CN116178870A - Heat-insulating waterproof composite material and preparation process thereof - Google Patents
Heat-insulating waterproof composite material and preparation process thereof Download PDFInfo
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- CN116178870A CN116178870A CN202211686771.1A CN202211686771A CN116178870A CN 116178870 A CN116178870 A CN 116178870A CN 202211686771 A CN202211686771 A CN 202211686771A CN 116178870 A CN116178870 A CN 116178870A
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- waterproof composite
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- 239000002131 composite material Substances 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 82
- 239000000839 emulsion Substances 0.000 claims abstract description 51
- 239000004005 microsphere Substances 0.000 claims abstract description 48
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 41
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 31
- 239000000945 filler Substances 0.000 claims abstract description 26
- 238000009833 condensation Methods 0.000 claims abstract description 9
- 230000005494 condensation Effects 0.000 claims abstract description 9
- 239000004793 Polystyrene Substances 0.000 claims abstract description 7
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000002091 cationic group Chemical group 0.000 claims abstract description 7
- 229920002223 polystyrene Polymers 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 60
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 49
- 238000003756 stirring Methods 0.000 claims description 40
- 238000002156 mixing Methods 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 26
- 239000000047 product Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 22
- 239000002270 dispersing agent Substances 0.000 claims description 20
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 15
- 239000003995 emulsifying agent Substances 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 15
- 238000004448 titration Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 13
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 11
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 11
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 11
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 11
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 11
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 10
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical group CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 5
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 239000001099 ammonium carbonate Substances 0.000 claims description 5
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical group [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 5
- 239000000347 magnesium hydroxide Substances 0.000 claims description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000011067 sorbitan monolaureate Nutrition 0.000 claims description 5
- 229950004959 sorbitan oleate Drugs 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000004321 preservation Methods 0.000 abstract description 5
- 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 abstract description 2
- 239000003063 flame retardant Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 13
- 238000000034 method Methods 0.000 description 8
- 238000009413 insulation Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012745 toughening agent Substances 0.000 description 2
- 229910003849 O-Si Inorganic materials 0.000 description 1
- 229910003872 O—Si Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000015784 hyperosmotic salinity response Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2439/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
- C08J2439/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
- C08J2439/06—Homopolymers or copolymers of N-vinyl-pyrrolidones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/19—Quaternary ammonium compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to the technical field of heat-insulating waterproof composite materials and provides a heat-insulating waterproof composite material and a preparation process thereof, wherein cationic polystyrene microspheres are used as templates, titanium dioxide particles formed by tetrabutyl titanate hydrolytic condensation are adsorbed on the surfaces of the microspheres for condensation, so that hollow titanium dioxide microspheres with hollow structures can be formed, and the hollow structures of the hollow titanium dioxide microspheres can play a good role in heat preservation, so that the hollow titanium dioxide microspheres are compounded with modified polyacrylate emulsion and the heat preservation performance of the polyacrylate emulsion can be improved; secondly, the filler component is added into the raw materials for preparing the heat-insulating waterproof composite material, so that antibacterial molecules and flame-retardant molecules in the filler component can be dispersed in molecular gaps of the heat-insulating waterproof composite material, and the heat-insulating waterproof composite material has stable antibacterial flame retardance on the basis of good waterproof heat-insulating performance.
Description
Technical Field
The invention relates to the technical field of heat-insulating waterproof composite materials, in particular to a heat-insulating waterproof composite material and a preparation process thereof.
Background
The composite material is a material with new properties, which is formed by two or more materials with different properties through a physical or chemical method. The materials complement each other in performance and generate a synergistic effect, so that the comprehensive performance of the composite material is superior to that of the original composition material, and various different requirements are met. Many composite materials with waterproof or heat insulation properties are widely applied to the building industry, such as wall coating, building heat insulation layers and the like, and many kinds of composite materials are manufactured into building heat insulation layer films for heat insulation of building walls. The composite material for preparing the heat-insulating layer film in the market at present has single performance, can simultaneously have good heat-insulating performance and waterproof performance, and can seldom exert the heat-insulating waterproof performance to the best effect in practical application even though the composite material can simultaneously have the heat-insulating waterproof performance.
