CN111187596A - Metal-organic framework composite phase change material for thermal management system and preparation method thereof - Google Patents
Metal-organic framework composite phase change material for thermal management system and preparation method thereof Download PDFInfo
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Abstract
The embodiment of the invention relates to the field of phase-change materials, in particular to a metal-organic framework composite phase-change material for a thermal management system and a preparation method thereof. The preparation method comprises the following steps: preparing a functionally modified metal-organic framework from raw materials comprising a functionally modified ligand and metal ions; the functionalized modified ligand is prepared from raw materials comprising an organic ligand and 1,3,5-benzene tricarboxychloride; the organic ligand includes: a functional substituent of 4-amino-benzoic acid; the functionalization includes: one or more of amination, alkylation or fluorination; the ligand is 4, 4' - [1,3, 5-benzanetriylis (carbonyimino) ] -trisbenzoic acid. The chemical properties of the pore channels of the metal-organic framework are regulated and controlled through functional modification, so that the obtained functional modified metal-organic framework has higher load capacity on a phase change core material when being used as a carrier material, and the prepared composite phase change material has better heat transfer performance, higher phase change latent heat, better stability and excellent thermal performance.
Description
Technical Field
The invention relates to the field of phase-change materials, in particular to a metal-organic framework composite phase-change material for a heat management system and a preparation method thereof.
Background
The heat storage/release technology is realized by utilizing the characteristic that Phase Change Materials (PCMs) can absorb or release a large amount of heat energy, and is an effective method for expanding heat energy application and overcoming energy crisis. However, large-scale application of phase change materials is often limited by disadvantages such as leakage, severe supercooling degree, insufficient heat transfer, low heat accumulation/release efficiency, and the like.
Therefore, the preparation of shaped composite phase change materials has attracted extensive attention from researchers. Various porous support materials such as porous carbon, graphene, diatomaceous earth, expanded vermiculite, etc. have been used to improve the thermal properties of composite phase change materials. But the synthesis method is complex and the packaging capacity is low, which seriously restricts the scale production of the composite phase-change material.
Metal Organic Frameworks (MOFs) materials are a new class of materials that can be used as functional matrices for encapsulating a variety of phase change materials. The prepared metal-organic framework composite phase change material with more excellent performance has wide application prospect in the fields of heat energy storage and heat management.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
Object of the Invention
In order to solve the above technical problems, an object of the present invention is to provide a metal-organic framework composite phase change material for a thermal management system and a method for preparing the same. According to the preparation method of the metal-organic framework composite phase-change material, the chemical properties of the pore channels of the metal-organic framework are regulated and controlled through functional modification, so that the obtained functional modified metal-organic framework is higher in the load capacity of a phase-change core material when being used as a carrier material, and the prepared composite phase-change material is better in heat transfer performance, higher in phase-change latent heat, better in stability and excellent in thermal performance.
Solution scheme
In order to achieve the purpose of the present invention, an embodiment of the present invention provides a preparation method of a metal-organic framework composite phase change material, including the following steps:
preparing a functionally modified metal-organic framework from raw materials comprising a functionally modified ligand and metal ions;
the functionalized modified ligand is prepared from raw materials comprising an organic ligand and 1,3,5-benzene tricarboxychloride;
the organic ligand includes: a functional substituent of 4-amino-benzoic acid;
the functionalization includes: one or more of amination, alkylation or fluorination;
the ligand is 4, 4' - [1,3, 5-benzanetriylimines (carbonyimino)]-trisbenzoic acid, hereinafter referred to as H3L·3H2O, the structure of which is shown in formula (1):
in one possible implementation manner of the above preparation method, the organic ligand includes: one or more of 3, 4-diamino-benzoic acid, 4-amino-3-methylbenzoic acid or 3-fluoro-4-aminobenzoic acid; optionally, the organic ligand comprises: one or more of 3, 4-diamino-benzoic acid or 3-fluoro-4-aminobenzoic acid; further optionally, the organic ligand comprises: 3, 4-diamino-benzoic acid.
In a possible implementation manner of the preparation method, the metal ions are Zn2+。
In one possible implementation mode, the functionalized and modified ligand is prepared by a method comprising the following steps: dissolving an organic ligand and triethylamine in an N, N-Dimethylacetamide (DMA) solution, adding 1,3,5-benzene trimethyl acyl chloride, and stirring at room temperature; adding water to generate precipitate, filtering, collecting and washing.
