CN114644906B - 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
The invention discloses a preparation method of a composite phase-change heat storage material, which comprises the following steps: mixing kaolin, talcum, andalusite and alumina, ball milling, adding expanded graphite, mixing, continuously adding a binder, a plasticizer and a pore-forming agent to obtain a mixture, foaming and curing the mixture, and heating the cured blank to 1300-1500 ℃ in vacuum or inert atmosphere to obtain a foam ceramic matrix material; b, mixing inorganic salt of the phase change material with the expanded graphite, and ball milling to obtain the phase change material; c, dipping the prepared foam ceramic matrix material and the phase change material in vacuum or inert atmosphere at the temperature higher than the phase change temperature of the phase change material to obtain the composite phase change heat storage material. The composite phase-change heat storage material prepared by the method has the advantages of high filling rate, corrosion resistance, good thermal conductivity, high heat filling and releasing rate, high heat storage density and low production cost.
Description
Technical Field
The invention belongs to the technical field of phase-change heat storage, and particularly relates to a composite phase-change heat storage material, and a preparation method of the composite phase-change heat storage material.
Background
The heat storage can alleviate the problems of discontinuous and unstable supply of clean energy and mismatch between peak-valley alternation of a power grid and power load intensity change. Compared with the sensible heat storage technology, the phase change heat storage technology increases the latent heat storage and release of heat in a phase change process in a state close to constant temperature, so that the phase change heat storage technology has important application value in the fields of building cold supply and heat supply, solar thermal power generation and valley electricity utilization. The core of the phase-change heat storage technology is a phase-change material, wherein inorganic salt is low in price, high in phase-change latent heat, high in specific heat and stable in chemical property, and the phase-change heat storage material is widely used. However, inorganic salts are easy to leak in the solid-liquid phase change process, and have poor heat conducting performance, so that the charge and discharge rate is affected.
Therefore, a composite phase-change heat storage material needs to be developed to solve the problems that the inorganic salt phase-change material is easy to leak and poor in heat conductivity in the use process.
Disclosure of Invention
The present invention has been made based on the findings and knowledge of the inventors regarding the following facts and problems: at present, the combination of the inorganic salt phase-change material and the matrix material with good compatibility is a main method for solving the problems that inorganic salt is easy to leak, has poor heat conducting property and has low charge and discharge rate in the solid-liquid phase change process. Although the prior art provides a basic idea of compounding a porous matrix and a phase-change material, the heat-conducting property of the matrix material and the phase-change material is not fundamentally solved at the same time, the bottleneck of low heat charging and discharging rate still exists, the material price of part of metals is high, the filling rate of part of materials is low due to the adoption of macroporous packaging phase-change materials, the potential leakage problem is accompanied, and the practical engineering application is still limited.
The present invention aims to solve at least one of the technical problems in the related art to some extent.
Therefore, the embodiment of the first aspect of the invention provides a preparation method of the composite phase-change heat storage material, which can solve the leakage problem of liquid inorganic salt, and meanwhile, the prepared composite phase-change heat storage material has the advantages of high filling rate, corrosion resistance, good thermal conductivity, high heat charging and discharging rate, high heat storage density and low production cost.
According to the preparation method of the composite phase-change heat storage material, the embodiment of the first aspect of the invention comprises the following steps:
a. preparing a matrix material: mixing and ball milling 7-15 parts by weight of kaolin, 8-15 parts by weight of talcum, 55-80 parts by weight of andalusite and 4-10 parts by weight of alumina, adding 0.5-1.3 parts by weight of expanded graphite, mixing, continuously adding a binder, a plasticizer and a pore-forming agent to obtain a mixture, foaming and curing the mixture, and heating the cured blank to 1300-1500 ℃ in vacuum or inert atmosphere to obtain a foamed ceramic matrix material;
b. preparing a phase change material: mixing 98-99 parts by weight of inorganic salt of a phase change material with 1-2 parts by weight of expanded graphite, and ball milling to obtain the phase change material;
c. preparing a composite phase change heat storage material: and c, under vacuum or inert atmosphere, soaking the foam ceramic matrix material prepared in the step a and the phase-change material prepared in the step b at a temperature higher than the phase-change temperature of the phase-change material to obtain the composite phase-change heat storage material.