The high molecular negative oxygen ion composite material disclosed in Chinese patent No. CN202111648812.3 comprises the following raw materials: the invention adds negative oxygen powder, glass powder, magnesium oxide, magnesium sulfate, stone powder, plant fiber, glass microsphere, waterproof toughening agent and functional agent, can change the plate structure, release negative oxygen ion, improve the human circulation, the invention adds glass powder and waterproof toughening agent, has good effects of heat preservation, heat insulation, waterproof, aging resistance and service life increase; the mechanical property of the stone powder can be enhanced by adding the stone powder and the functional agent; plant fiber and glass beads are added, so that the weight of the plate can be reduced, and the internal tension of the plate can be increased. However, the raw materials of the invention have a plurality of modification aids, and various modification aids cannot be connected in a stable connection mode, so that the heat insulation and waterproof performance of the prepared composite material is not stable enough, the composite material has no antibacterial property, is extremely easy to mildew in actual use, and is easy to cause material failure after mildew, so that the composite material needs to be improved.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a heat-insulating waterproof composite material and a preparation process thereof, and aims to ensure that the heat-insulating waterproof composite material prepared by the heat-insulating waterproof composite material has antibacterial and ultraviolet-resistant performances on the basis of stable heat-insulating waterproof performances.
Technical proposal
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the heat-insulating waterproof composite material comprises the following components in parts by weight: 55-60 parts of modified polyacrylate emulsion, 2-3 parts of hollow titanium dioxide microspheres, 0.2-0.3 part of polyvinylpyrrolidone, 1-2 parts of filler component and 0.1-0.2 part of dispersing agent;
the preparation method of the modified polyacrylate emulsion comprises the following steps:
1) Weighing a certain amount of composite emulsifier, itaconic acid and deionized water, stirring and mixing uniformly, heating to 50 ℃, adding a certain amount of modified calcium carbonate, then adding a certain amount of ethyl methacrylate, methyl methacrylate and ethyl acrylate with the same molar ratio, stirring for 30-40min at a constant temperature of 50 ℃ to prepare a pre-emulsion, and weighing a certain amount of potassium persulfate solution for later use;
2) Mixing 20% of the volume of the pre-emulsion and 15% of the volume of the potassium persulfate solution under the conditions of nitrogen introduction, stirring, reflux condensation, heating to 80 ℃, dropwise adding the rest pre-emulsion and the potassium persulfate solution, reacting for 3-4 hours at the constant temperature of 80 ℃ after the dropwise adding is completed, cooling to normal temperature, and dropwise adding sodium bicarbonate to adjust the pH to 7-8, thus obtaining the modified polyacrylate emulsion; wherein the mass fraction of the composite emulsifier is 1.5%, the mass fraction of itaconic acid is 2%, the mass fraction of modified calcium carbonate is 1.3%, the mass fraction of the total of ethyl methacrylate, methyl methacrylate and ethyl acrylate is 15%, and the mass fraction of potassium persulfate solution is 0.5%.
Still further, the complex emulsifier is OP-10, SDS and Span-20 according to 1:2:1 weight ratio.
Further, the preparation method of the modified calcium carbonate comprises the following steps:
step I, weighing 10-15 parts of calcium chloride, 10-12 parts of ammonium carbonate, 0.2-0.3 part of ethanolamine and 0.1-0.2 part of triethanolamine according to parts by weight, pouring the materials into a ball milling tank, and performing ball milling for 1h;
step II, filtering the product obtained in the step I, carrying out suction filtration and washing on the filtered product, then drying in a baking oven at 60 ℃ for 12 hours, and grinding and crushing to obtain calcium carbonate powder;
and III, weighing 3-aminopropyl triethoxysilane with the same weight and calcium carbonate powder in the step II, pouring the powder into a flask, adding an ethanol solution with the weight being 25-28 times of that of the powder, mixing and stirring for 7 hours, centrifugally washing the precipitate with absolute ethanol after stirring, drying the precipitate in a 100 ℃ oven for 12 hours, and grinding and crushing to obtain the modified calcium carbonate.
Further, the ethanol concentration of the ethanol solution in the step III is 95%, and the stirring speed in the step III is 500-600r/min.
Further, the preparation method of the hollow titanium dioxide microsphere comprises the following steps: firstly, adding 15-16 parts by weight of cationic polystyrene microsphere emulsion and 78-85 parts by weight of ammonia water into 100 parts by weight of absolute ethyl alcohol, uniformly mixing, transferring into a three-neck flask with a stirrer and a condenser tube, and stirring for 10min at a constant speed of 300r/min at room temperature; secondly, mixing 18-20 parts by weight of tetrabutyl titanate, 1-2 parts by weight of triethanolamine and 20 parts by weight of absolute ethyl alcohol to prepare a titration solution, dripping the titration solution into the three-neck flask by using a medical dropper, and heating to 80 ℃ for constant-temperature reaction for 8-10 hours after the dripping is finished; and (3) centrifugally washing the obtained product, drying the product in a drying oven at 70-75 ℃, and calcining the dried product at high temperature to obtain the hollow titanium dioxide microspheres.