In one possible implementation mode of the preparation method, the mass ratio of the organic ligand to the 1,3,5-benzene trimethyl acyl chloride is as follows: 1: 0.5 to 5, optionally 1 to 2; further optionally 1: 1.5-1.6.
In one possible implementation of the above preparation method, the metal-organic framework is prepared by a method comprising the following steps: adding metal salt into a Dimethylformamide (DMF) solution containing a functionalized and modified ligand, and carrying out solvothermal reaction to obtain crystals; filtering and collecting crystal blocks, and washing with DMF; drying in a vacuum drying oven.
In one possible implementation manner of the preparation method, the metal salt is Zn (NO)3)2·6H2O。
In a possible implementation manner of the preparation method, the mass ratio of the functionalized modified ligand to the metal salt is as follows: 1: 0.5 to 5; optionally 1: 1.5-3; further optionally 1: 2-2.5.
In a possible implementation manner, the preparation method further comprises the following steps: and adsorbing the phase-change core material by the prepared functionalized modified metal-organic framework.
In one possible implementation of the above preparation method, the adsorption comprises the following steps: dissolving the phase-change core material in a solvent, adding the prepared functionalized modified metal-organic framework, stirring, and drying in an oven.
In one possible implementation manner of the preparation method, the mass ratio of the phase-change core material to the functionally modified metal-organic framework is 1-100: 1-100; alternatively 50-90: 50-10 parts of; further optionally 70-85: 30-15.
In one possible implementation mode of the preparation method, the stirring time is 1-4 h.
In a possible implementation manner, the stirring temperature is higher than the phase-change temperature of the phase-change core material; alternatively, the stirring temperature is 60-120 ℃.
In a possible implementation manner, the drying temperature is higher than the phase-change temperature of the phase-change core material; optionally, the drying temperature is 60-120 ℃.
In one possible implementation mode of the preparation method, the drying time is 12-48 h.
In one possible implementation manner of the preparation method, the phase-change core material comprises: one or more of a polyol, a monohydric alcohol, a fatty acid or a paraffin wax; the polyol comprises one or more of polyethylene glycol (PEG) with an average molecular weight of 1000-; the monohydric alcohol comprises one or more of octadecanol or tetradecanol; the fatty acid comprises one or more of stearic acid, myristic acid, palmitic acid, capric acid, lauric acid or pentadecanoic acid; optionally, the phase change core material comprises PEG2000 or octadecanol.
The embodiment of the invention also provides the metal-organic framework composite phase-change material prepared by the preparation method.
The embodiment of the invention also provides the preparation method and the application of the metal-organic framework composite phase change material in a thermal management system.
Advantageous effects
(1) According to the preparation method of the metal-organic framework composite phase change material provided by the embodiment of the invention, 4' - [1,3, 5-zenetriylis (carbonyimino) ] -trisbenzoic acid ligand is selected as a raw material and is subjected to functional modification, so that a functionally modified metal-organic framework is further obtained, and the metal-organic framework has a three-dimensional porous network structure and high specific surface area and porosity; compared with an unmodified material, the functionalized modified metal-organic framework obtained by regulating and controlling the chemical properties of the pore channels of the metal-organic framework through functionalized modification has higher load capacity on a phase change core material when used as a carrier material, and the prepared composite phase change material has better heat transfer performance, higher phase change latent heat, better stability and excellent thermal performance.
(2) The preparation method of the metal-organic framework composite phase change material provided by the embodiment of the invention is used for preparing ligand H3L·3H2And O is subjected to amination, alkylation or fluorination modification, so that a weak hydrogen bond effect is generated between the metal-organic framework and the phase-change core material, and the phase-change core material is more favorably permeated, so that the loading capacity and the thermal property of the phase-change core material are improved.
Furthermore, the p-ligands H of 3, 4-diamino-benzoic acid, 4-amino-3-methylbenzoic acid and 3-fluoro-4-aminobenzoic acid were selected separately3L·3H2And O is subjected to amination, alkylation and fluorination modification, so that the chemical property of the pore channel of the metal-organic framework can be further optimized, and the loading capacity of the phase-change core material is improved.
