CN113861946A - Lotus root stalk biomass porous carbon composite phase change material and preparation method thereof - Google Patents
Lotus root stalk biomass porous carbon composite phase change material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a lotus root stem biomass porous carbon composite phase change material and a preparation method thereof2CO3Activating the lotus root rod, carbonizing at high temperature under argon atmosphere to obtain a lotus root rod porous carbon material, and adsorbing the inorganic hydrated salt phase change material by a water bath impregnation method by using the lotus root rod porous carbon material as a support material to prepare the composite phase change material. The preparation period is short, the prepared biomass porous carbon material is used as a supporting material, the specific surface area is large, the pore size is rich, and the liquid phase change material can be effectively adsorbed, so that the reduction of the phase change material is avoided, and the leakage problem is effectively solved; meanwhile, the heat conductivity coefficient of the composite phase change material can be improved.
Description
Technical Field
The invention relates to a phase-change material and a preparation method thereof, in particular to a lotus root stalk biomass porous carbon composite phase-change material and a preparation method thereof.
Background
With the continuous development of global economy, the demand of human beings on energy is increasing day by day, however, the exhaustion of non-renewable resources is inevitable, and in order to solve the contradiction between energy supply and demand, the heat energy storage technology is produced. Phase change materials are often used to store thermal energy and control temperature because they can absorb or release large amounts of heat during the phase change process. However, for the solid-liquid phase change material, during heat absorption and energy storage, the liquid phase is mostly leaked due to the solid-liquid phase change of the phase change material, so that the loss of the phase change material is reduced, and the cycle performance of the phase change material is reduced. The main solutions currently available are the microencapsulation method and the adsorption method. The microcapsule method is to wrap a layer of film with stable performance on the surface of phase change particles so as to form microcapsules with a core-shell structure. Although the leakage rate of the material can be effectively reduced, the preparation process is complex and the cost is high. The adsorption method is to load a phase-change material with a porous material, thereby solving the leakage problem. The method is easy to operate and has much lower overall cost than the microcapsule, so a large number of scholars research the method in recent years.
The existing porous material for loading the phase change material has small specific surface area, poor adsorption and easy leakage.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a lotus root stem biomass porous carbon composite phase change material and a preparation method thereof, and solves the problems that the existing porous phase change material is small in specific surface area and easy to leak.
The technical scheme is as follows: the lotus root stalk biomass porous carbon composite phase change material comprises a lotus root stalk biomass carbon material and an inorganic hydrated salt phase change material, wherein the mass fraction of the biomass carbon material is 1% -9%.
The inorganic hydrated salt phase-change material is at least one of disodium hydrogen phosphate dodecahydrate, sodium carbonate decahydrate, sodium thiosulfate pentahydrate and sodium acetate trihydrate.
The preparation method of the lotus root stalk biomass porous carbon composite phase change material comprises the following steps of:
(1) cleaning fresh lotus root stalks with deionized water, cutting into strips, and naturally drying;
(2) soaking the dried lotus root sticks in K2CO3Removing redundant impurities from the solution, and then soaking and cleaning the solution to be neutral by using deionized water;
(3) oven drying lotus root rod, and soaking in K2CO3Activating in the solution;
(4) heating the lotus root sticks obtained by activation to 700-900 ℃ at a heating rate of 3-5 ℃/min for 2-3h in a tubular furnace under an argon atmosphere;
(5) taking out the material treated in the step (4), cooling to room temperature, respectively washing with HCl and deionized water to neutrality, and drying to obtain the lotus root stalk porous biomass carbon material;
(6) pressing the prepared lotus root stalk porous biomass carbon material and the inorganic hydrated salt phase change material into blocks, putting the blocks into a beaker, putting the beaker into a water bath kettle, and preserving heat to finish soaking;
(7) and taking out the impregnated composite phase-change material, putting the impregnated composite phase-change material into an oven, removing the liquid on the surface of the composite phase-change material or the phase-change material which is not completely adsorbed, and continuously replacing filter paper until no liquid leaks, so as to obtain the lotus root stalk biomass porous carbon composite phase-change material.
Wherein the length of the strip in the step (1) is 2-3 cm.