According to the advantages and technical effects brought by the independent claims provided by the embodiment of the first aspect of the invention, 1, the foam ceramic matrix material is prepared by compounding porous ceramic and expanded graphite, has good compatibility with the phase change material, can fully adsorb the phase change material, and has high filling rate and low leakage rate; 2. the raw materials for preparing the matrix material in the embodiment of the invention adopt low-cost raw ores, the preparation cost is low, and the ceramic matrix material is a cordierite-mullite ceramic system, so that the ceramic matrix material has the advantage of good thermal shock resistance, and the problem that the common ceramic material is easy to crack when heated is avoided; 3. according to the method provided by the embodiment of the invention, the expanded graphite is added into the phase change material, so that the charging and discharging rate, the heat conductivity coefficient and the heat storage density of the composite material are obviously improved; 4. in the method provided by the embodiment of the invention, the foam ceramic matrix material and the phase-change material are immersed in vacuum or inert atmosphere, so that the filling rate and the heat conductivity coefficient of the phase-change material are improved, and a large number of air holes in the composite phase-change heat storage material are avoided.
According to the preparation method of the composite phase-change heat storage material, the preparation method of the expanded graphite in the step a and/or the step b comprises the following steps: placing the expandable graphite with the carbon mass content of more than 98% in a muffle furnace, and heating for 40-60 seconds at 750-850 ℃ to prepare the expandable graphite.
According to the preparation method of the composite phase-change heat storage material, in the first aspect of the embodiment of the invention, in the step a, the pore-forming agent is selected from at least one of sucrose, polystyrene, polyvinyl chloride, wood dust or carbon powder, and/or the addition amount of the pore-forming agent is 5-10 parts by weight.
According to the preparation method of the composite phase-change heat storage material, in the step a, the plasticizer is phthalate, and/or the adding amount of the plasticizer is 1-3 parts by weight.
According to the preparation method of the composite phase-change heat storage material, in the first aspect of the embodiment of the invention, in the step a, the binder is at least one selected from cellulose, polyvinyl alcohol, dextrin or clay, and/or the plasticizer is added in an amount of 2-8 parts by weight.
According to the preparation method of the composite phase-change heat storage material, which is provided by the embodiment of the first aspect of the invention, the porosity of the foam ceramic matrix material prepared in the step a is 70-90%.
According to the preparation method of the composite phase-change heat storage material, in the step b, the inorganic salt of the phase-change material is at least one selected from nitrate, carbonate or chloride.
According to the preparation method of the composite phase-change heat storage material, in the step b, the inorganic salt of the phase-change material is mixed carbonate of sodium carbonate and barium carbonate.
According to the preparation method of the composite phase-change heat storage material, in the step c, the soaking time is 1-2 h.
The embodiment of the second aspect of the invention also provides a composite phase-change heat storage material, which is prepared by adopting the preparation method of the embodiment of the first aspect of the invention.
According to the advantages and technical effects brought by the independent claims of the embodiment of the second aspect of the invention, the composite phase-change heat storage material of the embodiment of the invention has the excellent performances of high filling rate, corrosion resistance, good thermal conductivity, high heat charging and discharging rate and high heat storage density, and the preparation method is simple and the production cost is low.
Detailed Description
The following detailed description of embodiments of the invention is exemplary and intended to be illustrative of the invention and not to be construed as limiting the invention.
According to the preparation method of the composite phase-change heat storage material, the embodiment of the first aspect of the invention comprises the following steps:
a. preparing a matrix material: mixing and ball milling 7-15 parts by weight of kaolin, 8-15 parts by weight of talcum, 55-80 parts by weight of andalusite and 4-10 parts by weight of alumina, adding 0.5-1.3 parts by weight of expanded graphite, mixing, continuously adding a binder, a plasticizer and a pore-forming agent to obtain a mixture, foaming and curing the mixture, preferably, keeping the foaming and curing temperature at 180 ℃, keeping the temperature for 10-20 hours, and heating the cured blank to 1300-1500 ℃ in vacuum or inert atmosphere to obtain a foamed ceramic matrix material;
b. preparing a phase change material: mixing 98-99 parts by weight of inorganic salt of a phase change material with 1-2 parts by weight of expanded graphite, and ball milling to obtain the phase change material;
c. preparing a composite phase change heat storage material: and c, under vacuum or inert atmosphere, soaking the foam ceramic matrix material prepared in the step a and the phase-change material prepared in the step b at a temperature higher than the phase-change temperature of the phase-change material to obtain the composite phase-change heat storage material.
