CN114181666A - Modified expanded perlite-based phase-change composite material and preparation method and application thereof - Google Patents
Modified expanded perlite-based phase-change composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a modified expanded perlite-based phase-change material and a preparation method and application thereof. The invention relates to a preparation method of a modified expanded perlite-based phase change composite material, which comprises the following steps: s1: dissolving polyvinyl alcohol in water to form a polyvinyl alcohol aqueous solution; s2: soaking a polyvinyl alcohol aqueous solution into the macropores of the expanded perlite by a vacuum impregnation method, and freeze-drying to prepare modified expanded perlite with high porosity and graded porosity; s3: the modified expanded perlite adsorbs the phase change material by a vacuum impregnation method to prepare the modified expanded perlite-based phase change composite material. According to the invention, the aerogel preparation technology is organically combined with the porous mineral material, the constructed high-porosity graded porous modified expanded perlite can adsorb a large amount of phase change materials and effectively prevent the phase change materials from leaking, and meanwhile, the constructed modified expanded perlite based phase change thermal protection building material has excellent heat insulation performance.
Description
Technical Field
The invention relates to the technical field of phase-change materials, in particular to a modified expanded perlite-based phase-change composite material and a preparation method and application thereof.
Background
In recent years, energy crisis and environmental issues have received increasing attention from countries around the world. The construction industry not only consumes a large amount of energy, but also causes many environmental problems, such as excessive carbon dioxide emissions. In most countries, building energy consumption accounts for about 30% of total energy consumption, and even higher. Among all energy consumption of buildings, heating and air-conditioning cooling occupy most of the energy consumption, and therefore, reducing the energy consumption of heating and cooling is one of the main strategies to solve the current predicaments of human beings. Generally, the wall heat-insulating material is considered as an important factor influencing the energy conservation of buildings, and the selection of the high-efficiency energy-saving wall heat-insulating material is an important way for realizing the energy conservation of buildings. The organic phase change material has the characteristics of low heat conductivity coefficient and high latent heat, and has great potential in thermal protection application. The phase-change material is combined with the building material, so that heat transfer from the outside to the inside in summer can be effectively reduced, and the refrigeration energy consumption of an air conditioner is relieved; meanwhile, heat dissipation from indoor to outdoor in winter is reduced, and a heat preservation effect is achieved. The method can effectively relieve the energy consumption and the environmental problems caused by the energy consumption, and has wide application prospect.
However, organic phase change materials are prone to leakage during solid-liquid conversion, and application thereof is severely limited. Currently, combining organic phase change materials with porous support matrices is an effective leakage prevention strategy. However, porous carbon substrates such as graphene, carbon nanotubes, and expanded graphite are not conducive to thermal protection of buildings due to their high thermal conductivity. Porous minerals such as expanded vermiculite, diatomaceous earth and expanded perlite, although having low thermal conductivity, have limited their application due to the difficulty of maintaining high phase change material loadings for long periods of time due to the large pore effect.
Disclosure of Invention
The invention aims to provide a modified expanded perlite-based phase change composite material, a preparation method and application thereof, aiming at the defects in the prior art.
The invention relates to a preparation method of a modified expanded perlite-based phase change composite material, which comprises the following steps:
s1: dissolving polyvinyl alcohol in water to form a polyvinyl alcohol aqueous solution;
s2: soaking a polyvinyl alcohol aqueous solution into the macropores of the expanded perlite by a vacuum impregnation method, and freeze-drying to prepare modified expanded perlite with high porosity and graded porosity;
s3: the modified expanded perlite adsorbs the phase change material by a vacuum impregnation method to prepare the modified expanded perlite-based phase change composite material.
Further, in step S1, the mass concentration of the polyvinyl alcohol aqueous solution is 3 wt.% to 6 wt.%.
Further, in step S1, the polyvinyl alcohol is dissolved in water, the water bath heating temperature is 80-95 ℃, the stirring speed is 200-600 r/min, and the stirring time is 30-120 min.
