CN114539979B - Boron nitride aerogel-based composite shaping phase change material, preparation and application - Google Patents
Boron nitride aerogel-based composite shaping phase change material, preparation and application Download PDFInfo
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Abstract
The invention discloses preparation and application of a boron nitride aerogel-based high-heat-conductivity composite shaping phase-change material, which specifically comprises the following process steps: (1) And (3) hydrolyzing the organosilane and the boron nitride under an acidic condition to obtain hydrosol of composite boron nitride, freeze-drying the hydrosol to obtain composite boron nitride aerogel carrier boron nitride (2) mixing the phase change material with the composite boron nitride aerogel carrier obtained in the step (1), and placing the mixture in a vacuum oven to enable the phase change material to fully enter a carrier structure, so as to obtain the boron nitride aerogel-based high-heat-conductivity composite shaping phase change material. The boron nitride-based high-heat-conductivity composite shaping phase-change material prepared by the method is a white block-shaped object, has high phase-change material load and high heat conductivity, has electrical insulation property, has excellent heat storage performance and shaping effect, is simple in preparation method and low in operation requirement, and can be used for heat energy conversion and storage and functional substances of heat energy management equipment.
Description
Technical Field
The invention belongs to the field of composite shaping phase-change materials, and particularly relates to a preparation method for synthesizing a boron nitride aerogel-based high-heat-conductivity composite shaping phase-change material which can be used as a functional substance of thermal energy conversion and storage equipment through hydrolysis reaction, freeze drying, vacuum impregnation and other methods.
Background
The organic phase change material has a series of advantages of high heat storage density, wide selective range of phase change temperature, low supercooling degree, strong thermal stability and the like, and is widely used in the fields of building temperature control, solar photo-thermal conversion, electronic equipment thermal management and the like. However, in the application process, the phase change material has the problems of liquid flow leakage and low self heat conductivity coefficient in the phase change process, and the effect of the phase change material in practical application is greatly limited. Therefore, the improvement of the heat conductivity coefficient of the phase change material and the solution of the leakage problem thereof are necessary preconditions for promoting the practical application of the material.
At present, the shaped phase change material is the most common composite phase change material system, in the system, the phase change material can be protected from leakage and outflow in the phase change process by introducing the support carrier, and meanwhile, the additional addition of the high-heat-conductivity material can be inserted into the whole system to construct a heat-conductivity passage so as to improve the heat conductivity coefficient. Therefore, the aim of simultaneously realizing leakage prevention and heat conduction improvement is a hot spot of current research by directly preparing the high heat conduction material into the support carrier and introducing the support carrier into the phase change material system.
The preparation method takes organosilane and boron nitride as raw materials, and prepares the composite boron nitride aerogel through hydrolysis reaction and freeze drying; and then immersing the phase-change material into the phase-change material through vacuum impregnation to finally prepare the boron nitride aerogel-based composite shaping phase-change material. The boron nitride aerogel has the characteristic of graded porosity, so that the phase change material can be effectively wrapped, and meanwhile, the boron nitride aerogel has high heat conductivity coefficient and can effectively improve the heat conductivity; in the obtained composite phase-change material product, the phase-change material has high load, excellent heat storage performance and shaping effect, simultaneously, the heat conductivity coefficient is improved, the heat transmission rate is improved, meanwhile, the obtained composite phase-change material has electrical insulation property, the safety coefficient of practical use is improved to a certain extent, especially in the thermal management of electronic equipment, in addition, the preparation method is simple, the operation requirement is low, and the system can be used for heat energy conversion and storage and functional substances of heat energy management equipment.
Disclosure of Invention
The invention provides a preparation method of a boron nitride aerogel based composite shaping phase-change material, which is characterized in that organosilane and boron nitride are used as raw materials, the composite boron nitride aerogel is prepared through hydrolysis reaction and freeze drying, and then the phase-change material is immersed in the composite boron nitride aerogel based composite shaping phase-change material through vacuum impregnation.
The synthesized boron nitride aerogel-based composite sizing phase change material comprises the following steps:
(1) Adding organosilane and boron nitride with certain mass into aqueous solution, carrying out ultrasonic mixing uniformly, adding acid as a catalyst, stirring for a certain time to form uniform and stable hydrosol, preparing composite boron nitride aerogel by freeze drying, and preparing composite boron nitride aerogel by high-temperature reduction;
(2) And (3) mixing the phase-change material with the composite boron nitride aerogel carrier obtained in the step (1), and placing the mixture in a vacuum oven to enable the phase-change material to fully enter a carrier structure, so as to obtain the boron nitride aerogel-based high-heat-conductivity composite shaping phase-change material.
