CN115340331A - Preparation method of heat reflection cement-based material - Google Patents

Preparation method of heat reflection cement-based material Download PDF

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Publication number
CN115340331A
CN115340331A CN202210959464.XA CN202210959464A CN115340331A CN 115340331 A CN115340331 A CN 115340331A CN 202210959464 A CN202210959464 A CN 202210959464A CN 115340331 A CN115340331 A CN 115340331A
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cement
based material
heat
heat reflection
hollow glass
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钱春香
王莉
徐玉桂
石建华
于敏
彭贝贝
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Southeast University
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Southeast University
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04Portland cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/10Coating or impregnating
    • C04B20/1055Coating or impregnating with inorganic materials
    • C04B20/1066Oxides, Hydroxides

Abstract

The invention discloses a preparation method of a heat-reflecting cement-based material, which comprises the following steps: mixing a sodium hydroxide solution with the hollow glass microspheres, filtering and drying to obtain surface-treated hollow glass microspheres; mixing the hollow glass beads subjected to surface treatment with deionized water, stirring, dropwise adding a titanium source into the mixture, carrying out water bath reaction, filtering, and drying to obtain powder; calcining the powder at 500-900 ℃, grinding and sieving to obtain a load type heat reflection functional component; mixing, stirring and vibrating the heat reflection functional component, ordinary portland cement and water, placing the mixture in a mold for molding, curing under standard conditions, and then removing the mold to obtain the heat reflection cement-based material. The invention is green, environment-friendly and low-cost, and the heat reflection functional component is mixed into the cement-based material, and can automatically float to the surface of the cement-based material after being formed, thereby preparing the structure-function integrated heat reflection cement-based material with good heat reflection performance, and the structural performance and the durability of the cement-based material.

Description

Preparation method of heat reflection cement-based material
Technical Field
The invention relates to a preparation method of a heat reflection material, in particular to a preparation method of a heat reflection cement-based material.
Background
Under the strong irradiation of sunlight in summer, heat radiation energy can be gradually accumulated on the surface of a building, so that the surface temperature is continuously increased, heat is continuously transmitted to the indoor space, and the indoor living environment is influenced. In hot areas of China, the temperature of the outer wall of a building can reach 40-50 ℃ in summer, and the temperature of the metal surface can reach 70-80 ℃. Because the self heat insulation effect of the building is poor, the temperature in the building is high, and a large amount of electric energy is consumed by using a large amount of cooling equipment such as air conditioners, electric fans, air coolers and the like for building a comfortable living environment. According to statistics, the energy consumption of Chinese buildings accounts for about 25% of the total energy consumption, and about l5% of the power consumption is used for cooling and heating the buildings. Therefore, attention has been paid to how to reduce the heat of the building in summer and reduce the refrigeration energy consumption of the air conditioner so as to achieve the purposes of energy conservation and emission reduction.
The common measure for reducing the indoor temperature is generally to adopt a heat insulation coating, and the heat insulation coating is a novel functional coating and is widely applied to the fields of building outer walls, ship decks, automobile shells, oil tank outer walls, military aerospace and the like. The coating has good heat insulation effect, but has the problems of long drying period, great influence of weather and seasons on construction and the like. In practical application, a light-colored or white paint film has poor stain resistance; when the paint is used outdoors, the heat reflection performance is greatly reduced along with the dirtying, fading and aging of the paint film surface, and meanwhile, the decorative effect is poor. In addition, the composite material has the defects of weak impact resistance, easy damage and aging, large drying shrinkage, large fluctuation of thermal conductivity value and the like. Meanwhile, the internal structure is loose, the water absorption rate of the coating is high, and the thermal insulation effect is obviously poor after water absorption.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention aims to provide a preparation method of a heat reflection cement-based material which is green, environment-friendly, nontoxic, harmless and good in durability.
