CN112500836A - Composite phase-change heat storage material and preparation method thereof - Google Patents
Composite phase-change heat storage material and preparation method thereof Download PDFInfo
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Abstract
A composite phase-change heat storage material and a preparation method thereof are provided, wherein the composite phase-change heat storage material comprises: at least two layers of composite phase change layers from inside to outside; the composite phase change layer is formed by compounding eutectic salt and magnesium oxide; the content of eutectic salt in the composite phase change layer at the outermost layer is less than or equal to 20 wt%. The invention can effectively avoid the problems of moisture absorption and pulverization caused by the moisture absorption of eutectic salt, and obviously improve the moisture resistance.
Description
Technical Field
The invention relates to the field of heat storage materials, in particular to a composite phase-change heat storage material and a preparation method thereof.
Background
The composite phase-change heat storage material is mainly used for improving heat storage density by utilizing phase change of the material, storing electric energy, heat energy and the like, and releasing the energy when needed; therefore, the utilization of the composite phase-change heat storage material is an important means for solving the problems of intermittency and instability of renewable energy sources. The composite phase-change heat storage material can solve the contradiction between heat energy supply and demand mismatch, and effectively improves the energy utilization efficiency and the environment protection.
The composite phase-change heat storage material is divided into low temperature, medium temperature and high temperature, different types of composite phase-change heat storage materials exist according to the difference of application environments, and in the heat storage device, the composite phase-change material with the phase-change temperature of about 700 ℃ is a better choice in consideration of the temperature-resistant service life and the economical efficiency of accessories such as electric heating wires and the like. The fused salt phase-change heat storage material has the advantages of high heat storage density, high cost performance, easiness in operation control and management and the like, so that the fused salt phase-change heat storage material has great advantages in composite phase-change heat storage materials; however, eutectic salt in the fused salt phase-change heat storage material has a serious problem of hygroscopicity, so that the finally prepared composite phase-change heat storage material is easy to absorb moisture and pulverize when the relative humidity is higher than 50%, and the application range of the composite phase-change heat storage material is severely limited.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect that the eutectic salt doped phase-change material in the prior art is easy to absorb moisture and pulverize, so that the composite phase-change heat storage material which can not absorb moisture and pulverize even when the humidity is higher than 50% is provided, and the preparation method of the composite phase-change heat storage material is provided.
A composite phase-change heat storage material comprises at least two composite phase-change layers from inside to outside; the composite phase change layer is formed by compounding eutectic salt and magnesium oxide; the content of eutectic salt in the composite phase change layer at the outermost layer is less than or equal to 20 wt%.
The content of eutectic salt in the composite phase change layers of at least two layers from inside to outside is gradually reduced, and the difference of the content percentage of the eutectic salt in the composite phase change layers of two adjacent layers is not higher than 20 wt%.
The composite phase change layer comprises an inner layer, an intermediate layer and an outer layer, wherein the inner layer contains eutectic salt 40-60 wt%, the intermediate layer contains eutectic salt 20-40 wt%, and the outer layer contains eutectic salt not more than 20 wt%.
The eutectic salt is Na2CO3-K2CO3。
A preparation method of a composite phase-change heat storage material comprises the following steps:
preparing raw materials: obtaining eutectic salt and magnesium oxide, and respectively preparing composite raw materials of each composite phase change layer according to the proportion;
preparing an embryo body: preparing a blank body with at least two layers of composite phase change layers by adopting composite raw materials;
and (3) sintering: and pre-pressing and sintering the blank to obtain the composite phase change heat storage material.
The eutectic salt is Na2CO3-K2CO3The preparation process comprises the following steps: mixing and grinding sodium carbonate and potassium carbonate uniformly, and calcining to obtain the eutectic salt.
The composite raw material is obtained by blending eutectic salt and magnesium oxide, pre-sintering, crushing and grinding.
The pre-sintering temperature is 700-800 ℃, preferably 750 ℃; or, the crushed and ground composite raw material is sieved by a 150-mesh sieve; preferably, the milling is ball milling.
