CN113845886A - Intermediate-temperature phase-change heat storage material without supercooling and preparation method thereof - Google Patents
Intermediate-temperature phase-change heat storage material without supercooling and preparation method thereof Download PDFInfo
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- 238000005338 heat storage Methods 0.000 title claims abstract description 38
- 239000011232 storage material Substances 0.000 title claims abstract description 34
- 238000004781 supercooling Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000012782 phase change material Substances 0.000 claims abstract description 64
- 238000012360 testing method Methods 0.000 claims abstract description 47
- 238000003756 stirring Methods 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 28
- 230000008859 change Effects 0.000 claims abstract description 25
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000002667 nucleating agent Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 6
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- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 18
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- 238000002474 experimental method Methods 0.000 claims description 13
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- HEBKCHPVOIAQTA-ZXFHETKHSA-N ribitol Chemical compound OC[C@H](O)[C@H](O)[C@H](O)CO HEBKCHPVOIAQTA-ZXFHETKHSA-N 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- HEBKCHPVOIAQTA-IMJSIDKUSA-N L-arabinitol Chemical compound OC[C@H](O)C(O)[C@@H](O)CO HEBKCHPVOIAQTA-IMJSIDKUSA-N 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- VZWGHDYJGOMEKT-UHFFFAOYSA-J sodium pyrophosphate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O VZWGHDYJGOMEKT-UHFFFAOYSA-J 0.000 claims description 9
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- 239000001361 adipic acid Substances 0.000 claims description 8
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- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 claims description 6
- VQHSOMBJVWLPSR-JVCRWLNRSA-N lactitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@@H]1O[C@H](CO)[C@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-JVCRWLNRSA-N 0.000 claims description 6
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 6
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- 239000002184 metal Substances 0.000 claims description 5
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- 238000010438 heat treatment Methods 0.000 claims description 4
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 claims description 4
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 claims description 3
- KEZYHIPQRGTUDU-UHFFFAOYSA-N 2-[dithiocarboxy(methyl)amino]acetic acid Chemical compound SC(=S)N(C)CC(O)=O KEZYHIPQRGTUDU-UHFFFAOYSA-N 0.000 claims description 3
- SERLAGPUMNYUCK-YJOKQAJESA-N 6-O-alpha-D-glucopyranosyl-D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O SERLAGPUMNYUCK-YJOKQAJESA-N 0.000 claims description 3
- HEBKCHPVOIAQTA-NGQZWQHPSA-N D-Arabitol Natural products OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- HEBKCHPVOIAQTA-QWWZWVQMSA-N D-arabinitol Chemical compound OC[C@@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-QWWZWVQMSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-BXKVDMCESA-N L-mannitol Chemical compound OC[C@H](O)[C@H](O)[C@@H](O)[C@@H](O)CO FBPFZTCFMRRESA-BXKVDMCESA-N 0.000 claims description 3
- 229930182842 L-mannitol Natural products 0.000 claims description 3
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 3
- DGLRDKLJZLEJCY-UHFFFAOYSA-L disodium hydrogenphosphate dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].OP([O-])([O-])=O DGLRDKLJZLEJCY-UHFFFAOYSA-L 0.000 claims description 3
- FBPFZTCFMRRESA-GUCUJZIJSA-N galactitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-GUCUJZIJSA-N 0.000 claims description 3
- 239000000832 lactitol Substances 0.000 claims description 3
- 235000010448 lactitol Nutrition 0.000 claims description 3
- 229960003451 lactitol Drugs 0.000 claims description 3
- VQHSOMBJVWLPSR-WUJBLJFYSA-N maltitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-WUJBLJFYSA-N 0.000 claims description 3
- 239000000845 maltitol Substances 0.000 claims description 3
- 235000010449 maltitol Nutrition 0.000 claims description 3
- 229940035436 maltitol Drugs 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 229940087562 sodium acetate trihydrate Drugs 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 150000005846 sugar alcohols Chemical class 0.000 claims description 3
- 239000000811 xylitol Substances 0.000 claims description 3
- 235000010447 xylitol Nutrition 0.000 claims description 3
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 3
- 229960002675 xylitol Drugs 0.000 claims description 3
- 206010037660 Pyrexia Diseases 0.000 claims description 2
- 150000008064 anhydrides Chemical class 0.000 claims description 2
- 230000009972 noncorrosive effect Effects 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract 2
- 230000005496 eutectics Effects 0.000 abstract 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 24
- 230000000694 effects Effects 0.000 description 19
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- 229910001369 Brass Inorganic materials 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229930195725 Mannitol Natural products 0.000 description 2