According to the advantages and technical effects brought by the independent claims provided by the embodiment of the first aspect of the invention, 1, the foam ceramic matrix material is prepared by compounding porous ceramic and expanded graphite, has good compatibility with the phase change material, can fully adsorb the phase change material, and has high filling rate and low leakage rate; 2. the raw materials for preparing the matrix material in the embodiment of the invention adopt low-cost raw ores, the preparation cost is low, and the ceramic matrix material is a cordierite-mullite ceramic system, so that the ceramic matrix material has the advantage of good thermal shock resistance, and the problem that the common ceramic material is easy to crack when heated is avoided; 3. according to the method provided by the embodiment of the invention, the expanded graphite is added into the phase change material, so that the charging and discharging rate, the heat conductivity coefficient and the heat storage density of the composite material are obviously improved; 4. in the method provided by the embodiment of the invention, the foam ceramic matrix material and the phase-change material are immersed in vacuum or inert atmosphere, so that the filling rate and the heat conductivity coefficient of the phase-change material are improved, and a large number of air holes in the composite phase-change heat storage material are avoided.
According to the preparation method of the composite phase-change heat storage material, the preparation method of the expanded graphite in the step a and/or the step b comprises the following steps: placing the expandable graphite with the carbon mass content of more than 98% in a muffle furnace, and heating for 40-60 seconds at 750-850 ℃ to prepare the expandable graphite. In the embodiment of the invention, the expanded graphite is added into the matrix material and the phase change material, so that the heat charging and discharging rate, the heat conductivity coefficient and the heat storage density of the composite phase change heat storage material are obviously improved.
According to the preparation method of the composite phase-change heat storage material, in the first aspect of the embodiment of the invention, in the step a, the pore-forming agent is selected from at least one of sucrose, polystyrene, polyvinyl chloride, wood dust or carbon powder, and/or the addition amount of the pore-forming agent is 5-10 parts by weight. In the embodiment of the invention, the pore-forming agent is added, the pore-forming agent occupies a certain space in the blank, and after sintering, the pore-forming agent leaves the matrix to form pores. The amount of pore-forming agent used can affect the porosity and pore structure, and the amount of pore-forming agent used is too small, the porosity is too small, and the amount of pore-forming agent used is too large, so that the strength of the ceramic can be affected, and in the embodiment of the invention, the addition amount of pore-forming agent is preferably 5-10 parts by weight.
According to the preparation method of the composite phase-change heat storage material, in the first aspect of the embodiment of the invention, in the step a, the plasticizer is selected from phthalates, and/or the adding amount of the plasticizer is 1-3 parts by weight. According to the embodiment of the invention, the plasticizer is added, so that the toughness of the ceramic material can be enhanced by the plasticizer. Too little plasticizer is used to achieve plasticizing effect, and if too much is used, the ratio of the matrix material is reduced.
According to the preparation method of the composite phase-change heat storage material, in the first aspect of the embodiment of the invention, in the step a, the binder is at least one selected from cellulose, polyvinyl alcohol, dextrin or clay, and/or the plasticizer is added in an amount of 2-8 parts by weight.
According to the preparation method of the composite phase-change heat storage material, which is provided by the embodiment of the first aspect of the invention, the porosity of the foam ceramic matrix material prepared in the step a is 70-90%. The foam ceramic matrix material prepared by the method disclosed by the embodiment of the invention has high porosity, good compatibility with the phase-change material, capability of fully adsorbing the phase-change material and high filling rate of the phase-change material, so that the heat storage density is increased.
