CN114672283B - Phase-change temperature-control wet material and preparation method and application thereof - Google Patents
Phase-change temperature-control wet material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a phase-change temperature-control wet material and a preparation method and application thereof. The phase-change temperature-regulating and humidity-controlling material comprises the following components in percentage by mass: shaping the composite phase change material: 30% -70%; metal-organic framework material: 30 to 70 percent. The preparation method of the phase-change temperature-regulating and humidity-controlling material comprises the following steps: 1) Uniformly mixing the organic phase change material eutectic substance heated to a molten state with porous silicon dioxide, and then cooling and crushing to obtain a shaped composite phase change material; 2) And uniformly mixing the shaped composite phase change material and the metal-organic framework material to obtain the phase change temperature and humidity regulating material. The phase-change temperature and humidity regulating material has the advantages of controllable temperature and humidity, large phase-change enthalpy, good moisture absorption and dehumidification, no corrosion, no leakage, high stability, good cycle performance, no supercooling and phase separation phenomena and the like, can meet the requirement of human comfort, and is suitable for indoor temperature and humidity regulation.
Description
Technical Field
The invention relates to the technical field of temperature and humidity regulating materials, in particular to a phase-change temperature and humidity regulating material and a preparation method and application thereof.
Background
The temperature and humidity of the indoor environment directly affect the comfort and health of the human body, so that the regulation of the indoor temperature and humidity is very important. Technologies for adjusting indoor temperature and humidity mainly include two types: one is an active regulation technology adopting equipment such as an air conditioner, a humidifier and the like, and the other is a passive regulation technology adopting a material with the functions of temperature regulation and humidity regulation. The active regulation technology needs to consume a large amount of energy, while the passive regulation technology does not need to consume energy, and belongs to the green energy-saving skill.
At present, the passive temperature adjustment technology mainly adopts Phase Change Materials (PCMs), and the passive humidity adjustment technology adopts Humidity Control Materials (HCMs). PCMs can be divided into two broad categories, inorganic PCMs and organic PCMs, according to composition. Inorganic PCMs include hydrated salts, molten salts and eutectic salts thereof, have the advantages of high phase transition enthalpy (Δ H), flame retardancy, low price and the like, but have the problems of containing crystal water or having a high melting point, and are corrosive and cannot completely meet actual requirements. The organic PCMs have the advantages of higher enthalpy value, no corrosion, chemical inertness, high stability, no supercooling and phase separation phenomena and the like, can be used for indoor temperature regulation, but have the melting point (T) of the organic PCMs m ) High and easy to leak in the phase change melting process. The HCMs can be divided into silica gel, hydrated salt, inorganic mineral, organic polymer and the like according to the components, have the advantages of wide sources, low price and the like, but have the problems of low moisture absorption rate, large pore diameter, inconsistent pore diameter distribution, poor humidity controllability and the like. In addition, both PCMs and HCMs can only control temperature or humidity independently, and cannot control temperature and humidity simultaneously.
Therefore, the development of the temperature and humidity regulating material with large phase change enthalpy value, good moisture absorption and desorption, no corrosion and high stability has very important significance.
Disclosure of Invention
The invention aims to provide a phase-change temperature-control humidity material, and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
the phase-change temperature-control wet material comprises the following components in percentage by mass:
shaping the composite phase change material: 30% -70%;
metal-organic framework material: 30 to 70 percent.
Preferably, the phase-change temperature-control humidity-controlling material comprises the following components in percentage by mass:
shaping the composite phase change material: 40% -60%;
metal-organic framework material: 40 to 60 percent.
Preferably, the composition of the shaped composite phase change material comprises a carrier porous silicon dioxide and an organic phase change material eutectic compound. The porous silicon dioxide has the characteristics of large specific surface area and rich pore structures (mainly mesopores and macropores), and can be used as a carrier of the organic phase change material eutectic substance, the organic phase change material eutectic substance in a molten state can be adsorbed and fixed in a pore channel by utilizing the surface tension and the capillary action generated by the pores, and the organic phase change material eutectic substance can also form strong intermolecular hydrogen bonds with the porous silicon dioxide, so that a stable shape-stabilized composite phase change material can be obtained, and the shaped organic phase change material eutectic substance melts and absorbs heat to be converted into a liquid state when the indoor temperature is higher than the melting point and is tightly adsorbed in the pores by the porous silicon dioxide, so that leakage (shape fixation) cannot occur.