The technical scheme is as follows: the preparation method of the heat reflection cement-based material comprises the following steps:
(a) Mixing a sodium hydroxide solution and the hollow glass beads, filtering and drying to obtain surface-treated hollow glass beads;
(b) Mixing the hollow glass beads subjected to surface treatment with deionized water, stirring, dropwise adding a titanium source into the mixture, carrying out water bath reaction, filtering, and drying to obtain powder;
(c) Calcining the powder at 500-900 ℃, grinding and sieving to obtain a load type heat reflection functional component, wherein the load type heat reflection functional component is hollow glass beads coated with titanium dioxide powder;
(d) Mixing, stirring and vibrating the load-type heat reflection functional component, ordinary Portland cement and water, placing the mixture in a mold for molding, and removing the mold after curing under standard conditions to obtain the heat reflection cement-based material.
Further, in the step (a), the mass percent of the sodium hydroxide solution is 3-5 wt%, and the mass ratio of the sodium hydroxide solution to the hollow glass beads is 10-12.5. The drying temperature is 50-60 ℃, and the drying time is 24-36 h.
In step (b), the titanium source is any one of a titanium sulfate solution, a tetrabutyl titanate solution, and a titanium tetrachloride solution, and preferably a titanium sulfate solution. Firstly, compared with other titanium sources, the titanium sulfate is nontoxic and harmless, and is safe and easy to operate; secondly, titanium dioxide synthesized by titanium sulfate has higher reflectivity and less impurities; and thirdly, for cement-based materials, the addition of an inorganic titanium source has better effect without affecting the performance of the materials. The mass ratio of the titanium source to the hollow glass beads to the deionized water is 4-12. The temperature of the water bath reaction is 60-80 ℃, and the reaction time is 6-8 h.
Further, in the step (b), a magnetic heating stirrer is used for stirring, and the rotating speed is 400r/min.
Further, in the step (c), the calcining time is 2-3 h, and the sieving is 180-200 meshes.
Further, in the step (d), the mass ratio of the load-type heat reflection functional component to the ordinary portland cement is 1-10, and the water cement ratio is 0.3-0.5. The curing time is 1 to 2 days.
Furthermore, the sunlight reflectance of the heat reflection cement-based material is 41.2-62.3%.
The preparation principle is as follows: according to the light weight characteristic of the hollow glass microspheres, the load-type heat reflection functional component can be suspended on the surface of the cement-based material by using the vibration of the vibration table/the vibration rod/the vibrator in the preparation process of the heat reflection cement-based material. When external sunlight irradiates the surface of the heat-reflecting cement-based material, part of light beams can be reflected on the surface of the cement-based material, the rest of light beams can enter the inside of the cement-based material, and under the action of the heat-reflecting inorganic hollow particles, part of light beams can be scattered, the directions of the light beams are changed, and the absorption of the cement-based material to the sunlight is reduced.
Has the beneficial effects that: compared with the prior art, the invention has the following remarkable characteristics:
1. titanium dioxide powder is wrapped on the hollow glass beads through a heterogeneous precipitation method, so that the specific surface area of titanium dioxide is increased, the titanium dioxide is prevented from being directly added into a cement-based material to be agglomerated and covered, and the reflection and scattering capacities are improved;
2. the preparation process is green, environment-friendly and pollution-free, and the used materials are non-toxic and harmless;
3. the hollow glass beads are usually used as heat insulating materials due to the characteristic of low heat conductivity coefficient, so that the heat conduction effect can be reduced, and the heat transfer is prevented;
5. the heat reflection functional component loaded by the hollow glass beads is doped into the cement-based material, and the hollow glass beads are gathered in a specific area through vibration according to the light characteristic of the hollow glass beads of the carrier, namely, the hollow glass beads float on the surface of the cement-based material, so that the waste of the heat reflection functional component can be effectively avoided;
6. compared with the coating on the surface of the cement-based material, the internal doping method is simple and convenient to operate and can be completed in one step;
7. the prepared heat reflection cement-based material has good heat reflection performance, has the structural performance and the durability of the cement-based material, and realizes the integration of structure and function.
