CN117757323A - Colored heat-insulating coating with high reflection performance and high infrared radiation performance and preparation method thereof - Google Patents
Colored heat-insulating coating with high reflection performance and high infrared radiation performance and preparation method thereof Download PDFInfo
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- CN117757323A CN117757323A CN202311463450.XA CN202311463450A CN117757323A CN 117757323 A CN117757323 A CN 117757323A CN 202311463450 A CN202311463450 A CN 202311463450A CN 117757323 A CN117757323 A CN 117757323A
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- hollow glass
- titanium dioxide
- ferric oxide
- glass beads
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- 238000000576 coating method Methods 0.000 title claims abstract description 97
- 239000011248 coating agent Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 230000005855 radiation Effects 0.000 title claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 191
- 239000011521 glass Substances 0.000 claims abstract description 129
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 124
- 239000011324 bead Substances 0.000 claims abstract description 116
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 114
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 85
- 238000009413 insulation Methods 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000010410 layer Substances 0.000 claims abstract description 38
- 239000003973 paint Substances 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000011247 coating layer Substances 0.000 claims abstract description 13
- 239000002105 nanoparticle Substances 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 10
- 229920005989 resin Polymers 0.000 claims abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 239000002562 thickening agent Substances 0.000 claims abstract description 9
- 238000009736 wetting Methods 0.000 claims abstract description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011575 calcium Substances 0.000 claims abstract description 7
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 7
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 62
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000001354 calcination Methods 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000002002 slurry Substances 0.000 claims description 16
- 239000004005 microsphere Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 239000004094 surface-active agent Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 11
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 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 description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 239000000839 emulsion Substances 0.000 claims description 4
- 229920005646 polycarboxylate Polymers 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical group CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003929 acidic solution Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 6
- 238000002310 reflectometry Methods 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 8
- 239000011258 core-shell material Substances 0.000 abstract description 6
- 239000000049 pigment Substances 0.000 abstract description 6
- 238000013461 design Methods 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 63
- 239000000945 filler Substances 0.000 description 22
- 238000001000 micrograph Methods 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 238000005054 agglomeration Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 238000005202 decontamination Methods 0.000 description 6
- 230000003588 decontaminative effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- -1 iron ions Chemical class 0.000 description 5
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000012767 functional filler Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000879 optical micrograph Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012720 thermal barrier coating Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
The invention discloses a color heat insulation coating with high reflection performance and high infrared radiation performance and a preparation method thereof, and the color heat insulation coating comprises 35% -50% of water-based film forming resin, 10% -20% of ferric oxide and titanium dioxide double-layer coated hollow glass beads, 10% -20% of deionized water, 10% of rutile titanium dioxide nano particles, 5% -10% of talcum powder, 5% -10% of heavy calcium powder, 0.5% -2% of wetting dispersant and 0.5% -2% of thickener, wherein the hollow glass beads with the ferric oxide and the titanium dioxide double-layer coated hollow glass beads have a hollow core-shell structure, and the hollow heat insulation coating comprises an outermost titanium dioxide coating layer, a ferric oxide coating layer in a middle area and an innermost hollow glass bead in the hollow core-shell structure. The invention can endow the paint with color and good heat radiation performance, actively radiate material heat, and in addition, the core-shell structural design can also greatly reduce the influence of pigment such as ferric oxide on the high reflectivity of titanium dioxide, and the ferric oxide and the titanium dioxide have good synergistic effect, so that the respective performance characteristics can be fully volatilized.
Description
Technical Field
The invention belongs to the technical field of composite color heat insulation, and particularly relates to a preparation method and application of a color heat insulation coating for coating ferric oxide and titanium dioxide on hollow glass beads in a double-layer manner.
Background
When the heat-insulating coating is applied to the outer wall of a building, the energy loss of the building can be obviously reduced, and the heat-insulating coating is mainly divided into a barrier heat-insulating coating, a reflective heat-insulating coating and a radiation heat-insulating coating. The barrier heat-insulating coating mainly relies on functional filler with low heat conductivity in the coating to block the transmission of external heat, and the radiant heat-insulating coating mainly relies on high infrared radiation materials in the coating to actively emit heat to the outside to reduce the heat of a building. The reflective heat-insulating coating isolates heat outside a building by means of high reflectivity of solar radiation energy, and the direct addition of pigments of other colors or functional fillers with low reflectivity into the white heat-insulating coating generally affects the high reflectivity of the original coating, because the white reflective heat-insulating coating can reflect almost all light rays in a visible light range, and the pigments in the colored reflective heat-insulating coating can absorb part of the light rays in the visible light range, so the white reflective heat-insulating coating has better light and heat reflectivity compared with the reflective heat-insulating coatings of other colors. However, in practical application, color paint has better weather resistance and high artistic value, and people prefer to use color paint, so that a heat insulation paint with high light reflection performance and color is urgently needed in the market at present.
