CN115504771B - Radiation refrigeration material and preparation method and application thereof - Google Patents
Radiation refrigeration material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a radiation refrigeration material, a preparation method and application thereof, and belongs to the technical field of composite materials. The material comprises the following preparation raw materials: silicate esters, alkylalkoxysilanes, acids, and alumina; the state of the radiation refrigeration material is aerogel. The Silica Alumina Fiber Aerogels (SAFAs) synthesized by the sol-gel + blow-spinning process of the present invention provide up to 95% solar reflectance and 93% high atmospheric window emissivity due to scattered reflection and selective emission of the fiber network. In field testing, SAFAs were maintained at 8℃or more below ambient temperature, theoretically yielding 133.1W/m 2 Is used for cooling power by daytime radiation. In addition, SAFAs have high compression fatigue resistance, strong fireproof performance and excellent heat insulation performance, are low in cost, and can realize large-scale radiation refrigeration.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a radiation refrigeration material and a preparation method and application thereof.
Background
Radiation refrigeration is a passive cooling technology for directly radiating heat to the outer space, does not need extra energy input, and has important significance for reducing energy consumption. However, the radiation cooling of the material in the related art is easy to achieve at night, but it is difficult to achieve a cooling effect below ambient under daytime or sub-ambient conditions. And the radiation refrigeration material in the related art needs complex structural design, such as photon crystal and metamaterial, but the method has high cost and no expandability.
Therefore, there is a need to develop a radiation refrigeration material which has a good daytime refrigeration effect.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides the radiation refrigeration material which has good daytime refrigeration effect.
The invention also provides a preparation method of the radiation refrigeration material.
The invention also provides application of the radiation refrigeration material.
The method comprises the following steps: the first aspect of the invention provides a radiation refrigeration material, which comprises the following preparation raw materials: silicate esters, alkylalkoxysilanes, acids, and alumina; the radiation refrigeration material is aerogel.
According to one of the technical schemes of the radiation refrigeration material, the radiation refrigeration material has at least the following beneficial effects:
in the preparation raw materials provided by the invention, under the action of acid, silicate and alkyl alkoxy silane are polymerized and wrapped with aluminum oxide, and the aluminum oxide is formed after sintering, namely the type of the preparation raw materials determines the components of the obtained product, and the components of the product determine the reflection effect on specific wavelengths.
The radiation refrigeration material provided by the invention combines the components and the aerogel forms, so that the obtained radiation refrigeration material has good mechanical property and radiation refrigeration property, and particularly has good reflection effect on the wavelength of 8-13 mu m.
According to some embodiments of the invention, the radiation refrigeration material comprises the following preparation raw materials in percentage by mass:
according to some embodiments of the invention, the acid comprises about 0.01% of the preparation feedstock.
The invention realizes the control of toughness, strength, heat resistance and cycle compressibility of the material in the later stage by adjusting the dosage of each preparation raw material.
According to some preferred embodiments of the present invention, the radiation refrigeration material is prepared from the following raw materials in percentage by mass:
according to some further preferred embodiments of the present invention, the radiation refrigeration material comprises, in mass percent, raw materials for preparation comprising:
according to some embodiments of the invention, the silicate is at least one of methyl orthosilicate (CAS: 681-84-5), ethyl orthosilicate (CAS: 78-10-4), isopropyl orthosilicate (CAS: 1992-48-9), or butyl orthosilicate (CAS: 4766-57-8).
The silicate compound rapidly undergoes sol-gel reaction, so that the reaction time is greatly shortened.
According to some embodiments of the invention, the silicate is ethyl orthosilicate.
According to some embodiments of the invention, the alkylalkoxysilane is at least one of methyltrimethoxysilane (CAS: 1185-55-3), dimethyldimethoxysilane (CAS: 1112-39-6), methyltriethoxysilane (CAS: 2031-67-6), dimethyldiethoxysilane (CAS: 78-62-6), ethyltrimethylsilane (CAS: 3439-38-1), vinyltriethoxysilane (CAS: 78-08-0), propyltrimethoxysilane (CAS: 1067-25-0), or propyltriethoxysilane (CAS: 2550-02-9).
