22 parts of phenylphosphoryl dichloride, 0.3 part of dibutyltin oxide and 13 parts of triethylamine under the ice bath condition, reacting for 3 hours, continuing to react for 9 hours at room temperature, and obtaining an intermediate after precipitation, filtration, washing and drying;
And step C, uniformly mixing 10 parts of modified melamine, 14.5 parts of intermediate, 60 parts of toluene and 9 parts of triethylamine under the protection of nitrogen, reacting for 3 hours at 70 ℃, and filtering, washing and drying to obtain the flame retardant.
Embodiment 3a method for preparing a fire-proof composite board based on magnesium oxysulfide comprises the following processes:
Step S1, uniformly mixing 45 parts of light burned magnesium oxide and 25 parts of magnesium sulfate aqueous solution (density is 1.25g/cm 3), adding 3.0 parts of modifier (which is formed by compounding gluconic acid, hydroxyethylidene diphosphonic acid and sodium malate according to a mass ratio of 1:0.5:0.5), 15 parts of composite aerogel, 25 parts of active admixture (which is formed by compounding 10 parts of metakaolin and 15 parts of fly ash) and 0.5 part of foaming agent, and uniformly mixing to obtain modified magnesium oxysulfide cement slurry;
Step S2, sequentially laying a layer of non-woven fabric and a layer of alkali-resistant glass fiber mesh cloth on a template, pouring modified magnesium oxysulfide cement slurry, sequentially laying a layer of alkali-resistant glass fiber mesh cloth and a layer of non-woven fabric, performing primary curing and secondary curing (placing for 24 hours in an indoor environment with the temperature of 35 ℃ and the relative humidity of 70%, demolding, and then performing secondary curing for 14d and demolding in an environment with the temperature of 30 ℃ and the relative humidity of 80%) to obtain a fireproof composite board;
The preparation method of the composite aerogel comprises the following steps:
Mixing 100 parts of a 10mg/mL graphene oxide aqueous solution, 0.15 part of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.12 part of N-hydroxysuccinimide, performing ultrasonic treatment for 60min, adding a mixed solution of 5 parts of oleylamine, 100 parts of ethanol and 100 parts of deionized water, continuing ultrasonic treatment for 3h, stirring for 24h, centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
Uniformly mixing 8 parts of graphene oxide containing double bonds, 32 parts of flame retardant and 4 parts of photoinitiator, and irradiating with ultraviolet light (irradiation wavelength 400nm, irradiation time 2.0h, and irradiation intensity 35mW/cm 2) to obtain modified graphene oxide;
Uniformly mixing 500 parts of 3wt% carboxymethyl chitosan aqueous solution, 7.5 parts of modified graphene oxide, 15 parts of nanocellulose and 9 parts of hydroxyapatite nanowire, carrying out ultrasonic treatment for 2 hours, adding 7.5 parts of glutaraldehyde, uniformly stirring, standing for 5 hours to obtain composite hydrogel, pre-freezing the composite hydrogel in a refrigerator at-5 ℃ for 24 hours, and drying in a freeze dryer at-45 ℃ for 24 hours to obtain composite aerogel;
The preparation method of the flame retardant comprises the following steps:
Step A, uniformly mixing 32 parts of melamine and 224 parts of pyridine, heating to 50 ℃, introducing nitrogen, adding 22.4 parts of thioglycollic acid and 48 parts of dicyclohexylcarbodiimide, uniformly mixing, heating to 70 ℃, carrying out heat preservation reaction for 2 hours, and obtaining modified melamine after filtration, reduced pressure distillation and drying;
step B, uniformly mixing 48 parts of 4-hydroxyphenylboric acid and 480 parts of tetrahydrofuran, adding 76.8 parts of phenylphosphoryl dichloride, 1.44 parts of dibutyltin oxide and 48 parts of triethylamine under the ice bath condition, reacting for 4 hours, continuing to react for 10 hours at room temperature, and obtaining an intermediate after precipitation, filtration, washing and drying;
And step C, uniformly mixing 32 parts of modified melamine, 48 parts of intermediate, 224 parts of toluene and 32 parts of triethylamine under the protection of nitrogen, reacting for 4 hours at 75 ℃, and filtering, washing and drying to obtain the flame retardant.