According to the preparation method of the composite phase-change heat storage material, in the first aspect of the embodiment of the invention, in the step b, the inorganic salt of the phase-change material is selected from at least one of nitrate, carbonate or chloride, preferably mixed carbonate of sodium carbonate and barium carbonate.
According to the preparation method of the composite phase-change heat storage material, in the step c, the addition amount of the foam ceramic matrix material prepared in the step a is 45-40 parts by weight, and/or the addition amount of the phase-change material prepared in the step b is 55-60 parts by weight. In the embodiment of the invention, the adding amount of the phase-change material prepared in the step b is not particularly limited in the impregnation process of the matrix material and the phase-change material, and the phase-change material can be fully filled into the pore canal of the foamed ceramic only by adding enough phase-change material.
The embodiment of the second aspect of the invention also provides a composite phase-change heat storage material, which is prepared by adopting the preparation method of the embodiment of the first aspect of the invention.
According to the advantages and technical effects brought by the independent claims of the embodiment of the second aspect of the invention, the composite phase-change heat storage material of the embodiment of the invention has the excellent performances of high filling rate, corrosion resistance, good thermal conductivity, high heat charging and discharging rate and high heat storage density, and the preparation method is simple and the production cost is low.
The present invention will be described in detail with reference to examples.
Example 1
(1) Preparing expanded graphite: placing high-purity expandable graphite with granularity of more than 100 meshes and carbon mass content of more than 98% into a muffle furnace, and heating at 800 ℃ for 50 seconds to prepare the expanded graphite.
(2) Preparing a foam ceramic matrix material: mixing 10 parts by weight of kaolin, 10 parts by weight of talcum, 70 parts by weight of andalusite and 9 parts by weight of alumina ingredients, ball-milling, sieving with a 200-mesh sieve, adding 1 part by weight of expanded graphite, fully mixing, and adding a binder, a plasticizer and 10 parts by weight of sucrose to prepare a mixture. Heating the mixture to 180 ℃, preserving heat for 20 hours, foaming and curing, and heating the cured blank to 1500 ℃ in an inert atmosphere to obtain the foamed ceramic matrix material with the porosity of 80-90%.
(3) Preparing a phase change material: adding 98 parts by weight of mixed carbonate with the purity of more than 99% into 2 parts by weight of expanded graphite, mixing, ball milling and sieving with a 200-mesh sieve to obtain the phase change material, wherein the mixed carbonate comprises 46% of sodium carbonate and 54% of barium carbonate by mass.
(4) Preparing a composite phase change heat storage material: and (3) transferring a sufficient amount of phase change material and the foam ceramic matrix material into high-temperature vacuum equipment, and fully soaking at a temperature higher than 700 ℃, for example, 750 ℃ for 1h, so that the phase change material is filled into the pore channels of the foam ceramic matrix material, thereby obtaining the composite phase change heat storage material.
In the composite phase-change heat storage material prepared by the embodiment, the filling rate of the phase-change material is 65%, the thermal conductivity is 7.3W/m.K, the heat storage density is 835kJ/kg under the temperature difference condition of 450 ℃, and the leakage rate is less than 3% after 7500 times of cold and hot cycles.
Example 2
(1) Preparing expanded graphite: placing high-purity expandable graphite with granularity of more than 100 meshes and carbon mass content of more than 98% into a muffle furnace, and heating at 800 ℃ for 50 seconds to prepare the expanded graphite.
(2) Preparing a foam ceramic matrix material: mixing 7 parts by weight of kaolin, 8 parts by weight of talcum, 80% by weight of andalusite and 4 parts by weight of alumina ingredients, ball-milling, sieving with a 200-mesh sieve, mixing 1 part by weight of expanded graphite, fully mixing, and adding a binder, a plasticizer and 7 parts by weight of wood chips to prepare a mixture. Heating the mixture to 180 ℃, preserving heat for 15 hours, foaming and curing, and heating the cured blank to 1300 ℃ in an inert atmosphere to obtain the foamed ceramic matrix material with the porosity of 80-90%.