Titanium dioxide is often used as a functional filler for reflective thermal insulation coatings due to its high reflectivity and extremely strong hiding power. Ferric oxide is often used as a main component of inorganic pigment and infrared radiation powder in a coating, when the ferric oxide is directly added into a reflective heat-insulating coating in a powder form as pigment or high infrared radiation material, the reflective property of the reflective heat-insulating coating can be directly affected, and in addition, the directly added ferric oxide powder has the problem of agglomeration when dispersed in the coating.
When the solar rays irradiate the titanium dioxide of the outermost coating layer, the titanium dioxide has good reflection performance on the solar rays, and can isolate a large amount of solar energy. The intermediate coating layer ferric oxide can endow the paint with color and good heat radiation performance, can more actively emit material heat, and more importantly, as the ferric oxide is designed in the intermediate layer of the composite microsphere, the heat which can be absorbed by the ferric oxide is greatly reduced by the titanium dioxide in the outermost layer, and in addition, the influence of the pigment such as the ferric oxide on the high reflectivity of the titanium dioxide can be greatly reduced due to the structural design of a core shell, the problem that the agglomeration is caused by directly adding the ferric oxide powder into the paint is solved, the heat conductivity of the material is further reduced, and the ferric oxide and the titanium dioxide have good synergistic effect and can fully volatilize the respective performance characteristics. The hollow glass beads of the innermost layer have the characteristic of low heat conductivity, and can effectively isolate the transmission of external heat.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of the colored heat-insulating coating with high reflection performance and high infrared radiation performance.
In order to solve the technical problems, the invention provides the following technical scheme: a color heat-insulating coating with high reflection performance and high infrared radiation performance is characterized in that: comprising the steps of (a) a step of,
the paint comprises water-based film-forming resin, hollow glass beads coated by ferric oxide and titanium dioxide in a double-layer manner, deionized water, rutile titanium dioxide nano-particles, talcum powder, heavy calcium powder, wetting dispersant and thickener;
the water-based film-forming resin comprises, by mass, 35-50% of water-based film-forming resin, 10-20% of hollow glass beads coated with ferric oxide and titanium dioxide in a double-layer manner, 10% of rutile titanium dioxide nanoparticles, 5-10% of talcum powder, 5-10% of heavy calcium powder, 0.5-2% of wetting dispersant and 0.5-2% of thickener.
As a preferred embodiment of the preparation process according to the invention, there is provided: the preparation method of the hollow glass microsphere coated by ferric oxide and titanium dioxide comprises the following steps of,
ferric oxide coated hollow glass beads: decontaminating and drying the hollow glass beads by using a sodium hydroxide solution, preparing slurry with water, adding a surfactant and an acidic solution, adjusting the pH value of the solution by using the sodium hydroxide solution, carrying out suction filtration and drying treatment to obtain modified hollow glass beads, and calcining to obtain the ferric oxide coated hollow glass beads;
recoating of titanium dioxide: adding a surfactant into the hollow glass beads coated with ferric oxide, stirring, filtering and drying for later use;
adding tetrabutyl titanate and glacial acetic acid into ethanol, and fully stirring to obtain a solution A;
adding deionized water into ethanol, adding dilute hydrochloric acid to adjust the pH value of the solution, and fully stirring to obtain solution B;
and slowly dripping the solution B into the solution A, adding the hollow glass beads coated with the standby ferric oxide after the solution B is completely dripped into the solution A, fully stirring, standing until gel is formed, drying, and calcining to prepare the hollow glass beads coated with the ferric oxide and the titanium dioxide.
As a preferred embodiment of the preparation process according to the invention, there is provided: the hollow glass beads are decontaminated and dried by sodium hydroxide solution and then are prepared into slurry with water, wherein the diameter of the hollow glass beads is 20-80 mu m, the concentration of the sodium hydroxide solution is 0.1mol/L, and the mass fraction of the slurry is 10%.
As a preferred embodiment of the preparation process according to the invention, there is provided: the surfactant and the acid solution are added, and the pH value of the solution is regulated by the sodium hydroxide solution, wherein the surfactant is sodium dodecyl benzene sulfonate, the acid solution is ferric chloride with the concentration of 0.6mol/L, the concentration of the sodium hydroxide solution is 1.5mol/L, and the pH value is 4-7.
As a preferred embodiment of the preparation process according to the invention, there is provided: : and adding a surfactant into the hollow glass beads coated with the ferric oxide for standby, wherein the surfactant is triethoxysilane.
As a preferred embodiment of the preparation process according to the invention, there is provided: in the recoating of the titanium dioxide, the ethanol in the solution A is 80ml, the tetrabutyl titanate is 20ml, the glacial acetic acid is 5ml, the ethanol in the solution B is 35ml, the deionized water is 5ml, the concentration of the dilute hydrochloric acid is 0.1mol/L, and the dilute hydrochloric acid is added to adjust the PH of the solution to be 2-4.