When the number of the layers of the composite phase change layer is three; the specific process of the embryo body preparation is as follows:
laying the composite raw material of the outer layer at the bottom of the mould, and laying the composite raw material of the middle layer according to the position of the middle layer;
the diameter of the cylindrical metal sheet with the adjustable diameter is adjusted to be the same as the size of the inner layer, and the cylindrical metal sheet is placed above the composite raw material paved with the middle layer; injecting the composite raw material of the inner layer into the middle of the cylindrical metal sheet;
adjusting the diameter of the cylindrical metal sheet to be the same as the size of the middle layer, and injecting the composite raw material of the middle layer into the cylindrical metal sheet to completely cover the inner layer;
and finally, injecting the composite raw material of the outer layer to completely cover the middle layer to obtain a blank.
The pre-pressing pressure increasing mode is uniaxial pressing; if the pressure is too low or too short, the molding may not be performed, if the pressure is too high, the mold may be damaged, and if the pressure is too long, the efficiency may be affected, so that the object of the present invention may be achieved by preferably applying the pressure of 8t, preferably maintaining the pressure for 30s, and appropriately increasing the time, and the pressure for pre-pressing may be sufficient to ensure the molding.
The technical scheme of the invention has the following advantages:
1. the composite phase-change heat storage material provided by the invention adopts at least two composite phase-change layers arranged from inside to outside, and the content of eutectic salt in the outermost composite phase-change layer is set to be less than or equal to 20 wt%; the arrangement mode can arrange the composite phase change layer with high eutectic salt content on the inner layer, and the composite phase change heat storage material with higher heat storage density can be effectively obtained by compounding the eutectic salt and the magnesium oxide; meanwhile, because the content of eutectic salt in the outermost composite phase change layer is set to be less than or equal to 20 wt%, under the content condition, the moisture absorption of the eutectic salt can be effectively avoided, the moisture absorption is basically unchanged when the humidity is 80 RH% and the test is carried out for 120h, the moisture resistance is obviously improved, and the problems that the existing phase change heat storage material is easy to absorb moisture and pulverize in the environment with the humidity higher than 50% are solved.
2. The composite phase-change heat storage material provided by the invention further optimizes the difference of the content percentages of eutectic salts in the adjacent two composite phase-change layers, and when the difference is limited to be not more than 20 wt%, the thermal expansion coefficients between the layers can be effectively ensured to be basically consistent, so that the prepared composite phase-change heat storage material is not deformed and cracked, and further excellent thermal property is maintained.
3. In the preparation process of the composite phase-change heat storage material, the moisture resistance is further improved by optimizing the preparation process of the composite raw material, and meanwhile, the consistency of the thermal expansion coefficients between layers is better ensured, and the thermal property is better.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic cross-sectional view of a composite phase-change heat storage material according to embodiment 1 of the present invention;
fig. 2 is a schematic longitudinal sectional view of a composite phase-change heat storage material according to embodiment 1 of the present invention;
fig. 3 is an appearance diagram of a composite phase-change heat storage material after moisture absorption detection in embodiment 1 of the present invention;
fig. 4 is an appearance diagram of a composite phase-change heat storage material after moisture absorption detection in embodiment 2 of the present invention;
FIG. 5 is an appearance diagram of a composite phase-change heat storage material according to comparative example 1 of the present invention after moisture absorption detection;
fig. 6 is an appearance diagram of the composite phase-change heat storage material prepared in embodiment 5 of the present invention.