Further, in step S2, the size fraction of the expanded perlite is 0.5 to 4mm, and the mass ratio of the polyvinyl alcohol aqueous solution to the expanded perlite is 10 to 30: 1.
further, in step S2, the vacuum impregnation process includes: firstly, placing the expanded perlite in a vacuum impregnation device, vacuumizing for 10-30 min under the condition that the vacuum degree is less than-0.90 MPa, then injecting a polyvinyl alcohol aqueous solution, and continuously vacuumizing for 30-60 min.
Further, in step S3, the phase change material is paraffin, and the mass ratio of the modified expanded perlite to the phase change material is 20-35: 65-80.
Further, the vacuum impregnation process in step S3 is: the modified expanded perlite is firstly placed in a vacuum impregnation device, and is vacuumized for 10-30 min under the conditions that the vacuum degree is less than minus 0.90MPa and the room temperature, then the phase-change material is added, and the vacuum is continuously vacuumized for 30-60 min at the temperature of 50-70 ℃ and the vacuum degree is less than minus 0.90 MPa.
A modified expanded perlite-based phase-change composite material is prepared by adopting the preparation method.
A phase change thermal protection building material comprises the modified expanded perlite base phase change composite material.
The preparation method of the phase-change thermal protection building material comprises the steps of uniformly mixing the modified expanded perlite base phase-change composite material and an inorganic binder, forming, demoulding and maintaining to obtain the modified expanded perlite base phase-change thermal protection building material.
Further, the inorganic binder is water glass, and the mass ratio of the modified expanded pearl-based phase change composite material to the water glass is (4-6): 4 to 6.
The invention adsorbs polyvinyl alcohol (PVA) aqueous solution into a macroporous structure of expanded perlite by a vacuum impregnation method, freeze-solidifies the aqueous solution, freeze-dries the aqueous solution to construct a high-porosity graded porous material, further encapsulates an organic phase-change material, and is bonded, pressed and formed by an inorganic bonding material to prepare the high-performance modified expanded perlite-based phase-change thermal protection building material.
The modified expanded perlite-based phase change composite material constructed by the invention solves the problems of poor latent heat storage capacity and poor leakage prevention capacity of expanded perlite and low thermal protection performance, and has the advantages of simple preparation process, easy control, convenient industrial production and important application prospect in the field of building thermal protection.
According to the invention, the technology for preparing the aerogel is organically combined with the porous mineral expanded perlite, the expanded perlite can provide rigid framework support for the aerogel, the aerogel can regulate and control the pore structure of the expanded perlite, the modified organic expanded perlite can keep the high porosity of the aerogel and the expanded perlite, the phase-change material can be effectively adsorbed, and the phase-change material is prevented from leaking.
The loading capacity of the modified expanded perlite-based phase change composite material constructed by the invention reaches 73.3%, the loading capacity of the unmodified expanded perlite-based phase change composite material is 57.8%, the loading capacity is greatly improved, and the leakage-proof capability is improved. The time required for the modified expanded perlite base phase-change heat protection plate constructed by the invention to reach the target temperature (40 ℃) is 110min, the time required for the unmodified expanded perlite base phase-change heat protection plate to reach the target temperature (40 ℃) is only 65min, the time required for the unmodified expanded perlite base phase-change heat protection plate to reach the target temperature (40 ℃) is only 28min, and the heat insulation performance is greatly improved. When ambient temperature reduces, the heat that modified expanded perlite base phase transition heat guard plate can release the storage plays the heat preservation effect, and the modified expanded perlite base phase transition heat guard plate that this patent was constructed has superior thermal-insulated heat preservation performance.