Comparative example 1 the modified magnesium oxysulfate cement slurry comprises, by weight, 20 parts of light burned magnesium oxide, 25 parts of a magnesium sulfate aqueous solution, 15 parts of an active admixture, 0.1 part of a foaming agent and 0.1 part of a modifier, and compared with example 1, comparative example 1 is free of addition of composite aerogel, and the other steps and processes are the same as in example 1.
Comparative example 2A preparation method of a fire-proof composite board based on magnesium oxysulfide comprises the following processes:
compared with the example 2, the modifier in the comparative example 2 is prepared by compounding gluconic acid, hydroxyethylidene diphosphonic acid and sodium malate according to the mass ratio of 1:2:1, and other steps are the same as the example 2.
Comparative example 3A method for preparing a fire-proof composite board based on magnesium oxysulfide comprises the following processes:
The preparation method of the composite aerogel comprises the following steps:
uniformly mixing 300 parts of 3wt% carboxymethyl chitosan aqueous solution, 2.7 parts of graphene oxide, 6 parts of nanocellulose and 4.5 parts of hydroxyapatite nanowire, carrying out ultrasonic treatment for 1.5 hours, adding 3.6 parts of glutaraldehyde, uniformly stirring, standing for 4 hours to obtain composite hydrogel, pre-freezing the composite hydrogel in a refrigerator at-6 ℃ for 18 hours, and drying the composite hydrogel in a freeze dryer at-48 ℃ for 18 hours to obtain composite aerogel;
Comparative example 3 the modified graphene oxide was replaced with the same mass of graphene oxide as example 2, except that the procedure was the same as example 2.
The test comprises the steps of taking the fireproof composite boards obtained in examples 1-3 and comparative examples 1-3, preparing samples, respectively detecting the performances of the samples and recording detection results:
The flexural strength and the wet expansion rate are measured according to JC 688-2006 standard of glass magnesium plate, the specification of the sample is 2440mm multiplied by 1220mm multiplied by 8mm, and the fire resistance grade is measured according to GB 8624-2012 standard of building Material and product Combustion Performance Classification.
The test results were as follows:
From the data in the above table, the following conclusions can be clearly drawn:
Compared with examples 1-3, the flexural strength, wet expansion rate and fire resistance of the product obtained in comparative example 1 are all reduced, which shows that the composite aerogel prepared by the invention has remarkable advantages in mechanical property, water resistance and fire resistance, thereby improving the overall performance of the fire-proof composite board.
Compared with examples 1-3, the flexural strength of the product obtained in comparative example 2 is reduced, which shows that the addition of the modifier can obviously improve the flexural strength of magnesium oxysulfate cement, but the effect is influenced by the proportion of the components.