Soaking the mixture in the step (2) in 1mol/L K2CO3The solution is kept for 6 to 12 hours.
Soaking the mixture in the step (3) in 2-4mol/L K2CO3Activating in the solution for 12-24 h.
The mass concentration of HCl in the step (5) is 10%.
The temperature of the oven in the step (7) is 80 ℃.
The technical principle is as follows: the lotus root stalks are natural macroporous porous materials, a large number of micropores and mesopores can be generated after a series of treatments, the prepared biomass charcoal material has huge specific surface area and rich pore diameter structure, the leakage can be effectively solved by well adsorbing the solid-liquid phase change material, and K is utilized2CO3The principle of activation is as follows:
K2O+C→2K+CO
K2CO3+2C→2K+3CO
the above formula reaction occurs mainly with increasing temperature, K2CO3Is carbonized and reduced to K, K2O, CO and CO2And the like. And with the overflow of gas molecules, the consumption of C atoms, the volatilization and decomposition of intermediate products such as K simple substance and the like, a plurality of pores are formed on the surface of the material. Wherein the consumption of C atoms and the overflow of K simple substance form a large number of micropores.
Has the advantages that: according to the invention, a large amount of discarded agricultural waste lotus root stalks each year are used as raw materials, and are converted into a biomass porous carbon material through a series of treatments, and the biomass porous carbon material can be used as a supporting material to load a phase change material, and the lotus root stalks can be regenerated each year, so that the method is green, environment-friendly and low in cost; the prepared biomass porous carbon material is used as a supporting material, has large specific surface area and rich pore diameter, and can effectively adsorb the liquid phase-change material, thereby avoiding the reduction of the phase-change material and effectively solving the leakage problem; meanwhile, the heat conductivity coefficient of the composite phase change material can be improved.
Drawings
FIG. 1 is a nitrogen adsorption and desorption isotherm diagram of an alkali-modified lotus root stalk biomass carbon material in example 1;
FIG. 2 is a graph of the step size curve for the pure inorganic hydrated salt of example 1, curve A; curve B is the cold curve of inorganic hydrated salt/lotus root stalk carbon material;
FIG. 3 is a distribution diagram of the adsorption pore size of the biomass carbon material of lotus root stalk in example 1.
Detailed Description
The present invention will be further illustrated with reference to the following examples.
Example 1
The invention discloses a preparation process of a lotus root stalk biomass porous carbon composite phase change material, which comprises the following steps:
(1) cleaning the collected lotus root stalks with deionized water, cutting the lotus root stalks into strips of 2cm, and naturally drying the strips;
(2) soaking the lotus root stalks aired in the step 1 in 1mol/L K2CO3Removing excessive impurities in the solution for 6 hours, and then soaking and cleaning the solution to be neutral by using deionized water;
(3) drying lotus root rod, soaking in 3mol/L K2CO3Activating in the solution for 12 h;
(4) heating the lotus root sticks obtained by activation in the step 3 to 700-900 ℃ at a heating rate of 2 ℃/L by using a tube furnace in an argon atmosphere, and preserving heat for 2 h;
(5) taking out the material obtained in the step 4, cooling to room temperature, respectively washing with HCl with the mass concentration of 10% and deionized water to neutrality, and drying to obtain a porous biomass carbon material;
(6) putting the prepared porous biomass carbon material and disodium hydrogen phosphate dodecahydrate into a beaker, wherein the mass of the porous biomass carbon material is 9% of the whole mass, and putting the beaker into a water bath kettle to heat for 120min at 60 ℃;
(7) and taking out the impregnated composite phase change material.
(8) And (4) putting the impregnated composite phase change material in the step (7) into a drying oven at 60 ℃, and removing the liquid inorganic hydrated salt phase change material on the surface of the composite phase change material or the liquid which is not impregnated into the pores. The filter paper was changed continuously until no liquid leaked.
Example 2
Putting the prepared porous biomass carbon material and sodium acetate trihydrate into a beaker, and putting the beaker into a vacuum heating furnace to heat for 120min at 70 ℃;
and (3) putting the impregnated composite phase-change material into an oven at 70 ℃, and removing the liquid organic material on the surface of the composite phase-change material or the liquid which is not impregnated into the pores. The filter paper was changed continuously until no liquid leaked.