The alkyl alkoxy silane forms a hydrophobic structure on the surface of the aerogel, so that the surface of the pore structure of the aerogel is fully distributed with the hydrophobic groups.
According to some embodiments of the invention, the alkylalkoxysilane is methyltrimethoxysilane.
According to some embodiments of the invention, the acid is at least one of phosphoric acid, sulfuric acid, hydrogen chloride, hydrogen bromide, and hydrogen iodide.
The acid catalyst is selected, which is favorable for rapidly improving the hydrolysis of silicate, thereby improving the sol-gel reaction of the system.
According to some embodiments of the invention, the acid is phosphoric acid.
According to some embodiments of the invention, the daytime radiation cooling power of the radiation refrigeration material is more than or equal to 45W/m 2 ；
For example, 45 to 140W/m 2 Specifically, 120W/m 2 、110W/m 2 、100W/m 2 、80W/m 2 Or 56W/m 2 。
According to some embodiments of the invention, the solar reflectance of the radiant refrigerant material is greater than or equal to 80%;
for example, 80 to 95%, specifically 92%, 91%, 82%, 90% or 85%. According to some embodiments of the invention, the atmospheric window emissivity of the radiant refrigerant material is greater than or equal to 92%, such as 93%, 94%, or 97%.
According to some embodiments of the invention, the radiation refrigerating material may bring about an ambient temperature difference of 1.2 ℃ or more, for example, 6 ℃, 4 ℃, 3 ℃, 1.5 ℃, 5.5 ℃ or 2 ℃.
According to some embodiments of the invention, the radiation refrigerant material has a compressive strength of 60kPa or more, such as 100kPa, 110kPa or 70kPa.
According to some embodiments of the invention, the radiation refrigeration material can withstand high temperatures of greater than or equal to 800 ℃, and the specific withstand temperature can be 1200 ℃, 1000 ℃, or 850 ℃.
According to some embodiments of the invention, the radiant refrigerant material is tolerant of more than or equal to 300 cycles of compression, such as in particular 400 or 1000 cycles.
According to some embodiments of the invention, the radiant refrigerant material is a silica alumina fiber aerogel.
According to some embodiments of the invention, the fiber diameter of the radiation refrigerating material is between 75 and 110nm, for example, it may be particularly 80nm or 110nm.
The second aspect of the present invention provides a method for preparing the above radiation refrigeration material, comprising the steps of:
s1, mixing and dispersing the preparation raw materials of the radiation refrigeration material to prepare precursor gel; s2, blowing and spinning the precursor gel and sintering the precursor gel.
According to one of the technical schemes of the preparation method, the preparation method at least has the following beneficial effects:
the invention prepares sol gel by silicate and alkyl alkoxy silane, and under the condition of acid catalysis, the silicate and the alkyl alkoxy silane form a gel skeleton to fix alumina; thus, aerogel materials with excellent properties are produced.
The silicate reacts slowly with acid as catalyst; the production is easy to control. Meanwhile, silicate esters can stabilize silanol groups with large activity under acidic conditions, thereby improving storage stability.
The invention forms Silica Alumina Fiber Aerogel (SAFAs) by sol-gel; forming a fiber network through a blow spinning process; due to the scattered reflection and the selective emission of the fiber network, the material with high solar reflectivity and high atmospheric window emissivity is prepared. In addition, SAFAs have high compression fatigue resistance, strong fireproof performance and excellent heat insulation performance, are low in cost, and can realize large-scale radiation refrigeration.
According to some embodiments of the invention, the method of preparing the precursor gel comprises the steps of:
s01, mixing the silicate, the alkylalkoxysilane and the acid to prepare a first dispersion liquid;
s02, mixing the aluminum oxide with water to prepare second dispersion liquid;
s03, mixing the first dispersion liquid and the second dispersion liquid to prepare the precursor gel;
wherein; the steps S01 and S02 are only for convenience of expression, and there is no sequence between them.
According to some embodiments of the invention, in step S01, the mixing time is 2h to 4h.
According to some embodiments of the invention, in step S02, the mixing time is 4h to 6h.
According to some embodiments of the invention, in step S02, the temperature of the mixing is between 50 ℃ and 60 ℃.