Drawings
FIG. 1 is an SEM image of hollow glass microspheres of the present invention;
FIG. 2 is an SEM image of a supported heat reflective component of the present invention;
FIG. 3 is an EDS diagram of a supported heat reflective composition of the present invention;
FIG. 4 is a graph of the reflectance of a cement-based material of the present invention over a wavelength range of 300 to 2500 nm;
FIG. 5 is a graph of the flexural strength of the cement-based material of the present invention;
FIG. 6 is a graph of the compressive strength of the cement-based material of the present invention;
FIG. 7 is an SEM image of loading titanium dioxide on hollow glass microspheres according to the invention, wherein a is a calcination temperature of 1000 ℃ and b is a calcination temperature of 500 ℃;
FIG. 8 is an SEM image of a supported heat reflective component made according to comparative example 3;
figure 9 is an EDS plot of the supported heat reflective component prepared in comparative example 3.
Detailed Description
In the following examples, the hollow glass microspheres had a diameter of about 50 to 80 μm, as shown in FIG. 1. And c, calcining, wherein the crystal forms of the titanium dioxide coated on the surfaces of the hollow glass microspheres comprise rutile type and anatase type.
Example 1
A preparation method of a heat-reflecting cement-based material comprises the following steps:
a. firstly, preparing a sodium hydroxide solution with the mass fraction of 4wt%, mixing the sodium hydroxide solution and the hollow glass beads according to the mass ratio of 12.5;
b. mixing the hollow glass beads subjected to surface treatment with deionized water, placing the mixture into a magnetic heating stirrer with the temperature of 80 ℃ for stirring at the rotating speed of 400r/min, dropwise adding a titanium source titanium sulfate solution with the mass percent of 10wt%, wherein the mass ratio of the titanium source to the hollow glass beads to the deionized water is 8:1:10, performing water bath reaction for 6 hours, filtering and drying to obtain powder;
c. calcining the powder in a muffle furnace at 500 ℃ for 2h, grinding the powder and sieving the powder with a 200-mesh sieve to obtain a load-type heat reflection functional component, namely the hollow glass microspheres coated with titanium dioxide powder;
d. the method comprises the following steps of doping a load-type heat reflection functional component in a mode of replacing part of cement, mixing, stirring and vibrating the load-type heat reflection functional component, ordinary portland cement and water, wherein the mass ratio of the heat reflection functional component to the ordinary portland cement is 1.
Referring to fig. 2, when the microstructure and morphology of the sample are observed by an field Scanning Electron Microscope (SEM), it can be found that the surface of the hollow glass microsphere is coated with a layer of titanium dioxide.
As shown in fig. 3, the results of the surface scanning of the spectrometer show that the mass percentages of Al, si and Ti on the surface of the supported heat-reflecting functional component are 41.62wt%,35.31wt% and 23.07wt%, respectively, and the atomic percentages are 47.01%,38.31% and 14.68%, respectively.
The heat-reflective cement-based material prepared in this example was polished with sandpaper, and the reflectance in the wavelength range of 300nm to 2500nm was measured using an ultraviolet-visible near-infrared spectrophotometer, fig. 4. And calculating the solar light reflectance of the sample by referring to the technical conditions and the evaluation method of the heat reflecting material for the outer wall and the roof of the GB/T31389-2015 building. The solar reflectance of the heat-reflective cement-based material is calculated, the solar reflectance of the heat-reflective cement-based material prepared in the embodiment is 50.1%, and the solar reflectance of the cement-based material is 16.9%. Therefore, the cement-based material doped with the heat reflection functional component can obviously increase the reflection of sunlight and show better heat reflection performance.
Example 2
A preparation method of a heat-reflecting cement-based material comprises the following steps:
a. firstly, preparing a sodium hydroxide solution with the mass fraction of 4wt%, mixing the sodium hydroxide solution and the hollow glass beads according to the mass ratio of 12.5;
b. mixing the hollow glass beads subjected to surface treatment with deionized water, placing the mixture into a magnetic heating stirrer with the temperature of 60 ℃ for stirring at the rotating speed of 400r/min, dropwise adding a titanium source titanium sulfate solution with the mass percent of 10wt%, wherein the mass ratio of the titanium source to the hollow glass beads to the deionized water is 4:1:10, reacting in a water bath for 6 hours, filtering and drying to obtain powder;
c. calcining the powder in a muffle furnace at 500 ℃ for 2 hours, grinding the powder and sieving the powder with a 200-mesh sieve to obtain a load type heat reflection functional component, namely the hollow glass microspheres coated with titanium dioxide powder;
d. the method comprises the following steps of doping a load-type heat reflection functional component in a mode of replacing part of cement, mixing, stirring and vibrating the load-type heat reflection functional component, ordinary portland cement and water, wherein the mass ratio of the heat reflection functional component to the ordinary portland cement is 1.