The rest is the same as the step of the specific example 1.
Example 3
Putting the prepared porous biomass carbon material, sodium sulfate decahydrate and sodium acetate trihydrate mixed according to the ratio of 1:1 into a beaker, and putting the beaker into a vacuum heating furnace to heat for 120min at 70 ℃;
and (3) putting the impregnated composite phase-change material into an oven at 70 ℃, and removing the liquid inorganic material on the surface of the composite phase-change material or the liquid which is not impregnated into the pores. The filter paper was changed continuously until no liquid leaked.
The rest is the same as the step of the specific example 1.
The performance of the lotus root stalk biomass porous carbon composite phase change material prepared in example 1 is tested, the results are shown in fig. 1-3, and the test results show that the obtained composite phase change material Na2HPO4·12H2The phase transition temperature of the O/lotus root stalk biomass carbon is 21.2 ℃, and the specific surface area is 1724m2(ii)/g, maximum pore diameter of 354 nm. Through BET adsorption data and pore size distributionThe lotus root stalk biomass carbon material has excellent specific surface area and pore size distribution, and can be used as an adsorption material to improve the performance of a phase-change material; the step cooling curve shows that after the lotus root stalk biomass carbon material is added as the adsorption material, the integral supercooling degree is greatly reduced from 8.2 ℃ to 1.2 ℃, and the problem of supercooling of the phase change material is obviously solved.
Claims (7)
1. The lotus root stalk biomass porous carbon composite phase change material is characterized by comprising a lotus root stalk biomass carbon material and an inorganic hydrated salt phase change material, wherein the mass fraction of the biomass carbon material is 1% -9%.
2. The lotus root stalk biomass porous carbon composite phase change material as claimed in claim 1, wherein the inorganic hydrated salt phase change material is at least one of disodium hydrogen phosphate dodecahydrate, sodium carbonate decahydrate, sodium thiosulfate pentahydrate, and sodium acetate trihydrate.
3. The preparation method of the lotus root stalk biomass porous carbon composite phase change material as claimed in claim 1, characterized by comprising the following steps:
(1) cleaning fresh lotus root stalks with deionized water, cutting into strips, and naturally drying;
(2) soaking the dried lotus root sticks in K2CO3Removing redundant impurities from the solution, and then soaking and cleaning the solution to be neutral by using deionized water;
(3) oven drying lotus root rod, and soaking in K2CO3Activating in the solution;
(4) heating the lotus root sticks obtained by activation to 700-900 ℃ at a heating rate of 3-5 ℃/min for 2-3h in a tubular furnace under an argon atmosphere;
(5) taking out the material treated in the step (4), cooling to room temperature, respectively washing with HCl and deionized water to neutrality, and drying to obtain the lotus root stalk porous biomass carbon material;
(6) pressing the prepared lotus root stalk porous biomass carbon material and the inorganic hydrated salt phase change material into blocks, putting the blocks into a beaker, putting the beaker into a water bath kettle, and preserving heat to finish soaking;
(7) and taking out the impregnated composite phase-change material, putting the impregnated composite phase-change material into an oven, removing the liquid on the surface of the composite phase-change material or the phase-change material which is not completely adsorbed, and continuously replacing filter paper until no liquid leaks, so as to obtain the lotus root stalk biomass porous carbon composite phase-change material.
4. The lotus root stalk biomass porous carbon composite phase change material as claimed in claim 1, wherein the length of the strip in the step (1) is 2-3 cm.
5. The lotus root stalk biomass porous carbon composite phase change material as claimed in claim 1, wherein the soaking in the step (2) is performed at 1mol/L K2CO3The solution is kept for 6 to 12 hours.
6. The lotus root stalk biomass porous carbon composite phase change material as claimed in claim 1, wherein the soaking in the step (3) is performed at K of 2-4mol/L2CO3Activating in the solution for 12-24 h.
7. The lotus root stalk biomass porous carbon composite phase change material according to claim 1, wherein the mass concentration of HCl in the step (5) is 10%.
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