As a preferred embodiment of the preparation process according to the invention, there is provided: the hollow glass microsphere is coated by ferric oxide, wherein the thickness of the ferric oxide coating layer is 0.3-2 mu m, and the titanium dioxide is coated again, and the thickness of the titanium dioxide coating layer is 0.3-2 mu m.
As a preferred embodiment of the preparation process according to the invention, there is provided: the reaction temperature when the ferric oxide coats the hollow glass beads is more than or equal to 50 ℃, the calcination temperature is 500-800 ℃, and the calcination time is 2 hours; the reaction temperature in the recoating of the titanium dioxide is more than or equal to 50 ℃, the calcination temperature is 500-600 ℃, and the calcination time is 2h.
As a preferred embodiment of the preparation process according to the invention, there is provided: the wetting dispersant is of a polycarboxylate 5040 type; the aqueous film-forming resin is silicone-acrylic emulsion; the thickener is DH3100.
As a preferred embodiment of the preparation process according to the invention, there is provided: the diameter of the rutile titanium dioxide nano-particle is 40-100 nm.
It is still another object of the present invention to overcome the deficiencies of the prior art and to provide a product of a method for preparing a colored thermal barrier coating having high reflective and infrared radiation properties.
The invention further aims to overcome the defects in the prior art and provide the application of the product prepared by the preparation method of the colored heat-insulating coating with high reflection performance and high infrared radiation performance in the colored heat-insulating coating.
The invention has the beneficial effects that:
(1) The invention discloses a preparation method for coating hollow glass beads with ferric oxide and titanium dioxide in a double-layer manner, and application of the hollow glass beads in color heat insulation paint. The coating speed, the thickness of the coating layer and the size of the coated particles can be controlled by controlling the temperature and the pH value in the coating reaction. The coating layer is tightly coated and is not easy to fall off after being calcined at a proper calcining temperature, and the preparation process is simple and the preparation cost is low.
(2) The coating prepared by the invention is a color heat-insulating coating with three heat-insulating mechanisms of heat collection, heat radiation and heat reflection, and the titanium dioxide of the outermost coating layer has good reflection performance on solar rays and can isolate a large amount of solar energy. The intermediate coating layer ferric oxide can endow the paint with color and good heat radiation performance, can more actively emit material heat, and more importantly, as the ferric oxide is designed in the intermediate layer of the composite microsphere, the heat which can be absorbed by the ferric oxide can be greatly reduced by the titanium dioxide in the outermost layer, and in addition, the influence of the pigment such as the ferric oxide on the high reflectivity of the titanium dioxide can be greatly reduced due to the structural design of a core shell, the problem that the ferric oxide powder is directly added into the paint to generate agglomeration is solved, the heat conductivity of the material is further reduced, the ferric oxide and the titanium dioxide have good synergistic effect, and the respective performance characteristics can be fully volatilized. The hollow glass beads of the innermost layer have the characteristic of low heat conductivity, and can effectively isolate the transmission of external heat.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is a scanning electron microscope image of hollow glass beads before decontamination treatment;
FIG. 2 is a scanning electron microscope image of hollow glass beads before decontamination treatment;
FIG. 3 is a scanning electron microscope image of a hollow glass bead surface coated iron oxide film prepared in example 1;
FIG. 4 is a scanning electron microscope image and EDS data of a hollow glass bead double-layer coated with ferric oxide and titanium dioxide prepared in example 1;
FIG. 5 is an optical microscope image of a hollow glass microsphere double coated with ferric oxide and titanium dioxide prepared in comparative example 5;
FIG. 6 is a scanning electron microscope image of hollow glass beads coated with iron oxide and titanium dioxide prepared in example 7;
FIG. 7 is a scanning electron microscope image of the hollow glass beads double-coated with ferric oxide and titanium dioxide prepared in comparative example 13;
fig. 8 is an optical microscope image of hollow glass beads double coated with iron oxide and titanium dioxide prepared in comparative example 14.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The hollow glass beads used in the following examples and comparative examples were purchased from Saint Lai New Material Co., ltd., model HL38, the scanning electron microscope of which was shown in FIG. 1, and the surface contained a large amount of impurities, and the surface impurities were reduced as shown in FIG. 2 after the decontamination treatment with 1.5mol/L sodium hydroxide solution.
