CN114015418B - Thermochemical adsorption heat storage material with efficient mass and heat transfer and preparation method thereof - Google Patents
Thermochemical adsorption heat storage material with efficient mass and heat transfer and preparation method thereof Download PDFInfo
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Abstract
The invention provides a thermochemical adsorption heat storage material with high-efficiency mass and heat transfer and a preparation method thereof, belonging to the field of thermochemical heat storage; the preparation method adopts a step-by-step pore-forming method to increase the specific surface area and pore volume of the chemical adsorption material, improves the mass transfer performance of the composite material, and the prepared material has good mass transfer and heat transfer performance and high heat storage density. The material comprises the following components in percentage by mass: 35-60% of alkaline earth metal inorganic salt, 35-55% of modified diatomite, 3-15% of porous carbon-based heat conducting agent and 1-4% of binder; the method adopts the carbon dioxide and calcium oxide which are high-temperature pyrolysis products of calcium carbonate to perform pore-forming and pore structure regulation and control on diatomite step by step, and mainly adopts the principle that new pores are formed on the surface of the diatomite by the impact force of carbon dioxide generated by high-temperature pyrolysis of the calcium carbonate, and then calcium hydroxide is generated after calcium oxide is hydrated by soaking treatment and reacts with silicon dioxide in the diatomite to generate calcium silicate, so that the diatomite is further subjected to pore-forming and pore structure regulation and control.
Description
Technical Field
The invention belongs to the field of thermochemical heat storage, and particularly relates to a thermochemical adsorption heat storage material with efficient mass and heat transfer and a preparation method thereof.
Background
The rapid development of the modern industry consumes large amounts of fossil fuels, resulting in enormous environmental problems. However, to solve these problems, it is necessary to increase the utilization rate of renewable energy sources, such as solar energy, wind energy, etc., and convert them into electric energy and thermal energy to replace fossil energy sources. However, inconsistencies between the generation and consumption of renewable energy often lead to wasted resources.
Thermal energy storage offers a promising solution to address supply and demand mismatch. Thermal energy storage can be divided into three types, sensible heat storage, phase change heat storage and thermochemical heat storage. The thermochemical heat storage has the advantages of high energy density, small heat loss and the like, and is widely paid attention to people. Among the numerous thermochemical heat storage materials, hydrated salt thermochemical adsorption materials are one commonly used thermochemical heat storage material, whose heat storage and release processes are performed by hydration and dehydration, respectively. Compared with other thermochemical heat storage materials, the hydrated salt thermochemical adsorption material has the advantages of environmental protection, low cost, safety and the like, the reaction temperature range can be widely applied to the fields of solar cross-season heat storage, other low-grade heat recovery and the like, but the problems of expansion caking, low heat conduction performance and the like exist in the use process, so that the mass transfer and heat transfer performance of the material are reduced, the heat storage performance is rapidly attenuated in the long-period use process, and the large-scale commercial application of the material is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the thermochemical adsorption heat storage material with high-efficiency mass and heat transfer and the preparation method thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a thermochemical adsorption heat storage material with high-efficiency mass and heat transfer comprises the following components in percentage by mass:
35-60% of alkaline earth metal inorganic salt;
35-55% of modified diatomite;
3-15% of porous carbon-based heat conducting agent;
1-4% of adhesive.
Preferably, the thermochemical adsorption heat storage material comprises:
56.4% of alkaline earth metal inorganic salt;
35.6% of modified diatomite;
6.0% of porous carbon-based heat conducting agent;
2.0% of binder.
Specifically, the alkaline earth metal inorganic salt is magnesium sulfate, strontium bromide, strontium chloride or magnesium chloride;
the modified diatomite is diatomite subjected to pore-forming pretreatment, and the mass ratio of calcium silicate in the modified diatomite is 0.8% -5%;
the porous carbon-based heat conducting agent is expanded graphite or activated carbon;
the binder is carboxymethyl cellulose or starch;
preferably, the water vapor adsorption/desorption reaction temperature range of the thermochemical adsorption heat storage material for efficient mass and heat transfer is 30-120 ℃.