According to some embodiments of the invention, in step S02, the mass ratio of the alumina to the water is 1-2: 1.
according to some embodiments of the invention, in step S03, the mixing is performed under vacuum.
According to some embodiments of the invention, the vacuum environment has a pressure of 0.01Pa to 0.1Pa.
According to some embodiments of the invention, in step S03, the mixing time is 0.2h to 1h.
According to some embodiments of the invention, the temperature of the blow spinning is 20 ℃ to 50 ℃; therefore, the problems of rapid gelation reaction caused by overhigh temperature and blockage of spinning pinholes caused by the rapid gelation reaction can be fully avoided; the problems of excessively low temperature, reduced sol-gel reaction progress, incapability of molding caused by the reaction can be avoided. That is, in the above temperature range, the operability of the production method can be significantly improved.
According to some embodiments of the invention, the temperature of the blow spinning is 25-35 ℃.
According to some embodiments of the invention, the injection speed of the blow spinning is 5mL/h to 20mL/h.
According to some embodiments of the invention, the injection speed of the blow spinning is 10mL/h.
According to some embodiments of the invention, the moisture content of the blow-spun yarn is 30% to 50%.
According to some embodiments of the invention, the moisture content of the blow-spun yarn is 40%.
According to some embodiments of the invention, the pressure of the blow spinning is 5MPa to 10MPa.
According to some preferred embodiments of the invention, the pressure of the blow spinning is 8MPa to 10MPa.
According to some embodiments of the invention, the sintering temperature is 800 ℃ to 1200 ℃.
Preferably, the sintering temperature is 900-1100 ℃. Within the above range, there is a sufficiently high temperature to form crystalline SiO 2 The emissivity of the obtained radiation refrigeration material to an atmospheric window is improved; at the same time, the temperature is not sufficient to produce SiO 2 And the porous structure of the obtained aerogel is ensured by melting.
According to some embodiments of the invention, the sintering temperature is 1000 ℃.
According to some embodiments of the invention, the sintering time period is 1-3 hours; preferably, the sintering is for a period of about 2 hours.
The third aspect of the invention provides application of the radiation refrigeration material in preparing a daytime radiation refrigeration material.
The fiber aerogel is adopted for realizing daily radiation refrigeration for the first time, and compared with the common fragile aerogel, the fiber aerogel has good toughness and can be repeatedly folded and compressed. In addition, the material utilizes a porous structure similar to a photonic crystal, and realizes high reflectivity of sunlight and high emissivity of an atmospheric window. The network porous structure of aerogel and fiber is combined, and excellent mechanical property and heat insulation property are realized.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 shows SEM test results of the material prepared in example 1 of the present invention.
FIG. 2 shows SEM test results of the material prepared in example 1 of the present invention.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
In the description of the present invention, the descriptions of the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Specific embodiments of the present invention are described in detail below.
Example 1
The embodiment is a radiation refrigeration material and a preparation method thereof. The specific preparation materials are shown in table 1.
The preparation method of the radiation refrigeration material in the embodiment comprises the following steps:
s1, preparing a precursor by a sol-gel method:
mixing and stirring silicate, alkyl alkoxy silane and acid for 3 hours (with the rotating speed of 2000 rpm) to obtain a dispersion liquid A;
dissolving aluminum oxide powder (particle size range of 50-100 nm) in water, stirring at 60deg.C (rotating speed 1000 rpm) for 5 hr to obtain dispersion B, wherein the mass ratio of aluminum oxide to water is about 1.5:5;
the dispersion B was added to the dispersion A, and the mixture was stirred under vacuum (rotation speed 800 rpm) for 0.5 hours to obtain a precursor gel.
S2, preparing fiber aerogel by blow spinning:
carrying out blow spinning process processing and forming on the precursor gel to obtain fibers;
wherein the technological parameters of the blow spinning process are as follows:
the injection speed is 10ml/h, the air pressure is 10MPa, the temperature is 25 ℃, and the humidity is 40%.
Sintering the fiber at 1000 ℃ for 2 hours to obtain the fiber.
Example 2
This embodiment is a radiation refrigeration material and a preparation method thereof, and is different from embodiment 1 in that:
specific preparation raw materials are different and are shown in table 1.
