CN114806514A - Method for preparing discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material by adopting template method - Google Patents
Method for preparing discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material by adopting template method Download PDFInfo
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Abstract
A method for preparing a discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material by adopting a template method relates to the technical field of material science, in particular to a preparation method of a radiation refrigeration material. The invention aims to solve the problems that the preparation method of the radiation refrigeration material prepared by the prior art is not environment-friendly or the emission performance of an atmospheric window area is poor. The method is characterized in that: preparing a polymer mixed solution; molding to obtain a crude product of the radiation refrigeration material; and removing the pore-foaming agent to obtain the discontinuous scattering reinforced pore-sphere composite polymer-based radiation refrigeration material. The advantages are that: the reflectivity R of a solar spectrum (0.3-1 μm) can reach 68%, and compared with a single porous material, the emissivity is obviously improved in an atmospheric window wave band (8-13 μm); and the cooling effect at night can be as low as 5.8 ℃. The invention is mainly used for preparing the discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material.
Description
Technical Field
The invention relates to the technical field of material science, in particular to a preparation method of a radiation refrigeration material.
Background
The building energy consumption of China accounts for a large proportion of the total energy consumption of the whole society, wherein the air conditioner energy consumption accounts for 30-60% of the total energy consumption of the building. And the energy consumption for cooling in the global environment in 2050 years is expected to be 2 times of the current energy consumption, so that the research and development of a novel zero-carbon passive refrigeration technology for reducing the use of active preparation equipment of an air conditioner is vital to building energy conservation.
Radiation refrigeration has received wide attention as a novel passive refrigeration technology without energy consumption. The novel ideal daytime radiation refrigeration material radiates self heat into a huge outer space cold source through an atmospheric window (8-13 microns), does not need to consume any electric energy or heat energy, and has important significance for reducing refrigeration energy consumption and realizing zero-carbon environmental protection. The conventional radiation refrigeration material mainly has a multilayer structure, a metamaterial with a surface periodic structure, a randomly distributed particle structure and a porous structure. The porous structure material is a radiation refrigeration material with the best application and future commercialization prospect due to the advantages of good refrigeration effect, simple preparation method, low cost and large-scale preparation. However, for the existing porous material, the problems that the preparation method is not environment-friendly, the emissivity of the atmospheric window is not high and the like exist, so that the practical application of the porous material is limited.
China has disclosed a super-hydrophobic self-cleaning radiation cooling film and a preparation method thereof (application publication No. CN110483924A), and the method uses a phase inversion method to prepare a film with a micro-nano double porous structure. The organic solvents such as acetone and tetrahydrofuran used in the method are toxic and volatile, and are not environment-friendly.
China has disclosed a patent of ' a porous polydimethylsiloxane radiation refrigeration material and a preparation method thereof ' (application publication number: CN113072737A) ', which firstly synthesizes micron-sized NaCl pore-forming agents, and controls the distribution and the size of pores in the synthesized porous PDMS by controlling the size and the dosage of the micron-sized NaCl pore-forming agents, although the pores of the material can scatter the light in the solar spectrum wave band and isolate the heat exchange between a radiator and the surrounding environment, the emission performance of the material in the atmospheric window area is poor.
Disclosure of Invention
The invention aims to solve the problems that the preparation method of the radiation refrigeration material prepared by the prior art is not environment-friendly or the emission performance of an atmospheric window area is poor, and provides a method for preparing a discontinuous scattering reinforced pore-sphere composite polymer-based radiation refrigeration material by adopting a template method.
The method for preparing the discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material by adopting the template method is specifically completed according to the following steps:
firstly, preparing a polymer mixed solution: fully and uniformly mixing the polymer prepolymer and the curing agent, and vacuumizing in a vacuum machine to eliminate bubbles to prepare a polymer mixed solution; the volume ratio of the polymer prepolymer to the curing agent is 10 (1-6);
secondly, forming; uniformly mixing a pore-foaming agent and an inorganic microsphere material, then flatly paving the mixture in a container, uniformly pouring the polymer mixture obtained in the step one into the container, then placing the container in a vacuum machine for vacuumizing to eliminate bubbles, and finally performing curing molding to obtain a crude product of the radiation refrigeration material; the volume fraction of the pore-foaming agent in the crude product of the radiation refrigeration material is 30-60%; the volume fraction of the inorganic microsphere material in the crude product of the radiation refrigeration material is 6-20%;
thirdly, removing the pore-foaming agent: and soaking the crude product of the radiation refrigeration material in deionized water, heating to remove a pore-forming agent, and then putting the crude product of the radiation refrigeration material into an oven for drying to obtain the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material, wherein the thickness of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material is 400 mu m-5 mm.