A preparation method of a thermochemical adsorption heat storage material with high-efficiency mass and heat transfer comprises the following steps:
(1) Pore-forming: mixing diatomite and calcium carbonate according to a mass ratio of 10:0.1-10:0.5, and standing at a constant temperature of 950 ℃ for 3-10 hours, wherein the calcium carbonate is decomposed at the moment, carbon dioxide is quickly released and dissipated into the air, and new holes are formed in the diatomite under the action of airflow impact; mixing the mixture with deionized water in a volume ratio of 1:1-1:5, standing in a water bath at 50-90 ℃ for 5-30 min, carrying out hydration reaction on calcium oxide which is another decomposition product of calcium carbonate to generate calcium hydroxide, and reacting the calcium hydroxide with silicon dioxide in diatomite to generate calcium silicate, so that the size of pores in a carrier is enlarged, pores are further formed, and finally washing, filtering and drying at 120-150 ℃ to constant weight;
(2) Ball milling: ball milling the mixture subjected to pore forming in the step (1) for 1-3 hours at the rotating speed of 20-50 r/min, and then passing through a standard sieve with 100 meshes and 200 meshes to obtain a middle layer to obtain a carrier A; the porous carbon-based heat conducting agent passes through a 300-mesh standard sieve and a 400-mesh standard sieve in the same ball milling mode, and an intermediate layer is taken to obtain a carrier B;
(3) Mixing: mixing the carrier A and the carrier B subjected to ball milling in the step (2) according to a mass ratio of 55:1-7.5:1 to obtain a mixture C;
(4) Dipping: dissolving alkaline earth metal inorganic salt in water to obtain alkaline earth metal inorganic salt water solution with the mass concentration of 5-25%; dripping the obtained alkaline earth metal inorganic salt water solution into the mixture C until the material is just immersed, and continuously stirring the mixture C in the dripping process; finally, sealing and standing for 24-48 hours, and filtering to obtain a product D;
(5) Granulating: adding 1-4% of binder and 6-15% of deionized water into the product D obtained in the step (4), and then carrying out rotary granulation for 15-60 min at a rotating speed of 500-2500 r/min to obtain particles E;
(6) And (3) drying: and (3) drying the particles E in the step (5) at 120-150 ℃ for 1-5 h to obtain a finished product.
The beneficial effects are that: the invention provides a thermochemical adsorption heat storage material with high-efficiency mass and heat transfer and a preparation method thereof, and compared with the prior art, the thermochemical adsorption heat storage material has the following advantages:
1. according to the preparation method, the carbon dioxide and the calcium oxide which are high-temperature pyrolysis products of the calcium carbonate are utilized to perform pore-forming and pore structure regulation and control on the diatomite step by step, the main principle is that new pores are formed on the surface of the diatomite by the impact force of the carbon dioxide generated by the high-temperature pyrolysis of the calcium carbonate, then calcium hydroxide is generated after the calcium oxide is hydrated by soaking treatment and reacts with silicon dioxide in the diatomite to generate calcium silicate, the diatomite is further subjected to pore-forming and pore structure regulation and control, and the chemical reaction step-by-step pore-forming method increases the specific surface area and pore volume of the chemical adsorption material and improves the mass transfer performance of the composite material;
2. the porous carrier subjected to pore-forming pretreatment and the expanded porous carbon-based heat conducting agent are mixed and then are immersed together, so that the expanded porous carbon-based heat conducting agent can be uniformly distributed on the surfaces and the periphery of porous carrier particles, and simultaneously, an adsorbate high-heat-conductivity transmission channel among the porous carrier particles is established, and compared with a traditional single carrier immersion method, the heat transfer performance of the chemical adsorption material is further improved.
Drawings
FIG. 1 is a scanning electron microscope image of diatomaceous earth of example 1 without pore-forming pretreatment;
FIG. 2 is a scanning electron microscope image of the pretreated diatomaceous earth obtained in example 1;
FIG. 3 is a scanning electron microscope image of the composite chemisorbed thermal storage material obtained in example 1;
FIG. 4 is a DSC graph of the diatomite pore-forming pretreated composite chemisorbed heat storage material obtained in example 1;
FIG. 5 is a DSC graph of the diatomite pore-forming pretreated composite chemisorbed heat storage material obtained in example 2;
FIG. 6 is a scanning electron microscope image of the pretreated diatomaceous earth obtained in comparative example 1 after pore formation;
FIG. 7 is a DSC graph of the diatomite pore-forming pretreatment composite heat storage material obtained in comparative example 1;
FIG. 8 is a DSC graph of the diatomite untreated composite chemisorbed heat storage material obtained in comparative example 2.