(3) According to the preparation method of the metal-organic framework composite phase change material provided by the embodiment of the invention, the effective packaging of the phase change core material can be realized by adopting a low-cost solution impregnation method, the phase change core material is adsorbed and limited in the pore channel of the metal-organic framework material, the core material leakage can be effectively prevented, and the method is simple and rapid.
(4) According to the preparation method of the metal-organic framework composite phase-change material provided by the embodiment of the invention, the phase-change core material is various in selectable types and wide in application range.
Drawings
One or more embodiments are illustrated by the corresponding figures in the drawings, which are not meant to be limiting. The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
Fig. 1 is a Scanning Electron Microscope (SEM) scanning image of the metal-organic framework composite phase change material obtained in example 2 of the present invention.
Fig. 2 is a thermogravimetric analysis (TGA) of the metal-organic framework composite phase change material obtained in example 2 of the present invention.
FIG. 3 is a Differential Scanning Calorimetry (DSC) chart of the metal-organic framework composite phase-change material obtained in example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some embodiments, materials, elements, methods, means, and the like that are well known to those skilled in the art are not described in detail in order to not unnecessarily obscure the present invention.
In the following examples, all the raw materials used were commercially available raw materials.
1,3,5-benzene trimethyl acyl chloride CAS number 4422-95-1; 4-amino-benzoic acid CAS number 150-13-0; 3, 4-diamino-benzoic acid CAS number 619-05-6; CAS number of 4-amino-3-methylbenzoic acid is 2486-70-6; the CAS number of the 3-fluoro-4-aminobenzoic acid is 455-87-8.
Example 1
A preparation method of a metal-organic framework composite phase-change material comprises the following steps:
(1) preparation of unmodified metal-organic framework materials (Zn-MOFs):
4.2g (15.8mmol) of 1,3, 5-benzenetricarboxylic acid chloride are added to a solution of 6.5g (47.4mmol) of 4-amino-benzoic acid and 3.8mL of triethylamine in 80mL of N, N-Dimethylacetamide (DMA), and stirred at room temperature for 16 h; then adding 300mL water to generate precipitate, filtering and collecting, and then washing with acetone, water and methanol to obtain ligand H3L·3H2O。
62mg (0.208mmol) of Zn (NO)3)2·6H2O addition of 28mg H3L·3H2O in 5mL DMF; then sealing the solution in a heat-resistant glass tube container, and keeping the temperature at 95 ℃ for 1 d; after cooling to room temperature, filtering and collecting a colorless crystal block, and washing with DMF; and finally drying for 24 hours in a vacuum drying oven at 120 ℃ to obtain the unmodified Zn-MOFs carrier material.
(2) Preparing a metal-organic framework composite phase-change material:
dissolving 1g of PEG2000 in 50mL of absolute ethanol, and stirring at 80 ℃ for 1h to obtain a uniform solution;
adding 0.428g of the prepared unmodified Zn-MOFs carrier material into the uniform solution, and stirring for 1h at 80 ℃ to obtain a mixed solution; the phase-change material can fully enter the pore channels of the MOFs material by stirring, and the encapsulation speed and the encapsulation amount of the phase-change material can be improved by fully stirring;
then putting the mixed solution into an oven, drying for 24h at 80 ℃, and evaporating the solvent to obtain the metal-organic framework composite phase-change material; in the metal-organic framework composite phase change material, the loading amount of PEG2000 is 70%.
In the metal-organic framework composite phase change material of the present invention, the amount of the phase change core material is (mass of the phase change core material/mass of the metal-organic framework composite phase change material) × 100%.
Example 2
A preparation method of a metal-organic framework composite phase-change material comprises the following steps:
(1) preparation of amino-modified metal-organic framework materials (Zn-MOFs):
4.2g (15.8mmol) of 1,3, 5-benzenetricarboxylic acid chloride are added to a solution of 6.5g (42.7mmol) of 3, 4-diamino-benzoic acid and 3.8mL of triethylamine in 80mL of N, N-Dimethylacetamide (DMA) and stirred at room temperature for 16 h; then adding 300mL water to generate precipitation, filtering and collecting, and then washing with acetone, water and methanol to obtain the amino modified ligand H3L·3H2O。
62mg (0.208mmol) of Zn (NO)3)2·6H2O addition of H modified with 28mg of amino group3L·3H2O in 5mL DMF; then sealing the solution in a heat-resistant glass tube container, and keeping the temperature at 95 ℃ for 1 d; after cooling to room temperature, filtering and collecting a colorless crystal block, and washing with DMF; and finally drying for 24 hours in a vacuum drying oven at 120 ℃ to obtain the amino modified Zn-MOFs carrier material.
