CN116135813A - Flame-retardant modified polyphenyl particle light plastering gypsum and preparation method thereof - Google Patents
Flame-retardant modified polyphenyl particle light plastering gypsum and preparation method thereof Download PDFInfo
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- CN116135813A CN116135813A CN202310143780.4A CN202310143780A CN116135813A CN 116135813 A CN116135813 A CN 116135813A CN 202310143780 A CN202310143780 A CN 202310143780A CN 116135813 A CN116135813 A CN 116135813A
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- retardant
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- 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 title claims abstract description 53
- 239000003063 flame retardant Substances 0.000 title claims abstract description 53
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 50
- 239000010440 gypsum Substances 0.000 title claims abstract description 50
- 229920006389 polyphenyl polymer Polymers 0.000 title claims abstract description 31
- 239000002245 particle Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000000178 monomer Substances 0.000 claims description 37
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 18
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- 239000004593 Epoxy Substances 0.000 claims description 10
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 10
- 239000000920 calcium hydroxide Substances 0.000 claims description 10
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 10
- 229910021487 silica fume Inorganic materials 0.000 claims description 10
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 10
- FGZFESWHQXSPJU-UHFFFAOYSA-N 2-methyl-2-(3,3,3-trifluoropropyl)-1,3,5,2,4,6-trioxatrisilinane Chemical compound FC(F)(F)CC[Si]1(C)O[SiH2]O[SiH2]O1 FGZFESWHQXSPJU-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 8
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 8
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 8
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 8
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 7
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 7
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 7
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004078 waterproofing Methods 0.000 claims description 6
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical group COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- DWSWCPPGLRSPIT-UHFFFAOYSA-N benzo[c][2,1]benzoxaphosphinin-6-ium 6-oxide Chemical compound C1=CC=C2[P+](=O)OC3=CC=CC=C3C2=C1 DWSWCPPGLRSPIT-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 239000011159 matrix material Substances 0.000 abstract description 7
- -1 modified acrylic ester Chemical class 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 239000004566 building material Substances 0.000 abstract description 3
- 239000000839 emulsion Substances 0.000 abstract description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052731 fluorine Inorganic materials 0.000 abstract description 2
- 239000011737 fluorine Substances 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 238000002390 rotary evaporation Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000007792 addition Methods 0.000 description 6
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- DRRZZMBHJXLZRS-UHFFFAOYSA-N n-[3-[dimethoxy(methyl)silyl]propyl]cyclohexanamine Chemical compound CO[Si](C)(OC)CCCNC1CCCCC1 DRRZZMBHJXLZRS-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Chemical group CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 2
- ZXWHANCSQZVZCM-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;methanol Chemical compound OC.OC(=O)CC(O)(C(O)=O)CC(O)=O ZXWHANCSQZVZCM-UHFFFAOYSA-N 0.000 description 2
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011325 microbead Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- VDRSDNINOSAWIV-UHFFFAOYSA-N [F].[Si] Chemical group [F].[Si] VDRSDNINOSAWIV-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000011426 gypsum mortar Substances 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000009736 wetting 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
- C04B28/14—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
- C04B28/142—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 containing synthetic or waste calcium sulfate cements
- C04B28/144—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 containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being a flue gas desulfurization product
-
- 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
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00482—Coating or impregnation materials
- C04B2111/00508—Cement paints
-
- 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
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to flame-retardant modified polyphenyl particle light plastering gypsum and a preparation method thereof, belonging to the technical field of building materials, and comprising the following raw materials in parts by weight: 60-70 parts of gypsum, 6-7 parts of filler, 6-7 parts of vitrified micro bubbles, 1-1.2 parts of water reducer, 10-12 parts of waterproof agent and 7-10 parts of polyphenyl particles, and the waterproof agent is prepared and used for improving the water resistance of products; the interface binding fastness of the aggregate and the gypsum matrix can be improved, the gap between the aggregate and the gypsum matrix is filled, and the bonding force is enhanced as an interface treating agent, so that the strength of the formed material is improved. More prominently, the waterproof agent belongs to modified acrylic ester emulsion waterproof agents, belongs to high polymer materials with the advantages of acrylic ester, organic silicon and organic fluorine materials, and improves the applicability of the waterproof agent.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to flame-retardant modified polyphenyl particle light plastering gypsum and a preparation method thereof.