The thermal protection building material can effectively delay the rise of the surface temperature of the building material under the action of environmental heat flow, inhibit the heat flow from moving from the outdoor to the indoor, delay the rise of the indoor temperature, reduce the use of air conditioners in summer and reduce the refrigeration energy consumption of the air conditioners. In winter, the heat protection building material can absorb indoor heating heat to prevent the heat from being rapidly transferred outwards, and after the heating equipment is closed, the heat absorbed by the heat protection building material can be diffused indoors to delay the reduction of indoor temperature and reduce heating time, so that heating energy consumption is reduced.
Drawings
FIGS. 1a & b are scanning electron microscope images of Expanded Perlite (EP) and its local magnification;
FIGS. 1c & d are scanning electron microscope images of 3 wt.% polyvinyl alcohol solution modified expanded perlite (EPPVA3) and its local magnification;
FIGS. 1e & f are scanning electron microscope images of 4 wt.% polyvinyl alcohol solution modified expanded perlite (EPPVA4) and its local magnification;
FIGS. 1g & h are scanning electron microscope images of 5 wt.% polyvinyl alcohol solution modified expanded perlite (EPPVA5) and its local magnification;
FIGS. 1i & j are scanning electron microscope images of 6 wt.% polyvinyl alcohol solution modified expanded perlite (EPPVA6) and its local magnification;
FIG. 2a is a mercury intrusion curve of the expanded perlite EP and the modified expanded perlite EPPVA3, EPPVA4, EPPVA5 and EPPVA6 prepared in examples 1-4;
FIG. 2b is a mercury intrusion pore size distribution curve of the expanded perlite EP and the modified expanded perlite EPPVA3, EPPVA4, EPPVA5 and EPPVA6 prepared in examples 1-4;
FIG. 2c is a nitrogen adsorption and desorption curve of the expanded perlite EP and the modified expanded perlite EPPVA3, EPPVA4, EPPVA5 and EPPVA6 prepared in examples 1-4;
FIG. 2d is a BJH pore size distribution curve of the expanded perlite EP and the modified expanded perlite EPPVA3, EPPVA4, EPPVA5 and EPPVA6 prepared in examples 1-4;
FIG. 3a is a DSC curve of the modified expanded perlite based phase change composite materials P/EPPVA3, P/EPPVA4, P/EPPVA5 and P/EPPVA6 prepared in examples 1-4 and the unmodified expanded perlite phase change composite material P/EP prepared in comparative example 1;
FIG. 3b is a histogram of enthalpy corresponding to the modified expanded perlite based phase change composite materials P/EPPVA3, P/EPPVA4, P/EPPVA5 and P/EPPVA6 prepared in examples 1-4 and the unmodified expanded perlite phase change composite material P/EP prepared in comparative example 1;
FIG. 4 is a digital photograph of a modified expanded perlite base phase change thermal protection building material (P/EPP/B), an unmodified expanded perlite base phase change thermal protection building material (P/EP/B) and an expanded perlite thermal protection building material (EP/B) prepared by the technical solutions of example 5 and comparative examples 2-3;
FIG. 5 is a temperature-time distribution curve of P/EPP/B, P/EP/B and EP/B for thermal protection building materials prepared by the technical schemes of example 5 and comparative examples 2-3.
Detailed Description
The following are specific examples of the present invention, comparative examples, and technical solutions of the present invention are further described with reference to the drawings, but the present invention is not limited to these examples.
Example 1:
this example prepares a modified expanded perlite based phase change composite material P/EPPVA 5.
(1) 5g of polyvinyl alcohol (PVA) and 95mL of deionized water were weighed into a beaker and mixed and stirred at 95 ℃ for 60min to obtain a5 wt.% aqueous solution of polyvinyl alcohol (PVA 5).
(2) 2g of Expanded Perlite (EP) is weighed into a suction flask and evacuated for 10 min. Then 60mL of PVA aqueous solution is added through a separating funnel, the vacuum pumping is continued for 30min, and the redundant PVA solution is removed through suction filtration.
(3) The PVA modified expanded perlite is frozen in the lower layer of a refrigerator for 12h and then is placed in a freeze dryer for drying for 24h, and the graded porous modified expanded perlite (EPPVA5) with high porosity is prepared.
