CN116425496B - High-strength gypsum-based fiber board and preparation method thereof - Google Patents
High-strength gypsum-based fiber board and preparation method thereof Download PDFInfo
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- CN116425496B CN116425496B CN202310257060.0A CN202310257060A CN116425496B CN 116425496 B CN116425496 B CN 116425496B CN 202310257060 A CN202310257060 A CN 202310257060A CN 116425496 B CN116425496 B CN 116425496B
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- 239000010440 gypsum Substances 0.000 title claims abstract description 111
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 111
- 239000011094 fiberboard Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 70
- 239000000945 filler Substances 0.000 claims abstract description 67
- 239000000835 fiber Substances 0.000 claims abstract description 66
- 238000001035 drying Methods 0.000 claims abstract description 50
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 47
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 47
- 241001330002 Bambuseae Species 0.000 claims abstract description 47
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 47
- 239000011425 bamboo Substances 0.000 claims abstract description 47
- 238000002156 mixing Methods 0.000 claims abstract description 45
- 239000000243 solution Substances 0.000 claims abstract description 38
- 239000003610 charcoal Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002002 slurry Substances 0.000 claims abstract description 26
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 244000302661 Phyllostachys pubescens Species 0.000 claims abstract description 16
- 235000003570 Phyllostachys pubescens Nutrition 0.000 claims abstract description 16
- HSEYYGFJBLWFGD-UHFFFAOYSA-N 4-methylsulfanyl-2-[(2-methylsulfanylpyridine-3-carbonyl)amino]butanoic acid Chemical compound CSCCC(C(O)=O)NC(=O)C1=CC=CN=C1SC HSEYYGFJBLWFGD-UHFFFAOYSA-N 0.000 claims abstract description 13
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 13
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 13
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 11
- XVSBWQYHSLNOCU-UHFFFAOYSA-N ethenyl(dimethyl)silicon Chemical compound C[Si](C)C=C XVSBWQYHSLNOCU-UHFFFAOYSA-N 0.000 claims abstract description 11
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 9
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 239000011812 mixed powder Substances 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 33
- 238000005406 washing Methods 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 20
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 18
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 18
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 14
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 12
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- LFRDHGNFBLIJIY-UHFFFAOYSA-N trimethoxy(prop-2-enyl)silane Chemical compound CO[Si](OC)(OC)CC=C LFRDHGNFBLIJIY-UHFFFAOYSA-N 0.000 claims description 7
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 6
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 6
- 235000011151 potassium sulphates Nutrition 0.000 claims description 6
- 230000001680 brushing effect Effects 0.000 claims description 5
- 125000006850 spacer group Chemical group 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 14
- 230000008859 change Effects 0.000 abstract description 10
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 8
- 239000004917 carbon fiber Substances 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000010000 carbonizing Methods 0.000 abstract description 3
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 239000004566 building material Substances 0.000 abstract description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 20
- 238000005457 optimization Methods 0.000 description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 5
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- 229920000548 poly(silane) polymer Polymers 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 4
- 125000001841 imino group Chemical group [H]N=* 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 125000003827 glycol group Chemical group 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003139 buffering effect Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000006459 hydrosilylation reaction Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000008439 repair process Effects 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
- C04B28/14—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 calcium sulfate cements
- C04B28/145—Calcium sulfate hemi-hydrate with a specific crystal form
- C04B28/146—Calcium sulfate hemi-hydrate with a specific crystal form alpha-hemihydrate
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a high-strength gypsum-based fiber board and a preparation method thereof, and relates to the technical field of building materials. When the high-strength gypsum-based fiber board is prepared, firstly, dripping an aluminum ammonium sulfate solution and an tetraethoxysilane solution into an ammonium bicarbonate solution for reaction, filtering and calcining the mixture to obtain a nano porous filler, reacting the nano porous filler with triethoxysilane, then sequentially reacting the nano porous filler with vinyldimethylsilane and allyl trimethoxy to obtain a modified nano porous filler, carbonizing moso bamboo fibers, oxidizing the carbonized moso bamboo fibers with nitric acid, and finally aminating the carbonized moso bamboo fibers with ethylenediamine to obtain aminated bamboo carbon fibers; mixing gypsum, talcum powder, modified nano porous filler and aminated bamboo charcoal fiber, adding the mixed solution of pure water and silica sol, and stirring to form gypsum slurry; and (3) pouring the gypsum slurry into a plate-shaped mold coated with a release agent, drying, demolding and performing step-type roasting to prepare the high-strength gypsum-based fiber board. The high-strength gypsum-based fiber board prepared by the invention has excellent bending strength and temperature change resistance.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a high-strength gypsum-based fiber board and a preparation method thereof.
Background
The gypsum-based fiber board is a novel building board which takes building gypsum powder as a main raw material and various fibers as reinforcing materials. The gypsum-based fiber board can be used as drywall boards, wall liners, partition boards, back panels for tiles and bricks, prefabricated exterior cladding, ceiling blocks, floor fire doors and posts, wall panels, and special applications such as interior walls for trailers and boats, exterior insulation finishing systems.
However, due to the performance limitation of the gypsum material, the gypsum-based fiber board often has the defects of low bending strength, easy cracking and the like. The present application thus improves the performance of gypsum-based fiber board in all respects by modifying the fillers, fibers, and manufacturing processes used in the gypsum-based fiber board.
Disclosure of Invention
The invention aims to provide a high-strength gypsum-based fiber board and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
The high-strength gypsum-based fiber board is prepared by pouring gypsum slurry into a plate-shaped mold coated with a release agent, drying, demolding and performing step-type roasting; the gypsum slurry consists of gypsum mixed powder and mixed liquid; the isolating agent is prepared by the reaction of polyethylene glycol PEG400 and 1, 3-diethoxy-1, 3-tetramethyl disiloxane.
As optimization, the gypsum mixed powder is composed of gypsum, talcum powder, modified nano porous filler and aminated bamboo charcoal fiber; the mixed solution consists of pure water and silica sol.
As optimization, the modified nano porous filler is prepared by dripping an aluminum ammonium sulfate solution and an tetraethoxysilane solution into an ammonium bicarbonate solution for reaction, filtering and calcining the mixture to obtain the nano porous filler, reacting the nano porous filler with triethoxysilane, and then sequentially reacting with vinyldimethylsilane and allyltrimethoxy; the aminated bamboo carbon fiber is prepared by carbonizing moso bamboo fiber, oxidizing with nitric acid, and aminating with ethylenediamine.