Still further, the titration speed is 1-2 drops/s.
Still further, the filler component was dodecyltrimethylammonium chloride, dodecyldimethylbenzyl ammonium chloride, magnesium hydroxide, and aluminum hydroxide in a ratio of 3:2:1:2 by weight ratio through ball milling and mixing.
Still further, the dispersant is sorbitan oleate polyoxyethylene ether.
A preparation process of a heat-insulating waterproof composite material, which comprises the following steps:
step1, ultrasonically dispersing the hollow titanium dioxide microspheres, polyvinylpyrrolidone, a filler component and a dispersing agent in deionized water with the mass being 3-5 times of that of the hollow titanium dioxide microspheres, and marking the hollow titanium dioxide microspheres, the polyvinylpyrrolidone, the filler component and the dispersing agent as mixed components;
step2, pouring the modified polyacrylate emulsion in parts by weight into a three-neck flask, adding the mixed components in Step1, and stirring for 6 hours at a constant temperature of 80 ℃ to obtain a heat-insulating waterproof composite material base solution;
step3, pouring the basic liquid of the heat-insulating waterproof composite material in Step2 into a polytetrafluoroethylene plate to form a film at room temperature, and obtaining the film which is the heat-insulating waterproof composite material.
Further, the ultrasonic dispersion frequency in Step1 is 28-32kHz, and the ultrasonic dispersion time is 20-30min.
Advantageous effects
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the 3-aminopropyl triethoxy silane is used for modifying the calcium carbonate, so that the 3-aminopropyl triethoxy silane is connected with the calcium carbonate through Ca-O-Si bonds, the surface of the calcium carbonate contains reactive chemical bonds, and the modified calcium carbonate is added in the process of preparing the modified polyacrylate emulsion by taking ethyl methacrylate, methyl methacrylate and ethyl acrylate as raw materials, so that the modified calcium carbonate can be uniformly dispersed in a reaction solution, and the modified calcium carbonate is stably distributed in molecular gaps of the modified polyacrylate emulsion, so that the modified polyacrylate emulsion has better salt tolerance and corrosion resistance, and the mechanical property of the modified polyacrylate emulsion can be improved to a certain extent; secondly, a certain amount of itaconic acid is added into the raw materials for preparing the modified polyacrylate emulsion, so that the structure among molecular chains of the modified polyacrylate emulsion is more compact, and the tensile property and the thermal stability of the modified polyacrylate emulsion are improved.
2. According to the invention, the cationic polystyrene microsphere is used as a template, titanium dioxide particles formed by tetrabutyl titanate hydrolysis condensation are adsorbed on the surface of the titanium dioxide microsphere for condensation, so that the hollow titanium dioxide microsphere with a hollow structure can be formed, and as the hollow structure of the hollow titanium dioxide microsphere can play a good role in heat preservation, the hollow titanium dioxide microsphere is compounded with the modified polyacrylate emulsion and the heat preservation performance of the polyacrylate emulsion can be improved; secondly, the filler component is added into the raw materials for preparing the heat-insulating waterproof composite material, so that antibacterial molecules and flame-retardant molecules in the filler component can be dispersed in molecular gaps of the heat-insulating waterproof composite material, and the heat-insulating waterproof composite material has stable antibacterial flame retardance on the basis of good waterproof heat-insulating performance.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
the heat-insulating waterproof composite material comprises the following components in parts by weight: 55 parts of modified polyacrylate emulsion, 2 parts of hollow titanium dioxide microspheres, 0.2 part of polyvinylpyrrolidone, 1 part of filler component and 0.1 part of dispersing agent;
the preparation method of the modified polyacrylate emulsion comprises the following steps:
1) Weighing a certain amount of composite emulsifier, itaconic acid and deionized water, stirring and mixing uniformly, heating to 50 ℃, adding a certain amount of modified calcium carbonate, then adding a certain amount of ethyl methacrylate, methyl methacrylate and ethyl acrylate with the same molar ratio, stirring for 30min at a constant temperature of 50 ℃ to prepare a pre-emulsion, and then weighing a certain amount of potassium persulfate solution for later use;
2) Mixing 20% of the volume of the pre-emulsion and 15% of the volume of the potassium persulfate solution under the conditions of nitrogen introduction, stirring, reflux condensation, heating to 80 ℃, dropwise adding the rest of the pre-emulsion and the potassium persulfate solution, reacting for 3 hours at the constant temperature of 80 ℃ after the dropwise adding is completed, cooling to normal temperature, and dropwise adding sodium bicarbonate to adjust the pH to 7, thus obtaining the modified polyacrylate emulsion; wherein the mass fraction of the composite emulsifier is 1.5%, the mass fraction of itaconic acid is 2%, the mass fraction of modified calcium carbonate is 1.3%, the mass fraction of the total of ethyl methacrylate, methyl methacrylate and ethyl acrylate is 15%, and the mass fraction of potassium persulfate solution is 0.5%.