Further, the organosilane used in the step (1) is one or more than two of tetraethyl orthosilicate (TEOS), trimethoxymethylsilane (MTMS) or dimethoxydimethylsilane (DMDMDMS);
the mass ratio of the organosilane to the boron nitride in the step (1) is that: boron nitride = 1:10-10:1, a step of;
the ratio of the organosilane to the aqueous solution in the step (1) is: aqueous = 1g:50mL-1g:200mL;
the aqueous solution in the step (1) is an aqueous solution of ethanol, and the mass ratio of water to ethanol is: ethanol=1: 1-5:1, a step of;
the ultrasonic time in the step (1) is 2-4h;
further, the acid catalyst added in the step (1) is one or more of acetic acid, phosphoric acid and oxalic acid;
the pH range of the solution after adding the acid in the step (1) is 3-5;
the reaction time of adding acid in the step (1) is 3-5h;
further, the freeze drying temperature in the step (1) is minus 20 ℃ to minus 5 ℃ and the time is 48 to 72 hours; the method comprises the steps of carrying out a first treatment on the surface of the
Further, the phase change material in the step (2) is one or more than two of paraffin, polyethylene glycol, fatty alcohol, fatty acid and fatty amine;
further, the set temperature of the vacuum oven in the step (2) is 80-100 ℃, and the vacuum degree is-0.1 MPa;
the time of vacuum impregnation in the step (2) is 2-4 hours;
the finally prepared boron nitride aerogel-based composite shaping phase change material is a white block;
the boron nitride aerogel-based composite shaping phase-change material prepared by the method has high phase-change material load, excellent heat storage performance and shaping effect, and simultaneously improves the heat conductivity; the finally prepared boron nitride aerogel-based composite shaping phase change material has higher heat conductivity coefficient, and the heat conductivity coefficient is 1.2-2W/mK;
the preparation method is simple in reaction condition design, and low in operation requirement, and the prepared composite phase change material can be used for heat energy conversion and storage and functional substances of heat energy management equipment.
Drawings
FIG. 1 differential scanning calorimetry curve of example 1 boron nitride aerogel based composite set phase change material (paraffin wax, 90%).
Detailed Description
Example 1
(1) Adding 1g of ethyl orthosilicate and 1g of boron nitride into 100mL of aqueous solution (the mass ratio of water to ethanol is 4:1), carrying out ultrasonic treatment for 4 hours, uniformly mixing, adding oxalic acid to adjust the pH=3 of the mixed solution, and then stirring for 3 hours to form composite boron nitride sol; placing the sol into a freeze dryer, setting the temperature to be-10 ℃, and freeze-drying for 60 hours to obtain a boron nitride aerogel carrier;
(2) Adding a proper amount of paraffin (the mass ratio of the paraffin to the boron nitride aerogel is 20:1) into the carrier in the step (1), placing the carrier in a vacuum oven, and soaking the carrier for 4 hours at 80 ℃ under the vacuum degree of-0.1 MPa. And removing superfluous paraffin on the surface to finally obtain the boron nitride aerogel-based composite shaping phase change material.
The boron nitride aerogel-based composite shaping phase change material is a white block, wherein the mass percentage of paraffin accounts for 90%, and the differential scanning calorimeter curve of the boron nitride aerogel-based composite shaping phase change material is shown in figure 1; the heat conductivity coefficient is 1.5W/mK, and the heat conductivity is improved.
Example 2
(1) Adding 1g of ethyl orthosilicate and 0.5g of boron nitride into 100mL of aqueous solution (the mass ratio of water to ethanol is 2:1), carrying out ultrasonic treatment for 3 hours, uniformly mixing, adding oxalic acid to adjust the pH=4 of the mixed solution, and then stirring for 3 hours to form composite boron nitride sol; placing the sol into a freeze dryer, setting the temperature to be-10 ℃, and freeze-drying for 72 hours to obtain a boron nitride aerogel carrier;
(2) Adding a proper amount of stearyl alcohol (the mass ratio of the stearyl alcohol to the boron nitride aerogel is 20:1) into the carrier in the step (1), placing the carrier in a vacuum oven, and soaking the carrier for 3 hours at 80 ℃ under the vacuum degree of-0.1 MPa. And removing the superfluous octadecanol on the surface to finally obtain the boron nitride aerogel-based composite shaping phase change material.