The preparation method of the high-strength gypsum-based fiber board comprises the following preparation steps:
(1) Uniformly mixing nano porous filler, triethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:1 (6-8), adding ammonia water with the mass fraction of 15-20% and the mass of 6-8 times of the nano porous filler, stirring for 30-40 min at the temperature of 10-30 ℃ and the speed of 200-300 r/min, centrifugally separating, washing for 3-5 times by using the absolute ethyl alcohol, and drying for 4-6 h at the temperature of 60-70 ℃ to obtain pretreated porous filler; uniformly mixing the pretreated porous filler and a section of modified liquid according to the mass ratio of 1 (7-8), stirring at 70-80 ℃ for reaction for 4-6 hours at 500-800 r/min, centrifugally separating, washing with absolute ethyl alcohol for 3-5 times, drying at 60-70 ℃ for 4-6 hours, placing in a second section of modified liquid with the mass 7-8 times of the pretreated porous filler in a nitrogen atmosphere, and drying at 60-70 ℃ for 4-6 hours to obtain the modified nano porous filler;
(2) Immersing bamboo charcoal fiber in nitric acid with the mass fraction of 60-68%, stirring and reacting for 40-50 min at 70-80 ℃ and 300-500 r/min, filtering, washing with pure water and absolute ethyl alcohol for 3-5 times respectively, and drying for 3-4 h at 60-70 ℃ to obtain oxidized bamboo charcoal fiber; uniformly mixing oxidized bamboo charcoal fiber, ethylenediamine and pure water according to the mass ratio of 1:1 (15-20), stirring at 60-70 ℃ for reaction for 2-3 hours at 300-500 r/min, filtering, washing pure water and absolute ethyl alcohol for 3-5 times respectively, and drying at 60-70 ℃ for 3-4 hours to obtain aminated bamboo charcoal fiber;
(3) Uniformly mixing the alpha-hemihydrate gypsum with 200-300 meshes, talcum powder with 300-400 meshes, modified nano porous filler and aminated bamboo charcoal fiber according to the mass ratio of (5-6) to (1) (3-4) to (1), and stirring at the temperature of 10-30 ℃ for 2-3 min at the speed of 200-300 r/min to obtain gypsum mixed powder; pouring mixed liquid with the mass of 0.50-0.55 times of that of the gypsum mixed powder into the gypsum mixed powder, adding n-butyl alcohol with the mass of 0.0005-0.0006 times of that of the gypsum mixed powder and potassium sulfate with the mass of 0.02-0.03 times of that of the gypsum mixed powder, and stirring for 40-60 s at the temperature of 10-30 ℃ at the speed of 300-500 r/min to prepare gypsum slurry;
(4) Brushing a spacer agent with the thickness of 0.1-0.2 mm on the inner cavity of the plate-shaped mould, pouring gypsum slurry into the plate-shaped mould within 10-15 s, using a vibrating rod with the power of 800W to assist in exhausting for 2-3 min, naturally drying in air for 20-30 min, demoulding, drying at room temperature for 40-48 h, placing in a muffle furnace for step roasting, cooling to 10-20 ℃ at a constant speed of 30-40 ℃/h, and taking out to obtain the high-strength gypsum-based fiber board.
As optimization, the preparation method of the nano porous filler in the step (1) comprises the following steps: stirring 2mol/L ammonium bicarbonate solution at the temperature of 10-20 ℃ at the speed of 300-500 r/min, keeping stirring, dripping 0.1mol/L aluminum ammonium sulfate solution at the speed of 0.1-0.2 g/s, dripping 0.1mol/L tetraethoxysilane solution at the speed of 0.1-0.2 g/s, keeping the pH value at 9-10 by 15-20% of ammonia water in the dripping process, continuing stirring for 50-60 min after the dripping is finished, standing for 3-5 h, filtering, washing with pure water and absolute ethyl alcohol for 3-5 times respectively, drying at the temperature of 100-110 ℃ for 2-3 h, putting into a muffle furnace, heating to 1100-1200 ℃ at the heating rate of 60-70 ℃ for calcining for 14-18 h, cooling to room temperature, and taking out to prepare the product; the solvent of the ammonium bicarbonate and aluminum ammonium sulfate solution is water; the solvent of the ethyl orthosilicate solution is ethanol.
As optimization, the first-stage modified liquid in the step (1) is prepared by uniformly mixing vinyl dimethyl silane, n-hexane and chloroplatinic acid according to the mass ratio of 1 (6-8) (0.006-0.008); the second-stage modification liquid is prepared by uniformly mixing allyl trimethoxy silane, n-hexane and chloroplatinic acid according to the mass ratio of 1 (6-8) (0.006-0.008) in a nitrogen atmosphere.
As optimization, the preparation method of the bamboo charcoal fiber in the step (2) comprises the following steps: soaking moso bamboo fibers in 30-40% urea aqueous solution for 2-3 h, taking out, sequentially standing at 90-110 ℃ for 20-30 min in a nitrogen atmosphere, standing at 300-400 ℃ for 40-50 min, standing at 1000-1200 ℃ for 20-30 min, and cooling to room temperature to prepare the bamboo fiber; the moso bamboo fibers are in a fiber bundle form, the linear density is 30-40 dtex, and the fiber length is 80-120 mm.
As optimization, the mixed solution in the step (3) is prepared by uniformly mixing pure water and silica sol BJN-515 according to the mass ratio of 1 (0.3-0.35).
As optimization, the preparation method of the release agent in the step (4) comprises the following steps: uniformly mixing polyethylene glycol PEG400 and 1, 3-diethoxy-1, 3-tetramethyl disiloxane according to the mass ratio of 1 (0.5-0.6), adding p-toluenesulfonic acid with the mass of 0.004-0.006 times that of the ethylene glycol PEG400, stirring and reacting for 20-30 min at the temperature of 300-500 r/min at the temperature of 80-90 ℃ in nitrogen atmosphere, heating to 140-160 ℃ and continuously stirring and reacting for 6-8 h, cooling to the room temperature, and standing for 30-40 min at the temperature of 50-60 ℃ at the pressure of 1-2 kPa.