Background
The plastering gypsum is a plastering material for building inner walls and ceilings, which is prepared by taking gypsum as a main cementing material and adding sand stone, admixture, special composite additive and the like. As a novel wall plastering, the defects that the traditional plastering material is large in shrinkage, cracking, hollowing and the like and difficult to avoid are overcome, and the novel wall plastering has good workability, fluidity, water retention performance, heat preservation, heat insulation and sound insulation performance and proper fireproof performance, can be bonded with any base material, and is not limited by thickness.
The polyphenyl particles are light aggregate for preparing heat-insulating mortar, have good heat-insulating performance and low production cost, are commonly used as raw materials of plastering gypsum mortar, but have the problem of poor fire resistance, and the existing mortar also has the problems of low strength and poor water resistance, and the wall body starts to be pulverized and fall off from a plastering gypsum layer after being used for a period of time, so that similar problems are more likely to occur particularly under the condition of being wetted.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides flame-retardant modified polyphenyl particle light plastering gypsum and a preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
the flame-retardant modified polyphenyl particle light plastering gypsum comprises the following raw materials in parts by weight:
60-70 parts of desulfurized gypsum, 6-7 parts of filler, 6-7 parts of vitrified microbead, 1-1.2 parts of water reducer, 10-12 parts of waterproofing agent and 7-10 parts of polyphenyl granule,
the waterproof agent is prepared through the following steps:
adding a flame-retardant monomer into toluene under the protection of nitrogen, stirring and dispersing, heating to 50 ℃, adding a Karster catalyst, stirring for 50min, adding triethoxysilane, heating to 70 ℃, reacting for 48h, cooling and filtering after the reaction is finished, removing a solvent by rotary evaporation, and washing with ethanol to obtain a flame-retardant component; the flame-retardant monomer and triethoxysilane generate hydrosilylation under the catalysis of a Kanst catalyst to obtain a flame-retardant component;
setting the temperature at 80 ℃, adding 30% of mixed monomers, hexadecyl trimethyl ammonium bromide and nonylphenol polyoxyethylene ether into water under the protection of nitrogen, adding potassium persulfate, stirring for 30min, adding trifluoropropyl methyl cyclotrisiloxane, flame retardant components and the rest mixed monomers, keeping the temperature unchanged after the addition, continuously stirring and reacting for 4h, and regulating the pH value to 7 by using ammonia water after the reaction is finished to obtain the waterproof agent.
Further, the amount ratio of the flame retardant monomer, toluene, a Kanst catalyst and triethoxysilane was 4.5g:100mL:0.2mL:2.5g.
Further, in the second step, the dosage ratio of the mixed monomer, the cetyl trimethyl ammonium bromide, the polyoxyethylene nonylphenol ether, the water and the potassium persulfate is 80g:1g:0.5g:200mL:0.2g; the mass ratio of the mixed monomer to the trifluoropropyl methyl cyclotrisiloxane to the flame retardant component is 70:20:6-8.
Further, the mixed monomers are methyl methacrylate, butyl acrylate and vinyl trimethoxy silane according to the mass ratio of 5:2:1, and mixing. The waterproof agent belongs to modified acrylic emulsion;
further, the flame retardant monomer is prepared by the steps of:
under the ice water bath condition, DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) is added into dichloromethane, carbon tetrachloride is added into the dichloromethane for stirring and dispersing, triethylamine and hydroxyethyl acrylate are added into the dichloromethane, the temperature is raised to 20 ℃ after the addition, the stirring reaction is carried out for 12 hours, and after the reaction is finished, the solvent is removed by rotary evaporation after washing and drying, thus obtaining the flame-retardant monomer. P-H in DOPO reacts with-OH in hydroxyethyl acrylate, and terminal double bond is introduced into DOPO to obtain the flame-retardant monomer.