(3) Preparing a phase change material: adding 98 parts by weight of mixed chloride with the purity of more than 99% into 2 parts by weight of expanded graphite, mixing, ball milling and sieving with a 200-mesh sieve to obtain the phase change material, wherein the mixed chloride comprises 50% of sodium chloride and 50% of magnesium chloride by mass.
(4) Preparing a composite phase change heat storage material: and (3) transferring a sufficient amount of phase change material and the foam ceramic matrix material into high-temperature vacuum equipment, and fully soaking at a temperature higher than 300 ℃, for example, at 350 ℃ for 1.5 hours, so that the phase change material is filled into the pore channels of the foam ceramic matrix material, thereby obtaining the composite phase change heat storage material.
In the composite phase-change heat storage material prepared by the embodiment, the filling rate of the phase-change material is 65%, the thermal conductivity is 5.7W/m.K, the heat storage density is 647kJ/kg under the temperature difference condition of 250 ℃, and the leakage rate is less than 3% after 7500 times of cold and hot cycles.
Example 3
(1) Preparing expanded graphite: placing high-purity expandable graphite with granularity of more than 100 meshes and carbon mass content of more than 98% into a muffle furnace, and heating at 750 ℃ for 60 seconds to prepare the expanded graphite.
(2) Preparing a foam ceramic matrix material: 15 parts by weight of kaolin, 15 parts by weight of talcum, 58 parts by weight of andalusite and 10 parts by weight of alumina are mixed, ball-milled and sieved by a 200-mesh sieve, 2 parts by weight of expanded graphite is added, and after full mixing, a binder, a plasticizer and a pore-forming agent are added to prepare the mixture. Heating the mixture to 180 ℃, preserving heat for 20 hours, foaming and curing, and heating the cured blank to 1500 ℃ in an inert atmosphere to obtain the foamed ceramic matrix material with the porosity of 80-90%.
(3) Preparing a phase change material: adding 98 parts by weight of mixed carbonate with the purity of more than 99% into 2 parts by weight of expanded graphite, mixing, ball milling and sieving with a 200-mesh sieve to obtain the phase change material, wherein the mixed carbonate comprises 62% of sodium carbonate and 38% of barium carbonate by mass.
(4) Preparing a composite phase change heat storage material: and (3) transferring a sufficient amount of phase change material and the foam ceramic matrix material into high-temperature vacuum equipment, and fully soaking at a temperature higher than 700 ℃, for example, 750 ℃ for 1h, so that the phase change material is filled into the pore channels of the foam ceramic matrix material, thereby obtaining the composite phase change heat storage material.
In the composite phase-change heat storage material prepared by the embodiment, the filling rate of the phase-change material is 63%, the thermal conductivity is 5.9W/m.K, the heat storage density is 712kJ/kg under the temperature difference condition of 450 ℃, and the leakage rate is less than 3% after 7500 times of cold and hot cycles.
Comparative example 1
The same procedure as in example 1 was conducted except that the expanded graphite was not added to the ceramic base material prepared in step (2).
In the composite phase-change heat storage material prepared in the comparative example 1, the filling rate of the phase-change material is 65%, the thermal conductivity is 1.5W/m.K, the heat storage density is 835kJ/kg under the temperature difference condition of 450 ℃, and the leakage rate is 4% after 7500 times of cold and hot cycles.
Comparative example 2
The same method as that of comparative example 1 is different in that the phase change material prepared in step (3) is directly prepared by using mixed carbonate as the phase change material without adding expanded graphite.
In the composite phase-change heat storage material prepared in the comparative example 2, the filling rate of the phase-change material is 65%, the thermal conductivity is 1.7W/m.K, the heat storage density is 835kJ/kg under the temperature difference condition of 450 ℃, and the leakage rate is 4% after 7500 times of cold and hot cycles.
Comparative example 3
The same procedure as in example 1 was followed except that in the preparation of the ceramic base material in step (2), the cured green body was not limited to being heated to 1500℃under vacuum or an inert atmosphere.
In the composite phase-change heat storage material prepared in the comparative example 3, the filling rate of the phase-change material is 48%, the thermal conductivity is 7.1W/m.K, the heat storage density is 741kJ/kg under the temperature difference condition of 450 ℃, and the leakage rate is 7% after 7500 times of cold and hot cycles.