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000010951 brass Substances 0.000 description 2
- 239000010962 carbon steel Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000594 mannitol Substances 0.000 description 2
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- 239000003094 microcapsule Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920002732 Polyanhydride Polymers 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- ZUDYPQRUOYEARG-UHFFFAOYSA-L barium(2+);dihydroxide;octahydrate Chemical compound O.O.O.O.O.O.O.O.[OH-].[OH-].[Ba+2] ZUDYPQRUOYEARG-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
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- 239000012188 paraffin wax Substances 0.000 description 1
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Images
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention relates to a medium-temperature phase change heat storage material without supercooling and a preparation method thereof, wherein the preparation method comprises the steps of S1, preparing the material; step S2, preheating a reaction kettle; step S3, adding materials and stirring; step S4, pouring out and cooling; and step S5, testing. The method comprises the steps of carrying out eutectic mixing treatment by adopting two or more phase-change temperatures, then adding nucleating agents, in step S3, sequentially adding two or more phase-change materials into a reaction kettle from low to high according to the phase-change temperatures for melting and stirring, adding the nucleating agents after uniformly mixing, in step S4, pouring out a mixture in the reaction kettle, and cooling to room temperature to finish the preparation of the supercooling-free medium-temperature phase-change heat-storage material.
Description
Technical Field
The invention relates to the technical field of phase change energy storage, in particular to an intermediate-temperature phase change heat storage material without supercooling and a preparation method thereof.
Background
The phase-change heat storage technology has wide application prospect due to the advantages of large heat storage capacity, constant temperature in the heat storage and release process and the like, the phase-change material is a carrier of the phase-change heat storage technology, the phase-change temperature of the phase-change material for heat storage is required to be consistent with the temperature required by application in the application process so as to ensure the efficient utilization of energy, and the phase-change material can be divided into four types of solid-gas, liquid-gas, solid-solid and solid-liquid phase-change materials according to the basic form of phase-state transformation of the material in the working process; the solid-liquid phase change material stores heat and releases heat by utilizing the phase change of a substance, and when the external temperature is higher than the phase change temperature of the phase change material, the phase change of the material absorbs heat and stores the heat; when the external temperature is lower than the phase change temperature, the material releases the energy stored by the material; in the solid-liquid phase change process, the phase change enthalpy of a substance is large, the volume change is small, and the phase change process is mild and easy to control; solid-liquid phase change materials can be divided into organic and inorganic phase change materials from chemical compositions; the organic solid-liquid phase-change material mainly comprises paraffin, alcohols, fatty acid agents and esters thereof, and the inorganic solid-liquid phase-change material mainly comprises crystalline hydrated salt, molten metal (alloy) and the like; solid-liquid phase change materials can be divided into low-temperature, medium-temperature and high-temperature phase change materials according to the working temperature range; in the medium-temperature phase-change heat storage material, when the melting point of the hydrated salt (or hydrate) phase-change material containing crystal water is higher and is close to the boiling point of water, the material is easy to gasify, so that the composition and the thermal physical property of phase change are influenced, certain corrosivity exists, the requirement on the material of a storage container is high, the use cost is higher, the safety is relatively low, and the application of the material in practice is greatly influenced.
Literature "huaweisan, chapter school coming, liufeng, korea super, yuan wei li, wanhang. preparation and thermal properties [ J ] of phase change material composite barium hydroxide octahydrate, 2018.37 (11); 4384 & gt 4389 & gt to find a container for storing phase change materials of ba (oh) 2.8H 2O, 4 metal materials of 20# carbon steel, T2 red copper, H62 brass and 304 stainless steel were selected as test objects, and after 4 metals were immersed in a molten ba (oh) 2.8H 2O solution for 18 days, the weight loss of the 20# carbon steel, T2 red copper, H62 brass and 304 stainless steel was 6.286, 4.084, 6.66 and 0.09mg/cm3, respectively, so that the ba (oh) 2.8H 2O solution had different degrees of corrosivity to the 4 metals.