(4) 6g of modified expanded perlite is weighed into a suction flask and vacuumized for 10min at room temperature. Weighing 24g of paraffin (P) and placing the paraffin (P) in a separating funnel on a filter flask, opening the separating funnel to transfer the paraffin into the filter flask, then vacuumizing for 30min under the condition of 60 ℃ water bath, carrying out oven heat filtration for 24h at 60 ℃, and replacing filter paper for multiple times to prepare the modified expanded perlite-based phase-change composite material (P/EPPVA 5).
Example 2:
this example prepares a modified expanded perlite based phase change composite material P/EPPVA 3.
3g of polyvinyl alcohol (PVA) and 97mL of deionized water were weighed into a beaker and mixed and stirred at 95 ℃ for 60min to obtain a3 wt.% aqueous solution of polyvinyl alcohol (PVA 3). Steps (2), (3) and (4) are the same as those in example 1.
Example 3:
this example prepares a modified expanded perlite based phase change composite material P/EPPVA 4.
4g of polyvinyl alcohol (PVA) and 96mL of deionized water were weighed into a beaker and mixed and stirred at 95 ℃ for 60min to give a4 wt.% aqueous solution of polyvinyl alcohol (PVA 4). Steps (2), (3) and (4) are the same as those in example 1.
Example 4:
this example prepares a modified expanded perlite based phase change composite material P/EPPVA 6.
6g of polyvinyl alcohol (PVA) and 94mL of deionized water were weighed into a beaker and mixed and stirred at 95 ℃ for 60min to give a6 wt.% aqueous solution of polyvinyl alcohol (PVA 6). Steps (2), (3) and (4) are the same as those in example 1.
Example 5:
the modified expanded perlite base phase change thermal protection building material P/EPP/B is prepared by the embodiment.
Weighing 65g of modified expanded perlite phase change composite material (P/EPPVA5) and 65g of water glass, uniformly mixing and stirring, placing the mixture in a mould, pressing into a 100X 60X 20mm plate, placing in an oven with the temperature controlled at 60 +/-1 ℃ and curing for 24h to obtain the modified expanded perlite base phase change thermal protection building material (P/EPP/B).
Comparative example 1:
compared with the embodiment 1, the expanded perlite-based phase change composite material P/EP prepared by the comparative example has no structural regulation on the expanded perlite.
6g of expanded perlite raw ore is weighed into a suction flask and vacuumized for 10min at room temperature. Weighing 24g of paraffin (P) and placing the paraffin (P) in a separating funnel on a filter flask, opening the separating funnel to transfer the paraffin into the filter flask, then vacuumizing for 30min under the condition of 60 ℃ water bath, carrying out hot filtration for 24h in a 60 ℃ oven, and replacing filter paper for multiple times to prepare the expanded perlite-based phase-change composite material (P/EP).
Comparative example 2:
the difference between the P/EP/B prepared by the comparative example and the example 5 is that: the phase-change thermal protection building material is prepared from the unmodified expanded perlite base phase-change composite material.
Weighing 65g of expanded perlite base phase change composite material (P/EP) and 65g of water glass, uniformly mixing and stirring, placing the mixture in a mold, pressing into a 100 x 60 x 20mm plate, placing in an oven with the temperature controlled at 60 ℃ and maintaining for 24h to obtain the expanded perlite base phase change thermal protection building material (P/EP/B).
Comparative example 3:
this comparative example prepares an expanded perlite thermal protective building material EP/B, which differs from example 5 in that: the phase-change thermal protection building material is prepared by using expanded perlite raw ore. Weighing 30g of Expanded Perlite (EP) and 100g of water glass, uniformly mixing and stirring, placing the mixture in a mould to be pressed into a 100X 60X 20mm plate, and placing the plate in an oven with the temperature controlled at 60 ℃ to be maintained for 24 hours to obtain the expanded perlite heat protection plate (EP/B).