Further, the dosage ratio of DOPO to dichloromethane was 2.5g:10mL; the molar ratio of DOPO, carbon tetrachloride, triethylamine and hydroxyethyl acrylate is 1:1.2:1.2:1.2.
further, the filler comprises silica fume and calcium hydroxide, and the mass ratio of the silica fume to the calcium hydroxide is 1:1.
further, the water reducer is prepared by the following steps:
mixing hydroxyethyl cellulose and water, adding a sodium hydroxide aqueous solution to adjust the pH value to 9, adding an organosilicon epoxy quaternary ammonium salt to set the temperature to 55 ℃, stirring and reacting for 3 hours, centrifuging after the reaction is finished, neutralizing with a citric acid methanol solution, and drying to constant weight at 40 ℃ to obtain the water reducer. The water reducer is a cationic high molecular water reducer which is prepared by taking hydroxyethyl cellulose as a matrix and organic silicon epoxy quaternary ammonium salt as a cationization monomer and reacting, has good high and low temperature resistance and water resistance, has surface covering and encapsulating effects on dispersed fillers and aggregates, plays a role in wetting, reduces water consumption, and meanwhile, hydroxyl and ether bonds in the structure of the water reducer can be strongly adsorbed on the surfaces of the fillers or aggregates, reduces aggregation, sedimentation and other phenomena, and can play a role in diluting slurry.
Further, the dosage ratio of hydroxyethyl cellulose, water and organosilicon epoxy quaternary ammonium salt is 1g:20mL:0.3g.
The organosilicon epoxy quaternary ammonium salt is prepared by the following steps:
under the protection of nitrogen, mixing N, N-diethyl amine propyl methyl dimethoxy silane and absolute methanol, heating to 55 ℃, adding epoxy chloropropane, stirring for reaction for 6 hours, removing the methanol by rotary evaporation after the reaction is finished, washing with absolute ethyl ether, and drying in vacuum after the washing is finished to obtain the organosilicon epoxy quaternary ammonium salt. Wherein, the dosage ratio of the N, N-diethyl amine propyl methyl dimethoxy silane to the anhydrous methanol is 1:20mL; the dosage mole ratio of the N, N-diethyl amine propyl methyl dimethoxy silane to the epichlorohydrin is 1:1.2.
further, the gypsum is desulfurized gypsum which is obtained after calcining for 2 hours at 180 ℃ and then aging for 7 days under natural conditions.
A preparation method of flame-retardant modified polyphenyl particle light plastering gypsum comprises the following steps: the raw materials are mixed according to the weight parts to obtain the flame-retardant modified polyphenyl granule light plastering gypsum.
The invention has the beneficial effects that:
in order to solve the problems in the background technology, the invention prepares a waterproof agent for improving the water resistance of the product; in addition, the polystyrene particles and the vitrified microbeads are used as the light aggregate and the interface clearance of the gypsum matrix in the preparation process is larger, the waterproof agent added in the invention can improve the interface binding fastness of the aggregate and the gypsum matrix, fill the gap between the aggregate and the gypsum matrix and serve as an interface treating agent to enhance the binding force, thereby improving the strength of the formed material. More prominently, the waterproof agent in the invention belongs to modified acrylic ester emulsion waterproof agents, belongs to high polymer materials with the advantages of acrylic ester, organic silicon and organic fluorine materials, adjusts the source of raw materials in the preparation process, adds trifluoropropyl methyl cyclotrisiloxane and flame retardant components into the raw materials, and introduces-Si-O-chain segments on the chains of the polymer; meanwhile, the flame retardant component is introduced on the basis of introducing the fluorine silicon group, so that the applicability of the waterproof agent is improved.
In addition, the polyphenyl particles and the vitrified micro bubbles are all lightweight aggregates for preparing the lightweight plastering gypsum, wherein the polyphenyl particles have good heat insulation performance but poor fire resistance, and the vitrified micro bubbles have good fire resistance but poor heat insulation performance, and are compounded in the invention for improving the performance.
The water reducer is a cationic high-molecular water reducer which is prepared by taking hydroxyethyl cellulose as a matrix and organic silicon epoxy quaternary ammonium salt as a cationization monomer through reaction, has good high and low temperature resistance and water resistance, and meanwhile, the part of the hydroxyethyl cellulose in the water reducer has a promotion effect on toughening of materials, so that the flexural strength can be improved to a certain extent.