The composite emulsifier is OP-10, SDS and Span-20 according to the following ratio of 1:2:1 weight ratio.
The preparation method of the modified calcium carbonate comprises the following steps:
step I, weighing 10 parts of calcium chloride, 10 parts of ammonium carbonate, 0.2 part of ethanolamine and 0.1 part of triethanolamine according to parts by weight, pouring the materials into a ball milling tank, and performing ball milling for 1h;
step II, filtering the product obtained in the step I, carrying out suction filtration and washing on the filtered product, then drying in a baking oven at 60 ℃ for 12 hours, and grinding and crushing to obtain calcium carbonate powder;
and III, weighing 3-aminopropyl triethoxysilane with the same weight and calcium carbonate powder in the step II, pouring the powder into a flask, adding an ethanol solution with the weight being 25 times of that of the powder, mixing and stirring for 7 hours, centrifugally washing the precipitate with absolute ethanol after stirring, drying the obtained precipitate in a drying oven at 100 ℃ for 12 hours, and grinding and crushing to obtain the modified calcium carbonate.
The ethanol concentration of the ethanol solution in step III was 95%, and the stirring speed in step III was 500r/min.
The preparation method of the hollow titanium dioxide microsphere comprises the following steps: firstly, adding 15 parts by weight of cationic polystyrene microsphere emulsion and 78 parts by weight of ammonia water into 100 parts by weight of absolute ethyl alcohol, uniformly mixing, transferring into a three-neck flask with a stirrer and a condenser tube, and stirring at a constant speed of 300r/min for 10min at room temperature; secondly, 18 parts by weight of tetrabutyl titanate, 1 part by weight of triethanolamine and 20 parts by weight of absolute ethyl alcohol are mixed to prepare a titration solution, a medical dropper is used for dripping the titration solution into the three-neck flask, and the temperature is raised to 80 ℃ for constant-temperature reaction for 8 hours after the dripping is finished; and (3) centrifugally washing the obtained product, drying the product in a drying oven at 70 ℃, and calcining the dried product at high temperature to obtain the hollow titanium dioxide microspheres.
The titration speed was 1 drop/s.
The filler comprises dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride, magnesium hydroxide and aluminum hydroxide according to the proportion of 3:2:1:2 by weight ratio through ball milling and mixing.
The dispersing agent is sorbitan oleate polyoxyethylene ether.
A preparation process of a heat-insulating waterproof composite material comprises the following steps:
step1, ultrasonically dispersing the hollow titanium dioxide microspheres, polyvinylpyrrolidone, a filler component and a dispersing agent in deionized water with the mass being 3 times that of the hollow titanium dioxide microspheres, and marking the hollow titanium dioxide microspheres, the polyvinylpyrrolidone, the filler component and the dispersing agent as mixed components;
step2, pouring the modified polyacrylate emulsion in parts by weight into a three-neck flask, adding the mixed components in Step1, and stirring for 6 hours at a constant temperature of 80 ℃ to obtain a heat-insulating waterproof composite material base solution;
step3, pouring the basic liquid of the heat-insulating waterproof composite material in Step2 into a polytetrafluoroethylene plate to form a film at room temperature, and obtaining the film which is the heat-insulating waterproof composite material.
The ultrasonic dispersion frequency in Step1 is 28kHz, and the ultrasonic dispersion time is 20min.