Description of reference numerals:
1-inner layer, 2-middle layer, 3-outer layer.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
A composite phase change heat storage material comprises a composite phase change layer with a three-layer structure from inside to outside, namely an inner layer 1, an intermediate layer 2 and an outer layer 3, as shown in figures 1 and 2; the inner layer is formed by compounding 60 wt% of eutectic salt and 40 wt% of magnesium oxide, the middle layer is formed by compounding 40 wt% of eutectic salt and 60 wt% of magnesium oxide, and the outer layer is formed by compounding 20 wt% of eutectic salt and 60 wt% of magnesium oxide. The diameter of the composite phase-change heat storage material is 50mm, and the height of the composite phase-change heat storage material is 25 mm; wherein, the diameter of the inner layer is 42mm, the height is 17mm, and the diameter of the intermediate layer is 46mm, the height is 21 mm. The preparation process of the composite phase-change heat storage material is as follows:
(1) preparing raw materials: mixing industrial-grade sodium carbonate and potassium carbonate according to a mass ratio of 52: 48, uniformly mixing and grinding the mixture according to the mass ratio, calcining the mixture to obtain binary eutectic salt, uniformly mixing the binary eutectic salt and magnesium oxide according to the mass ratio to respectively prepare premixed powder of an inner layer, an intermediate layer and an outer layer, prepressing the premixed powder at the prepressing pressure of 8t for 30s, putting the premixed powder on an alumina ceramic plate, putting the alumina ceramic plate into an air atmosphere electric furnace for presintering at the presintering temperature of 750 ℃, crushing and ball-milling the presintering block at the ball-milling rotation speed of 175r/min for 3h to obtain uniform powder, wherein the powder is a composite raw material; wherein the ratio of the eutectic salt in the composite raw material of the inner layer is 60 wt%, the ratio of the eutectic salt in the composite raw material of the intermediate layer is 40 wt%, and the ratio of the eutectic salt in the composite raw material of the outer layer is 20 wt%.
(2) Preparing an embryo body: put into the bottom tiling of mould with the composite raw materials in bottom and form the bottom material that highly is 2mm, then put into the composite raw materials tiling in intermediate level and form the intermediate level material that highly is 2mm, at last through the cylindrical foil of diameter adjustable, adjust its diameter to the diameter size of inlayer, pour into the composite raw materials of inlayer, accomplish the inlayer and set up the back, the shim size, set up it to the diameter in intermediate level, then pour into the composite raw materials in intermediate level into, accomplish the composite raw materials in intermediate level and pour into the back, pour into outer composite raw materials into at last, and then form the idiosome.
(3) And (3) sintering: pressing the blank into a cylindrical sample by a uniaxial pressing method, wherein the applied pressure is 8t, and the dwell time is 30 s; and sintering in air atmosphere to obtain the final composite phase-change heat storage material.
Example 2
The present example is different from example 1 in the compounding ratio of the inner layer 1, the intermediate layer 2 and the outer layer 3, specifically, the inner layer is composed of 40 wt% eutectic salt and 60 wt% magnesium oxide, the intermediate layer is composed of 20 wt% eutectic salt and 80 wt% magnesium oxide, and the outer layer is composed of 0 wt% eutectic salt and 100 wt% magnesium oxide.
Example 3
The present embodiment is different from embodiment 1 in that the number of layers of the composite phase change layer in the present embodiment is different, and the number of the composite phase change layers is set as four layers, which is specifically set as follows:
a composite phase change heat storage material comprises a composite phase change layer with four layers from inside to outside, and an inner layer, a first intermediate layer, a second intermediate layer and an outer layer are sequentially arranged from inside to outside; the inner layer is formed by compounding 60 wt% of eutectic salt and 40 wt% of magnesium oxide, the first middle layer is formed by compounding 45 wt% of eutectic salt and 55 wt% of magnesium oxide, the second middle layer is formed by compounding 35 wt% of eutectic salt and 65 wt% of magnesium oxide, and the outer layer is formed by compounding 20 wt% of eutectic salt and 80 wt% of magnesium oxide. The diameter of the composite phase-change heat storage material is 50mm, and the height of the composite phase-change heat storage material is 25 mm; wherein the diameter of the inner layer is 42mm, the height is 17mm, the diameter of the first intermediate layer is 44mm, the height is 19mm, the diameter of the second intermediate layer is 46mm, the height is 21 mm. The preparation process of the composite phase-change heat storage material is as follows:
(1) preparing raw materials: mixing industrial-grade sodium carbonate and potassium carbonate according to a mass ratio of 52: 48, uniformly mixing and grinding the mixture according to the mass ratio, calcining the mixture to obtain binary eutectic salt, uniformly mixing the binary eutectic salt and magnesium oxide according to the mass ratio to respectively prepare premixed powder of an inner layer, an intermediate layer and an outer layer, prepressing the premixed powder at the prepressing pressure of 8t for 30s, putting the premixed powder on an alumina ceramic plate, putting the alumina ceramic plate into an air atmosphere electric furnace for presintering at the presintering temperature of 750 ℃, crushing and ball-milling the presintering block at the ball-milling rotation speed of 175r/min for 3h to obtain uniform powder, wherein the powder is a composite raw material; wherein the ratio of the eutectic salt in the composite raw material of the inner layer is 60 wt%, the ratio of the eutectic salt in the composite raw material of the first intermediate layer is 45 wt%, the ratio of the eutectic salt in the composite raw material of the second intermediate layer is 35 wt%, and the ratio of the eutectic salt in the composite raw material of the outer layer is 20 wt%.