Example 1
The embodiment relates to a preparation method of double-layer coating of ferric oxide and titanium dioxide on hollow glass beads, which comprises the following steps:
preparation of double-layer coating of ferric oxide and titanium dioxide on hollow glass beads:
(1) The decontamination pretreatment of the hollow glass beads comprises the steps of adding 20ml of 0.1mol/L sodium hydroxide solution into 5g of hollow glass beads, rotating for 10 minutes at the speed of 300 revolutions per minute by using an electric stirrer, oscillating for 10 minutes by using an ultrasonic cleaner, filtering and washing by using deionized water, and drying for 8 hours at the temperature of 100 ℃ in a vacuum drying oven for later use.
(2) Ferric oxide coated hollow glass beads: preparing 50ml of 0.6mol/L ferric chloride acid solution (ferric oxide precursor) and 100ml of 1.5mol/L sodium hydroxide solution in advance, preparing slurry with the mass fraction of the hollow glass beads and water of 10% obtained in the step (1), adding 0.5g of active agent sodium dodecyl benzene sulfonate, rotating for 10 minutes at the speed of 300 revolutions per minute by using an electric stirrer, vibrating for 10 minutes by using an ultrasonic cleaner, and placing a beaker filled with the hollow glass bead slurry into a magnetic stirring water bath, wherein the temperature of the magnetic stirring water bath is set to 70 ℃, the rotating speed is set to 300 revolutions per minute, and the rotating speed is set to 5 minutes.
The pH value of the slurry is monitored in real time by inserting a pH measuring instrument into the hollow glass bead slurry, 0.6mol/L ferric chloride acid solution is dripped into the slurry at the speed of 1 second and 1 drop, meanwhile, 1.5mol/L sodium hydroxide solution is continuously dripped into the hollow glass bead slurry, when the ferric chloride acid solution and the sodium hydroxide solution are dripped into the hollow glass bead slurry together, the pH value of the hollow glass bead slurry is ensured to be 5, and after 50ml of the 0.6mol/L ferric chloride acid solution is completely dripped, and the pH value of the hollow glass bead slurry is regulated to be 5, the dripping of the 1.5mol/L sodium hydroxide solution is stopped. And (3) continuously stirring for 30 minutes, then carrying out filtration treatment, and putting the hollow glass microspheres obtained after filtration into a vacuum drying oven to be dried for 8 hours at the temperature of 100 ℃ for standby.
(3) And (3) carrying out active treatment on the hollow glass microspheres coated with ferric oxide: and (3) placing the hollow glass beads dried in the step (2) into a muffle furnace, calcining at 600 ℃ for two hours, and taking out, wherein the surfaces of the hollow glass beads are coated with a layer of ferric oxide film. Preparing slurry with the mass fraction of 20% by using the hollow glass beads calcined at high temperature and deionized water, adding 0.15g of triethoxysilane serving as an active agent, rotating for 10 minutes at the speed of 300 revolutions per minute by using an electric stirrer, then oscillating for 10 minutes by using an ultrasonic cleaner, filtering, and drying the hollow glass beads in a vacuum drying oven at the temperature of 100 ℃ for 8 hours for later use.
(4) Recoating of titanium dioxide: 20ml of tetrabutyl titanate was added to 80ml of ethanol, and the mixture was rotated at 800 rpm for 10 minutes with an electric stirrer, followed by 5ml of glacial acetic acid, and further rotated at 800 rpm for 10 minutes, and then placed in a magnetic stirring water bath at a temperature of 60℃at 800 rpm, which was designated as solution A. 5ml of deionized water was added to 35ml of ethanol and the mixture was stirred with an electric stirrer at 800 rpm for 10 minutes, followed by 0.1mol/L of dilute hydrochloric acid to give a mixed solution of ethanol and deionized water having a pH of 2.5, and after 10 minutes of rotation, stirring was stopped to give solution B. Adding the solution B into the solution A at a speed of 1 second and 1 drop, rotating the water bath at 800 revolutions per minute, rotating the water bath at 300 revolutions per minute after the solution B is completely dropped, slowly adding the hollow glass microspheres which are prepared by surface active treatment in the step (3), stopping stirring for one hour (stirring is stopped immediately when gel is formed by the solution in the stirring process and loses fluidity), taking the solution out of the water bath, standing for 8 hours, and putting the solution into a vacuum drying box for drying at 100 ℃ for 6 hours after standing. And taking out the dried hollow glass microspheres, calcining the hollow glass microspheres for 2 hours at 500 ℃ in a muffle furnace, and taking out the hollow glass microspheres at a calcining temperature of 500 ℃. At the moment, the hollow glass beads are attached with ferric oxide films and titanium dioxide films, and the hollow glass beads coated by ferric oxide and titanium dioxide in a double-layer manner are prepared.
The heat-insulating coating 1 is prepared by taking the hollow glass beads coated with the ferric oxide and the titanium dioxide in double layers as heat-insulating fillers.