Detailed Description
The invention is described in detail below with reference to the attached drawings and the specific embodiments:
example 1
Mixing untreated diatomite and calcium carbonate according to a mass ratio of 10:0.3, standing at 950 ℃ for 5 hours, mixing the mixture and deionized water according to a volume ratio of 1:3, standing in a water bath at 80 ℃ for 15 minutes, washing, filtering and drying at 150 ℃ to constant weight; ball milling the mixture after pore forming for 2 hours, wherein the rotation speed of the ball mill is 30r/min, and then passing through a standard sieve with 100 meshes and 200 meshes, and taking an intermediate layer to obtain a carrier A; the expanded graphite passes through a 300-mesh standard sieve and a 400-mesh standard sieve in the same ball milling mode, and an intermediate layer is taken to obtain a carrier B; mixing the carrier A and the carrier B according to a mass ratio of 35.6:6 to obtain a mixture C; dissolving magnesium sulfate in water to obtain a solution with the mass concentration of 25%, and then dropwise adding the solution into the mixture C until the material is just immersed, and continuously stirring the mixture C in the dropwise adding process; finally, sealing and standing for 24 hours, and filtering to obtain a product D; adding 2% of carboxymethyl cellulose and 10% of deionized water into the D, and performing rotary granulation at a rotating speed of 1500r/min for 30min to obtain particles E; and drying the particles E at 150 ℃ for 2 hours to obtain the composite thermochemical adsorption spherical particles with the average particle size of 3-5 mm.
The scanning electron microscope of untreated diatomite is shown in figure 1, the scanning electron microscope of diatomite after pore-forming treatment is shown in figure 2, and the comparison of figures 1 and 2 shows that the size of pores of diatomite pretreated by the method of the invention is increased, and the number of pores is more; a typical scanning electron microscope image of the composite chemical adsorption heat storage material prepared by the invention is shown in figure 3, and magnesium sulfate enters the pore canal of diatomite and is uniformly distributed on the surface of a carrier.
The DSC test results of the composite thermochemical adsorption material obtained in the embodiment are shown in FIG. 4, and the initial temperature of the water vapor desorption reaction is 32.5 ℃, 66.6 ℃ and 110.9 ℃ respectively, the desorption reaction heat is 813.1kJ/kg, and the composite thermochemical adsorption material shows higher heat storage performance. The pore structure test results of the composite thermochemical adsorption material obtained by the embodiment are shown in table 1, the heat conduction test results are shown in table 2, the obtained composite thermochemical adsorption material has the largest specific surface area, pore volume and average pore diameter after the two-step chemical reaction pore-forming pretreatment, and meanwhile, the heat conduction test results have higher heat conduction coefficients and accord with the expectation of the invention.
Example 2
Mixing untreated diatomite and calcium carbonate according to a mass ratio of 10:0.3, standing at 950 ℃ for 3 hours, mixing the mixture and deionized water according to a volume ratio of 1:3, standing in a water bath at 80 ℃ for 15 minutes, washing, filtering and drying at 130 ℃ to constant weight; ball milling the mixture after pore forming for 1.5h, wherein the rotation speed of the ball mill is 30r/min, and then passing through a standard sieve with 100 meshes and 200 meshes, and taking an intermediate layer to obtain a carrier A; the expanded graphite passes through a 300-mesh standard sieve and a 400-mesh standard sieve in the same ball milling mode, and an intermediate layer is taken to obtain a carrier B; mixing the carrier A and the carrier B according to a mass ratio of 5:1 to obtain a mixture C; dissolving magnesium sulfate in water to obtain a solution with the mass concentration of 25%, and then dropwise adding the solution into the mixture C until the material is just immersed, and continuously stirring the mixture C in the dropwise adding process; finally, sealing and standing for 24 hours, and filtering to obtain a product D; adding 2% of carboxymethyl cellulose and 15% of deionized water into the D, and performing rotary granulation at a rotating speed of 1500r/min for 60min to obtain particles E; and drying the particles E at 150 ℃ for 1.5 hours to obtain the composite thermochemical adsorption spherical particles with the average particle size of 3-5 mm.