As optimization, the technological parameters of the step-type roasting in the step (4) are as follows: sequentially roasting for 1h at 50-60 ℃, 2h at 100-120 ℃, 2h at 200-220 ℃, 2h at 300-320 ℃ and the heating rate in the roasting process is 80-100 ℃/h.
Compared with the prior art, the invention has the following beneficial effects:
The invention is used for preparing the high-strength gypsum-based fiber board; mixing gypsum, talcum powder, modified nano porous filler and aminated bamboo charcoal fiber into gypsum mixed powder; mixing pure water and silica sol to prepare a mixed solution; the gypsum slurry is prepared by mixing and stirring gypsum mixed powder and mixed liquid; and (3) pouring the gypsum slurry into a plate-shaped mold coated with a release agent, drying, demolding and performing step-type roasting to prepare the high-strength gypsum-based fiber board.
Firstly, dropwise adding an aluminum ammonium sulfate solution and an tetraethoxysilane solution into an ammonium bicarbonate solution for reaction, filtering and calcining to obtain a nano porous filler, reacting the nano porous filler with triethoxysilane, then sequentially reacting with vinyldimethylsilane and allyltrimethoxy to obtain a modified nano porous filler, polymerizing and growing vinyldimethylsilane on the surface of the nano porous composite filler through hydrosilylation reaction, forming polysilane branched chains on the surface, reacting with allyltrimethoxy silane, hydrolyzing the edge end into silicon hydroxyl groups in the subsequent process, hydrophilizing and forming silica connection with other components of gypsum slurry, wherein the middle polysilane chain segment has good flexibility and high temperature resistance, and can play a role of buffering when the volume is changed due to temperature change, thereby improving the bending strength and the temperature change resistance.
Secondly, carbonizing moso bamboo fibers, oxidizing the carbonized moso bamboo fibers by nitric acid, and aminating the carbonized moso bamboo fibers by ethylenediamine to obtain aminated bamboo carbon fibers, wherein the surface of the aminated bamboo carbon fibers is provided with more amino groups and imino groups, the aminated bamboo carbon fibers are not agglomerated and uniformly dispersed in the whole, the amino groups and the imino groups are easy to form covalent bonds with metal ions, and a complexation reaction occurs, so that the dissolution rate of calcium in gypsum slurry is improved, the compactness is improved, and the supersaturation of calcium hydroxide generated by the gypsum slurry is improved due to the formation of a complex, so that the hydration of gypsum is effectively prevented from generating a loose crystalline phase structure, the compactness is further improved, and the bending strength and the temperature change resistance are improved; compared with silicon oil, the release agent prepared by reacting polyethylene glycol PEG400 and 1, 3-diethoxy-1, 3-tetramethyl disiloxane has the advantages that polyethylene glycol chain segments in the release agent remained on the surface can pass through after demolding, so that water molecules can be dried conveniently, and the release agent is cracked into small molecular gas at high temperature, so that the generated chain segments can be connected with silicon on the surface of a gypsum board to repair surface gaps and defects, and the bending strength is improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, 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.
Example 1
The preparation method of the high-strength gypsum-based fiber board mainly comprises the following preparation steps:
(1) Stirring 2mol/L ammonium bicarbonate solution at the temperature of 10 ℃ and the rotating speed of 300r/min, keeping stirring, dripping 0.1mol/L aluminum ammonium sulfate solution at the speed of 0.1g/s, dripping 0.1mol/L tetraethoxysilane solution at the speed of 0.1g/s, keeping the pH at 9 through 20 mass percent of ammonia water in the dripping process, continuously stirring for 50min after the dripping is finished, standing for 5h, filtering, washing with pure water and absolute ethyl alcohol for 3 times respectively, drying for 3h at 100 ℃, putting in a muffle furnace, heating to 1100 ℃ at the heating rate of 60 ℃/h, calcining for 18h, cooling to room temperature, and taking out to obtain the nano porous filler; uniformly mixing nano porous filler, triethoxysilane and absolute ethyl alcohol according to a mass ratio of 1:1:6, adding ammonia water with a mass fraction of 15% and 6 times that of the nano porous filler, stirring for 40min at 10 ℃ and 200r/min, centrifugally separating, washing with absolute ethyl alcohol for 3 times, and drying at 60 ℃ for 6h to obtain pretreated porous filler; uniformly mixing vinyl dimethyl silane, n-hexane and chloroplatinic acid according to the mass ratio of 1:6:0.006 to prepare a section of modified liquid; in a nitrogen atmosphere, uniformly mixing allyl trimethoxy silane, n-hexane and chloroplatinic acid according to the mass ratio of 1:6:0.006 to prepare a two-stage modified liquid; uniformly mixing the pretreated porous filler and a section of modified liquid according to the mass ratio of 1:7, stirring at 70 ℃ for reaction for 6 hours at 500r/min, centrifugally separating, washing with absolute ethyl alcohol for 3 times, drying at 60 ℃ for 6 hours, placing in a second section of modified liquid with the mass 7 times of that of the pretreated porous filler in a nitrogen atmosphere, and drying at 60 ℃ for 6 hours to obtain the modified nano porous filler;
(2) Soaking moso bamboo fibers with the linear density of 30dtex and the fiber length of 80mm in a urea aqueous solution with the mass fraction of 30% for 3 hours, taking out, sequentially standing at 90 ℃ for 30min, at 300 ℃ for 50min, at 1000 ℃ for 30min in a nitrogen atmosphere, and cooling to room temperature to obtain bamboo charcoal fibers; immersing the bamboo charcoal fiber in 60% nitric acid by mass, stirring at 70deg.C and 300r/min for reacting for 50min, filtering, washing with pure water and absolute ethanol for 3 times, and drying at 60deg.C for 4 hr to obtain oxidized bamboo charcoal fiber; uniformly mixing oxidized bamboo charcoal fiber, ethylenediamine and pure water according to a mass ratio of 1:1:15, stirring at 60 ℃ and 300r/min for reaction for 3 hours, filtering, washing the mixture with pure water and absolute ethyl alcohol for 3 times respectively, and drying the mixture at 60 ℃ for 4 hours to obtain aminated bamboo charcoal fiber;