The boron nitride aerogel-based composite shaping phase change material is a white block, wherein the mass percentage of stearyl alcohol is 85%; the heat conductivity coefficient is 2W/mK, and the heat conductivity is improved.
Example 3
(1) Adding 1g of ethyl orthosilicate and 0.8g of boron nitride into 150mL of aqueous solution (the mass ratio of water to ethanol is 4:1), carrying out ultrasonic treatment for 2 hours, uniformly mixing, adding oxalic acid to adjust the pH=5 of the mixed solution, and then stirring for 4 hours to form composite boron nitride sol; placing the sol into a freeze dryer, setting the temperature to-10 ℃, and freeze-drying for 48 hours to obtain a boron nitride aerogel carrier;
(2) Adding a proper amount of octadecanoic acid (the mass ratio of the octadecanoic acid to the boron nitride aerogel is 20:1) into the carrier in the step (1), placing the carrier in a vacuum oven, and soaking the carrier for 3 hours at 80 ℃ under the vacuum degree of-0.1 MPa. And removing the superfluous octadecanoic acid on the surface to finally obtain the boron nitride aerogel-based composite shaping phase change material.
The boron nitride aerogel-based composite shaping phase change material is a white block, wherein the mass percentage of the stearic acid is 92%; the heat conductivity coefficient is 1.2W/mK, and the heat conductivity is improved.
Example 4
(1) Adding 1g of ethyl orthosilicate and 0.5g of boron nitride into 200mL of aqueous solution (the mass ratio of water to ethanol is 4:1), carrying out ultrasonic treatment for 3 hours, uniformly mixing, adding oxalic acid to adjust the pH=3 of the mixed solution, and then stirring for 3 hours to form composite boron nitride sol; placing the sol into a freeze dryer, setting the temperature to-10 ℃, and freeze-drying for 48 hours to obtain a boron nitride aerogel carrier;
(2) Adding a proper amount of eicosane (the mass ratio of eicosane to boron nitride aerogel is 20:1) into the carrier in the step (1), placing the carrier in a vacuum oven, and soaking the carrier for 4 hours at 80 ℃ under the vacuum degree of-0.1 MPa. And removing the superfluous eicosane on the surface to finally obtain the boron nitride aerogel-based composite shaping phase change material.
The boron nitride aerogel-based composite shaping phase change material is a white block, wherein the mass percentage of the stearic acid is 90%; the heat conductivity coefficient is 1.6W/mK, and the heat conductivity is improved.
Example 5
(1) Adding 1g of ethyl orthosilicate into 150mL of aqueous solution (the mass ratio of water to ethanol is 4:1), uniformly mixing, adding oxalic acid to adjust the pH=4 of the mixed solution, and stirring for 4 hours to form sol; placing the sol into a freeze dryer, setting the temperature to-10 ℃, and freeze drying for 48 hours to obtain a support carrier material;
(2) Adding a proper amount of stearyl alcohol (the mass ratio of the stearyl alcohol to the carrier is 20:1) into the carrier in the step (1), placing the carrier in a vacuum oven, and soaking the carrier for 3 hours at 80 ℃ under the vacuum degree of-0.1 MPa. And removing the superfluous octadecanoic acid on the surface to finally obtain the composite shaping phase change material.
The composite shaping phase change material obtained by the invention is a white block, wherein the mass percentage of the stearyl alcohol accounts for 60 percent; the thermal conductivity is 0.4W/mK.
Example 6
(1) Adding 0.8g of boron nitride into 150mL of aqueous solution (the mass ratio of water to ethanol is 4:1), uniformly mixing, adding oxalic acid to adjust the pH=4 of the mixed solution, and stirring for 4 hours to form boron nitride dispersion; placing the mixture in a freeze dryer, setting the temperature to be-10 ℃, and freeze-drying the mixture for 48 hours to obtain a boron nitride carrier;
(2) Adding a proper amount of stearic acid (the mass ratio of the stearic acid to the boron nitride is 20:1) into the carrier in the step (1), placing the carrier in a vacuum oven, and immersing the carrier for 3 hours at 80 ℃ under the vacuum degree of-0.1 MPa. Removing the superfluous octadecanoic acid on the surface to finally obtain the carbon nano tube-based composite shaping phase change material.