Referring to the attached figure 1, it is a scanning electron microscope photograph of the materials prepared in the technical schemes of examples 1-4 and comparative example 1: (a) the raw Expanded Perlite (EP), the modified expanded perlite (EPPVA3), the modified expanded perlite (EPPVA4), the modified expanded perlite (EPPVA5) and the modified expanded perlite (EPPVA6) are respectively used as the raw (EP), (e), (g) and (i); (b) the (d), (f), (h) and (j) are expanded perlite raw ore (EP), modified expanded perlite (EPPVA3), modified expanded perlite (EPPVA4), modified expanded perlite (EPPVA5) and modified expanded perlite (EPPVA6) which are partially enlarged. As can be seen from (a) and (b), the expanded perlite raw ore has a macroporous structure of 20-200 μm. As can be seen from (c) - (j), as the concentration of PVA increases, the PVA forms a gradually increased small pore structure in EP, and the EP primary macropores gradually decrease. The pore structure of the expanded perlite can be regulated by controlling the concentration of PVA to achieve the desired pore size. The PVA solutions with the concentrations of 3 wt.%, 4 wt.%, 5 wt.% and 6 wt.% are prepared, and comparison shows that as the concentration of the PVA increases, the micron-sized macropores gradually decrease, the mesoporous aperture increases, and the mesoporous pore volume increases, so that the phase-change material is favorably adsorbed and stabilized.
Referring to the attached FIG. 2 and Table 1, it is a graph showing the pore structure change of the materials prepared by the technical schemes of examples 1-4 and comparative example 1: (a) - (d) mercury intrusion curves, mercury intrusion pore size distributions, nitrogen sorption desorption curves and BJH pore size distributions of EP, EPPVA3, EPPVA4, EPPVA5 and EPPVA6, respectively. The expanded perlite raw ore has large porosity and pore size distribution of 2-200 mu m. After the modification of PVA with different concentrations, the pore size distribution of EPPVA3, EPPVA4, EPPVA5 and EPPVA6 is mainly concentrated between 1-55 μm, 1-20 μm, 1-15 μm and 1-28 μm, and is far smaller than the pore size distribution of EP. Meanwhile, the specific surface areas of the EPPVA3, the EPPVA4, the EPPVA5 and the EPPVA6 are increased, the number of mesopores is increased, the pore diameter of the mesopores is increased, and the pore volume is increased, so that the phase change material can be adsorbed in a large amount and prevented from leaking.
Refer to the attached figure 3 and table 2, which are DSC curves and corresponding enthalpy value histograms of P/EP, P/EPPVA3, P/EPPVA4, P/EPPVA5 and P/EPPVA6 of the materials prepared by the technical schemes of examples 1-4 and comparative example 1. It can be seen that the prepared modified expanded perlite-based phase change composite material has excellent latent heat storage capacity, and the latent heat storage capacity is enhanced along with the increase of the concentration of the modified PVA.
Referring to the attached figure 4, the digital photos of the modified expanded perlite base phase change thermal protection building material (P/EPP/B), the unmodified expanded perlite base phase change thermal protection building material (P/EP/B) and the expanded perlite thermal protection building material (EP/B) prepared by the technical schemes of the embodiment 5 and the comparative examples 2-3 are shown.
Refer to the attached FIG. 5, which is a time-temperature curve of the materials P/EPP/B, P/EP/B and EP/B prepared by the technical schemes of the example 5 and the comparative examples 2-3. By setting the temperature of the heating plate, the sample was placed on the heating plate and the change in the surface temperature of the sample over time was recorded with a thermocouple. The time required for the modified expanded perlite base phase-change heat protection plate constructed by the invention to reach the target temperature (40 ℃) is 110min, the time required for the unmodified expanded perlite base phase-change heat protection plate to reach the target temperature (40 ℃) is 65min, the time required for the unmodified expanded perlite base phase-change heat protection plate to reach the target temperature (40 ℃) is only 28min, and the latent heat insulation performance is improved. When the ambient temperature reduces, the modified expanded perlite base phase transition heat protection plate can release the heat of storage, plays the heat preservation effect, and the modified expanded perlite base phase transition heat protection plate that this patent was constructed has superior thermal protection performance.