(3) Pure water and silica sol BJN-515 are uniformly mixed according to the mass ratio of 1:0.3 to prepare mixed solution; uniformly mixing 200-mesh alpha-type semi-hydrated gypsum, 300-mesh talcum powder, modified nano porous filler and aminated bamboo charcoal fiber according to the mass ratio of 5:1:3:1, and stirring at 10 ℃ for 3min at 200r/min to obtain gypsum mixed powder; pouring mixed liquid with the mass of 0.50 times of that of the gypsum mixed powder into the gypsum mixed powder, adding n-butanol with the mass of 0.0005 times of that of the gypsum mixed powder and potassium sulfate with the mass of 0.02 times of that of the gypsum mixed powder, and stirring at 10 ℃ for 60s at 300r/min to prepare gypsum slurry;
(4) Uniformly mixing polyethylene glycol PEG400 and 1, 3-diethoxy-1, 3-tetramethyl disiloxane according to a mass ratio of 1:0.5, adding p-toluenesulfonic acid with the mass of 0.004 times that of the ethylene glycol PEG400, stirring and reacting for 30min at 80 ℃ and 300r/min in a nitrogen atmosphere, heating to 140 ℃ and continuously stirring and reacting for 8h, cooling to room temperature, and standing for 40min at 50 ℃ and 1kPa to prepare the release agent; brushing a spacer agent with the thickness of 0.1mm on the inner cavity of the plate-shaped mould, pouring gypsum slurry into the plate-shaped mould within 10 seconds, using a vibrating rod with the power of 800W to assist in exhausting for 3 minutes, naturally drying for 20 minutes in air, demoulding, drying for 40 hours at room temperature, placing in a horse fluorine furnace, sequentially roasting for 1 hour at 50 ℃,2 hours at 100 ℃,2 hours at 200 ℃,2 hours at 300 ℃, and taking out after the temperature is uniformly reduced to 10 ℃ at the temperature reducing rate of 30 ℃/h, thereby obtaining the high-strength gypsum-based fiber board.
Example 2
The preparation method of the high-strength gypsum-based fiber board mainly comprises the following preparation steps:
(1) Stirring 2mol/L ammonium bicarbonate solution at 15 ℃ and 400r/min, keeping stirring, dropwise adding 0.1mol/L aluminum ammonium sulfate solution at the speed of 0.15g/s, dropwise adding 0.1mol/L tetraethoxysilane solution at the speed of 0.15g/s, keeping the pH at 9.5 through 18% ammonia water by mass fraction in the dropwise adding process, continuing stirring for 55min after the dropwise adding process, standing for 4h, filtering, washing with pure water and absolute ethyl alcohol for 4 times, drying at 105 ℃ for 2.5h, placing in a muffle furnace, heating to 1150 ℃ at the heating rate of 65 ℃/h, calcining for 16h, cooling to room temperature, and taking out to obtain the nano porous filler; uniformly mixing nano porous filler, triethoxysilane and absolute ethyl alcohol according to a mass ratio of 1:1:7, adding ammonia water with mass fraction of 18% and mass ratio of 7 times of the nano porous filler, stirring for 35min at 20 ℃ and 250r/min, centrifugally separating, washing with absolute ethyl alcohol for 4 times, and drying for 5h at 65 ℃ to obtain pretreated porous filler; uniformly mixing vinyl dimethyl silane, normal hexane and chloroplatinic acid according to the mass ratio of 1:7:0.007 to prepare a section of modified liquid; in a nitrogen atmosphere, uniformly mixing allyl trimethoxy silane, n-hexane and chloroplatinic acid according to the mass ratio of 1:7:0.007 to prepare a two-stage modified liquid; uniformly mixing the pretreated porous filler and a first-stage modified liquid according to the mass ratio of 1:7.5, stirring at 75 ℃ for reaction for 5 hours at 650r/min, centrifugally separating, washing with absolute ethyl alcohol for 4 times, drying at 65 ℃ for 5 hours, placing in a second-stage modified liquid with the mass 7.5 times that of the pretreated porous filler in a nitrogen atmosphere, and drying at 65 ℃ for 5 hours to obtain the modified nano porous filler;
(2) Soaking moso bamboo fibers with the linear density of 35dtex and the fiber length of 100mm in a urea aqueous solution with the mass fraction of 35% for 2.5h, taking out, sequentially standing at 100 ℃ for 25min, at 350 ℃ for 45min, at 1100 ℃ for 25min, and cooling to room temperature to obtain bamboo charcoal fibers; immersing the bamboo charcoal fiber in 64% nitric acid by mass, stirring at 75deg.C and 400r/min for reacting for 45min, filtering, washing with pure water and absolute ethanol for 4 times, and drying at 65deg.C for 3.5 hr to obtain oxidized bamboo charcoal fiber; uniformly mixing oxidized bamboo charcoal fiber, ethylenediamine and pure water according to a mass ratio of 1:1:18, stirring at 65 ℃ and 400r/min for reaction for 2.5h, filtering, washing pure water and absolute ethyl alcohol for 4 times respectively, and drying at 65 ℃ for 3.5h to obtain aminated bamboo charcoal fiber;
(3) Pure water and silica sol BJN-515 are uniformly mixed according to the mass ratio of 1:0.32 to prepare mixed solution; uniformly mixing 250-mesh alpha-type semi-hydrated gypsum, 350-mesh talcum powder, modified nano porous filler and aminated bamboo charcoal fiber according to the mass ratio of 5.5:1:3.5:1, and stirring at 20 ℃ for 2.5min at 250r/min to obtain gypsum mixed powder; pouring mixed liquid with the mass of 0.52 times of that of the gypsum mixed powder into the gypsum mixed powder, adding n-butyl alcohol with the mass of 0.00055 times of that of the gypsum mixed powder and potassium sulfate with the mass of 0.025 times of that of the gypsum mixed powder, and stirring at 20 ℃ for 50s at 400r/min to prepare gypsum slurry;
(4) Uniformly mixing polyethylene glycol PEG400 and 1, 3-diethoxy-1, 3-tetramethyl disiloxane according to a mass ratio of 1:0.55, adding p-toluenesulfonic acid with the mass of 0.005 times that of the ethylene glycol PEG400, stirring and reacting for 25min at 85 ℃ and 400r/min in a nitrogen atmosphere, heating to 150 ℃ and continuously stirring and reacting for 7h, cooling to room temperature, and standing for 35min at 55 ℃ and 1.5kPa to prepare the release agent; brushing a spacer agent with the thickness of 0.15mm on the inner cavity of the plate-shaped mould, pouring gypsum slurry into the plate-shaped mould within 12 seconds, using a vibrating rod with the power of 800W to assist in exhausting for 2.5 minutes, naturally drying for 25 minutes in air, demoulding, drying for 44 hours at room temperature, placing in a horse fluorine furnace, sequentially roasting for 1 hour at 55 ℃, roasting for 2 hours at 110 ℃, roasting for 2 hours at 210 ℃, roasting for 2 hours at 310 ℃, heating up at 90 ℃/h in the roasting process, cooling down to 15 ℃ at a constant speed at a cooling rate of 35 ℃/h, and taking out to obtain the high-strength gypsum-based fiber board.