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
And (3) preparing a water reducing agent:
under the protection of nitrogen, mixing N, N-diethyl amine propyl methyl dimethoxy silane and absolute methanol, heating to 55 ℃, adding epoxy chloropropane, stirring for reaction for 6 hours, removing the methanol by rotary evaporation after the reaction is finished, washing with absolute ethyl ether, and drying in vacuum after the washing is finished to obtain the organosilicon epoxy quaternary ammonium salt. Wherein, the dosage ratio of the N, N-diethyl amine propyl methyl dimethoxy silane to the anhydrous methanol is 1:20mL; the dosage mole ratio of the N, N-diethyl amine propyl methyl dimethoxy silane to the epichlorohydrin is 1:1.2;
mixing hydroxyethyl cellulose and water, adding a sodium hydroxide aqueous solution to adjust the pH value to 9, adding an organosilicon epoxy quaternary ammonium salt to set the temperature to 55 ℃, stirring and reacting for 3 hours, centrifuging after the reaction is finished, neutralizing with a citric acid methanol solution, and drying to constant weight at 40 ℃ to obtain the water reducer; the dosage ratio of the hydroxyethyl cellulose, the water and the organosilicon epoxy quaternary ammonium salt is 1g:20mL:0.3g.
Example 2
Preparing a flame retardant monomer:
under the ice water bath condition, DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) is added into dichloromethane, carbon tetrachloride is added into the dichloromethane for stirring and dispersing, triethylamine and hydroxyethyl acrylate are added into the dichloromethane, the temperature is raised to 20 ℃ after the addition, the stirring reaction is carried out for 12 hours, and after the reaction is finished, the solvent is removed by rotary evaporation after washing and drying, thus obtaining the flame-retardant monomer. Wherein, the dosage ratio of DOPO and dichloromethane is 2.5g:10mL; the molar ratio of DOPO, carbon tetrachloride, triethylamine and hydroxyethyl acrylate is 1:1.2:1.2:1.2.
example 3
Preparing a waterproof agent:
adding the flame-retardant monomer prepared in the embodiment 2 into toluene under the protection of nitrogen, stirring and dispersing, heating to 50 ℃, adding a Karster catalyst, stirring for 50min, adding triethoxysilane, heating to 70 ℃, reacting for 48h, cooling and filtering after the reaction is finished, removing a solvent by rotary evaporation, and washing with ethanol to obtain a flame-retardant component; wherein the dosage ratio of the flame retardant monomer, toluene, the Kanst catalyst and the triethoxysilane is 4.5g:100mL:0.2mL:2.5g.
Setting the temperature at 80 ℃, adding 30% of mixed monomers, hexadecyl trimethyl ammonium bromide and nonylphenol polyoxyethylene ether into water under the protection of nitrogen, adding potassium persulfate, stirring for 30min, adding trifluoropropyl methyl cyclotrisiloxane, flame retardant components and the rest mixed monomers, keeping the temperature unchanged after the addition, continuously stirring and reacting for 4h, and regulating the pH value to 7 by using ammonia water after the reaction is finished to obtain the waterproof agent. Wherein, the dosage ratio of the mixed monomer, the cetyl trimethyl ammonium bromide, the nonylphenol polyoxyethylene ether, the water and the potassium persulfate is 80g:1g:0.5g:200mL:0.2g; the mass ratio of the mixed monomer to the trifluoropropyl methyl cyclotrisiloxane to the flame retardant component is 70:20:6. the mixed monomer is methyl methacrylate, butyl acrylate and vinyl trimethoxy silane according to the mass ratio of 5:2:1, and mixing.
Example 4
Preparing a waterproof agent:
adding the flame-retardant monomer prepared in the embodiment 2 into toluene under the protection of nitrogen, stirring and dispersing, heating to 50 ℃, adding a Karster catalyst, stirring for 50min, adding triethoxysilane, heating to 70 ℃, reacting for 48h, cooling and filtering after the reaction is finished, removing a solvent by rotary evaporation, and washing with ethanol to obtain a flame-retardant component; wherein the dosage ratio of the flame retardant monomer, toluene, the Kanst catalyst and the triethoxysilane is 4.5g:100mL:0.2mL:2.5g.