The light reflection performance of the heat reflection cement-based material prepared in the embodiment is tested by using the test method of the embodiment 1, and the result shows that the sunlight reflection ratio is similar to that of the embodiment 1 and is 47.9%. When the water bath temperature is 60 ℃, the conversion rate of the hydrolysis reaction of the titanium particles is high without the hydrolysis reaction at 80 ℃, namely when the water bath temperature is 60 ℃, less titanium dioxide is synthesized, and the reflection ratio is lower.
Example 3
A preparation method of a heat-reflecting cement-based material comprises the following steps:
a. firstly, preparing a sodium hydroxide solution with the mass fraction of 4wt%, mixing the sodium hydroxide solution and the hollow glass beads according to the mass ratio of 12.5;
b. mixing the hollow glass beads subjected to surface treatment with deionized water, placing the mixture into a magnetic heating stirrer with the temperature of 80 ℃ for stirring at the rotating speed of 400r/min, dropwise adding a titanium source titanium sulfate solution with the mass percent of 10wt%, wherein the mass ratio of the titanium source to the hollow glass beads to the deionized water is 6:1:10, performing water bath reaction for 6 hours, filtering and drying to obtain powder;
c. calcining the powder in a muffle furnace at 900 ℃ for 2h, grinding the powder and sieving the powder with a 200-mesh sieve to obtain a load-type heat reflection functional component, namely the hollow glass microspheres coated with titanium dioxide powder;
d. the method comprises the following steps of doping a load-type heat reflection functional component in a mode of replacing part of cement, mixing, stirring and vibrating the load-type heat reflection functional component, ordinary portland cement and water, wherein the mass ratio of the heat reflection functional component to the ordinary portland cement is 1.
The light reflection performance of the heat reflection cement-based material prepared in the embodiment is tested by using the test method of the embodiment 1, and the result shows that the sunlight reflection ratio is close to that of the embodiment 1 and is 45%.
Example 4
A preparation method of a heat-reflecting cement-based material comprises the following steps:
a. firstly, preparing a sodium hydroxide solution with the mass fraction of 4wt%, mixing the sodium hydroxide solution and the hollow glass beads according to the mass ratio of 12.5;
b. mixing the hollow glass beads subjected to surface treatment with deionized water, placing the mixture into a magnetic heating stirrer with the temperature of 80 ℃ for stirring at the rotating speed of 400r/min, dropwise adding a titanium source titanium sulfate solution with the mass percent of 10wt%, wherein the mass ratio of the titanium source to the hollow glass beads to the deionized water is 12:1:10, reacting in a water bath for 6 hours, filtering and drying to obtain powder;
c. calcining the powder in a muffle furnace at 500 ℃ for 2 hours, grinding the powder and sieving the powder with a 200-mesh sieve to obtain a load type heat reflection functional component, namely the hollow glass microspheres coated with titanium dioxide powder;
d. the method comprises the following steps of doping a load-type heat reflection functional component in a mode of replacing part of cement, mixing, stirring and vibrating the load-type heat reflection functional component, ordinary portland cement and water, wherein the mass ratio of the heat reflection functional component to the ordinary portland cement is 1.
The light reflection performance of the heat reflection cement-based material prepared in the example was tested by the test method of example 1, and the result showed that the solar light reflection ratio was 58.4%. This indicates that: the mixing amount of the heat reflection material is increased, and the reflection of sunlight can be obviously enhanced.