The invention has the advantages that:
the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material prepared by the invention has a pore scatterer and a microsphere scatterer, wherein the pore scatterer has a strong Mie scattering effect and can strongly scatter light in a solar spectrum waveband, and pores in the pore scatterer can isolate the heat exchange between the scatterer and the surrounding environment. The microsphere scatterer can strongly scatter light in a solar spectrum wave band through a Mie scattering effect and can also strongly emit light in an atmospheric window wave band through a surface phonon polarization resonance effect, so that the daytime radiation refrigeration effect is realized.
Secondly, the reflectivity R of the solar spectrum (0.3-1 μm) of the prepared discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material can reach 68%, and compared with a single porous material (such as embodiment 3), the emissivity of the prepared discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material in an atmospheric window waveband (8-13 μm) is obviously improved; and the cooling effect at night can be as low as 5.8 ℃.
The discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material prepared by the invention has a single-layer film structure, and is simple in structure and good in stability.
The preparation method is simple to operate, low in cost, environment-friendly and capable of being prepared and applied in a large scale.
Drawings
FIG. 1 is a photograph of a discontinuous scattering enhanced hole-sphere composite polymer-based radiation refrigeration material obtained in example 1;
FIG. 2 is a graph of an atmospheric window area emissivity spectrum, in which A shows the atmospheric window area emissivity spectrum of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material prepared in example 1, B shows the atmospheric window area emissivity spectrum of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material prepared in example 2, and C shows the atmospheric window area emissivity spectrum of a pure porous material prepared in comparative example 1;
FIG. 3 is a spectrum of reflectance in the solar spectral region of the discontinuous scattering-enhanced pore-sphere composite polymer-based radiation refrigeration material obtained in example 1.
Detailed Description
The first embodiment is as follows: the embodiment is a method for preparing a discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material by adopting a template method, which is specifically completed by the following steps:
firstly, preparing a polymer mixed solution: fully and uniformly mixing the polymer prepolymer and the curing agent, and vacuumizing in a vacuum machine to eliminate bubbles to prepare a polymer mixed solution; the volume ratio of the polymer prepolymer to the curing agent is 10 (1-6);
secondly, forming; uniformly mixing a pore-foaming agent and an inorganic microsphere material, then flatly paving the mixture in a container, uniformly pouring the polymer mixture obtained in the step one into the container, then placing the container in a vacuum machine for vacuumizing to eliminate bubbles, and finally performing curing molding to obtain a crude product of the radiation refrigeration material; the volume fraction of the pore-foaming agent in the crude product of the radiation refrigeration material is 30-60%; the volume fraction of the inorganic microsphere material in the crude product of the radiation refrigeration material is 6-20%;
thirdly, removing the pore-foaming agent: and soaking the crude product of the radiation refrigeration material in deionized water, heating to remove a pore-forming agent, and then putting the crude product of the radiation refrigeration material into an oven for drying to obtain the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material, wherein the thickness of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material is 400 mu m-5 mm.