Example 2:
the heat-insulating waterproof composite material comprises the following components in parts by weight: 60 parts of modified polyacrylate emulsion, 3 parts of hollow titanium dioxide microspheres, 0.3 part of polyvinylpyrrolidone, 2 parts of filler component and 0.2 part of dispersing agent;
the preparation method of the modified polyacrylate emulsion comprises the following steps:
1) Weighing a certain amount of composite emulsifier, itaconic acid and deionized water, stirring and mixing uniformly, heating to 50 ℃, adding a certain amount of modified calcium carbonate, then adding a certain amount of ethyl methacrylate, methyl methacrylate and ethyl acrylate with the same molar ratio, stirring for 40min at a constant temperature of 50 ℃ to prepare a pre-emulsion, and then weighing a certain amount of potassium persulfate solution for later use;
2) Mixing 20% of the volume of the pre-emulsion and 15% of the volume of the potassium persulfate solution under the conditions of nitrogen introduction, stirring, reflux condensation, heating to 80 ℃, dropwise adding the rest of the pre-emulsion and the potassium persulfate solution, reacting for 4 hours at the constant temperature of 80 ℃ after the dropwise adding is completed, cooling to normal temperature, and dropwise adding sodium bicarbonate to adjust the pH to 8, thus obtaining the modified polyacrylate emulsion; wherein the mass fraction of the composite emulsifier is 1.5%, the mass fraction of itaconic acid is 2%, the mass fraction of modified calcium carbonate is 1.3%, the mass fraction of the total of ethyl methacrylate, methyl methacrylate and ethyl acrylate is 15%, and the mass fraction of potassium persulfate solution is 0.5%.
The composite emulsifier is OP-10, SDS and Span-20 according to the following ratio of 1:2:1 weight ratio.
The preparation method of the modified calcium carbonate comprises the following steps:
step I, weighing 15 parts of calcium chloride, 12 parts of ammonium carbonate, 0.3 part of ethanolamine and 0.2 part of triethanolamine according to parts by weight, pouring the mixture into a ball milling tank, and performing ball milling for 1h;
step II, filtering the product obtained in the step I, carrying out suction filtration and washing on the filtered product, then drying in a baking oven at 60 ℃ for 12 hours, and grinding and crushing to obtain calcium carbonate powder;
and III, weighing 3-aminopropyl triethoxysilane with the same weight and calcium carbonate powder in the step II, pouring the powder into a flask, adding an ethanol solution with the weight being 28 times of that of the powder, mixing and stirring for 7 hours, centrifugally washing the precipitate with absolute ethanol after stirring, drying the obtained precipitate in a drying oven at 100 ℃ for 12 hours, and grinding and crushing to obtain the modified calcium carbonate.
The ethanol concentration of the ethanol solution in step III was 95%, and the stirring speed in step III was 600r/min.
The preparation method of the hollow titanium dioxide microsphere comprises the following steps: firstly, adding 16 parts by weight of cationic polystyrene microsphere emulsion and 85 parts by weight of ammonia water into 100 parts by weight of absolute ethyl alcohol, uniformly mixing, transferring into a three-neck flask with a stirrer and a condenser tube, and stirring at a constant speed of 300r/min for 10min at room temperature; secondly, mixing 20 parts by weight of tetrabutyl titanate, 2 parts by weight of triethanolamine and 20 parts by weight of absolute ethyl alcohol to prepare a titration solution, dripping the titration solution into the three-neck flask by using a medical dropper, and heating to 80 ℃ for constant-temperature reaction for 10 hours after the dripping is finished; and (3) centrifugally washing the obtained product, drying the product in an oven at 75 ℃, and calcining the dried product at high temperature to obtain the hollow titanium dioxide microspheres.
The titration speed was 2 drops/s.
The filler comprises dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride, magnesium hydroxide and aluminum hydroxide according to the proportion of 3:2:1:2 by weight ratio through ball milling and mixing.
The dispersing agent is sorbitan oleate polyoxyethylene ether.
A preparation process of a heat-insulating waterproof composite material comprises the following steps:
step1, ultrasonically dispersing the hollow titanium dioxide microspheres, polyvinylpyrrolidone, a filler component and a dispersing agent in deionized water with the mass being 5 times of that of the hollow titanium dioxide microspheres, and marking the hollow titanium dioxide microspheres, the polyvinylpyrrolidone, the filler component and the dispersing agent as mixed components;
step2, pouring the modified polyacrylate emulsion in parts by weight into a three-neck flask, adding the mixed components in Step1, and stirring for 6 hours at a constant temperature of 80 ℃ to obtain a heat-insulating waterproof composite material base solution;
step3, pouring the basic liquid of the heat-insulating waterproof composite material in Step2 into a polytetrafluoroethylene plate to form a film at room temperature, and obtaining the film which is the heat-insulating waterproof composite material.
The ultrasonic dispersion frequency in Step1 is 32kHz, and the ultrasonic dispersion time is 30min.