Preferably, the mass percentage content of the porous silicon dioxide in the shaped composite phase change material is 20-40%.
Further preferably, the mass percentage of the porous silicon dioxide in the shaped composite phase change material is 25% -35%. The content of the porous silicon dioxide in the shaped composite phase change material is low, although the phase change enthalpy value is large, the shaped effect is poor (eutectic substances of the organic phase change material are easy to overflow in the phase change melting process), and the content of the porous silicon dioxide is high, although the better shaped effect can be obtained, the phase change enthalpy value of the shaped composite phase change material is small.
Preferably, the porous silica is selected from at least one of hydrophilic fumed silica, hydrophobic fumed silica, and ordered mesoporous silica (e.g., MCM-41 molecular sieve, SBA-15 molecular sieve). The porous silica is used for shaping the organic phase change material eutectic, preventing it from leaking during the phase change melting process.
Further preferably, the porous silica is hydrophilic fumed silica. The price of the ordered mesoporous silica is too high, and the compatibility between the hydrophobic fumed silica and the humidity control material is poor, so that the hydrophilic fumed silica is most suitable.
Preferably, the organic phase change material eutectic compound is formed by compounding at least two of alkane wax, fatty acid and fatty alcohol. The melting point of the single organic phase change material is too high, and the melting point can be adjusted by forming eutectic compounds through compounding.
Preferably, the melting point of the organic phase change material eutectic is 28-32 ℃.
Preferably, the phase change enthalpy value of the organic phase change material eutectic compound is greater than 180J/g.
Preferably, the alkane wax is a mixture of alkanes having 18 to 34 carbon atoms.
Preferably, the fatty acid is a monocarboxylic acid having 10 to 18 carbon atoms.
Further preferably, the fatty acid is selected from at least one of lauric acid, palmitic acid, stearic acid (stearic acid).
Preferably, the aliphatic alcohol is a monohydric alcohol having 14 to 18 carbon atoms.
Further preferably, the fatty alcohol is at least one selected from tetradecanol and hexadecanol.
Preferably, the organic phase change material eutectic compound is formed by compounding two of dodecanoic acid, hexadecanoic acid and octadecanoic acid with at least one of tetradecanol and hexadecanol.
Preferably, the metal-organic framework material is selected from at least one of MIL-101 (Cr), MIL-100 (Fe), al-MOF fumarate, CAU-10 (Al). The metal-organic framework material has a microporous structure, has the advantages of high adsorption quantity, low desorption temperature and the like when being used as a moisture absorbent, has S-shaped water vapor adsorption isothermal characteristic, and is an ideal humidity control material.
Further preferably, the metal-organic framework material is MIL-101 (Cr). From the aspects of raw material price, adsorption capacity, adsorption and desorption curve (a steep curve in the range of 30-65% of relative humidity) and the like, the MIL-101 (Cr) is most suitable (the saturated capacity of water vapor adsorption is more than 0.8g/g, the moisture absorption-desorption rate is high, and the hysteresis loop is small).
The preparation method of the phase-change temperature-regulating and humidity-controlling material comprises the following steps:
1) Uniformly mixing the organic phase change material eutectic substance heated to a molten state with porous silicon dioxide, and then cooling and crushing to obtain a shaped composite phase change material;
2) And uniformly mixing the shaped composite phase change material and the metal-organic framework material to obtain the phase change temperature and humidity regulating material.
The building material comprises the phase-change temperature and humidity regulating material.
The beneficial effects of the invention are: the phase-change temperature and humidity regulating material has the advantages of controllable temperature and humidity, large phase-change enthalpy, good moisture absorption and dehumidification, no corrosion, no leakage, high stability, good cycle performance, no supercooling and phase separation phenomena and the like, can meet the requirement of human comfort, and is suitable for indoor temperature and humidity regulation.