The carbon nano tube-based composite shaping phase change material is a white block, wherein the mass percentage of the octadecanoic acid is 20%, and the boron nitride is 80%; the thermal conductivity is 3W/mK. The boron nitride prepared under the condition does not have a porous network, so that the boron nitride has no leakage-proof function of the shaped phase change material.
Claims (14)
1. The preparation method of the boron nitride gel-based composite shaping phase change material is characterized by comprising the following specific process steps:
(1) Adding organosilane and boron nitride into the aqueous solution, carrying out ultrasonic mixing uniformly, adding acid serving as a catalyst, stirring to form hydrosol, and carrying out freeze drying to obtain composite boron nitride aerogel; the mass ratio of the organosilane to the boron nitride in the step (1) is that: boron nitride = 1:10-10:1, the aqueous solution in the step (1) is an aqueous solution of ethanol, and the mass ratio of water to ethanol is: ethanol=1: 1-5:1, the ratio of the organosilane to the aqueous solution in the step (1) is: aqueous = 1g:50mL-1g:200mL; the pH range of the solution after the acid is added in the step (1) is 3-5,
(2) And (3) mixing the phase-change material with the composite boron nitride aerogel carrier obtained in the step (1), and placing the mixture in a vacuum oven to enable the phase-change material to fully enter a carrier structure, so as to obtain the boron nitride aerogel-based composite shaping phase-change material.
2. The method of manufacturing according to claim 1, characterized in that: the organosilane used in the step (1) is one or more than two of tetraethyl orthosilicate (TEOS), trimethoxymethylsilane (MTMS) or dimethoxydimethylsilane (DMDMDMS);
the mass ratio of the organosilane to the boron nitride in the step (1) is that: boron nitride = 1:1-3:1.
3. the preparation method according to claim 1 or 2, characterized in that:
the ratio of the organosilane to the aqueous solution in the step (1) is: aqueous = 1g: 80-120 mL;
the aqueous solution in the step (1) is an aqueous solution of ethanol, and the mass ratio of water to ethanol is: ethanol=2: 1-4:1, a step of;
the ultrasonic time in the step (1) is 2-4h.
4. A method of preparation according to claim 3, characterized in that:
the ultrasonic time in the step (1) is 3-4h.
5. The method of manufacturing according to claim 1, characterized in that: the acid catalyst added in the step (1) is one or more than two of acetic acid, phosphoric acid and oxalic acid;
the pH of the solution after adding the acid in the step (1) is 3;
the reaction time of adding acid in the step (1) is 3-5h.
6. The method of manufacturing according to claim 1, characterized in that: the freeze drying temperature in the step (1) is-20 ℃ to-5 ℃ and the time is 48-72h.
7. The method of manufacturing according to claim 6, wherein: the freeze drying temperature in the step (1) is-15 ℃ to-10 ℃ and the time is 48 to 60 hours.
8. The method of manufacturing according to claim 1, characterized in that: the phase change material in the step (2) is one or more than two of paraffin, polyethylene glycol, fatty alcohol, fatty acid and fatty amine, wherein the loading amount of the phase change material is 85% -95%.
9. The method of manufacturing according to claim 8, wherein:
when the phase change material is one or more than two of polyethylene glycol, fatty acid and fatty amine, the loading capacity of the phase change material is 85-90%.
10. The method of manufacturing according to claim 8, wherein: when the phase change material is one or more than two of paraffin and fatty acid, the loading capacity of the phase change material is 90-95%.
11. The method of manufacturing according to claim 1, characterized in that: the set temperature of the vacuum oven in the step (2) is 80-100 ℃, and the vacuum degree is-0.1 MPa;
the time of vacuum impregnation in the step (2) is 2-4h.
12. The method of manufacturing according to claim 1, characterized in that: the set temperature of the vacuum oven in the step (2) is 80-90 ℃;
the time of vacuum impregnation in the step (2) is 3-4h.
13. A boron nitride aerogel-based high thermal conductivity composite shaped phase change material prepared by the preparation method of any one of claims 1-12.
14. Use of a boron nitride aerogel based high thermal conductivity composite set phase change material according to claim 13 as a functional material for a thermal energy conversion, storage or thermal energy management device.
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