The second embodiment is as follows: the present embodiment differs from the first embodiment in that: in the step one, the polymer prepolymer is one of epoxy resin prepolymer, polyester resin prepolymer, polyacrylate resin prepolymer, polyamide resin prepolymer, polyurethane resin prepolymer, polyolefin resin prepolymer, fluororesin prepolymer or silicone resin prepolymer. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: in the first step, the curing agent is one or more of benzoyl peroxide, azodiisobutyronitrile, methyl ethyl ketone peroxide and triethylene diamine. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: in the first step, the vacuum is pumped in a vacuum machine until the vacuum degree is 0.02MPa to 0.04MPa, and bubbles are eliminated for 0.8h to 1.5h under the vacuum degree of 0.02MPa to 0.04 MPa. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: in the second step, the pore-forming agent is one or two of NaCl and sugar. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: in the second step, the inorganic microsphere material is SiO 2 Powder, BaSO 4 Powder, CaCO 3 Powder, MgO powder, Al 2 O 3 Powder, Si 3 N 4 One or more of powder, titanium dioxide, talcum powder, aluminum silicate powder and ceramic powder, and the particle size of the inorganic microsphere material is 0.4-2 microns. The rest is the same as the first to fifth embodiments.
The seventh concrete implementation mode: the difference between this embodiment and one of the first to sixth embodiments is: and step two, the vacuum pump is arranged in a vacuum machine for vacuum pumping until the vacuum degree is 0.02MPa to 0.04MPa, and bubbles are eliminated for 0.8h to 1.5h under the vacuum degree of 0.02MPa to 0.04 MPa. The rest is the same as the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: and in the second step, curing is carried out at the temperature of 80-120 ℃. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: and step three, soaking the crude product of the radiation refrigeration material in deionized water, and heating for 2-8 h at the temperature of 40-80 ℃. The others are the same as the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and the first to ninth embodiments is: and drying for 0.5-2 h at the temperature of 50-100 ℃ in the third step. The rest is the same as the first to ninth embodiments.
The invention is not limited to the above embodiments, and one or a combination of several embodiments may also achieve the object of the invention.
The following experiments are adopted to verify the effect of the invention:
example 1: the method for preparing the discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material by adopting the template method is specifically completed according to the following steps:
firstly, preparing a polymer mixed solution: fully and uniformly mixing the polymer prepolymer and the curing agent, vacuumizing in a vacuum machine until the vacuum degree is 0.02MPa, and eliminating bubbles for 1h under the vacuum degree of 0.02MPa to prepare a polymer mixed solution; the volume ratio of the polymer prepolymer to the curing agent is 10: 1;
secondly, forming; uniformly mixing a pore-foaming agent and an inorganic microsphere material, paving the mixture in a container, uniformly pouring the polymer mixed solution obtained in the step one into the container, then placing the container in a vacuum machine for vacuumizing until the vacuum degree is 0.02MPa, eliminating bubbles for 1 hour under the vacuum degree of 0.02MPa, and finally performing curing molding at the temperature of 100 ℃ to obtain a crude product of the radiation refrigeration material; the volume fraction of the pore-foaming agent in the crude product of the radiation refrigeration material is 50 percent; the volume fraction of the inorganic microsphere material in the crude product of the radiation refrigeration material is 13 percent;
thirdly, removing the pore-foaming agent: and (3) soaking the crude radiation refrigeration material in deionized water, heating at 80 ℃ for 8h to remove a pore-forming agent, then putting the radiation refrigeration material into a drying oven, and drying at 80 ℃ for 1h to obtain the discontinuous scattering enhanced pore-sphere composite polymer-based radiation refrigeration material, wherein the thickness of the discontinuous scattering enhanced pore-sphere composite polymer-based radiation refrigeration material is 2.5 mm.
In the first step of this embodiment, the polymer prepolymer is a PDMS prepolymer.
In the first step of this embodiment, the curing agent is benzoyl peroxide.
In the second step of this embodiment, the pore-forming agent is sugar.
In the second step of this embodiment, the inorganic microsphere material is SiO 2 Powder, and the average grain diameter of the inorganic microsphere material is 4 mu m.
Fig. 1 is a photograph of a real object of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material obtained in example 1, and the average pore diameter of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material obtained in example 1 is about 280 μm by performing pore amplification analysis on the photograph.
The reflectivity of the discontinuous scattering-reinforced hole-sphere composite polymer-based radiation refrigeration material obtained in example 1 is detected by a fiber optic spectrometer (CHS-5000/200 μm), and the result is shown in fig. 3, fig. 3 is a solar spectrum area reflectivity spectrogram of the discontinuous scattering-reinforced hole-sphere composite polymer-based radiation refrigeration material obtained in example 1, and it can be seen from fig. 3 that the reflectivity R can reach 68% in the solar spectrum (0.3 μm to 1 μm).