Setting the temperature at 80 ℃, adding 30% of mixed monomers, hexadecyl trimethyl ammonium bromide and nonylphenol polyoxyethylene ether into water under the protection of nitrogen, adding potassium persulfate, stirring for 30min, adding trifluoropropyl methyl cyclotrisiloxane, flame retardant components and the rest mixed monomers, keeping the temperature unchanged after the addition, continuously stirring and reacting for 4h, and regulating the pH value to 7 by using ammonia water after the reaction is finished to obtain the waterproof agent. Wherein, the dosage ratio of the mixed monomer, the cetyl trimethyl ammonium bromide, the nonylphenol polyoxyethylene ether, the water and the potassium persulfate is 80g:1g:0.5g:200mL:0.2g; the mass ratio of the mixed monomer to the trifluoropropyl methyl cyclotrisiloxane to the flame retardant component is 35:10:4. the mixed monomer is methyl methacrylate, butyl acrylate and vinyl trimethoxy silane according to the mass ratio of 5:2:1, and mixing.
Comparative example 1
Compared with example 4, the flame retardant component is not added in the preparation process of the waterproof agent, and the rest raw materials and the preparation process remain the same as those of example 4.
Example 5
A preparation method of flame-retardant modified polyphenyl particle light plastering gypsum comprises the following steps: 60 parts of desulfurized gypsum, 6 parts of filler, 6 parts of vitrified micro bubbles, 1 part of water reducer prepared in example 1, 10 parts of waterproofing agent prepared in example 3 and 7 parts of polyphenyl particles are mixed according to parts by weight, so that the flame-retardant modified polyphenyl particle light plastering gypsum is obtained.
The filler comprises silica fume and calcium hydroxide, and the mass ratio of the silica fume to the calcium hydroxide is 1:1, a step of; the gypsum is desulfurized gypsum, calcined for 2 hours at 180 ℃, and then aged for 7 days under natural conditions to obtain the gypsum.
Example 6
A preparation method of flame-retardant modified polyphenyl particle light plastering gypsum comprises the following steps: 65 parts of desulfurized gypsum, 6.5 parts of filler, 6.5 parts of vitrified micro bubbles, 1 part of water reducer prepared in example 1, 10-12 parts of waterproofing agent prepared in example 4 and 7-10 parts of polyphenyl particles are mixed according to parts by weight, so as to obtain the flame-retardant modified polyphenyl particle light plastering gypsum.
The filler comprises silica fume and calcium hydroxide, and the mass ratio of the silica fume to the calcium hydroxide is 1:1, a step of; the gypsum is desulfurized gypsum, calcined for 2 hours at 180 ℃, and then aged for 7 days under natural conditions to obtain the gypsum.
Example 7
A preparation method of flame-retardant modified polyphenyl particle light plastering gypsum comprises the following steps: 70 parts of desulfurized gypsum, 7 parts of filler, 7 parts of vitrified micro bubbles, 1.2 parts of water reducer prepared in example 1, 12 parts of waterproofing agent prepared in example 4 and 10 parts of polyphenyl particles are mixed according to parts by weight, so that the flame-retardant modified polyphenyl particle light plastering gypsum is obtained.
The filler comprises silica fume and calcium hydroxide, and the mass ratio of the silica fume to the calcium hydroxide is 1:1, a step of; the gypsum is desulfurized gypsum, calcined for 2 hours at 180 ℃, and then aged for 7 days under natural conditions to obtain the gypsum.
Comparative example 2
In comparison with example 6, the waterproofing agent was changed to the sample prepared in comparative example 1, and the remaining raw materials and the preparation process were kept the same as in example 6.
Comparative example 3
The water reducer was replaced with a commercially available basf water reducer f10 as compared with example 6, and the other raw materials and the preparation process were the same as those of example 6.