Example 3
The preparation method of the high-strength gypsum-based fiber board mainly comprises the following preparation steps:
(1) Stirring 2mol/L ammonium bicarbonate solution at a speed of 500r/min at 20 ℃, keeping stirring, dropwise adding 0.1mol/L aluminum ammonium sulfate solution at a speed of 0.2g/s, dropwise adding 0.1mol/L tetraethoxysilane solution at a speed of 0.2g/s, keeping the pH at 10 by 20 mass percent of ammonia water in the dropwise adding process, continuously stirring for 60min after the dropwise adding, standing for 3h, filtering, washing with pure water and absolute ethyl alcohol for 5 times, drying at 110 ℃ for 2h, placing in a muffle furnace, heating to 1200 ℃ at a heating rate of 70 ℃/h, calcining for 14h, cooling to room temperature, and taking out to obtain the nano porous filler; uniformly mixing nano porous filler, triethoxysilane and absolute ethyl alcohol according to a mass ratio of 1:1:8, adding ammonia water with a mass fraction of 20% and 8 times that of the nano porous filler, stirring for 30min at 30 ℃ and 300r/min, centrifugally separating, washing with absolute ethyl alcohol for 5 times, and drying at 70 ℃ for 4 hours to obtain pretreated porous filler; uniformly mixing vinyl dimethyl silane, normal hexane and chloroplatinic acid according to the mass ratio of 1:8:0.008 to prepare a first-stage modified liquid; in a nitrogen atmosphere, uniformly mixing allyl trimethoxy silane, n-hexane and chloroplatinic acid according to the mass ratio of 1:8:0.008 to prepare a two-stage modified liquid; uniformly mixing the pretreated porous filler and a section of modified liquid according to the mass ratio of 1:8, stirring at 80 ℃ for reaction for 4 hours at 800r/min, centrifugally separating, washing with absolute ethyl alcohol for 5 times, drying at 70 ℃ for 4 hours, placing in a second section of modified liquid with the mass 8 times that of the pretreated porous filler in a nitrogen atmosphere, and drying at 70 ℃ for 4 hours to obtain the modified nano porous filler;
(2) Soaking moso bamboo fibers with the linear density of 40dtex and the fiber length of 120mm in a urea aqueous solution with the mass fraction of 40% for 3 hours, taking out, sequentially standing at 110 ℃ for 20min, at 400 ℃ for 40min, at 1200 ℃ for 20min, and cooling to room temperature to obtain bamboo charcoal fibers; immersing the bamboo charcoal fiber in 68% nitric acid at 80deg.C, stirring at 500r/min for reaction for 40min, filtering, washing with pure water and absolute ethanol for 5 times, and drying at 70deg.C for 3 hr to obtain oxidized bamboo charcoal fiber; uniformly mixing oxidized bamboo charcoal fiber, ethylenediamine and pure water according to a mass ratio of 1:1:20, stirring at 70 ℃ for reaction for 2 hours at 500r/min, filtering, washing pure water and absolute ethyl alcohol for 5 times respectively, and drying at 70 ℃ for 3 hours to obtain aminated bamboo charcoal fiber;
(3) Pure water and silica sol BJN-515 are uniformly mixed according to the mass ratio of 1:0.35 to prepare mixed solution; uniformly mixing 300-mesh alpha-type semi-hydrated gypsum, 400-mesh talcum powder, modified nano porous filler and aminated bamboo charcoal fiber according to the mass ratio of 6:1:4:1, and stirring at 30 ℃ for 2min at 300r/min to obtain gypsum mixed powder; pouring mixed liquid with the mass of 0.55 times of the gypsum mixed powder into the gypsum mixed powder, adding n-butyl alcohol with the mass of 0.0006 times of the gypsum mixed powder and potassium sulfate with the mass of 0.03 times of the gypsum mixed powder, and stirring at 30 ℃ for 40s at 500r/min to prepare gypsum slurry;
(4) Uniformly mixing polyethylene glycol PEG400 and 1, 3-diethoxy-1, 3-tetramethyl disiloxane according to a mass ratio of 1:0.6, adding p-toluenesulfonic acid with the mass of 0.006 times that of the ethylene glycol PEG400, stirring and reacting for 20min at 90 ℃ and 500r/min in a nitrogen atmosphere, heating to 160 ℃ and continuously stirring and reacting for 6h, cooling to room temperature, and standing for 30min at 60 ℃ and 2kPa to prepare the release agent; brushing a spacer agent with the thickness of 0.2mm on the inner cavity of the plate-shaped mould, pouring gypsum slurry into the plate-shaped mould within 15 seconds, using a vibrating rod with the power of 800W to assist in exhausting for 3 minutes, naturally drying for 30 minutes in air, demoulding, drying for 40 hours at room temperature, placing in a horse fluorine furnace, sequentially roasting for 1 hour at 60 ℃, roasting for 2 hours at 120 ℃, roasting for 2 hours at 220 ℃, roasting for 2 hours at 320 ℃, heating up to 100 ℃/h in the roasting process, cooling down to 20 ℃ at a constant speed at a cooling rate of 40 ℃/h, and taking out to obtain the high-strength gypsum-based fiber board.