DSC test results of the composite thermochemical adsorption material obtained by this example are shown in FIG. 5; the initial temperature of the vapor desorption reaction was found to be 40.7 ℃, 64.6 ℃ and 104.3 ℃ respectively, and the heat of the desorption reaction was found to be 748.9kJ/kg. The pore structure test results of the composite thermochemical adsorption material obtained by the example are shown in table 1, the heat conduction test results are shown in table 2, and as the mass fraction of the expanded graphite becomes larger, the material has the highest heat conduction coefficient, however, the specific surface area, the pore volume and the average pore diameter are reduced due to the reduction of the mass fraction of the diatomite, so that the mass transfer performance is reduced; therefore, the heat storage performance of the composite material is obviously reduced under the condition of the same sulfate content.
Comparative example 1
Mixing untreated diatomite and calcium carbonate according to a mass ratio of 10:0.8, standing at 950 ℃ for 5 hours, mixing the mixture and deionized water according to a volume ratio of 1:3, standing in a water bath at 80 ℃ for 15 minutes, washing, filtering and drying at 150 ℃ to constant weight; ball milling the mixture after pore forming for 2 hours, wherein the rotation speed of the ball mill is 30r/min, and then passing through a standard sieve with 100 meshes and 200 meshes, and taking an intermediate layer to obtain a carrier A; the expanded graphite passes through a 300-mesh standard sieve and a 400-mesh standard sieve in the same ball milling mode, and an intermediate layer is taken to obtain a carrier B; mixing the carrier A and the carrier B according to a mass ratio of 35.6:6 to obtain a mixture C; dissolving magnesium sulfate in water to obtain a solution with the mass concentration of 25%, and then dropwise adding the solution into the mixture C until the material is just immersed, and continuously stirring the mixture C in the dropwise adding process; finally, sealing and standing for 24 hours, and filtering to obtain a product D; adding 2% of carboxymethyl cellulose and 10% of deionized water into the D, and performing rotary granulation at a rotating speed of 1500r/min for 30min to obtain particles E; and drying the particles E at 150 ℃ for 2 hours to obtain the composite thermochemical adsorption spherical particles with the average particle size of 3-5 mm.
The diatomite subjected to pore-forming treatment obtained in the embodiment is shown in fig. 6, and it can be seen that after the content of calcium carbonate exceeds the mass fraction given by the invention, the impact force generated by the carbon dioxide released by the decomposition reaction of calcium carbonate damages the disk structure of the diatomite. DSC test results of the composite thermochemical adsorption material are shown in FIG. 7, the initial temperature of the composite material steam desorption reaction is 29.0 ℃, 63.9 ℃ and 110.3 ℃, and the desorption reaction heat is 594.0kJ/kg. The pore structure test results of the composite thermochemical adsorption material obtained by this comparative example are shown in table 1, the heat conduction test results are shown in table 2, and as the diatomite disc results are destroyed, the specific surface area and pore volume are reduced, and the heat conduction performance is obviously reduced.
As can be seen from comparing comparative example 1 with example 1, the total heat storage density of the material was greatly reduced except for the mass fraction of calcium carbonate under the other preparation conditions same as example 1, and the object of the present invention was not achieved.
Comparative example 2
Washing and filtering untreated diatomite and drying the diatomite at 150 ℃ to constant weight; ball milling is carried out for 2 hours, the rotating speed of the ball mill is 30r/min, and then a carrier A is obtained by passing through a standard sieve with 100 meshes and 200 meshes and taking the middle layer; the expanded graphite passes through a 300-mesh standard sieve and a 400-mesh standard sieve in the same ball milling mode, and an intermediate layer is taken to obtain a carrier B; mixing the carrier A and the carrier B according to a mass ratio of 35.6:6 to obtain a mixture C; dissolving magnesium sulfate in water to obtain a solution with the mass concentration of 25%, and then dropwise adding the solution into the mixture C until the material is just immersed, and continuously stirring the mixture C in the dropwise adding process; finally, sealing and standing for 24 hours, and filtering to obtain a product D; adding 2% of carboxymethyl cellulose and 10% of deionized water into the D, and performing rotary granulation at a rotating speed of 1500r/min for 30min to obtain particles E; and drying the particles E at 150 ℃ for 2 hours to obtain the composite thermochemical adsorption spherical particles with the average particle size of 3-5 mm.