(2) Preparing a metal-organic framework composite phase-change material:
dissolving 1g of PEG2000 in 50mL of absolute ethanol, and stirring at 80 ℃ for 1h to obtain a uniform solution;
adding 0.25g of the prepared amino modified Zn-MOFs carrier material into the uniform solution, and stirring for 1h at 80 ℃ to obtain a mixed solution;
then putting the mixed solution into an oven, drying for 24h at 80 ℃, and evaporating the solvent to obtain the metal-organic framework composite phase-change material; in the metal-organic framework composite phase change material, the loading amount of PEG2000 is 80%; the metal-organic framework composite phase change material is marked as 80% PEG2000@ Zn-MOFs.
The preparation method of the metal-organic framework composite phase change material (marked as 85% PEG2000@ Zn-MOFs) with the PEG2000 loading of 85% is the same as that in the step (2), and only the difference is that the addition amount of the amino modified Zn-MOFs carrier material is 0.177 g.
The preparation method of the metal-organic framework composite phase change material (marked as 70% PEG2000@ Zn-MOFs) with the PEG2000 loading of 70% is the same as the step (2), and only the difference is that the addition amount of the amino modified Zn-MOFs carrier material is 0.428 g.
Scanning results of a Scanning Electron Microscope (SEM) of the prepared metal-organic framework composite phase change material are shown in figure 1, wherein a in figure 1 is an amino modified Zn-MOFs carrier material without loading PEG, b is 70% PEG2000@ Zn-MOFs, c is 80% PEG2000@ Zn-MOFs, and d is 85% PEG2000@ Zn-MOFs; as can be seen from SEM scanning pictures, after the phase change core material is soaked, the appearance of the composite phase change material is more compact than that of the original Zn-MOFs material, and the surface and the edge become smooth. PEG2000 is uniformly distributed in the composite phase-change material, and PEG molecules, hydroxyl functional groups and amino functional groups generate hydrogen bond action to be anchored in a framework. When the mass ratio of PEG is increased to 85%, some PEG molecules are inevitably dispersed on the surface of the carrier material, thereby indirectly determining the optimal carrying capacity of Zn-MOFs. The porous structure of the modified Zn-MOFs provides powerful support for the composite phase change material, so that the shape stability of the composite phase change material is maintained and the composite phase change material is prevented from leaking, and the composite material has good shape stability.
The thermogravimetric analysis (TGA) result is shown in figure 2, and the PEG and the composite phase-change material do not show obvious thermal decomposition at the temperature of below 253 ℃, thereby showing the high thermal stability of the composite phase-change material.
The results of Differential Scanning Calorimetry (DSC) are shown in FIG. 3. DSC (differential scanning calorimetry) test results show that the phase change temperature of the 85% PEG2000@ Zn-MOFs composite phase change material is 50.4/23.8 ℃, and the latent heat of phase change is 159.8/149.5J/g.
Example 3
(1) Preparation of alkyl-modified Metal-organic framework materials (Zn-MOFs):
the same as in example 2, except that 6.5g (43.0mmol) of 4-amino-3-methylbenzoic acid was added; preparing the alkyl modified Zn-MOFs carrier material.
(2) Preparing a metal-organic framework composite phase-change material:
dissolving 1g of PEG2000 in 50mL of absolute ethyl alcohol, and stirring for 1h at 80 ℃ to obtain a uniform solution;
adding 0.428g of the prepared alkyl modified Zn-MOFs carrier material into the uniform solution, and stirring for 1h at 80 ℃ to obtain a mixed solution;
then putting the mixed solution into an oven, drying for 24h at 80 ℃, and evaporating the solvent to obtain the metal-organic framework composite phase-change material; in the metal-organic framework composite phase change material, the loading amount of PEG2000 is 70%.
Example 4
(1) Preparation of fluorine-modified Metal-organic framework materials (Zn-MOFs):
the same as in example 2, except that 6.5g (42.0mmol) of 3-fluoro-4-aminobenzoic acid was added; preparing the fluorine modified Zn-MOFs carrier material.