(2) Preparing an embryo body: placing the composite raw material of the bottom layer into the bottom of a mould, tiling to form a bottom layer material with the height of 2mm, placing the composite raw material of a second intermediate layer on the bottom layer material, tiling to form a second intermediate layer material with the height of 1mm, placing the composite raw material of a first intermediate layer on the second intermediate layer material, tiling to form a first intermediate layer material with the height of 1mm, finally adjusting the diameter of the cylindrical metal sheet with adjustable diameter to the diameter size of the inner layer, placing the cylindrical metal sheet at the middle position of the first intermediate layer material, injecting the composite raw material of the inner layer, adjusting the size of the sheet to be the diameter of the first intermediate layer after the inner layer is set, then injecting the composite raw material of the first intermediate layer, adjusting the size of the sheet to be the diameter of the second intermediate layer after the composite raw material of the first intermediate layer is injected, then injecting the composite raw material of the second intermediate layer into the sheet, and finally injecting the composite raw material of, thereby forming a blank.
(3) And (3) sintering: pressing the blank into a cylindrical sample by a uniaxial pressing method, wherein the applied pressure is 8t, and the dwell time is 30 s; and sintering in air atmosphere to obtain the final composite phase-change heat storage material.
Example 4
The difference between this example and example 1 is that the process for preparing raw materials in this example is different, and the specific configuration is as follows:
in the preparation process of the raw materials, industrial-grade sodium carbonate and potassium carbonate are directly mixed according to the mass ratio of 52: 48, mixing, grinding uniformly, and calcining to obtain binary eutectic salt; then uniformly mixing the binary eutectic salt and magnesium oxide according to the required mass ratio to respectively prepare premixed powder of an inner layer, an intermediate layer and an outer layer, carrying out ball milling on the premixed powder, wherein the ball milling rotation speed is 175r/min, the ball milling time is 3h, and obtaining uniform powder after ball milling, wherein the powder is a composite raw material.
Example 5
The difference between this embodiment and embodiment 1 is that the number of layers of the composite phase change layer in this embodiment is different, the number of the composite phase change layers is set as two layers, and the difference between the contents of eutectic salt between two adjacent layers is greater than 20 wt%, and the specific setting is as follows:
a composite phase change heat storage material comprises a composite phase change layer with a structure from inside to outside, namely an inner layer 1 and an outer layer 3; the inner layer is formed by compounding 60 wt% of eutectic salt and 40 wt% of magnesium oxide, and the outer layer is formed by compounding 20 wt% of eutectic salt and 60 wt% of magnesium oxide. The diameter of the composite phase-change heat storage material is 50mm, and the height of the composite phase-change heat storage material is 25 mm; wherein, the diameter of the inner layer is 42mm, and the height is 17 mm. The preparation process of the composite phase-change heat storage material is as follows:
(1) preparing raw materials: mixing industrial-grade sodium carbonate and potassium carbonate according to a mass ratio of 52: 48, uniformly mixing and grinding the mixture according to the mass ratio, calcining the mixture to obtain binary eutectic salt, uniformly mixing the binary eutectic salt and magnesium oxide according to the mass ratio to respectively prepare premixed powder of an inner layer, an intermediate layer and an outer layer, prepressing the premixed powder at the prepressing pressure of 8t for 30s, putting the premixed powder on an alumina ceramic plate, putting the alumina ceramic plate into an air atmosphere electric furnace for presintering at the presintering temperature of 750 ℃, crushing and ball-milling the presintering block at the ball-milling rotation speed of 175r/min for 3h to obtain uniform powder, wherein the powder is a composite raw material; wherein the ratio of the eutectic salt in the composite raw material of the inner layer is 60 wt%, the ratio of the eutectic salt in the composite raw material of the intermediate layer is 40 wt%, and the ratio of the eutectic salt in the composite raw material of the outer layer is 20 wt%.