Example 5
A preparation method of a heat-reflecting cement-based material comprises the following steps:
a. firstly, preparing a sodium hydroxide solution with the mass fraction of 4wt%, mixing the sodium hydroxide solution and the hollow glass beads according to the mass ratio of 11;
b. mixing the hollow glass beads subjected to surface treatment with deionized water, placing the mixture into a magnetic heating stirrer with the temperature of 70 ℃ for stirring at the rotating speed of 400r/min, dropwise adding a titanium source titanium sulfate solution with the mass percent of 10wt%, wherein the mass ratio of the titanium source to the hollow glass beads to the deionized water is 8:1:10, performing water bath reaction for 8 hours, filtering and drying to obtain powder;
c. calcining the powder in a muffle furnace at 700 ℃ for 3h, grinding the powder and sieving the powder with a 200-mesh sieve to obtain a load-type heat reflection functional component, namely the hollow glass microspheres coated with titanium dioxide powder;
d. the method comprises the following steps of doping a load-type heat reflection functional component in a mode of replacing part of cement, mixing, stirring and vibrating the load-type heat reflection functional component, ordinary portland cement and water, wherein the mass ratio of the heat reflection functional component to the ordinary portland cement is 1.
The light reflection performance of the heat reflection cement-based material prepared in the embodiment is tested by using the test method of the embodiment 1, and the result shows that the sunlight reflection ratio is 62.3%. The group of embodiments is the group which has the best effect on the cement-based material by internally mixing the heat reflection functional component.
The internal doped heat reflection functional component is not only beneficial to improving the heat reflection performance of the cement-based material, but also beneficial to the mechanical property of the cement-based material. Referring to fig. 5 to 6, the flexural strength and compressive strength of the cement-based material itself, the cement-based material doped with 10% of the heat reflective material prepared in example 1, and the cement-based materials 3d and 7d doped with 20% of the heat reflective material prepared in this example are shown. Because of TiO 2 The high specific surface area of the nano particles provides a nucleation effect for cement hydration, promotes the formation of cement hydration products, and enables the cement stone structure to be more compact. Particularly, the compressive strength is obviously improved along with the doping of the titanium dioxide in the early stage of hydration. At higher titanium dioxide contents, tiO 2 The large amount of agglomeration causes certain defects to the composite system, so that the increase amplitude of the compressive strength is reduced. In general, the addition of titanium dioxide not only improves the heat reflection performance, but also contributes to the improvement of the strength
Example 6
A preparation method of a heat-reflecting cement-based material comprises the following steps:
a. firstly, preparing a sodium hydroxide solution with the mass fraction of 3wt%, mixing the sodium hydroxide solution and the hollow glass beads according to the mass ratio of 10;
b. mixing the hollow glass beads subjected to surface treatment with deionized water, placing the mixture into a magnetic heating stirrer with the temperature of 70 ℃ for stirring at the rotating speed of 400r/min, dropwise adding a titanium source tetrabutyl titanate solution with the mass percent of 8wt%, wherein the mass ratio of the titanium source to the hollow glass beads to the deionized water is 3;
c. calcining the powder in a muffle furnace at 700 ℃ for 3 hours, grinding the powder and sieving the powder with a 180-mesh sieve to obtain a load type heat reflection functional component, namely the hollow glass microspheres coated with titanium dioxide powder;
d. the method comprises the following steps of doping a load-type heat reflection functional component in a mode of replacing part of cement, mixing, stirring and vibrating the load-type heat reflection functional component, ordinary portland cement and water, wherein the mass ratio of the heat reflection functional component to the ordinary portland cement is 1, the water cement ratio is 0.3, placing the mixture in a mold for molding, and demolding after curing for 2 days under standard conditions to obtain the heat reflection cement-based material.
The light reflection performance of the heat reflection cement-based material prepared in the example was tested by the test method of example 1, and the result showed that the solar light reflection ratio was 41.2%.
Example 7
A preparation method of a heat-reflecting cement-based material comprises the following steps:
a. firstly, preparing a sodium hydroxide solution with the mass fraction of 5wt%, mixing the sodium hydroxide solution and the hollow glass beads according to the mass ratio of 11;
b. mixing the hollow glass beads subjected to surface treatment with deionized water, placing the mixture into a magnetic heating stirrer with the temperature set to be 75 ℃ for stirring at the rotating speed of 400r/min, dropwise adding a titanium source titanium tetrachloride solution with the mass percent of 12wt%, wherein the mass ratio of the titanium source to the hollow glass beads to the deionized water is 6;
c. calcining the powder in a muffle furnace at 600 ℃ for 2.5h, grinding the powder and sieving the powder with a 180-mesh sieve to obtain a load type heat reflection functional component, namely the hollow glass microspheres coated with titanium dioxide powder;
d. and (2) doping a load-type heat reflection functional component in a manner of replacing part of cement, mixing, stirring and vibrating the load-type heat reflection functional component, the ordinary Portland cement and water, wherein the mass ratio of the heat reflection functional component to the ordinary Portland cement is 1 and the water cement ratio is 0.4, placing the mixture in a mold for molding, and removing the mold after curing for 2 days under standard conditions to obtain the heat reflection cement-based material.