Example 3
The embodiment is a radiation refrigeration material and a preparation method thereof,
the difference from example 1 is that:
specific preparation raw materials are different and are shown in table 1.
Example 4
The embodiment is a radiation refrigeration material and a preparation method thereof.
The radiation refrigeration material preparation raw material in this example was the same as in example 1.
The difference between the preparation method of the radiation refrigeration material in this embodiment and embodiment 1 is that: the temperature in the blowing spinning process in the step S2 is 45 ℃.
Example 5
The embodiment is a radiation refrigeration material and a preparation method thereof.
The radiation refrigeration material preparation raw material in this example was the same as in example 1.
The difference between the preparation method of the radiation refrigeration material in this embodiment and embodiment 1 is that: the pressure intensity in the blowing spinning process in the step S2 is 5MPa.
Example 6
The embodiment is a radiation refrigeration material and a preparation method thereof.
The radiation refrigeration material preparation raw material in this example was the same as in example 1.
The difference between the preparation method of the radiation refrigeration material in this embodiment and embodiment 1 is that: the sintering temperature in step S2 was 1200 ℃.
Example 7
The embodiment is a radiation refrigeration material and a preparation method thereof.
The radiation refrigeration material preparation raw material in this example was the same as in example 1.
The difference between the preparation method of the radiation refrigeration material in this embodiment and embodiment 1 is that: the sintering temperature in step S2 was 800 ℃.
Table 1 composition (parts by weight) of the raw materials for preparation used in examples 1 to 3
| - | Silicate esters | Alkylalkoxysilane | Alumina oxide | Phosphoric acid |
| Example 1 | 22 | 7.99 | 70 | 0.01 |
| Example 2 | 25 | 7.99 | 67 | 0.01 |
| Example 3 | 25 | 4.99 | 70 | 0.01 |
In table 1, the silicate is tetraethyl orthosilicate (TEOS);
the alkylalkoxysilane is methyltrimethoxysilane (MTMS);
phosphoric acid, available from aladine, analytically pure, about 87 mass percent;
the D50 of alumina was about 50nm, available from Guangzhou New Metallurgical chemical Co.
Comparative example 1
The comparative example is a radiation refrigeration material and a preparation method thereof. The specific differences from example 1 are that:
excluding alumina.
Test case
The first aspect of the present test example tests the morphology of the radiation refrigeration material obtained in example 1, and the test results are shown in fig. 1 to 2. The result shows that the radiation refrigeration material provided by the invention is formed by winding fibrous materials, wherein the diameter of the fibers is between 0.5 and 1.5 mu m. The fibers are intertwined, pores exist among the fibers, the test example also counts the sizes of the pores (the maximum spanned size of the pores) in the visual field of fig. 2, the specific pore size is about 5 mu m (average value), and the pore sizes are in Gaussian distribution and have a certain rule, so that the obtained radiation refrigeration material has a structure similar to a photonic crystal.
The present test example also tested the performance of the radiant refrigerant materials produced in examples 1-7 and comparative example 1, wherein:
daytime radiant cooling power is carried out in accordance with the method in ANSI/ASHRAE Standard 138;
the emissivity of the air window is tested by adopting a reflectometer, and the infrared emissivity (the emissivity of the air window) of 7-14 mu m wavelength is specifically tested;
the reflectance (solar reflectance) of the sample for light in the 300-2500 nm band was measured using a UV-VIS-NIR spectrometer (integrating sphere).
Fiber diameter was read by electron microscopy and counting software (Nano measurement).
Thermocouples (VC 6801) were used to test the cooling effect (temperature difference) between day and night and calculate the average of the environmental temperature differences.
Compressive strength was carried out in accordance with the method provided in GB/T4740.
The heat resistance test method comprises the following steps: the material is kept at the corresponding temperature for 30min, and the change degree of the solar reflectivity of the material is within 2 percent.
Cyclic compressibility is carried out in accordance with the method provided in GB/T2423.1-2001.
The results of the performance test of the radiation refrigerating materials prepared in examples 1 to 7 of the present invention and comparative example 1 are shown in Table 2.