Specifically, the method comprises the following steps:
1) The phase-change temperature and humidity control material has the advantages that the phase-change temperature accords with the thermal comfort range of a human body, the phase-change enthalpy value is large, and the phenomena of corrosion, chemical inertia, high stability, supercooling and phase separation are avoided;
2) The phase-change temperature and humidity regulating material has the advantages of accurate indoor temperature and humidity regulation, good moisture absorption-dehumidification performance, no corrosion and leakage problem, good cycle performance and the like, and can reduce the energy consumption of an air conditioner and realize the energy conservation of a building as a functional building material;
3) The phase-change temperature-regulating and humidity-controlling material disclosed by the invention is simple in preparation method, mild in process conditions, low in cost and suitable for large-scale production and application.
Drawings
FIG. 1 is a DSC curve of the ternary organic phase change material eutectic compound in examples 1-3.
FIG. 2 is a plot of pore size distribution for MIL-101 (Cr) and hydrophilic fumed silica.
FIG. 3 is a water vapor sorption isotherm for MIL-101 (Cr).
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
MIL-101 (Cr) in examples 1 to 7 was prepared by the following method: 1) 2.007g of Cr (NO) 3 ) 3 ·9H 2 Adding O into 25mL of deionized water, and stirring at room temperature for 10min to obtain a chromium nitrate solution; 2) 0.823g of terephthalic acid (H) 2 BDC) is added into 5mL of N, N-dimethyl amide (DMF), and the mixture is stirred for 10min at room temperature to obtain N, N-dimethyl amide solution of terephthalic acid; 3) Adding an N, N-dimethylamide solution of terephthalic acid into a chromium nitrate solution, stirring for 30min, dropwise adding 0.38mL of 49 mass percent hydrofluoric acid (HF), continuously stirring for 10min, transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, reacting for 24h at 160 ℃, naturally cooling to room temperature, adding 150mL of deionized water, transferring into a constant-temperature water bath kettle, stirring and washing for 6h at 60 ℃, performing suction filtration on the separated product by using a G4 funnel, stirring and washing for 6h by using 100mL of DMF, repeating the washing operation twice, performing suction filtration, adding the filtered solid into a forced air drying oven, and drying for 24h at 120 ℃ to obtain MIL-101 (Cr).
Example 1:
a phase-change temperature-control humidity-control material is prepared by the following steps:
1) Mixing 6.4g of dodecanoic acid, 1.6g of stearic acid and 2.0g of hexadecanol, placing the mixture in a constant-temperature water bath kettle, stirring the mixture for 2 hours at the temperature of 60 ℃, and naturally cooling the mixture to room temperature to obtain a ternary organic phase change material eutectic compound;
2) 3.5g of the ternary organic phase change material eutectic compound obtained in the step 1) is placed in a constant-temperature water bath kettle and stirred for 30min at 60 ℃, then 1.5g of hydrophilic fumed silica is added, the stirring is continued for 2h, the mixture is naturally cooled to room temperature, and the mechanical crushing is carried out, so as to obtain the shaped composite phase change material;
3) Adding 5g of MIL-101 (Cr) into the shaped composite phase change material obtained in the step 2), and uniformly stirring to obtain the phase change temperature and humidity regulating material.
Example 2:
a phase-change temperature-control humidity-control material is prepared by the following steps:
1) Mixing 5.6g of dodecanoic acid, 1.4g of stearic acid and 3.0g of hexadecanol, placing the mixture in a constant-temperature water bath kettle, stirring the mixture for 2 hours at the temperature of 60 ℃, and naturally cooling the mixture to room temperature to obtain a ternary organic phase change material eutectic crystal;
2) Placing 3.5g of the ternary organic phase change material eutectic compound obtained in the step 1) in a constant-temperature water bath kettle, stirring for 30min at 60 ℃, adding 1.5g of hydrophilic fumed silica, continuously stirring for 2h, naturally cooling to room temperature, and mechanically crushing to obtain a shaped composite phase change material;
3) Adding 5g of MIL-101 (Cr) into the shaped composite phase change material obtained in the step 2), and uniformly stirring to obtain the phase change temperature and humidity regulating material.