Example 3:
the heat-insulating waterproof composite material comprises the following components in parts by weight: 58 parts of modified polyacrylate emulsion, 2 parts of hollow titanium dioxide microspheres, 0.3 part of polyvinylpyrrolidone, 2 parts of filler component and 0.1 part of dispersing agent;
the preparation method of the modified polyacrylate emulsion comprises the following steps:
1) Weighing a certain amount of composite emulsifier, itaconic acid and deionized water, stirring and mixing uniformly, heating to 50 ℃, adding a certain amount of modified calcium carbonate, then adding a certain amount of ethyl methacrylate, methyl methacrylate and ethyl acrylate with the same molar ratio, stirring for 35min at a constant temperature of 50 ℃ to prepare a pre-emulsion, and then weighing a certain amount of potassium persulfate solution for later use;
2) Mixing 20% of the volume of the pre-emulsion and 15% of the volume of the potassium persulfate solution under the conditions of nitrogen introduction, stirring, reflux condensation, heating to 80 ℃, dropwise adding the rest of the pre-emulsion and the potassium persulfate solution, reacting for 4 hours at the constant temperature of 80 ℃ after the dropwise adding is completed, cooling to normal temperature, and dropwise adding sodium bicarbonate to adjust the pH to 7, thus obtaining the modified polyacrylate emulsion; wherein the mass fraction of the composite emulsifier is 1.5%, the mass fraction of itaconic acid is 2%, the mass fraction of modified calcium carbonate is 1.3%, the mass fraction of the total of ethyl methacrylate, methyl methacrylate and ethyl acrylate is 15%, and the mass fraction of potassium persulfate solution is 0.5%.
The composite emulsifier is OP-10, SDS and Span-20 according to the following ratio of 1:2:1 weight ratio.
The preparation method of the modified calcium carbonate comprises the following steps:
step I, 13 parts of calcium chloride, 11 parts of ammonium carbonate, 0.2 part of ethanolamine and 0.2 part of triethanolamine are weighed according to parts by weight and poured into a ball milling tank for ball milling for 1h;
step II, filtering the product obtained in the step I, carrying out suction filtration and washing on the filtered product, then drying in a baking oven at 60 ℃ for 12 hours, and grinding and crushing to obtain calcium carbonate powder;
and III, weighing 3-aminopropyl triethoxysilane with the same weight and calcium carbonate powder in the step II, pouring the powder into a flask, adding an ethanol solution with the weight being 27 times of that of the powder, mixing and stirring for 7 hours, centrifugally washing the precipitate with absolute ethanol after stirring, drying the obtained precipitate in a drying oven at 100 ℃ for 12 hours, and grinding and crushing to obtain the modified calcium carbonate.
The ethanol concentration of the ethanol solution in step III was 95%, and the stirring speed in step III was 600r/min.
The preparation method of the hollow titanium dioxide microsphere comprises the following steps: firstly, adding 16 parts by weight of cationic polystyrene microsphere emulsion and 81 parts by weight of ammonia water into 100 parts by weight of absolute ethyl alcohol, uniformly mixing, transferring into a three-neck flask with a stirrer and a condenser tube, and stirring at a constant speed of 300r/min for 10min at room temperature; secondly, mixing 19 parts by weight of tetrabutyl titanate, 2 parts by weight of triethanolamine and 20 parts by weight of absolute ethyl alcohol to prepare a titration solution, dripping the titration solution into the three-neck flask by using a medical dropper, and heating to 80 ℃ for constant-temperature reaction for 9 hours after the dripping is finished; and (3) centrifugally washing the obtained product, drying the product in a drying oven at 73 ℃, and calcining the dried product at high temperature to obtain the hollow titanium dioxide microsphere.
The titration speed was 2 drops/s.
The filler comprises dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride, magnesium hydroxide and aluminum hydroxide according to the proportion of 3:2:1:2 by weight ratio through ball milling and mixing.
The dispersing agent is sorbitan oleate polyoxyethylene ether.
A preparation process of a heat-insulating waterproof composite material comprises the following steps:
step1, ultrasonically dispersing the hollow titanium dioxide microspheres, polyvinylpyrrolidone, a filler component and a dispersing agent in deionized water with the mass being 4 times that of the hollow titanium dioxide microspheres, and marking the hollow titanium dioxide microspheres, the polyvinylpyrrolidone, the filler component and the dispersing agent as mixed components;
step2, pouring the modified polyacrylate emulsion in parts by weight into a three-neck flask, adding the mixed components in Step1, and stirring for 6 hours at a constant temperature of 80 ℃ to obtain a heat-insulating waterproof composite material base solution;
step3, pouring the basic liquid of the heat-insulating waterproof composite material in Step2 into a polytetrafluoroethylene plate to form a film at room temperature, and obtaining the film which is the heat-insulating waterproof composite material.
The ultrasonic dispersion frequency in Step1 is 30kHz, and the ultrasonic dispersion time is 25min.