(2) Preparing an embryo body: the bottom of putting into the mould with the compound raw materials of bottom lay tiling and form the bottom material that the height is 2mm, then through diameter adjustable cylindrical foil, adjust its diameter to the diameter size of inlayer, pour into the compound raw materials of inlayer into, after accomplishing the inlayer and setting up, pour into outer compound raw materials into again, and then form the idiosome.
(3) And (3) sintering: pressing the blank into a cylindrical sample by a uniaxial pressing method, wherein the applied pressure is 8t, and the dwell time is 30 s; and sintering in air atmosphere to obtain the final composite phase-change heat storage material.
Comparative example 1
This example is different from example 1 in the compounding ratio of the inner layer 1, the intermediate layer 2 and the outer layer 3, specifically, the inner layer is composed of 70 wt% eutectic salt and 30 wt% magnesium oxide, the intermediate layer is composed of 50 wt% eutectic salt and 50 wt% magnesium oxide, and the outer layer is composed of 30 wt% eutectic salt and 70 wt% magnesium oxide.
Test examples
The composite phase change heat storage materials prepared in the above examples and comparative examples are tested for moisture absorption and thermal expansion performance, and the testing method is as follows: moisture absorption: at 25 deg.C and humidity of 80% RH, testing with a Giant Force humiture tester (model: ETH-1000) for 120h, and calculating its powdering rate. The specific pulverization rate calculation method comprises the following steps: weighing a test sample, placing the test sample in a temperature and humidity box, adjusting the humidity of the temperature and humidity box to 80%, adjusting the temperature to 25 ℃, placing the test sample in the temperature and humidity box for 120 hours, taking out the test sample, placing the test sample in an oven, drying the test sample at the temperature of 120 ℃ for 24 hours, taking out the test sample, recovering and weighing a pulverized part of the high-temperature composite material by using a brush, and calculating the pulverization rate, wherein the pulverization rate is the weight of the pulverized part/the weight of the test sample. The appearance of the composite phase-change heat storage material after moisture absorption detection in example 1 is shown in fig. 3, the appearance of the composite phase-change heat storage material after moisture absorption detection in example 2 is shown in fig. 4, the appearance of the composite phase-change heat storage material after moisture absorption detection in comparative example 1 is shown in fig. 5, and the appearance of the composite phase-change heat storage material prepared in example 5 is shown in fig. 6.
Thermal expansion performance: and (3) directly observing the appearance condition of the composite phase change heat storage material obtained by sintering, and observing whether deformation or cracks exist.
The phase change enthalpy of the composite phase change heat storage material is detected under the condition of normal temperature (25 ℃), and the detection result is shown in table 1.
The test results obtained by the above test method are shown in table 1 below.
TABLE 1
| Powdering ratio | Thermal expansion performance | Enthalpy of phase change (J/g) | |
| Example 1 | 1.0％ | No deformation and no crack | 78 |
| Example 2 | 0.8％ | No deformation and no crack | 52 |
| Example 3 | 1.0％ | No deformation and no crack | 83 |
| Example 4 | 1.3％ | No deformation and no crack | 78 |
| Example 5 | 1.1％ | Deformation and surface cracking | - (Performance reasons not tested) |
| Comparative example 1 | 5％ | No deformation and no crack | - (Performance reasons not tested) |
The results in table 1 show that: the embodiment of the invention can achieve higher performance of preventing moisture absorption, is not easy to absorb moisture and pulverize when the humidity reaches 80 percent, and has high stability.