Example 3:
a phase-change temperature-control humidity-control material is prepared by the following steps:
1) Mixing 4.8g of dodecanoic acid, 1.2g of stearic acid and 4.0g of hexadecanol, stirring for 2 hours at 60 ℃ in a constant-temperature water bath kettle, and naturally cooling to room temperature to obtain a ternary organic phase change material eutectic compound;
2) 3.5g of the ternary organic phase change material eutectic compound obtained in the step 1) is placed in a constant-temperature water bath kettle and stirred for 30min at 60 ℃, then 1.5g of hydrophilic fumed silica is added, the stirring is continued for 2h, the mixture is naturally cooled to room temperature, and the mechanical crushing is carried out, so as to obtain the shaped composite phase change material;
3) Adding 5g of MIL-101 (Cr) into the shaped composite phase change material obtained in the step 2), and uniformly stirring to obtain the phase change temperature and humidity regulating material.
Example 4:
a phase-change temperature-control humidity-control material is prepared by the following steps:
1) Placing 3.75g of ternary organic phase change material eutectic compound (the preparation method is the same as that of the embodiment 2) in a constant-temperature water bath kettle, stirring for 30min at 60 ℃, adding 1.25g of hydrophilic fumed silica, continuously stirring for 2h, naturally cooling to room temperature, and mechanically crushing to obtain a shaped composite phase change material;
2) Adding 5g of MIL-101 (Cr) into the shaped composite phase change material obtained in the step 2), and uniformly stirring to obtain the phase change temperature and humidity regulating material.
Example 5:
a phase-change temperature-control humidity-control material is prepared by the following steps:
1) Placing 3.25g of ternary organic phase change material eutectic compound (the preparation method is the same as that in example 2) in a constant-temperature water bath kettle, stirring for 30min at 60 ℃, adding 1.75g of hydrophilic fumed silica, continuously stirring for 2h, naturally cooling to room temperature, and mechanically crushing to obtain a shaped composite phase change material;
2) Adding 5g of MIL-101 (Cr) into the shaped composite phase change material obtained in the step 2), and uniformly stirring to obtain the phase change temperature and humidity regulating material.
Example 6:
a phase-change temperature-control humidity-control material is prepared by the following steps:
1) Placing 3.5g of ternary organic phase change material eutectic compound (the preparation method is the same as that of the embodiment 2) in a constant-temperature water bath kettle, stirring for 30min at 60 ℃, adding 1.5g of hydrophilic fumed silica, continuously stirring for 2h, naturally cooling to room temperature, and mechanically crushing to obtain a shaped composite phase change material;
2) Adding 3.33g of MIL-101 (Cr) into the shaped composite phase change material obtained in the step 2), and uniformly stirring to obtain the phase change temperature and humidity regulating material.
Example 7:
a phase-change temperature-control humidity-control material is prepared by the following steps:
1) Placing 3.5g of ternary organic phase change material eutectic compound (the preparation method is the same as that in example 2) in a constant-temperature water bath kettle, stirring for 30min at 60 ℃, adding 1.5g of hydrophilic fumed silica, continuously stirring for 2h, naturally cooling to room temperature, and mechanically crushing to obtain a shaped composite phase change material;
2) Adding 7.5g of MIL-101 (Cr) into the shaped composite phase change material obtained in the step 2), and uniformly stirring to obtain the phase change temperature and humidity regulating material.
And (4) performance testing:
1) The Differential Scanning Calorimetry (DSC) curves of the ternary organic phase change material eutectics (abbreviated as "eutectics 1-3") in examples 1-3 are shown in FIG. 1.