Comparative example 1
The method for preparing the high-strength gypsum-based fiber board of comparative example 1 differs from example 2 only in the step (1), and the step (1) is modified as follows: stirring 2mol/L ammonium bicarbonate solution at 15 ℃ and 400r/min, keeping stirring, dripping 0.1mol/L aluminum ammonium sulfate solution at the speed of 0.15g/s, dripping 0.1mol/L tetraethoxysilane solution at the speed of 0.15g/s, keeping the pH at 9.5 through 18 mass percent of ammonia water in the dripping process, continuing stirring for 55min after dripping, standing for 4h, filtering, washing with pure water and absolute ethyl alcohol for 4 times, drying at 105 ℃ for 2.5h, putting in a muffle furnace, heating to 1150 ℃ at the heating rate of 65 ℃/h, calcining for 16h, cooling to room temperature, and taking out to obtain the nano porous filler. And in step (4) a "nanoporous filler" was used directly, the rest of the procedure being as in example 2.
Comparative example 2
The method for preparing the high-strength gypsum-based fiber board of comparative example 2 differs from example 2 only in the step (1), and the step (1) is modified as follows: stirring 2mol/L ammonium bicarbonate solution at 15 ℃ and 400r/min, keeping stirring, dropwise adding 0.1mol/L aluminum ammonium sulfate solution at the speed of 0.15g/s, dropwise adding 0.1mol/L tetraethoxysilane solution at the speed of 0.15g/s, keeping the pH at 9.5 through 18% ammonia water by mass fraction in the dropwise adding process, continuing stirring for 55min after the dropwise adding process, standing for 4h, filtering, washing with pure water and absolute ethyl alcohol for 4 times, drying at 105 ℃ for 2.5h, placing in a muffle furnace, heating to 1150 ℃ at the heating rate of 65 ℃/h, calcining for 16h, cooling to room temperature, and taking out to obtain the nano porous filler; uniformly mixing nano porous filler, triethoxysilane and absolute ethyl alcohol according to a mass ratio of 1:1:7, adding ammonia water with mass fraction of 18% and mass ratio of 7 times of the nano porous filler, stirring for 35min at 20 ℃ and 250r/min, centrifugally separating, washing with absolute ethyl alcohol for 4 times, and drying for 5h at 65 ℃ to obtain pretreated porous filler; uniformly mixing vinyl dimethyl silane, normal hexane and chloroplatinic acid according to the mass ratio of 1:7:0.007 to prepare a section of modified liquid; uniformly mixing the pretreated porous filler and a section of modified liquid according to the mass ratio of 1:7.5, stirring at 75 ℃ and 650r/min for reaction for 5 hours, centrifugally separating, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 5 hours to obtain the modified nano porous filler. The rest of the procedure is the same as in example 2.
Comparative example 3
The method for preparing the high-strength gypsum-based fiber board of comparative example 3 is different from example 2 in that step (2) is modified as follows: soaking moso bamboo fibers with the linear density of 35dtex and the fiber length of 100mm in a urea aqueous solution with the mass fraction of 35% for 2.5h, taking out, sequentially standing at 100 ℃ for 25min, at 350 ℃ for 45min, at 1100 ℃ for 25min, and cooling to room temperature to obtain the bamboo charcoal fibers. And in the step (4), bamboo charcoal fiber is directly used, and the rest steps are the same as in the example 2.
Comparative example 4
The method for preparing the high strength gypsum-based fiber board of comparative example 4 differs from example 2 only in the step (4), and the step (4) is modified as follows: the inner cavity of the plate-shaped mould is coated with H201 methyl silicone oil with the thickness of 0.15mm, gypsum slurry is poured into the plate-shaped mould within 12 seconds, and is assisted to exhaust for 2.5 minutes by a vibrating rod with the power of 800W, naturally dried in air for 25 minutes, demolded, dried at room temperature for 44 hours, placed in a horse fluorine furnace, baked at 55 ℃ for 1 hour, baked at 110 ℃ for 2 hours, baked at 210 ℃ for 2 hours, baked at 310 ℃ for 2 hours, the temperature rising rate in the baking process is 90 ℃/H, cooled to 15 ℃ at a constant speed at the cooling rate of 35 ℃/H, and taken out, thus obtaining the high-strength gypsum-based fiber board.
Comparative example 5
The preparation method of the high-strength gypsum-based fiber board mainly comprises the following preparation steps:
(1) Stirring 2mol/L ammonium bicarbonate solution at 15 ℃ and 400r/min, keeping stirring, dropwise adding 0.1mol/L aluminum ammonium sulfate solution at the speed of 0.15g/s, dropwise adding 0.1mol/L tetraethoxysilane solution at the speed of 0.15g/s, keeping the pH at 9.5 through 18% ammonia water by mass fraction in the dropwise adding process, continuing stirring for 55min after the dropwise adding process, standing for 4h, filtering, washing with pure water and absolute ethyl alcohol for 4 times, drying at 105 ℃ for 2.5h, placing in a muffle furnace, heating to 1150 ℃ at the heating rate of 65 ℃/h, calcining for 16h, cooling to room temperature, and taking out to obtain the nano porous filler;
(2) Soaking moso bamboo fibers with the linear density of 35dtex and the fiber length of 100mm in a urea aqueous solution with the mass fraction of 35% for 2.5h, taking out, sequentially standing at 100 ℃ for 25min, at 350 ℃ for 45min, at 1100 ℃ for 25min, and cooling to room temperature to obtain bamboo charcoal fibers;
(3) Pure water and silica sol BJN-515 are uniformly mixed according to the mass ratio of 1:0.32 to prepare mixed solution; uniformly mixing 250-mesh alpha-type semi-hydrated gypsum, 350-mesh talcum powder, nano porous filler and bamboo charcoal fiber according to the mass ratio of 5.5:1:3.5:1, and stirring at 20 ℃ for 2.5min at 250r/min to obtain gypsum mixed powder; pouring mixed liquid with the mass of 0.52 times of that of the gypsum mixed powder into the gypsum mixed powder, adding n-butyl alcohol with the mass of 0.00055 times of that of the gypsum mixed powder and potassium sulfate with the mass of 0.025 times of that of the gypsum mixed powder, and stirring at 20 ℃ for 50s at 400r/min to prepare gypsum slurry;
(4) The inner cavity of the plate-shaped mould is coated with H201 methyl silicone oil with the thickness of 0.15mm, gypsum slurry is poured into the plate-shaped mould within 12 seconds, and is assisted to exhaust for 2.5 minutes by a vibrating rod with the power of 800W, naturally dried in air for 25 minutes, demolded, dried at room temperature for 44 hours, placed in a horse fluorine furnace, baked at 55 ℃ for 1 hour, baked at 110 ℃ for 2 hours, baked at 210 ℃ for 2 hours, baked at 310 ℃ for 2 hours, the temperature rising rate in the baking process is 90 ℃/H, cooled to 15 ℃ at a constant speed at the cooling rate of 35 ℃/H, and taken out, thus obtaining the high-strength gypsum-based fiber board.