The thermocouple (VC6801) is adopted to test the cooling effect of the discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material obtained in the embodiment 1, and the cooling effect at night can be as low as 5.8 ℃.
Example 2: the method for preparing the discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material by adopting the template method is specifically completed according to the following steps:
firstly, preparing a polymer mixed solution: fully and uniformly mixing the polymer prepolymer and the curing agent, vacuumizing in a vacuum machine until the vacuum degree is 0.02MPa, and eliminating bubbles for 1h under the vacuum degree of 0.02MPa to prepare a polymer mixed solution; the volume ratio of the polymer prepolymer to the curing agent is 10: 1;
secondly, forming; uniformly mixing a pore-foaming agent and an inorganic microsphere material, then spreading the mixture in a container, uniformly pouring the polymer mixed solution obtained in the step one in the container, then placing the container in a vacuum machine for vacuumizing until the vacuum degree is 0.02MPa, eliminating bubbles for 1h under the vacuum degree of 0.02MPa, and finally performing curing molding at the temperature of 100 ℃ to obtain a crude product of the radiation refrigeration material; the volume fraction of the pore-foaming agent in the crude product of the radiation refrigeration material is 50 percent; the volume fraction of the inorganic microsphere material in the crude product of the radiation refrigeration material is 10 percent;
thirdly, removing the pore-foaming agent: and soaking the crude product of the radiation refrigeration material in deionized water, heating at 80 ℃ for 8h to remove a pore-forming agent, then putting the crude product into a drying oven, and drying at 80 ℃ for 1h to obtain the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material, wherein the thickness of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material is 2.5 mm.
In the first step of this embodiment, the polymer prepolymer is a PDMS prepolymer.
In the first step of this embodiment, the curing agent is benzoyl peroxide.
In the second step of this embodiment, the pore-forming agent is sugar.
In the second step of this embodiment, the inorganic microsphere material is SiO 2 Powder, and the average grain diameter of the inorganic microsphere material is 4 mu m.
Comparative example 1: comparison without adding inorganic microsphere material:
firstly, preparing a polymer mixed solution: fully and uniformly mixing the polymer prepolymer and the curing agent, vacuumizing in a vacuum machine until the vacuum degree is 0.02MPa, and eliminating bubbles for 1h under the vacuum degree of 0.02MPa to prepare a polymer mixed solution; the volume ratio of the polymer prepolymer to the curing agent is 10: 1;
secondly, forming; firstly, flatly paving a pore-foaming agent in a container, uniformly pouring the polymer mixed solution obtained in the step one into the container, then placing the container in a vacuum machine for vacuumizing until the vacuum degree is 0.02MPa, eliminating bubbles for 1h under the vacuum degree of 0.02MPa, and finally carrying out curing molding at the temperature of 100 ℃ to obtain a crude product of the radiation refrigeration material; the volume fraction of the pore-foaming agent in the crude product of the radiation refrigeration material is 50 percent;
thirdly, removing the pore-foaming agent: and soaking the crude product of the radiation refrigeration material in deionized water, heating at 80 ℃ for 8h to remove a pore-forming agent, then putting the crude product into a drying oven, and drying at 80 ℃ for 1h to obtain the pure porous material, wherein the thickness of the pure porous material is 2.5 mm.
In the first step of this embodiment, the polymer prepolymer is a PDMS prepolymer.
In the first step of this embodiment, the curing agent is benzoyl peroxide.
In the second step of this embodiment, the pore-forming agent is sugar.
The emissivity of the solar spectrum region of the discontinuous scattering reinforced pore-sphere composite polymer-based radiation refrigeration materials prepared in examples 1 and 2 and the emissivity of the pure porous material prepared in comparative example 1 were measured by a fourier spectrometer, and the results are shown in fig. 2; fig. 2 is a graph of an atmospheric window area emissivity spectrum, in which a shows the atmospheric window area emissivity spectrum of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material prepared in example 1, B shows the atmospheric window area emissivity spectrum of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material prepared in example 2, and C shows the atmospheric window area emissivity spectrum of the pure porous material prepared in comparative example 1, and compared with comparative example 1, the emissivity of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material prepared in the invention is significantly improved in an atmospheric window waveband (8 μm-13 μm).