TABLE 1 pore Structure parameters of the expanded perlite EP and the modified expanded perlite EPPVA3, EPPVA4, EPPVA5 and EPPVA6 prepared in examples 1 to 4
Table 2 phase transition thermal performance parameters corresponding to P/EP of modified expanded perlite-based phase transition composite materials P/EPPVA3, P/EPPVA4, P/EPPVA5 and P/EPPVA6 prepared in examples 1-4 and unmodified expanded perlite phase transition composite material P/EP prepared in comparative example 1
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A preparation method of a modified expanded perlite-based phase-change composite material is characterized by comprising the following steps: the method comprises the following steps:
s1: dissolving polyvinyl alcohol in water to form a polyvinyl alcohol aqueous solution;
s2: soaking a polyvinyl alcohol aqueous solution into the macropores of the expanded perlite by a vacuum impregnation method, and freeze-drying to prepare modified expanded perlite with high porosity and graded porosity;
s3: the modified expanded perlite adsorbs the phase change material by a vacuum impregnation method to prepare the modified expanded perlite-based phase change composite material.
2. The method for preparing a modified expanded perlite-based phase change composite material as claimed in claim 1, wherein the method comprises the following steps: in step S1, the mass concentration of the polyvinyl alcohol aqueous solution is 3 wt.% to 6 wt.%.
3. The method for preparing a modified expanded perlite-based phase change composite material as claimed in claim 1, wherein the method comprises the following steps: in the step S2, the size fraction of the expanded perlite is 0.5-4 mm, and the mass ratio of the polyvinyl alcohol aqueous solution to the expanded perlite is 10-30: 1.
4. The method for preparing a modified expanded perlite-based phase change composite material as claimed in claim 1, wherein the method comprises the following steps: in step S2, the vacuum impregnation process is: firstly, placing the expanded perlite in a vacuum impregnation device, vacuumizing for 10-30 min under the condition that the vacuum degree is less than-0.90 MPa, then injecting a polyvinyl alcohol aqueous solution, and continuously vacuumizing for 30-60 min.
5. The method for preparing a modified expanded perlite-based phase change composite material as claimed in claim 1, wherein the method comprises the following steps: in the step S3, the phase-change material is paraffin, and the mass ratio of the modified expanded perlite to the phase-change material is 20-35: 65-80.
6. The method for preparing a modified expanded perlite based phase change composite as claimed in claim 5 wherein: the vacuum impregnation process in step S3 is: the modified expanded perlite is firstly placed in a vacuum impregnation device, and is vacuumized for 10-30 min under the conditions that the vacuum degree is less than minus 0.90MPa and the room temperature, then the phase-change material is added, and the vacuum is continuously vacuumized for 30-60 min at the temperature of 50-70 ℃ and the vacuum degree is less than minus 0.90 MPa.
7. A modified expanded perlite-based phase-change composite material is characterized in that: prepared by the preparation method as described in any one of claims 1 to 6.
8. A phase change thermal protective building material, characterized in that: comprising a modified expanded perlite based phase change composite as claimed in claim 7.
9. A method of making a phase change thermal protective building material of claim 8, comprising: and uniformly mixing the modified expanded perlite base phase change composite material with an inorganic binder, molding, demolding and maintaining to obtain the modified expanded perlite base phase change thermal protection building material.
10. The method for preparing a phase change thermal protective building material of claim 9, wherein: the inorganic binder is water glass, and the mass ratio of the modified expanded pearl-based phase change composite material to the water glass is (4-6): 4 to 6.
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| CN117303938A (en) * | 2023-09-26 | 2023-12-29 | 中国地质大学（武汉） | Expanded perlite composite aerogel and preparation method thereof |
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