Samples prepared in examples 5-7 and comparative examples 2-3 were tested according to 1:0.3, mixing water, and testing performance; testing the strength in a wet state, curing the test piece under the standard condition for 7 days, curing the test piece in a constant temperature and constant humidity curing box with the temperature of (20+/-5) ℃ and the air humidity of (85+/-5)% for 7 days, taking out the test piece, and testing the flexural strength according to GB/T28627 within 30 minutes; the fireproof performance test is carried out according to the standard GB/T5464-2010 'method for testing incombustibility of building materials'; the test results are shown in table 1 below:
TABLE 1
| Example 5 | Example 6 | Example 7 | Comparative example 2 | Comparative example 3 | |
| Flexural Strength/MPa | 4.06 | 4.10 | 4.08 | 3.97 | 3.75 |
| Flexural Strength/MPa | 3.21 | 3.24 | 3.25 | 3.12 | 2.87 |
| Fire rating | A1 | A1 | A1 | A2 | A1 |
The test result shows that the product prepared by the invention has good strength performance, excellent water resistance and good fire resistance under the condition of high air humidity.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (7)
1. The flame-retardant modified polyphenyl particle light plastering gypsum is characterized by comprising the following raw materials in parts by weight: 60-70 parts of gypsum, 6-7 parts of filler, 6-7 parts of vitrified micro bubbles, 1-1.2 parts of water reducer, 10-12 parts of waterproofing agent and 7-10 parts of polyphenyl particles,
the waterproof agent is prepared through the following steps:
adding a flame-retardant monomer into toluene under the protection of nitrogen, stirring and dispersing, heating to 50 ℃, adding a Karster catalyst, stirring for 50min, adding triethoxysilane, heating to 70 ℃, and reacting for 48h to obtain a flame-retardant component;
setting the temperature at 80 ℃, adding 30% of mixed monomers, hexadecyl trimethyl ammonium bromide and nonylphenol polyoxyethylene ether into water under the protection of nitrogen, then adding potassium persulfate, stirring for 30min, then adding trifluoropropyl methyl cyclotrisiloxane, flame retardant components and the rest mixed monomers, keeping the temperature unchanged after the addition, continuing stirring and reacting for 4h, and adjusting the pH value to 7 to obtain the waterproof agent; the mixed monomer is methyl methacrylate, butyl acrylate and vinyl trimethoxy silane according to the mass ratio of 5:2:1, and mixing.
2. The flame-retardant modified polyphenyl particle light plastering gypsum according to claim 1, wherein the dosage ratio of the mixed monomer, the cetyltrimethylammonium bromide, the nonylphenol polyoxyethylene ether, the water and the potassium persulfate in the second step is 80g:1g:0.5g:200mL:0.2g; the mass ratio of the mixed monomer to the trifluoropropyl methyl cyclotrisiloxane to the flame retardant component is 70:20:6-8.
3. The flame retardant modified polyphenyl granule light plastering gypsum according to claim 1, wherein the flame retardant monomer is prepared by the following steps:
under the ice water bath condition, DOPO is added into dichloromethane, then carbon tetrachloride is added into the dichloromethane for stirring and dispersing, triethylamine and hydroxyethyl acrylate are added into the dichloromethane, the temperature is raised to 20 ℃ after the addition, and the reaction is carried out for 12 hours under stirring, so that the flame-retardant monomer is obtained.
4. The flame-retardant modified polyphenyl particle light plastering gypsum according to claim 1, wherein the filler comprises silica fume and calcium hydroxide, and the mass ratio of the silica fume to the calcium hydroxide is 1:1.
5. the flame retardant modified polyphenyl granule light plastering gypsum according to claim 1, wherein the water reducing agent is prepared by the following steps:
and mixing hydroxyethyl cellulose with water, adding a sodium hydroxide aqueous solution to adjust the pH value to 9, adding an organosilicon epoxy quaternary ammonium salt, setting the temperature to 55 ℃, and stirring and reacting for 3 hours to obtain the water reducer.
6. The flame-retardant modified polyphenyl granule light plastering gypsum according to claim 1, wherein the gypsum is obtained by calcining desulfurized gypsum at 180 ℃ for 2 hours and then aging for 7 days under natural conditions.
7. The method for preparing the flame-retardant modified polyphenyl granule light plastering gypsum according to claim 1, which is characterized by comprising the following steps: the raw materials are mixed according to the weight parts to obtain the flame-retardant modified polyphenyl granule light plastering gypsum.
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