Compared with examples 1-3, the flexural strength, the wet expansion rate and the fire resistance of the product obtained in the comparative example 3 are all reduced, and compared with graphene oxide, the modified graphene oxide prepared by the invention has better flame retardant effect and hydrophobic property, thereby effectively improving the fire resistance and the water resistance of the material.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. A preparation method of a fireproof composite board based on magnesium oxysulfide is characterized by comprising the following steps:
Step S1, uniformly mixing light burned magnesia and magnesium sulfate aqueous solution, adding a modifier, composite aerogel, an active admixture and a foaming agent, and uniformly mixing to obtain modified magnesium oxysulfide cement slurry;
Step S2, sequentially laying a layer of non-woven fabric and a layer of alkali-resistant glass fiber mesh cloth on the template, pouring modified magnesium oxysulfide cement slurry, sequentially laying a layer of alkali-resistant glass fiber mesh cloth and a layer of non-woven fabric, and performing primary curing and secondary curing to obtain the fireproof composite board;
the modified magnesium oxysulfate cement slurry comprises, by weight, 20-45 parts of light burned magnesium oxide, 25-50 parts of a magnesium sulfate aqueous solution, 5-15 parts of composite aerogel, 15-25 parts of an active admixture, 0.1-0.5 part of a foaming agent and 0.1-3.0 parts of a modifier;
The preparation method of the composite aerogel comprises the following steps:
mixing graphene oxide aqueous solution, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, performing ultrasonic treatment for 30-60 min, adding a mixed solution of oleylamine, ethanol and deionized water, continuing ultrasonic treatment for 2-3 h, stirring for 22-24 h, and centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
uniformly mixing graphene oxide containing double bonds, a flame retardant and a photoinitiator, and irradiating with ultraviolet light to obtain modified graphene oxide;
Uniformly mixing carboxymethyl chitosan aqueous solution, modified graphene oxide, nanocellulose and hydroxyapatite nanowire, performing ultrasonic treatment for 1-2 hours, adding glutaraldehyde, uniformly stirring, and standing for 3-5 hours to obtain composite hydrogel;
the preparation method of the flame retardant comprises the following steps:
Uniformly mixing melamine and pyridine, heating to 40-50 ℃, introducing nitrogen, adding thioglycollic acid and dicyclohexylcarbodiimide, uniformly mixing, heating to 60-70 ℃, reacting for 1-2 hours at a constant temperature, filtering, distilling under reduced pressure, and drying to obtain modified melamine;
Step B, uniformly mixing 4-hydroxyphenylboric acid and tetrahydrofuran, adding phenylphosphoryl dichloride, dibutyltin oxide and triethylamine under the ice bath condition, reacting for 2-4 hours, continuing to react for 8-10 hours at room temperature, precipitating, filtering, washing and drying to obtain an intermediate;
step C, under the protection of nitrogen, uniformly mixing modified melamine, an intermediate, toluene and triethylamine, reacting for 2-4 hours at 65-75 ℃, and filtering, washing and drying to obtain a flame retardant;
the modifier is formed by compounding (0.5-1.0) of gluconic acid, hydroxyethylidene diphosphonic acid and sodium malate according to the mass ratio of (0.3-0.5).
2. The method for preparing the magnesium oxysulfate-based fireproof composite board as claimed in claim 1, wherein the magnesium sulfate aqueous solution is a magnesium sulfate aqueous solution with a density of 1.2-1.3 g/cm 3.
3. The preparation method of the magnesium oxysulfide-based fireproof composite board is characterized in that in the step (2), the mass ratio of graphene oxide containing double bonds, a flame retardant and a photoinitiator is 1 (2-4) (0.3-0.5).
4. The preparation method of the magnesium oxysulfide-based fireproof composite board is characterized in that in the step (3), the mass ratio of carboxymethyl chitosan, modified graphene oxide, nanocellulose and hydroxyapatite nanowires is 1 (0.3-0.5) (0.5-1.0), and the concentration of carboxymethyl chitosan aqueous solution is 3wt%.
5. The method for preparing the magnesium oxysulfide-based fireproof composite board as claimed in claim 1, wherein the active admixture is compounded by 5-10 parts of metakaolin and 10-15 parts of fly ash.
6. The fire-proof composite board based on magnesium oxysulfide prepared by the preparation method according to any one of claims 1-5.
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| CN113979715A (en) * | 2021-11-25 | 2022-01-28 | 响水华夏特材科技发展有限公司 | Aerogel modified magnesium oxysulfate fireproof insulation board and preparation method thereof |
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| CN106752681B (en) * | 2016-11-23 | 2019-05-14 | 厦门大学 | A kind of Water-borne inflation type refractory coating and preparation method thereof based on modified graphene oxide |
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| CN113979715A (en) * | 2021-11-25 | 2022-01-28 | 响水华夏特材科技发展有限公司 | Aerogel modified magnesium oxysulfate fireproof insulation board and preparation method thereof |
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