(2) Preparing a metal-organic framework composite phase-change material:
dissolving 1g of PEG2000 in 50mL of absolute ethyl alcohol, and stirring for 1h at 80 ℃ to obtain a uniform solution;
adding 0.176g of the prepared fluorine modified Zn-MOFs carrier material into the uniform solution, and stirring for 1h at 80 ℃ to obtain a mixed solution;
then putting the mixed solution into an oven, drying for 24h at 80 ℃, and evaporating the solvent to obtain the metal-organic framework composite phase-change material; in the metal-organic framework composite phase change material, the loading amount of PEG2000 is 85%.
In the above examples, the phase change core material used is PEG2000, and in addition to PEG2000, octadecanol, paraffin, PEG with other molecular weights, stearic acid, and the like may be used.
The thermal performance parameters of the metal-organic framework composite phase change materials prepared in examples 1-4 are shown in Table 1:
TABLE 1
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a metal-organic framework composite phase-change material comprises the following steps:
preparing a functionally modified metal-organic framework from raw materials comprising a functionally modified ligand and metal ions;
the functionalized modified ligand is prepared from raw materials comprising an organic ligand and 1,3,5-benzene tricarboxychloride;
the organic ligand includes: a functional substituent of 4-amino-benzoic acid;
the functionalization includes: one or more of amination, alkylation or fluorination;
the ligand structure is shown as formula (1):
2. the method of claim 1, wherein: the organic ligand includes: one or more of 3, 4-diamino-benzoic acid, 4-amino-3-methylbenzoic acid or 3-fluoro-4-aminobenzoic acid; optionally, the organic ligand comprises: one or more of 3, 4-diamino-benzoic acid or 3-fluoro-4-aminobenzoic acid; further optionally, the organic ligand comprises: 3, 4-diamino-benzoic acid.
3. The method of claim 1, wherein: the metal ion is Zn2+；
And/or the mass ratio of the organic ligand to the 1,3,5-benzene trimethyl acyl chloride is as follows: 1: 0.5-5.
4. The method of claim 1, wherein: the functionalized modified ligand is prepared by a method comprising the following steps: dissolving an organic ligand and triethylamine in an N, N-dimethylacetamide solution, adding 1,3,5-benzene trimethyl acyl chloride, and stirring at room temperature; adding water to generate precipitate, filtering, collecting and washing.
5. The method of claim 1, wherein: the metal-organic framework is prepared by a process comprising the steps of: adding metal salt into a dimethylformamide solution containing a functionalized and modified ligand, and carrying out solvothermal reaction to obtain crystals; filtering and collecting crystal blocks, and washing with dimethylformamide; drying in a vacuum drying oven;
optionally, the metal salt is Zn (NO)3)2·6H2O；
Optionally, the mass ratio of the functionalized modified ligand to the metal salt is: 1: 0.5-5.
6. The method of claim 1, wherein: the preparation method also comprises the following steps: and adsorbing the phase-change core material by the prepared functionalized modified metal-organic framework.
7. The method of claim 6, wherein: the mass ratio of the phase-change core material to the functionalized modified metal-organic framework is 1-100: 1-100; alternatively 50-90: 50-10 parts of;
and/or, the phase change core material comprises: one or more of a polyol, a monohydric alcohol, a fatty acid or a paraffin wax; the polyhydric alcohol comprises one or more of polyethylene glycol with the average molecular weight of 1000-; the monohydric alcohol comprises one or more of octadecanol or tetradecanol; the fatty acid comprises one or more of stearic acid, myristic acid, palmitic acid, capric acid, lauric acid or pentadecanoic acid;
and/or, the adsorption comprises the following steps: dissolving the phase-change core material in a solvent, adding the prepared functionalized modified metal-organic framework, stirring, and drying in an oven.
8. The method of claim 7, wherein: stirring for 1-4 h;
and/or the stirring temperature is higher than the phase-change temperature of the phase-change core material;
and/or the drying temperature is higher than the phase-change temperature of the phase-change core material;
and/or the drying time is 12-48 h.
9. The metal-organic framework composite phase-change material prepared by the preparation method of any one of claims 1 to 8.
10. Use of the preparation method of any one of claims 1 to 8 or the metal-organic framework composite phase change material of claim 9 in a thermal management system.
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