The organic polymer phase-change material has the characteristics of large heat energy storage capacity, small temperature volume change, easy combination with other materials and the like, so that the organic polymer phase-change material is widely applied to civil and military fields such as solar energy storage and utilization, building heat storage and heating, energy storage cookers and the like. The main defects are that the thermal conductivity is low, the large temperature difference exists between the melting temperature and the solidification temperature of the material, the energy utilization efficiency of the material is reduced, and the large-scale popularization and application of the material are limited. For example, in the literature of Yi Wang, ShuangLi, TingZhang, DeyiZhang, Hui Ji. Super consuming and thermal behavor improvement of erythritol as phase change material for thermal Energy storage [ J ]. Solar Energy Materials and sol Cells,2017,171, in order to solve the supercooling problem of erythritol in the organic mesophilic phase change material, a microencapsulation method is adopted, silica is used as a shell material of the microcapsule to wrap erythritol, and a white microcapsule powder material is prepared, so that the phase change temperature difference between melting and solidification of erythritol is reduced from 90 ℃ to 13.7 ℃, but the preparation process is complicated and the manufacturing cost is high by the micro-gelling method, and the industrial mass production is not suitable.
Disclosure of Invention
Therefore, the invention provides a medium-temperature phase-change heat storage material without supercooling and a preparation method thereof, which are used for solving the problems that the medium-temperature phase-change heat storage material in the prior art is corrosive and has supercooling.
In order to achieve the above objects, the present invention provides a medium temperature phase change heat storage material without supercooling and a method for preparing the same, comprising,
step S1, preparing materials, namely preparing a first phase-change material, a second phase-change material and a nucleating agent, wherein the first phase-change material and the second phase-change material account for 80-95% by mass, and the nucleating agent accounts for 5-20% by mass;
s2, preheating the reaction kettle to 220 ℃ for 150-;
step S3, adding materials and stirring, namely adding the first phase-change material into the reaction kettle, heating until the first phase-change material is completely melted, stirring, slowly adding the second phase-change material into the reaction kettle while stirring until the second phase-change material is completely melted, slowly adding the nucleating agent into the reaction kettle while stirring, and stirring for 60-120 minutes after the nucleating agent is completely added into the reaction kettle;
step S4, pouring out and cooling, pouring out the mixture mixed in the reaction kettle, cooling to room temperature, and finishing the preparation of the heat storage material;
and step S5, testing, namely performing DSC test and step cooling experiment test on the prepared heat storage material.
Further, the first phase change material is a sugar alcohol substance, and the second phase change material is a fatty acid substance or an ester substance.
Further, the first phase change material is one or more of xylitol, sorbitol, L-arabitol, D-arabitol, ribitol, erythritol, galactitol, lactitol, D-lactitol monohydrate, maltitol, L-mannitol, D-mannitol, isomaltitol, D-threitol and mannitol.
Further, when the second phase change material is a fatty acid substance, the second phase change material is one or more of adipic acid, azelaic acid, polysebacic polyanhydride and sebacic acid.
Further, when the second phase change material is an ester, the second phase change material is dimethyl terephthalate. .
Further, the nucleating agent is one or more of sodium pyrophosphate decahydrate, sodium sulfate decahydrate, sodium acetate trihydrate, disodium hydrogen phosphate dodecahydrate, sodium metasilicate pentahydrate and porous graphite.
Further, in the step S3, the stirring speed is 300-900 rpm.
Compared with the prior art, the invention has the beneficial effects that the prepared supercooling-free medium-temperature phase change heat storage material is nontoxic and harmless, has no corrosion to metal, and is safe and environment-friendly.
Furthermore, in DSC test, the temperature difference between the melting temperature and the solidification temperature of the medium-temperature phase-change material prepared by the invention is small, and the problem of obvious supercooling is avoided.