Comparative example 1:
the ingredients and the preparation method of the heat-insulating waterproof composite material provided by the embodiment are approximately the same as those of the embodiment 1, and the main differences are that: the formulation of comparative example 1 does not contain hollow titanium dioxide microspheres in the formulation of example 1.
Comparative example 2:
the ingredients and the production method of the heat-insulating waterproof composite material provided by the embodiment are approximately the same as those of the embodiment 2, and the main differences are that: the formulation of comparative example 2 does not contain the filler component of the formulation of example 2.
Comparative example 3:
the heat-insulating waterproof composite material provided by the embodiment is a composite material film with heat-insulating waterproof performance which is randomly extracted in the market.
Performance detection
The heat insulating and waterproof composite materials prepared by examples 1 to 3 in the present invention were respectively designated as examples 1 to 3, the heat insulating and waterproof composite materials prepared by comparative examples 1 to 2 were designated as comparative examples 1 to 2, the composite material film in comparative example 3 was designated as comparative example 3, and then the relevant properties were examined for examples 1 to 3 and comparative examples 1 to 3, and the obtained data are recorded in the following table:
as shown by the data in the table, the heat-insulating waterproof composite material produced in the embodiments 1-3 has better heat-conducting property and ultraviolet-proof property compared with the comparative example 1, thereby showing the heat-insulating and ultraviolet-proof effects which can be achieved by adding the hollow titanium dioxide microspheres; secondly, compared with comparative example 2, the heat-insulating waterproof composite material produced in the examples 1-3 has good antibacterial effect, so that the addition of the filler component can lead the heat-insulating waterproof composite material to have better antibacterial performance; finally, the heat-insulating waterproof composite material produced in the embodiment 1-3 is superior to the film of the composite material of the comparative example 3 in all performances, so that the heat-insulating waterproof composite material prepared by the invention is better in performance and better in market popularization value.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The heat-insulating waterproof composite material is characterized by comprising the following components in parts by weight: 55-60 parts of modified polyacrylate emulsion, 2-3 parts of hollow titanium dioxide microspheres, 0.2-0.3 part of polyvinylpyrrolidone, 1-2 parts of filler component and 0.1-0.2 part of dispersing agent;
the preparation method of the modified polyacrylate emulsion comprises the following steps:
1) Weighing a certain amount of composite emulsifier, itaconic acid and deionized water, stirring and mixing uniformly, heating to 50 ℃, adding a certain amount of modified calcium carbonate, then adding a certain amount of ethyl methacrylate, methyl methacrylate and ethyl acrylate with the same molar ratio, stirring for 30-40min at a constant temperature of 50 ℃ to prepare a pre-emulsion, and weighing a certain amount of potassium persulfate solution for later use;
2) Mixing 20% of the volume of the pre-emulsion and 15% of the volume of the potassium persulfate solution under the conditions of nitrogen introduction, stirring, reflux condensation, heating to 80 ℃, dropwise adding the rest pre-emulsion and the potassium persulfate solution, reacting for 3-4 hours at the constant temperature of 80 ℃ after the dropwise adding is completed, cooling to normal temperature, and dropwise adding sodium bicarbonate to adjust the pH to 7-8, thus obtaining the modified polyacrylate emulsion; wherein the mass fraction of the composite emulsifier is 1.5%, the mass fraction of itaconic acid is 2%, the mass fraction of modified calcium carbonate is 1.3%, the mass fraction of the total of ethyl methacrylate, methyl methacrylate and ethyl acrylate is 15%, and the mass fraction of potassium persulfate solution is 0.5%.
2. The heat-insulating and water-proof composite material according to claim 1, wherein the composite emulsifier is OP-10, SDS and Span-20 according to 1:2:1 weight ratio.
3. The heat-insulating waterproof composite material according to claim 1, wherein the preparation method of the modified calcium carbonate comprises the following steps:
step I, weighing 10-15 parts of calcium chloride, 10-12 parts of ammonium carbonate, 0.2-0.3 part of ethanolamine and 0.1-0.2 part of triethanolamine according to parts by weight, pouring the materials into a ball milling tank, and performing ball milling for 1h;
step II, filtering the product obtained in the step I, carrying out suction filtration and washing on the filtered product, then drying in a baking oven at 60 ℃ for 12 hours, and grinding and crushing to obtain calcium carbonate powder;
and III, weighing 3-aminopropyl triethoxysilane with the same weight and calcium carbonate powder in the step II, pouring the powder into a flask, adding an ethanol solution with the weight being 25-28 times of that of the powder, mixing and stirring for 7 hours, centrifugally washing the precipitate with absolute ethanol after stirring, drying the precipitate in a 100 ℃ oven for 12 hours, and grinding and crushing to obtain the modified calcium carbonate.