The light reflection performance of the heat reflection cement-based material prepared in the example was tested by the test method of example 1, and the result showed that the solar light reflectance was 45.6%.
Example 8
A preparation method of a heat-reflecting cement-based material comprises the following steps:
a. firstly, preparing a sodium hydroxide solution with the mass fraction of 3wt%, mixing the sodium hydroxide solution and the hollow glass beads according to the mass ratio of 12;
b. mixing the hollow glass beads subjected to surface treatment with deionized water, placing the mixture into a magnetic heating stirrer with the temperature of 65 ℃ for stirring at the rotation speed of 400r/min, dropwise adding a titanium source titanium tetrachloride solution with the mass percent of 11wt%, wherein the mass ratio of the titanium source to the hollow glass beads to the deionized water is 5;
c. calcining the powder in a muffle furnace at 800 ℃ for 2.5h, grinding the powder and sieving the powder with a 180-mesh sieve to obtain a load type heat reflection functional component, namely the hollow glass microspheres coated with titanium dioxide powder;
d. and (2) doping a load-type heat reflection functional component in a manner of replacing part of cement, mixing, stirring and vibrating the load-type heat reflection functional component, the ordinary Portland cement and water, wherein the mass ratio of the heat reflection functional component to the ordinary Portland cement is 1, the water cement ratio is 0.5, placing the mixture in a mold for molding, and removing the mold after curing for 2 days under standard conditions to obtain the heat reflection cement-based material.
The light reflection performance of the heat reflection cement-based material prepared in the embodiment is tested by using the test method of the embodiment 1, and the result shows that the sunlight reflection ratio is 48.3%.
Example 9
The remaining steps of this comparative example are the same as example 5, except that: in the step b, the titanium source is tetrabutyl titanate solution, and the sunlight reflectance of the prepared cement-based material is 48.9%.
Example 10
The remaining steps of this comparative example are the same as example 5, except that: in the step b, the titanium source is titanium tetrachloride solution, and the solar light reflectance of the prepared cement-based material is 50.6%.
From the reflectance ratios calculated in examples 5, 9 and 10, it can be seen that the titanium sulfate solution is selected as the titanium source, the reflectivity of the synthesized titanium dioxide is high, the impurities are few, the other properties of the cement-based material are not affected, and the titanium sulfate solution is non-toxic, harmless, safe and easy to operate.
Comparative example 1
The remaining steps of this comparative example are the same as example 5, except that: in the step c, the calcination temperature is 400 ℃, and the sunlight reflectance of the prepared cement-based material is 41.17%, which indicates that the reflection and scattering capabilities of the cement-based material are poor. At a calcination temperature of 400 c, the titanium dioxide synthesized at this time was anatase type, and rutile type titanium dioxide was little or no, resulting in poor reflection effect, so that the solar reflectance was relatively low.
Comparative example 2
The remaining steps of this comparative example are the same as example 5, except that: in the step c, the calcination temperature is 1000 ℃, and the solar reflectance of the prepared cement-based material is 35.17%, which indicates that the reflection and scattering capabilities of the cement-based material are poor. When the calcination temperature is 1000 ℃, the spheres are shrunk due to the formation of quartz crystals and mullite in the glass, the core-shell is separated to a certain extent, and the performance of the hollow glass microspheres is reduced, so that the calcination temperature is not too high, and as shown in fig. 7, SEM images of loading titanium dioxide on the hollow glass microspheres at the calcination temperatures of 1000 ℃ and 500 ℃ respectively are shown. As can be seen from fig. 7 (a) and (b), the calcination temperature is also one of the important factors influencing the reflectivity, and too high calcination temperature causes the performance of the microspheres to be reduced, and the hollow microspheres are crushed seriously, so that the carrier does not play a role, the reflection effect is not obvious, and the solar light reflection ratio is greatly reduced.