Further, in a step cooling experiment, the medium-temperature phase-change material prepared by the invention has only slight temperature fluctuation in a solidification heat release curve, and does not have a supercooling problem.
Drawings
FIG. 1 is a flow chart of a method for preparing a medium-temperature phase-change heat storage material without supercooling according to the present invention;
FIG. 2 is a graph showing the effect of DSC test in example 1;
FIG. 3 is a graph showing the test effect of the step cold test in example 1;
FIG. 4 is a graph showing the effect of DSC test in example 2;
FIG. 5 is a graph showing the test effect of the step-by-step cold test in example 2;
FIG. 6 is a graph showing the effect of DSC test in example 3;
FIG. 7 is a graph showing the test effect of the step-by-step cold test in example 3;
FIG. 8 is a graph showing the effect of DSC test in example 4;
FIG. 9 is the test result of the step-by-step cold experiment in example 4.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described below with reference to examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Referring to fig. 1, which is a flowchart illustrating a method for preparing a medium-temperature phase-change thermal storage material without supercooling according to the present invention, the present invention discloses a method for preparing a medium-temperature phase-change thermal storage material without supercooling, comprising,
step S1, preparing materials, namely preparing a first phase-change material, a second phase-change material and a nucleating agent, wherein the first phase-change material and the second phase-change material account for 80-95% by mass, and the nucleating agent accounts for 5-20% by mass;
s2, preheating the reaction kettle to 220 ℃ for 150-;
step S3, adding materials and stirring, namely adding the first phase-change material into the reaction kettle, heating until the first phase-change material is completely melted, stirring, slowly adding the second phase-change material into the reaction kettle while stirring until the second phase-change material is completely melted, slowly adding the nucleating agent into the reaction kettle while stirring, and stirring for 60-120 minutes after the nucleating agent is completely added into the reaction kettle;
step S4, pouring out and cooling, pouring out the mixture mixed in the reaction kettle, cooling to room temperature, and finishing the preparation of the heat storage material; and step S5, testing, namely performing DSC test and step cooling experiment test on the prepared heat storage material.
Specifically, the first phase change material is a sugar alcohol substance, and the second phase change material is a fatty acid substance or an ester substance.
Specifically, the first phase change material is one or more of xylitol, sorbitol, L-arabitol, D-arabitol, ribitol, erythritol, galactitol, lactitol, D-lactitol monohydrate, maltitol, L-mannitol, D-mannitol, isomaltitol, D-threitol and mannitol.
Specifically, when the second phase change material is a fatty acid substance, the second phase change material is one or more of adipic acid, azelaic acid, polysebacic anhydride and sebacic acid.
Specifically, when the second phase change material is an ester species, the second phase change material is dimethyl terephthalate. .
Specifically, the nucleating agent is one or more of sodium pyrophosphate decahydrate, sodium sulfate decahydrate, sodium acetate trihydrate, disodium hydrogen phosphate dodecahydrate, sodium metasilicate pentahydrate and porous graphite.
Specifically, in the step S3, the stirring speed is 300-900 rpm.
Example 1
Referring to fig. 2 and fig. 3, wherein fig. 2 is a DSC test result of example 1, and fig. 3 is a test result of a step-cooling experiment of example 1, the present invention discloses a medium-temperature phase-change heat storage material without supercooling, which is prepared by the following steps of quality material,
the method comprises the steps of firstly predicting a reaction kettle to 170 ℃, pouring 85g of L-arabitol into the reaction kettle through a feeding port, stirring after the L-arabitol is completely heated and melted, slowly adding 8g of adipic acid into the reaction kettle, stirring until all the adipic acid is melted, slowly pouring 5g of sodium sulfate decahydrate into the reaction kettle, stirring while adding, stirring for 30 minutes after the L-arabitol is fully melted, adding 2g of porous graphite, stirring for 60 minutes, pouring, cooling to room temperature, and then carrying out DSC test and step cooling test.
The melting temperature, melting enthalpy value, solidifying temperature and solidifying enthalpy value are tested by using a Differential Scanning Calorimetry (DSC), and a DSC test effect chart shown in figure 2 is obtained, and the step cooling experiment test effect is shown in figure 3.