4. A heat insulating and waterproof composite material according to claim 3, wherein the ethanol concentration of the ethanol solution in the step III is 95%, and the stirring speed in the step III is 500-600r/min.
5. The heat-insulating waterproof composite material according to claim 1, wherein the preparation method of the hollow titanium dioxide microspheres comprises the following steps: firstly, adding 15-16 parts by weight of cationic polystyrene microsphere emulsion and 78-85 parts by weight of ammonia water into 100 parts by weight of absolute ethyl alcohol, uniformly mixing, transferring into a three-neck flask with a stirrer and a condenser tube, and stirring for 10min at a constant speed of 300r/min at room temperature; secondly, mixing 18-20 parts by weight of tetrabutyl titanate, 1-2 parts by weight of triethanolamine and 20 parts by weight of absolute ethyl alcohol to prepare a titration solution, dripping the titration solution into the three-neck flask by using a medical dropper, and heating to 80 ℃ for constant-temperature reaction for 8-10 hours after the dripping is finished; and (3) centrifugally washing the obtained product, drying the product in a drying oven at 70-75 ℃, and calcining the dried product at high temperature to obtain the hollow titanium dioxide microspheres.
6. The heat insulating and water resistant composite material according to claim 5, wherein said titration speed is 1-2 drops/s.
7. The heat-insulating and waterproof composite material according to claim 1, wherein the filler component is dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride, magnesium hydroxide and aluminum hydroxide according to a weight ratio of 3:2:1:2 by weight ratio through ball milling and mixing.
8. The heat-insulating and waterproof composite material according to claim 1, wherein the dispersing agent is sorbitan oleate polyoxyethylene ether.
9. The process for preparing a heat-insulating waterproof composite material according to any one of claims 1 to 8, characterized in that it comprises the following steps:
step1, ultrasonically dispersing the hollow titanium dioxide microspheres, polyvinylpyrrolidone, a filler component and a dispersing agent in deionized water with the mass being 3-5 times of that of the hollow titanium dioxide microspheres, and marking the hollow titanium dioxide microspheres, the polyvinylpyrrolidone, the filler component and the dispersing agent as mixed components;
step2, pouring the modified polyacrylate emulsion in parts by weight into a three-neck flask, adding the mixed components in Step1, and stirring for 6 hours at a constant temperature of 80 ℃ to obtain a heat-insulating waterproof composite material base solution;
step3, pouring the basic liquid of the heat-insulating waterproof composite material in Step2 into a polytetrafluoroethylene plate to form a film at room temperature, and obtaining the film which is the heat-insulating waterproof composite material.
10. The process for preparing the heat-insulating waterproof composite material according to claim 9, wherein the ultrasonic dispersion frequency in Step1 is 28-32kHz, and the ultrasonic dispersion time is 20-30min.
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| CN104761741A (en) * | 2015-04-17 | 2015-07-08 | 陕西科技大学 | Preparation method for hollow titanium dioxide/polyacrylate composite film with insulation performance |
| CN106866992A (en) * | 2017-03-31 | 2017-06-20 | 陕西科技大学 | A kind of preparation method of the titania modified polyacrylate dispersion of hollow spheres |
| CN112225247A (en) * | 2020-10-20 | 2021-01-15 | 桂林理工大学 | Nano titanium dioxide open hollow sphere and preparation method thereof |
| CN115260858A (en) * | 2022-07-15 | 2022-11-01 | 嘉宝莉化工集团股份有限公司 | Reflective heat insulation coating, reflective heat insulation film, preparation method of reflective heat insulation film and heat insulation product |
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Patent Citations (4)
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|---|---|---|---|---|
| CN104761741A (en) * | 2015-04-17 | 2015-07-08 | 陕西科技大学 | Preparation method for hollow titanium dioxide/polyacrylate composite film with insulation performance |
| CN106866992A (en) * | 2017-03-31 | 2017-06-20 | 陕西科技大学 | A kind of preparation method of the titania modified polyacrylate dispersion of hollow spheres |
| CN112225247A (en) * | 2020-10-20 | 2021-01-15 | 桂林理工大学 | Nano titanium dioxide open hollow sphere and preparation method thereof |
| CN115260858A (en) * | 2022-07-15 | 2022-11-01 | 嘉宝莉化工集团股份有限公司 | Reflective heat insulation coating, reflective heat insulation film, preparation method of reflective heat insulation film and heat insulation product |
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