Test case
1. Flexural Strength test
Preparation of flexural Strength samples: the mould size was 70mm x 22.36mm x 11.18mm according to the cuboid sample specified by the JB/T8583-2008 standard.
The testing method comprises the following steps: the bending strength is tested by a three-point bending resistance method, the experimental equipment adopts a WDW-50Y microcomputer to control an electronic universal testing machine, the measurement span is 60mm, the moving speed of a cutter head is 1mm/min, and the calculation formula of the bending strength is as follows:
σ＝(3FL)/(2bh2)
Wherein: sigma-flexural strength in units of MPa;
f a maximum load in units (N) of sample fracture;
L is a span, in units of mm;
b a width of the cross section of the sample in units of (mm);
h is the height of the cross section of the sample in units of mm.
2. Testing of temperature-resistance-change properties
Preparation of a temperature-resistant modified performance sample: the die dimensions were 160mm by 40mm according to cuboid specimens specified by inorganic nonmetallic standard GBT 9776-2008.
The testing method comprises the following steps: placing the sample into a box-type furnace at 100 ℃ for 3 hours, then rapidly placing the sample into a muffle furnace at 300 ℃, preserving the heat for 30 minutes, opening a furnace door to observe the surface of the sample, and grading whether cracks or collapse blocks exist.
The assessment criteria are divided into four levels, each level of criteria being characterized by:
the first surface of the level 1 is smooth and has no crack or has only very tiny crack;
the class 2 one surface has dendritic or netlike tiny cracks, the crack width is less than 0.5mm, and the sample has no collapse and falling phenomenon;
the 3-level surface is provided with dendritic or netlike cracks, the width of the cracks is less than 1mm, the cracks are deeper, no through coarse cracks exist along the transverse direction (namely the horizontal direction) or the longitudinal direction, and the sample does not collapse and fall off;
The 4-level surface is provided with dendritic or netlike cracks, the crack width is larger than 1mm, the longitudinal or transverse directions are provided with through cracks, and the sample can be collapsed and fall off;
The following table 1 gives the results of performance analysis of flexural strength and resistance to temperature change of high strength gypsum-based fiber boards employing examples 1 to 3 of the present invention and comparative examples 1 to 5.
TABLE 1
| Flexural Strength | Grade of temperature change resistance | Flexural Strength | Grade of temperature change resistance | ||
| Example 1 | 5.72MPa | Level 1 | Comparative example 1 | 4.51MPa | 3 Grade |
| Example 2 | 5.73MPa | Level 1 | Comparative example 2 | 3.27MPa | Grade 4 |
| Example 3 | 5.69MPa | Level 1 | Comparative example 3 | 4.15MPa | Level 2 |
| Comparative example 4 | 5.40MPa | Level 2 | |||
| Comparative example 5 | 2.34MPa | 3 Grade |
As can be seen from a comparison of the experimental data of examples 1 to 3 and comparative examples 1 to 5 in Table 1, the high-strength gypsum-based fiber board prepared by the present invention has good flexural strength and temperature change resistance.
From the comparison of experimental data of examples 1,2 and 3 and comparative examples 1 and 2, the examples 1,2 and 3 have low bending strength and poor temperature resistance, which shows that the modified nano porous composite filler is modified by only one section of modified liquid, vinyl dimethyl silane in the first section of modified liquid undergoes polymerization growth on the surface of the nano porous composite filler through hydrosilylation reaction, and polysilane branched chains are formed on the surface, but are hydrophobic and cannot be uniformly dispersed in gypsum slurry, so that the bending strength and the temperature resistance are reduced, the two sections of modified liquid react the edge of the polysilane branched chains on the surface with allyl trimethoxysilane, silicon hydroxyl groups can be hydrolyzed in the subsequent process, hydrophilic and form silicon-oxygen connection with other components of the gypsum slurry, and the middle polysilane chain has good flexibility and high temperature resistance, and plays a role in buffering when the volume change is caused by temperature change, so that the bending strength and the temperature resistance are improved; from comparison of experimental data of examples 1,2 and 3 and comparative example 3, the examples 1,2 and 3 have low bending strength and poor temperature resistance, and the fact that after oxidation and amination are carried out on bamboo carbon fibers, the surfaces of the aminated bamboo carbon fibers have more amino groups and imino groups, the bamboo carbon fibers are not agglomerated, are uniformly dispersed in the whole, the amino groups and the imino groups are easy to form covalent bonds with metal ions, and a complex reaction occurs, so that the dissolution rate of calcium in gypsum slurry is improved, the compactness is improved, and the supersaturation degree of calcium hydroxide generated by the gypsum slurry is improved due to the formation of complex, so that hydration of gypsum is effectively prevented from generating a loose crystalline phase structure, the compactness is further improved, and the bending strength and the temperature resistance are improved; from comparison of experimental data of examples 1,2 and 3 and comparative example 4, it can be found that the bending strength of examples 1,2 and 3 compared with comparative example 4 is low, which means that the release agent synthesized by polyethylene glycol and 1, 3-diethoxy-1, 3-tetramethyl disiloxane is used, compared with silicone oil, after demolding, the silicone oil remained on the surface is hydrophobic to affect drying, and polyethylene glycol chain segments in the release agent can pass water molecules to facilitate drying, and then the polyethylene glycol chain segments are cracked into small molecular gas at high temperature of the release agent, and the generated chain segments can be connected on the surface of gypsum board to form silica so as to play a role in repairing surface gaps and defects, thereby improving the bending strength.