As can be seen from fig. 1: the dodecanoic acid, the stearic acid and the hexadecanol in a certain proportion can form a eutectic compound with a single melting point, the phase transition temperature (melting point) of the eutectic compound is within the range of 30.53-31.35 ℃, and the phase transition enthalpy value is within the range of 184.92 kJ/kg-201.39 kJ/kg, so that the eutectic compound meets the requirement of phase transition temperature control.
2) MIL-101 (Cr) and hydrophilic fumed silica (SiO for short) 2 ") holesThe diameter size distribution curve is shown in fig. 2.
As can be seen from fig. 2: the hydrophilic gas phase silicon dioxide has a large amount of micropores and mesopores, takes the mesopores as the main part, has the average pore diameter of 8.14nm and the specific surface area as high as 151.8m 2 Is suitable for being used as a shaping carrier of a ternary organic phase change material eutectic crystal, and the pore diameter of MIL-101 (Cr) is concentrated into micropores, the average pore diameter is 1.926nm, and the specific surface area is up to 1972m 2 Is suitable for being used as a moisture absorbent to absorb the small molecular water vapor.
3) The water vapor adsorption isotherm of MIL-101 (Cr) is shown in FIG. 3.
As can be seen from fig. 3: the MIL-101 (Cr) adsorption curve is represented by three stages: at P/P 0 When the adsorption quantity is less than 0.3, the adsorption quantity and the adsorption rate are lower, which shows that the desorption performance is excellent, and P/P 0 The adsorption rate is obviously increased in the range of 0.3-0.5, but the rate is gradually reduced after the adsorption rate exceeds 0.6, and an S-shaped water vapor adsorption isotherm is formed on the whole, which shows that MIL-101 (Cr) has excellent humidity regulation capacity when the indoor relative humidity is 30-65%, and is suitable for being used as a humidity control material.
4) The thermal properties and adsorption data of the phase change temperature and humidity control materials of examples 1 to 7 are shown in the following table:
TABLE 1 thermophysical properties and adsorption data of the phase change thermoregulation humidity control materials of examples 1-7
As can be seen from Table 1: the addition of the hydrophilic fumed silica can further reduce the phase change temperature of the ternary organic phase change material eutectic compound; the shaped composite phase-change material obtained by compounding the two materials is further mixed with a metal organic framework, the melting point of the prepared phase-change temperature and humidity control material is in the range of 25.50-27.39 ℃, the melting point is basically consistent with the thermal comfort range (20-27 ℃) of a human body, and the phase-change enthalpy of the material is still at a higher level of the same material; in addition, the MIL101 (Cr) adsorbent is added into the shaped composite phase-change material, and the prepared phase-change temperature and humidity regulating material still has strong water absorption capacity (for example, the saturated adsorption capacity of the phase-change temperature and humidity regulating material in the embodiment 2 can reach 0.5g/g when the relative humidity is 60%); in conclusion, the phase-change temperature and humidity regulating material is suitable for being used as an indoor temperature and humidity control material and completely meets the requirement of human body comfort.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (3)
1. The phase-change temperature-control wet material is characterized by comprising the following components in percentage by mass:
shaping the composite phase change material: 30% -70%;
metal-organic framework material: 30% -70%;
the composition of the shaped composite phase change material comprises carrier porous silicon dioxide and an organic phase change material eutectic compound;
the mass percentage content of the porous silicon dioxide in the shape-stabilized composite phase change material is 20-40%;
the porous silica is hydrophilic fumed silica;
the organic phase change material eutectic compound is formed by compounding two of dodecanoic acid, hexadecanoic acid and octadecanoic acid with at least one of tetradecanol and hexadecanol;
the metal-organic framework material is MIL-101 (Cr).
2. The method for preparing the phase-change temperature and humidity regulating material according to claim 1, which comprises the following steps:
1) Uniformly mixing the organic phase change material eutectic substance heated to a molten state with porous silicon dioxide, and then cooling and crushing to obtain a shaped composite phase change material;
2) And uniformly mixing the shaped composite phase change material and the metal-organic framework material to obtain the phase change temperature and humidity regulating material.
3. A building material, the composition comprising the phase change temperature and humidity regulating material of claim 1.
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