The heat-insulating coating 1 comprises the following components in percentage by mass: 45% of aqueous film-forming resin silicone-acrylic emulsion, 15% of ferric oxide and titanium dioxide double-layer coated hollow glass beads, 15% of deionized water, 10% of rutile titanium dioxide nano particles, 5% of talcum powder, 5% of heavy calcium powder, 1% of polycarboxylate 5040 type wetting dispersant and 1% of DH3100 thickener.
The specific preparation process of the heat-insulating paint 1 is as follows:
according to the mass percentage, 1% polycarboxylate 5040 type wetting agent dispersing agent and 15% deionized water are sequentially added into a beaker, then the mixture is fully stirred for ten minutes at the speed of 600 revolutions per minute by an electric magnetic stirrer, then 45% of aqueous film forming substance silicone-acrylic emulsion, 15% of ferric oxide and titanium dioxide double-layer coated hollow glass beads, 10% of rutile titanium dioxide nano particles, 5% of talcum powder and 5% of heavy calcium powder are sequentially added, the rotating speed of the electric stirrer is adjusted to 300 revolutions per minute, the electric stirrer rotates for 30 minutes, and finally after 1% of DH3100 thickener is added, the rotating speed of the electric stirrer is 300 revolutions per minute, and the preparation is completed after 10 minutes of rotation.
FIG. 1 is a scanning electron microscope image of hollow glass beads before decontamination treatment; FIG. 2 is a scanning electron microscope image of hollow glass beads before decontamination treatment; the scanning electron microscope image of the hollow glass bead coated with ferric oxide prepared in the step (2) of the embodiment is shown in fig. 3, and the surface of the hollow glass bead is coated with a layer of ferric oxide film.
The scanning electron microscope image and EDS data of the hollow glass bead double-layer coated with ferric oxide and titanium dioxide prepared in the step (4) of the embodiment are shown in fig. 4, and the core-shell layer of the hollow glass bead detects iron element and titanium element, so that the coating success is confirmed.
Comparative example 1
The difference from example 1 is that: the hollow glass beads coated by the ferric oxide and the titanium dioxide serving as the heat insulation filler are changed into the hollow glass beads coated by the ferric oxide, and the hollow glass beads coated by the ferric oxide and the titanium dioxide prepared by the comparative example are used as the heat insulation filler to prepare the heat insulation coating 2.
Comparative example 2
The difference from example 1 is that: the hollow glass beads coated by the heat insulation filler of ferric oxide and titanium dioxide are changed into hollow glass beads, and 2 mass percent of ferric oxide powder is added into the heat insulation coating 9, so that the hollow glass beads are prepared as the heat insulation filler to prepare the heat insulation coating 3.
Comparative example 3
The difference from example 1 is that: the heat insulation coating 4 was prepared by changing the hollow glass beads coated with the heat insulation filler of ferric oxide and titanium dioxide into the hollow glass beads coated with titanium dioxide and adding 2% by mass of ferric oxide powder into the heat insulation coating 11, and using the hollow glass beads coated with titanium dioxide prepared in the comparative example as the heat insulation filler.
Comparative example 4
The difference from example 1 is that: the hollow glass bead coated by the double layers of ferric oxide and titanium dioxide serving as the heat insulation filler is changed into the hollow glass bead coated by titanium dioxide, and the hollow glass bead coated by the double layers of ferric oxide and titanium dioxide prepared in the comparative example is used as the heat insulation filler to prepare the heat insulation coating 5.
Comparative example 5
The difference from example 1 is that: and (3) changing the pH value of the reaction condition of the hollow glass beads coated by the ferric oxide in the step (2) from 5 to 2, and preparing the heat-insulating coating 6 by taking the hollow glass beads coated by the ferric oxide and the titanium dioxide prepared in the comparative example as heat-insulating filler.
The optical microscopic diagram of the hollow glass bead coated by the ferric oxide and the titanium dioxide prepared in the comparative example is shown in fig. 5, and the reaction rate is greatly reduced because the pH value of the reaction condition of the hollow glass bead coated by the ferric oxide is changed from 5 to 2, and the ferric oxide is not completely coated.
Comparative example 6
The difference from example 1 is that: and (3) changing the pH value of the reaction condition of the hollow glass beads coated by the ferric oxide in the step (2) from 5 to 11, and preparing the heat-insulating coating 7 by taking the hollow glass beads coated by the ferric oxide and the titanium dioxide prepared in the comparative example as heat-insulating filler.
Comparative example 7
The present example relates to a preparation of double-layer coating of ferric oxide and titanium dioxide on hollow glass beads, which is different from example 1 in that: the temperature of calcination in the step (4) when the titanium dioxide is recoated is changed from 500 ℃ to 800 ℃, and the hollow glass beads coated with the ferric oxide and the titanium dioxide prepared in the comparative example are used as heat insulation filler to prepare the heat insulation coating 8.