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. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (3)
1. The preparation method of the high-strength gypsum-based fiber board is characterized by comprising the following preparation steps of:
(1) Uniformly mixing nano porous filler, triethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:1 (6-8), adding ammonia water with the mass fraction of 15-20% and the mass of 6-8 times of the nano porous filler, stirring for 30-40 min at the temperature of 10-30 ℃ and the speed of 200-300 r/min, centrifugally separating, washing for 3-5 times by using the absolute ethyl alcohol, and drying for 4-6 h at the temperature of 60-70 ℃ to obtain pretreated porous filler; uniformly mixing the pretreated porous filler and a section of modified liquid according to the mass ratio of 1 (7-8), stirring at 70-80 ℃ for reaction for 4-6 hours at 500-800 r/min, centrifugally separating, washing with absolute ethyl alcohol for 3-5 times, drying at 60-70 ℃ for 4-6 hours, placing in a second section of modified liquid with the mass 7-8 times of the pretreated porous filler in a nitrogen atmosphere, and drying at 60-70 ℃ for 4-6 hours to obtain the modified nano porous filler;
(2) Immersing bamboo charcoal fiber in nitric acid with the mass fraction of 60-68%, and at 70-80 ℃,
Stirring for reacting for 40-50 min at 300-500 r/min, filtering, washing with pure water and absolute ethyl alcohol for 3-5 times, and drying at 60-70 ℃ for 3-4 h to obtain oxidized bamboo charcoal fibers; uniformly mixing oxidized bamboo charcoal fiber, ethylenediamine and pure water according to the mass ratio of 1:1 (15-20), stirring at 60-70 ℃ for reaction for 2-3 hours at 300-500 r/min, filtering, washing pure water and absolute ethyl alcohol for 3-5 times respectively, and drying at 60-70 ℃ for 3-4 hours to obtain aminated bamboo charcoal fiber;
(3) Uniformly mixing the alpha-hemihydrate gypsum with 200-300 meshes, talcum powder with 300-400 meshes, modified nano porous filler and aminated bamboo charcoal fiber according to the mass ratio of (5-6) to (1) (3-4) to (1), and stirring at the temperature of 10-30 ℃ for 2-3 min at the speed of 200-300 r/min to obtain gypsum mixed powder; pouring mixed liquid with the mass of 0.50-0.55 times of that of the gypsum mixed powder into the gypsum mixed powder, adding n-butyl alcohol with the mass of 0.0005-0.0006 times of that of the gypsum mixed powder and potassium sulfate with the mass of 0.02-0.03 times of that of the gypsum mixed powder, and stirring for 40-60 s at the temperature of 10-30 ℃ at the speed of 300-500 r/min to prepare gypsum slurry;
(4) Brushing a spacer agent with the thickness of 0.1-0.2 mm on the inner cavity of the plate-shaped mould, pouring gypsum slurry into the plate-shaped mould within 10-15 s, using a vibrating rod with the power of 800W to assist in exhausting for 2-3 min, naturally drying in air for 20-30 min, demoulding, drying at room temperature for 40-48 h, placing in a muffle furnace for step roasting, uniformly cooling to 10-20 ℃ at the cooling rate of 30-40 ℃/h, and taking out to obtain the high-strength gypsum-based fiber board;
The preparation method of the nano porous filler in the step (1) comprises the following steps: stirring 2mol/L ammonium bicarbonate solution at the temperature of 10-20 ℃ at the speed of 300-500 r/min, keeping stirring, dripping 0.1mol/L aluminum ammonium sulfate solution at the speed of 0.1-0.2 g/s, dripping 0.1mol/L tetraethoxysilane solution at the speed of 0.1-0.2 g/s, keeping the pH value at 9-10 by 15-20% of ammonia water in the dripping process, continuing stirring for 50-60 min after the dripping is finished, standing for 3-5 h, filtering, washing with pure water and absolute ethyl alcohol for 3-5 times respectively, drying at the temperature of 100-110 ℃ for 2-3 h, putting into a muffle furnace, heating to 1100-1200 ℃ at the heating rate of 60-70 ℃ for calcining for 14-18 h, cooling to room temperature, and taking out to prepare the product; the solvent of the ammonium bicarbonate and aluminum ammonium sulfate solution is water; the solvent of the ethyl orthosilicate solution is ethanol;
The first-stage modified liquid in the step (1) is prepared by uniformly mixing vinyl dimethyl silane, normal hexane and chloroplatinic acid according to the mass ratio of 1 (6-8) (0.006-0.008); the second-stage modification liquid is prepared by uniformly mixing allyl trimethoxy silane, n-hexane and chloroplatinic acid according to the mass ratio of 1 (6-8) (0.006-0.008) in a nitrogen atmosphere;
The preparation method of the bamboo charcoal fiber in the step (2) comprises the following steps: soaking moso bamboo fibers in 30-40% urea aqueous solution for 2-3 h, taking out, sequentially standing at 90-110 ℃ for 20-30 min in a nitrogen atmosphere, standing at 300-400 ℃ for 40-50 min, standing at 1000-1200 ℃ for 20-30 min, and cooling to room temperature to prepare the bamboo fiber; the moso bamboo fibers are in a fiber bundle form, the linear density is 30-40 dtex, and the fiber length is 80-120 mm;
the mixed solution in the step (3) is prepared by uniformly mixing pure water and silica sol BJN-515 according to the mass ratio of 1 (0.3-0.35);
The preparation method of the release agent in the step (4) comprises the following steps: uniformly mixing polyethylene glycol PEG400 and 1, 3-diethoxy-1, 3-tetramethyl disiloxane according to the mass ratio of 1 (0.5-0.6), adding p-toluenesulfonic acid with the mass of 0.004-0.006 times that of the ethylene glycol PEG400, stirring and reacting for 20-30 min at the temperature of 300-500 r/min at the temperature of 80-90 ℃ in nitrogen atmosphere, heating to 140-160 ℃ and continuously stirring and reacting for 6-8 h, cooling to the room temperature, and standing for 30-40 min at the temperature of 50-60 ℃ at the pressure of 1-2 kPa.
2. The method for preparing a high strength gypsum-based fiber board of claim 1, wherein the step firing in step (4) comprises the following process parameters: sequentially roasting for 1h at 50-60 ℃, 2h at 100-120 ℃, 2h at 200-220 ℃, 2h at 300-320 ℃ and the heating rate in the roasting process is 80-100 ℃/h.
3. A high strength gypsum-based fiber board prepared by the method of preparing a high strength gypsum-based fiber board according to claim 1 or 2.
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