Claims (10)
1. The method for preparing the discontinuous scattering reinforced hole-sphere composite polymer-based radiation refrigeration material by adopting the template method is characterized by comprising the following steps of:
firstly, preparing a polymer mixed solution: fully and uniformly mixing the polymer prepolymer and the curing agent, and vacuumizing in a vacuum machine to eliminate bubbles to prepare a polymer mixed solution; the volume ratio of the polymer prepolymer to the curing agent is 10 (1-6);
secondly, forming; uniformly mixing a pore-foaming agent and an inorganic microsphere material, then flatly paving the mixture in a container, uniformly pouring the polymer mixture obtained in the step one into the container, then placing the container in a vacuum machine for vacuumizing to eliminate bubbles, and finally performing curing molding to obtain a crude product of the radiation refrigeration material; the volume fraction of the pore-foaming agent in the crude product of the radiation refrigeration material is 30-60%; the volume fraction of the inorganic microsphere material in the crude product of the radiation refrigeration material is 6-20%;
thirdly, removing the pore-foaming agent: and soaking the crude product of the radiation refrigeration material in deionized water, heating to remove a pore-forming agent, and then putting the crude product of the radiation refrigeration material into an oven for drying to obtain the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material, wherein the thickness of the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material is 400 mu m-5 mm.
2. The method for preparing a discontinuous scattering-reinforced hole-sphere composite polymer-based radiation refrigeration material according to claim 1, wherein in the step one, the polymer prepolymer is one of epoxy resin prepolymer, polyester resin prepolymer, polyacrylate resin prepolymer, polyamide resin prepolymer, polyurethane resin prepolymer, polyolefin resin prepolymer, fluororesin prepolymer or silicone resin prepolymer.
3. The method for preparing the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material by adopting the template method as claimed in claim 2, wherein the curing agent in the step one is one or more of benzoyl peroxide, azobisisobutyronitrile, methyl ethyl ketone peroxide and triethylene diamine.
4. The method for preparing the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material by adopting the template method as claimed in claim 3, wherein in the step one, the vacuum machine is vacuumized until the vacuum degree is 0.02MPa to 0.04MPa, and bubbles are eliminated for 0.8h to 1.5h under the vacuum degree of 0.02MPa to 0.04 MPa.
5. The method for preparing the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material by adopting the template method according to claim 1 or 4, wherein the pore-forming agent in the second step is one or both of NaCl and sugar.
6. The method for preparing the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material by adopting the template method as claimed in claim 5, wherein the inorganic microsphere material in the second step is SiO 2 Powder, BaSO 4 Powder, CaCO 3 Powder, MgO powder, Al 2 O 3 Powder, Si 3 N 4 One or more of powder, titanium dioxide, talcum powder, aluminum silicate powder and ceramic powder, and the particle size of the inorganic microsphere material is 0.4-2 mu mm。
7. The method for preparing the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material by adopting the template method according to claim 6, wherein in the second step, the material is placed in a vacuum machine for vacuum pumping until the vacuum degree is 0.02MPa to 0.04MPa, and bubbles are eliminated for 0.8h to 1.5h under the vacuum degree of 0.02MPa to 0.04 MPa.
8. The method for preparing the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material by adopting the template method as claimed in claim 7, wherein the curing is carried out at a temperature of 80-120 ℃ in the second step.
9. The method for preparing the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material by adopting the template method according to claim 1 or 8, characterized in that in the third step, the crude product of the radiation refrigeration material is immersed in deionized water and heated at the temperature of 40-80 ℃ for 2-8 h.
10. The method for preparing the discontinuous scattering-reinforced pore-sphere composite polymer-based radiation refrigeration material by adopting the template method according to claim 9, wherein the drying is carried out at the temperature of 50-100 ℃ for 0.5-2 h in the third step.
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