The DSC result of the diatomite untreated composite chemical adsorption heat storage material is shown in figure 8, the initial temperature of water vapor desorption is 39.2 ℃, 76.9 ℃ and 110.0 ℃, and the total heat storage density is 660.4kJ/kg; comparing comparative example 2 with examples 1 and 2, it can be found that the specific surface area and pore volume are reduced, the thermal conductivity is significantly reduced by about 19% and the total heat storage density of the composite is reduced, which does not achieve the object of the present invention.
TABLE 1
TABLE 2
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. The preparation method of the thermochemical adsorption heat storage material with high-efficiency mass and heat transfer is characterized by comprising the following steps of:
(1) Pore-forming: mixing diatomite and calcium carbonate according to a mass ratio of 10:0.1-10:0.5, placing at a constant temperature of 950 ℃ for 3-10 hours, mixing with deionized water according to a volume ratio of 1:1-1:5, standing at 50-90 ℃ for 5-30 minutes, washing, filtering and drying to constant weight;
(2) Ball milling: ball milling the mixture obtained in the step (1) to obtain a carrier A; ball-milling the porous carbon-based heat conducting agent in the same ball-milling mode to obtain a carrier B;
(3) Mixing: mixing the carrier A and the carrier B obtained in the step (2) according to a certain proportion to obtain a mixture C;
(4) Dipping: dissolving alkaline earth metal inorganic salt in water to obtain alkaline earth metal inorganic salt water solution with the mass concentration of 5-25%; dropwise adding the obtained alkaline earth metal inorganic salt water solution into the mixture C until the material is just immersed, continuously stirring the mixture C in the dropwise adding process, finally sealing and standing for 24-48 h, and filtering to obtain a product D;
(5) Granulating: adding 1-4% of binder and 6-15% of deionized water into the product D obtained in the step (4) for granulating to obtain particles E, and drying to obtain the thermochemical adsorption heat storage material with high-efficiency mass and heat transfer, wherein the thermochemical adsorption heat storage material comprises the following components in percentage by mass:
35-60% of alkaline earth metal inorganic salt;
35-55% of modified diatomite;
3-15% of a porous carbon-based heat conducting agent;
1-4% of a binder.
2. The method for preparing a thermochemical adsorption heat storage material with high efficiency of mass and heat transfer according to claim 1, wherein the ball milling time in the step (2) is 1-3h, and the rotation speed of the ball mill is 20-50 r/min; ball milling, passing through a standard sieve with 100 meshes and 200 meshes, and taking an intermediate layer to obtain a carrier A; and (3) ball milling, and then passing through a standard sieve with 300 meshes and 400 meshes, and taking an intermediate layer to obtain a carrier B.
3. The method for producing a thermochemical adsorption heat storage material for efficient mass and heat transfer according to claim 1, wherein the granulating process in step (5) is: and (5) carrying out rotary granulation for 15-60 min at the rotating speed of 500-2500 r/min.
4. A thermochemical adsorption heat storage material of high efficiency mass and heat transfer prepared by the method as claimed in any one of claims 1 to 3, characterized by comprising the following components in mass percent:
35-60% of alkaline earth metal inorganic salt;
35-55% of modified diatomite;
3-15% of a porous carbon-based heat conducting agent;
1-4% of a binder.
5. The thermochemical adsorption heat storage material of high efficiency mass and heat transfer according to claim 4, comprising the following components in mass percent:
56.4% of alkaline earth metal inorganic salt;
35.6% of modified diatomite;
6.0% of porous carbon-based heat conducting agent;
2.0% of binder.
6. The efficient mass and heat transfer thermochemical adsorption heat storage material according to claim 4 or 5, wherein the alkaline earth metal inorganic salt is magnesium sulfate, strontium bromide, strontium chloride or magnesium chloride; the porous carbon-based heat conducting agent is expanded graphite or activated carbon; the binder is carboxymethyl cellulose or starch.
7. The efficient mass and heat transfer thermochemical adsorption heat storage material according to claim 4 or 5, wherein the modified diatomite comprises 0.8% -5% of calcium silicate by mass.
8. The thermochemical adsorption heat storage material of claim 6 wherein the temperature range of the water vapor adsorption/desorption reaction of the thermochemical adsorption heat storage material of high efficiency mass and heat transfer is 30-120 ℃.
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| CN116162446B (en) * | 2023-02-03 | 2023-12-01 | 南京航空航天大学 | High-power-density low-cost calcium-based heat storage particles based on solid waste utilization and preparation method thereof |
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