The scanning electron microscope diagram of the hollow glass bead coated with the ferric oxide and the titanium dioxide in the double-layer prepared in the comparative example is shown in fig. 6, and the calcining temperature is changed from 500 ℃ to 800 ℃ when the titanium dioxide in the step (4) is coated again, so that the hollow glass bead is molten and damaged due to the overhigh calcining temperature.
Comparative example 8
The difference from example 1 is that: the temperature of calcination in the step (4) when the titanium dioxide is recoated is changed from 500 ℃ to 400 ℃, and the hollow glass beads coated with the ferric oxide and the titanium dioxide prepared in the comparative example are used as heat insulation filler to prepare the heat insulation coating 9.
Comparative example 9
The difference from example 1 is that: the temperature of calcination in the coating of the ferric oxide in the step (2) is changed from 600 ℃ to 900 ℃, and the hollow glass beads coated with the ferric oxide and the titanium dioxide in double layers prepared in the comparative example are used as heat insulation fillers to prepare the heat insulation coating 10.
Comparative example 10
The difference from example 1 is that: the temperature of calcination in the coating of the ferric oxide in the step (2) is changed from 600 ℃ to 400 ℃, and the hollow glass beads coated with the ferric oxide and the titanium dioxide in double layers prepared in the comparative example are used as heat insulation fillers to prepare the heat insulation coating 11.
Comparative example 11
The difference from example 1 is that: and (3) adding dilute hydrochloric acid in the step (4) to adjust the ph of ethanol and deionized water to be changed from 2.5 to 5, and preparing the heat-insulating coating 12 by taking the hollow glass beads coated with the ferric oxide and the titanium dioxide prepared in the comparative example as heat-insulating fillers.
Comparative example 12
The difference from example 1 is that: and (3) adding dilute hydrochloric acid in the step (4) to adjust the ph of ethanol and deionized water to be changed from 2.5 to 1, and preparing the heat-insulating coating 13 by taking the hollow glass beads coated with the ferric oxide and the titanium dioxide prepared in the comparative example as heat-insulating fillers.
Comparative example 13
The difference from example 1 is that: the heat-insulating paint 14 was prepared by changing 0.6mol/L ferric chloride of the iron source provided by the preparation of ferric oxide in the step (2) into 0.6mol/L ferric nitrate nonahydrate, and using the hollow glass beads coated with the double layers of ferric oxide and titanium dioxide prepared in the comparative example as heat-insulating filler.
The scanning electron microscope image of the hollow glass bead coated with ferric oxide prepared in the step (2) of the comparative example is shown in fig. 7, a layer of ferric oxide film is coated on the surface of the hollow glass bead, but the ferric oxide is not completely coated, and a plurality of burrs exist on the surface, because the solubility of ferric nitrate nonahydrate and ferric chloride in water are inconsistent, and the concentration of free iron ions in water does not reach the optimal coating concentration.
Comparative example 14
The difference from example 1 is that: the reaction temperature of the hollow glass beads coated with the ferric oxide in the step (2) is changed from 60 ℃ to 20 ℃, and the hollow glass beads coated with the ferric oxide and the titanium dioxide prepared in the comparative example are used as heat insulation filler to prepare the heat insulation coating 15.
The optical microscope image of the hollow glass bead coated with ferric oxide prepared in the step (2) of the comparative example is shown in fig. 8, and the surface of the hollow glass bead is coated with a layer of ferric oxide, so that the coating of ferric oxide is very little, and the ferric oxide is not completely coated because ferric ions generated by the hydrolysis of ferric chloride are insufficient and the reduction of the reaction temperature is unfavorable for the generation of reactants under the condition of the coating temperature of 60 ℃. The scanning electron microscope diagram of the hollow glass bead coated by the ferric oxide and the titanium dioxide prepared in the embodiment is shown in fig. 6, and as the reaction temperature of the hollow glass bead coated by the ferric oxide is changed from 60 ℃ to 20 ℃, the reaction rate is reduced, and the ferric oxide is not completely coated.
Comparative example 15
The present example relates to a preparation of double-layer coating of ferric oxide and titanium dioxide on hollow glass beads, which is different from example 1 in that: the reaction temperature of the titanium dioxide coated hollow glass beads in the step (4) is changed from 70 ℃ to 20 ℃, and the ferric oxide and titanium dioxide double-layer coated hollow glass beads prepared in the comparative example are used as heat insulation filler to prepare the heat insulation coating 16.
Comparative example 16
The difference from example 1 is that: the addition amount of the rutile titanium dioxide nano-particles is adjusted to be increased from 10% to 15%. The heat-insulating paint 17 was prepared by using the hollow glass beads double-coated with ferric oxide and titanium dioxide prepared in this comparative example as a heat-insulating filler.
Performance testing
The heat-insulating coatings prepared in the above examples and comparative examples were subjected to performance tests, specifically: the coatings were applied to the same stainless steel plate using a coater to form a coating of 800 μm thickness, and the hemispherical emissivity, heat insulating property and reflectivity thereof were measured.