TABLE 2 Performance test results of the radiation refrigeration materials prepared in examples 1 to 7 and comparative example 1 of the present invention
As is clear from the results of Table 1, examples 1 to 7 of the present invention all obtained 45W/m or more 2 The reflectivity of the solar radiation cooling power is more than or equal to 80 percent, the average value of the environmental temperature difference is also more than or equal to 1.2 ℃, the average value is as high as 6 ℃ (average value in daytime and at night), wherein the temperature difference of the daytime condition can be as high as 8 ℃; in addition, the fiber has excellent heat resistance, compressive strength, cyclic compressibility and moderate fiber diameter. Thus, can bring significant technical advantages as a radiation refrigeration material.
If alumina is not included in the raw materials to be prepared (comparative example 1), there is a significant decrease in the overall performance in all aspects due to the inability to form a synergistic effect with other materials.
In addition, although all of the radiation refrigeration materials prepared in examples 1 to 7 can meet industrial use, the change of conditions in the preparation process also brings about the change of properties, in particular, compared with example 1:
the proportion of alumina used in example 2 was reduced, and therefore, the reflectance was lowered to some extent, and the heat resistance was deteriorated. In example 3, the proportion of alkylalkoxysilane used was reduced, resulting in a decrease in emissivity and an increase in brittleness of the material. In example 4, the blow spinning temperature was too high, the sol-gel process was accelerated, the fiber size was unstable, and the overall performance was reduced; in example 5, the blow spinning pressure was too low, the sol-gel process slowed down, the fiber size was unstable, and the overall performance was reduced;
in example 6, the sintering temperature is too high, amorphous silicon dioxide is subjected to melt crystallization, the reflectivity is subjected to unstable change, the compression resistance of the material is reduced, and the compression cycle stability is reduced; in example 7, the sintering temperature was too low, no two-phase fusion of silica and alumina occurred to form a sialyl phase, and the two-phase compatibility was poor, and the emissivity and emissivity were low.
In summary, the Silica Alumina Fiber Aerogel (SAFAs) synthesized by the sol-gel+blow spinning process of the present invention can be used as a radiation refrigerating material, and has a solar reflectance of up to 95% and a high atmospheric window emissivity of 97%, due to scattered reflection and selective emission of the fiber network. In field testing, SAFAs were maintained at 8℃or more below ambient temperature, theoretically yielding 133.1W/m 2 Is used for cooling power by daytime radiation. In addition, SAFAs have high compression fatigue resistance, strong fireproof performance and excellent heat insulation performance, are low in cost, and can realize large-scale radiation refrigeration.
While the embodiments of the present invention have been described in detail with reference to the specific embodiments, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (8)
1. A radiant refrigerant material characterized by: the radiation refrigeration material comprises the following preparation raw materials in parts by weight:
20-25 parts of silicate;
4.5-8 parts of alkyl alkoxy silane;
60-70 parts of aluminum oxide;
0.005-0.015 parts of acid;
the radiation refrigeration material is prepared by a preparation method comprising the following steps:
s1, mixing and dispersing the preparation raw materials of the radiation refrigeration material to prepare precursor gel;
s2, blowing and spinning the precursor gel and then sintering;
the temperature of the blowing spinning is 25-35 ℃;
the pressure of the blow spinning is 8-10 MPa;
the sintering temperature is 900-1100 ℃.
2. A radiant refrigerant material as set forth in claim 1 wherein: the silicate is at least one of methyl orthosilicate, ethyl orthosilicate, isopropyl orthosilicate or butyl orthosilicate.
3. A radiant refrigerant material as set forth in claim 1 wherein: the alkyl alkoxy silane is at least one of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, ethyl trimethyl silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane.
4. A radiant refrigerant material as set forth in claim 1 wherein: the acid is at least one of phosphoric acid, sulfuric acid, hydrogen chloride, hydrogen bromide and hydrogen iodide.
5. A radiant refrigerant material as set forth in claim 1 wherein: the humidity of the blow spinning is 30% -50%.
6. A radiant refrigerant material as set forth in claim 1 wherein: the injection speed of the blow spinning is 5 mL/h-20 mL/h.
7. A radiant refrigerant material as set forth in claim 1 wherein: the sintering time is 1-3 h.
8. Use of a radiant refrigerant material as defined in any one of claims 1 to 7 for the preparation of a diurnal radiant refrigerant material.
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