Heat storage performance: in example 5, the content difference of eutectic salt between two adjacent layers is higher than 20%, so that the difference of expansion coefficients between the two layers is large, the thermal property is also large, and the problem of deformation or/and cracking of the prepared heat storage material is caused.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The composite phase change heat storage material is characterized by comprising at least two layers of composite phase change layers from inside to outside; the composite phase change layer is formed by compounding eutectic salt and magnesium oxide; the content of eutectic salt in the composite phase change layer at the outermost layer is less than or equal to 20 wt%.
2. The composite phase-change heat storage material as claimed in claim 1, wherein the content of eutectic salt in the composite phase-change layers of at least two layers from inside to outside decreases in sequence, and the difference of the content percentage of eutectic salt in the composite phase-change layers of two adjacent layers is not higher than 20 wt%.
3. The composite phase-change heat storage material as claimed in claim 1 or 2, wherein the number of the composite phase-change layers is three, namely an inner layer, an intermediate layer and an outer layer, wherein the content of eutectic salt in the inner layer is 40-60 wt%, the content of eutectic salt in the intermediate layer is 20-40 wt%, and the content of eutectic salt in the outer layer is less than or equal to 20 wt%.
4. The composite phase-change heat storage material as claimed in any one of claims 1 to 3, wherein the eutectic salt is Na2CO3-K2CO3。
5. The method for preparing a composite phase-change heat storage material as claimed in any one of claims 1 to 4, comprising:
preparing raw materials: obtaining eutectic salt and magnesium oxide, and respectively preparing composite raw materials of each composite phase change layer according to the proportion;
preparing an embryo body: preparing a blank body with at least two layers of composite phase change layers by adopting composite raw materials;
and (3) sintering: and pre-pressing and sintering the blank to obtain the composite phase change heat storage material.
6. The method of claim 5 wherein the eutectic salt is Na2CO3-K2CO3The preparation process comprises the following steps: mixing and grinding sodium carbonate and potassium carbonate uniformly, and calcining to obtain the eutectic salt.
7. The method for preparing a composite phase-change heat storage material according to claim 5 or 6, wherein the composite raw material is obtained by blending eutectic salt and magnesium oxide, pre-sintering, crushing and grinding.
8. The preparation method of the composite phase-change heat storage material as claimed in claim 7, wherein the pre-sintering temperature is 700-800 ℃, preferably 750 ℃; or, the crushed and ground composite raw material is sieved by a 150-mesh sieve; preferably, the milling is ball milling.
9. The method for preparing a composite phase-change heat storage material according to any one of claims 5 to 8, wherein when the number of layers of the composite phase-change layer is three; the specific process of the embryo body preparation is as follows:
laying the composite raw material of the outer layer at the bottom of the mould, and laying the composite raw material of the middle layer according to the position of the middle layer;
the diameter of the cylindrical metal sheet with the adjustable diameter is adjusted to be the same as the size of the inner layer, and the cylindrical metal sheet is placed above the composite raw material paved with the middle layer; injecting the composite raw material of the inner layer into the middle of the cylindrical metal sheet;
adjusting the diameter of the cylindrical metal sheet to be the same as the size of the middle layer, and injecting the composite raw material of the middle layer into the cylindrical metal sheet to completely cover the inner layer;
and finally, injecting the composite raw material of the outer layer to completely cover the middle layer to obtain a blank.
10. The method for preparing a composite phase change heat storage material according to any one of claims 5 to 9, wherein the pre-pressing pressure is increased by uniaxial pressing; preferably, the applied pressure is 8t and the dwell time is 30 s.
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| CN116814225A (en) * | 2023-08-31 | 2023-09-29 | 北京智慧能源研究院 | High-heat-conductivity composite structure heat storage material applicable to high-cold high-altitude areas and preparation method thereof |
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Application publication date: 20210316 |