Hemispherical emissivity test: the measurement is carried out at room temperature by adopting an IR-2 dual-band infrared emissivity tester, and the measurement is carried out at room temperature by coating the coating on a round iron sheet with the diameter of 8 cm.
Thermal insulation performance test: the paint is sprayed on the stainless steel plate by using an applicator, one surface coated with the paint is upwards placed in a heat insulation film temperature tester, and a temperature probe below the glass plate collects the temperature before and after irradiation of an infrared lamp and displays the temperature difference.
Reflectance test: C84-II reflectance meter reflectance measurements were performed on coatings on stainless steel plates.
Adhesion test: the execution standard is GB/T1720-79.
The test results are shown in table 1 below:
table 1 results of performance test of heat-insulating coating prepared in examples and comparative examples
As can be seen from the test results in Table 1, the heat-insulating coating 1 prepared in example 1 was red in color, good in color hiding power, highest in reflectivity and hemispherical emissivity, and best in heat-insulating effect.
As can be seen from the performance test results in table 1, comparative example 1 changed the hollow glass bead coated with the heat insulation filler of ferric oxide and titanium dioxide into the hollow glass bead coated with ferric oxide, and the outer layer of the hollow glass bead was not coated with highly reflective titanium dioxide, so that the reflectivity of the heat insulation coating was greatly reduced, and the heat insulation effect was greatly reduced. Comparative example 2 and comparative example 3 comparative example 1 both add ferric oxide powder directly into the heat-insulating coating to impart color and high emissivity to the coating, but the directly added ferric oxide powder tends to cause agglomeration during dispersion, which results in a decrease in coating color hiding power, a decrease in radiant surface area, and a decrease in hemispherical emissivity, as compared with example 1, and the directly added ferric oxide also interferes with efficient reflection of titanium dioxide on solar rays, thereby reducing the reflectivity and heat-insulating ability of the heat-insulating coating. Comparative example 4 comparative example 1 changes the hollow glass bead coated with titanium dioxide from the double-layer coated hollow glass bead coated with titanium dioxide and the hemispherical emissivity of comparative example 4 is far lower than that of example 1, the active heat radiation ability is weak, the paint color is white, and the heat insulation effect is inferior to that of example 1. Comparative example 5 when the reaction pH of the iron oxide coating was adjusted from 5 to 2, the reaction of iron ions and hydroxyl groups in water was slow, the effectively coated iron oxide was little, the coating color was pale red, and the hemispherical emissivity was also lower than that of experimental example 1. Comparative example 6 when the reaction pH of the iron sesquioxide coating was adjusted from 5 to 9, the reaction of the iron ions with the hydroxide in water was too rapid, the generated iron sesquioxide particles were too large, effective coating was difficult to complete, and the agglomeration phenomenon was aggravated. Comparative example 6 is inferior to example 1 in both reflectivity and heat insulating effect. The calcination temperatures in the coating process are increased or reduced in comparative examples 7, 8 and 9 and comparative example 10, too low calcination temperature results in the coating being not tight, the coating layer is easy to fall off, the hollow glass beads are easy to crack at too high calcination temperature, and the thermal conductivity of the material is rapidly increased, so that the heat insulation performance is reduced. Comparative example 11 in which the pH of ethanol and deionized water was adjusted from 2.5 to 5 by adding diluted hydrochloric acid in step (4), the formation of titania was too fast to be advantageous for coating of titania, and comparative example 12 in which the pH of ethanol and deionized water was adjusted from 2.5 to 1 by adding diluted hydrochloric acid in step (4), the formation of titania was too slow to be advantageous for coating of titania, and the reflectivity of comparative example 11 and comparative example 12 were both lower than that of example 1, and the heat insulation effect was also poor. In comparative example 13, ferric nitrate nonahydrate was lower in solubility in water than ferric chloride, so that when ferric nitrate nonahydrate was used in comparative example 13, the efficiency of coating hollow glass microspheres with ferric oxide of comparative example 13 was lower than that of example 1 using ferric chloride at the same concentration, and the subsequent coating with titanium dioxide was affected, the infrared radiation ability was also lower than that of experimental example 1, and the color hiding power was lower than that of example 1 to appear pale red. Compared with example 1, the reaction temperature of the ferric oxide coating in comparative example 14 is adjusted from 60 ℃ to 20 ℃, the coating reaction rate is reduced, free iron ions in water are reduced, the ferric oxide which is effectively coated is little, the paint is light red, and the hemispherical emissivity is lower than that of example 1. Compared with example 1, comparative example 15 was prepared by adjusting the reaction temperature of the titanium oxide coating from 70 ℃ to 20 ℃, the coating reaction rate was reduced, free titanium ions in water were reduced, the effectively coated titanium oxide was reduced, and the reflectance was lower than in example 1. In comparative example 16, when the proportion of rutile titanium dioxide nanoparticles in the heat-insulating coating is increased, an agglomeration phenomenon tends to occur at an excessively high proportion, resulting in a decrease in reflectance and a decrease in heat-insulating effect, as compared with example 1.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, and it should be covered in the scope of the present invention.