Comparative example 4
The same ceramic material matrix composition and phase change material inorganic salt adopted in example 1 are adopted, except that after mixing kaolin, talcum, andalusite, alumina and mixed carbonate, ball milling and sieving with a 200-mesh sieve, adding binder, plasticizer and sucrose, adding the expanded graphite prepared in step (1), and sintering at 750 ℃ in high-temperature vacuum equipment, thus obtaining the composite phase change heat storage material.
In the composite phase-change heat storage material prepared in the comparative example 4, the filling rate of the phase-change material is 53%, the thermal conductivity is 3.2W/m.K, the heat storage density is 732kJ/kg under the temperature difference condition of 450 ℃, and the leakage rate is 4% after 7500 times of cold and hot cycles.
Comparative example 5
The same procedure as in example 1 is followed except that in step (4), the phase change material and the ceramic foam matrix material are impregnated under a non-vacuum or inert atmosphere.
The composite phase-change heat storage material prepared in comparative example 5 contains a large number of air holes, the filling rate of the phase-change material is 30%, the thermal conductivity is 5.2W/m.K, the heat storage density is 687kJ/kg under the temperature difference condition of 450 ℃, and the leakage rate is 7% after 7500 times of cold and hot cycles.
For purposes of this disclosure, the terms "one embodiment," "some embodiments," "example," "a particular example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (8)
1. The preparation method of the composite phase-change heat storage material is characterized by comprising the following steps of:
a. preparing a matrix material: mixing and ball milling 7-15 parts by weight of kaolin, 8-15 parts by weight of talcum, 55-80 parts by weight of andalusite and 4-10 parts by weight of alumina, adding 0.5-1.3 parts by weight of expanded graphite for mixing, continuously adding a binder, a plasticizer and a pore-forming agent to obtain a mixture, foaming and curing the mixture, and heating the cured blank to 1300-1500 ℃ in vacuum or inert atmosphere to obtain a foamed ceramic matrix material;
b. preparing a phase change material: mixing 98-99 parts by weight of inorganic salt of a phase-change material with 1-2 parts by weight of expanded graphite, and ball-milling to obtain the phase-change material, wherein the inorganic salt of the phase-change material is at least one of nitrate, carbonate or chloride;
c. preparing a composite phase change heat storage material: c, under vacuum or inert atmosphere, soaking the foam ceramic matrix material prepared in the step a and the phase-change material prepared in the step b at a temperature higher than the phase-change temperature of the phase-change material to obtain a composite phase-change heat storage material;
the preparation method of the expanded graphite in the step a and/or the step b comprises the following steps: placing the expandable graphite with the carbon mass content of more than 98% in a muffle furnace, and heating for 40-60 seconds at 750-850 ℃ to prepare the expandable graphite.
2. The method for preparing a composite phase-change heat storage material according to claim 1, wherein in the step a, the pore-forming agent is at least one selected from sucrose, polystyrene, polyvinyl chloride, wood dust and carbon powder, and/or the addition amount of the pore-forming agent is 5-10 parts by weight.
3. The method for preparing a composite phase-change heat storage material according to claim 1, wherein in the step a, the plasticizer is phthalate esters and/or the plasticizer is added in an amount of 1-3 parts by weight.
4. The method for preparing a composite phase-change heat storage material according to claim 1, wherein in the step a, the binder is at least one selected from cellulose, polyvinyl alcohol, dextrin and clay, and/or the plasticizer is added in an amount of 2-8 parts by weight.
5. The method for preparing the composite phase-change heat storage material according to claim 1, wherein the porosity of the foamed ceramic matrix material prepared in the step a is 70-90%.
6. The method for preparing a composite phase-change heat storage material according to claim 1, wherein in the step b, the inorganic salt of the phase-change material is a mixed carbonate of sodium carbonate and barium carbonate.
7. The method for preparing a composite phase-change heat storage material according to claim 1, wherein in the step c, the soaking time is 1-2 hours.
8. A composite phase change heat storage material, characterized in that it is produced by the production method according to any one of claims 1 to 7.
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