Comparative example 3
A preparation method for coating titanium dioxide powder on hollow glass beads comprises the following steps:
a. mixing ethanol with tetrabutyl titanate and glacial acetic acid, stirring vigorously for 15min to obtain solution A, and mixing anhydrous ethanol with deionized water to obtain solution B. In the experimental process, dropwise adding the solution B into the solution A at a constant speed for reaction, continuously stirring to obtain uniform light yellow transparent sol, continuously stirring the obtained light yellow transparent sol for 30min, and standing at room temperature;
b. after a certain standing time, the sol still needs to keep a certain fluidity, hollow glass microspheres are added, stirred for 1 hour, filtered by a 200-mesh filter screen, and dried in an oven at 60 ℃ for 24 hours;
c. and calcining the glass microspheres coated with the titanium dioxide gel in a muffle furnace for 2 hours to obtain the load type heat reflection functional component, namely the hollow glass microspheres coated with the titanium dioxide powder.
The heat reflection functional components prepared by the sol-gel method, namely the hollow glass beads coated with the titanium dioxide powder, are respectively subjected to SEM and EDS image characterization. As shown in fig. 8 to 9, the coating effect of the heat reflective functional component prepared by comparative example 3 was poor, much less than that of the titanium dioxide powder coated in fig. 2. The titanium content measured by a surface scanning method on the hollow glass microspheres coated with the titanium dioxide powder is also low. The calcined sample was a pale yellow powder, not a white powder, so the reflectance was low.

Claims (10)

1. A preparation method of the heat reflection cement-based material is characterized by comprising the following steps:
(a) Mixing a sodium hydroxide solution with the hollow glass microspheres, filtering and drying to obtain surface-treated hollow glass microspheres;
(b) Mixing the hollow glass beads subjected to surface treatment with deionized water, stirring, dropwise adding a titanium source, carrying out water bath reaction, filtering, and drying to obtain powder;
(c) Calcining the powder at 500-900 ℃, grinding and sieving to obtain a load type heat reflection functional component, wherein the load type heat reflection functional component is hollow glass beads coated with titanium dioxide powder;
(d) Mixing, stirring and vibrating the load-type heat reflection functional component, ordinary Portland cement and water, placing the mixture in a mold for molding, and removing the mold after curing under standard conditions to obtain the heat reflection cement-based material.
2. The method of claim 1, wherein the step of preparing a heat-reflecting cementitious material comprises: in the step (a), the mass percent of the sodium hydroxide solution is 3-5 wt%, and the mass ratio of the sodium hydroxide solution to the hollow glass beads is 10-12.5.
3. A method of producing a heat reflective cementitious material according to claim 1 or 2, characterised in that: in the step (a), the drying temperature is 50-60 ℃, and the drying time is 24-36 h.
4. The method of claim 1, wherein the step of preparing a heat-reflecting cementitious material comprises: in the step (b), the titanium source is any one of a titanium sulfate solution, a tetrabutyl titanate solution and a titanium tetrachloride solution.
5. The method of claim 1, wherein the step of preparing a heat-reflecting cementitious material comprises: in the step (b), the mass ratio of the titanium source, the hollow glass beads and the deionized water is 4-12.
6. A method of producing a heat reflective cementitious material according to claim 1 or 5, characterised in that: in the step (b), the temperature of the water bath reaction is 60-80 ℃, and the reaction time is 6-8 h.
7. The method of claim 1, wherein the step of preparing a heat-reflecting cementitious material comprises: in the step (c), the calcining time is 2-3 h, and the sieving is 180-200 meshes.
8. The method of claim 1, wherein the step of preparing a heat-reflecting cementitious material comprises: in the step (d), the mass ratio of the load-type heat reflection functional component to the ordinary portland cement is 1.
9. The method of claim 1, wherein the step of preparing a heat-reflecting cementitious material comprises: in the step (d), the curing time is 1 to 2 days.
10. The method of claim 1, wherein the step of preparing a heat-reflecting cementitious material comprises: the solar light reflection ratio of the heat reflection cement-based material is 41.2% -62.3%.
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