Claims (10)
1. A color heat-insulating coating with high reflection performance and high infrared radiation performance is characterized in that: comprising the steps of (a) a step of,
the paint comprises water-based film-forming resin, hollow glass beads coated by ferric oxide and titanium dioxide in a double-layer manner, deionized water, rutile titanium dioxide nano-particles, talcum powder, heavy calcium powder, wetting dispersant and thickener;
the water-based film-forming resin comprises, by mass, 35-50% of water-based film-forming resin, 10-20% of hollow glass beads coated with ferric oxide and titanium dioxide in a double-layer manner, 10% of rutile titanium dioxide nanoparticles, 5-10% of talcum powder, 5-10% of heavy calcium powder, 0.5-2% of wetting dispersant and 0.5-2% of thickener.
2. The colored thermal insulation coating of claim 1, wherein: the preparation method of the hollow glass microsphere coated by ferric oxide and titanium dioxide comprises the following steps of,
ferric oxide coated hollow glass beads: decontaminating and drying the hollow glass beads by using a sodium hydroxide solution, preparing slurry with water, adding a surfactant and an acidic solution, adjusting the pH value of the solution by using the sodium hydroxide solution, carrying out suction filtration and drying treatment to obtain modified hollow glass beads, and calcining to obtain the ferric oxide coated hollow glass beads;
recoating of titanium dioxide: adding a surfactant into the hollow glass beads coated with ferric oxide, stirring, filtering and drying for later use;
adding tetrabutyl titanate and glacial acetic acid into ethanol, and fully stirring to obtain a solution A;
adding deionized water into ethanol, adding dilute hydrochloric acid to adjust the pH value of the solution, and fully stirring to obtain solution B;
and slowly dripping the solution B into the solution A, adding the hollow glass beads coated with the standby ferric oxide after the solution B is completely dripped into the solution A, fully stirring, standing until gel is formed, drying, and calcining to prepare the hollow glass beads coated with the ferric oxide and the titanium dioxide.
3. The method of manufacturing as claimed in claim 2, wherein: the hollow glass beads are decontaminated and dried by sodium hydroxide solution and then are prepared into slurry with water, wherein the diameter of the hollow glass beads is 20-80 mu m, the concentration of the sodium hydroxide solution is 0.1mol/L, and the mass fraction of the slurry is 10%.
4. The method of manufacturing as claimed in claim 2, wherein: the surfactant and the acid solution are added, and the pH value of the solution is regulated by the sodium hydroxide solution, wherein the surfactant is sodium dodecyl benzene sulfonate, the acid solution is ferric chloride with the concentration of 0.6mol/L, the concentration of the sodium hydroxide solution is 1.5mol/L, and the pH value is 4-7.
5. The method of manufacturing as claimed in claim 2, wherein: and adding a surfactant into the hollow glass beads coated with the ferric oxide for standby, wherein the surfactant is triethoxysilane.
6. The method of manufacturing as claimed in claim 2, wherein: in the recoating of the titanium dioxide, the ethanol in the solution A is 80ml, the tetrabutyl titanate is 20ml, the glacial acetic acid is 5ml, the ethanol in the solution B is 35ml, the deionized water is 5ml, the concentration of the dilute hydrochloric acid is 0.1mol/L, and the dilute hydrochloric acid is added to adjust the PH of the solution to be 2-4.
7. The method of manufacturing as claimed in claim 2, wherein: the hollow glass microsphere is coated by ferric oxide, wherein the thickness of the ferric oxide coating layer is 0.3-2 mu m, and the titanium dioxide is coated again, and the thickness of the titanium dioxide coating layer is 0.3-2 mu m.
8. The method of manufacturing as claimed in claim 2, wherein: the reaction temperature when the ferric oxide coats the hollow glass beads is more than or equal to 50 ℃, the calcination temperature is 500-800 ℃, and the calcination time is 2 hours; the reaction temperature in the recoating of the titanium dioxide is more than or equal to 50 ℃, the calcination temperature is 500-600 ℃, and the calcination time is 2h.
9. The colored thermal insulation coating of claim 1, wherein: the wetting dispersant is of a polycarboxylate 5040 type; the aqueous film-forming resin is silicone-acrylic emulsion; the thickener is DH3100.
10. The colored thermal insulation coating of claim 1, wherein: the diameter of the rutile titanium dioxide nano-particle is 40-100 nm.
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