Example 2
With reference to fig. 4 and 5, fig. 4 is a DSC test result of example 2, and fig. 5 is a test result of a step-by-step cooling experiment of example 2, the present invention discloses a medium-temperature phase change heat storage material without supercooling, which is prepared by the following steps of quality material,
adopting 72g of L-arabitol, 15g of azelaic acid, 11g of sodium pyrophosphate decahydrate and 2g of porous graphite, firstly predicting the temperature of a reaction kettle to 150 ℃, pouring 72g of L-arabitol into the reaction kettle through a feeding port, stirring after the L-arabitol is completely heated and melted, slowly adding 15g of azelaic acid into the reaction kettle, stirring until the azelaic acid is completely melted, then slowly pouring 11g of sodium pyrophosphate decahydrate into the reaction kettle, stirring while adding, stirring for 30 minutes after the L-arabitol is fully melted, then adding 2g of porous graphite, stirring for 60 minutes, pouring out, cooling to room temperature, and then carrying out DSC test and step cooling experimental test.
The melting temperature, melting enthalpy value, solidifying temperature and solidifying enthalpy value are tested by using a Differential Scanning Calorimetry (DSC), and a DSC test effect graph shown in figure 4 is obtained, and the step cooling experiment test effect graph is shown in figure 5.
Example 3
Referring to fig. 6 and 7, wherein fig. 6 is a graph showing the DSC test effect of example 3, and fig. 7 is a graph showing the test effect of the step-by-step cooling experiment of example 3, the present invention discloses a medium-temperature phase change heat storage material without supercooling, which is prepared by the following steps of quality material,
adopting 90g of ribitol, 5g of adipic acid, 3g of sodium pyrophosphate decahydrate and 2g of porous graphite, firstly predicting a reaction kettle to 170 ℃, pouring 90g of ribitol into the reaction kettle through a feeding port, stirring after the ribitol is completely heated and melted, slowly adding 5g of adipic acid into the reaction kettle, stirring until all the adipic acid is melted, then slowly pouring 3g of sodium pyrophosphate decahydrate into the reaction kettle, stirring while adding, stirring for 30 minutes after the ribitol is completely melted, then adding 2g of porous graphite, stirring for 60 minutes, pouring out, cooling to room temperature, and then carrying out DSC test and step cooling experimental test.
The melting temperature, melting enthalpy value, solidifying temperature and solidifying enthalpy value are tested by using a differential thermal scanner (DSC), and a DSC test effect graph shown in figure 6 is obtained, and the step cooling experiment test effect is shown in figure 7.
Example 4
With reference to fig. 8 and fig. 9, in which fig. 8 is a graph of the DSC test effect of example 4, and fig. 9 is a graph of the test effect of the cooling experiment of example 4, the present invention discloses a medium-temperature phase change heat storage material without supercooling, which is prepared by the following steps of quality material,
adopting 84g of ribitol, 6g of azelaic acid, 8g of sodium pyrophosphate decahydrate and 2g of porous graphite, firstly predicting a reaction kettle to 150 ℃, pouring 84g of ribitol into the reaction kettle through a feeding port, stirring after the ribitol is completely heated and melted, slowly adding 6g of azelaic acid into the reaction kettle, stirring until the azelaic acid is completely melted, then slowly pouring 8g of sodium pyrophosphate decahydrate into the reaction kettle, stirring while adding, stirring for 30 minutes after the ribitol is completely melted, then adding 2g of porous graphite, stirring for 60 minutes, pouring out, cooling to room temperature, and then carrying out DSC test and step cooling experimental test.
The melting temperature, melting enthalpy value, solidifying temperature and solidifying enthalpy value are tested by using a differential thermal scanner (DSC), and a DSC test effect graph shown in figure 8 is obtained, and the step cooling experiment test effect is shown in figure 9.
Please continue to refer to table 1, which is a table of the thermophysical data of the non-supercooling medium-temperature phase change heat storage material of examples 1-4, wherein the data of the melting temperature, melting enthalpy, freezing temperature and freezing enthalpy of the materials tested by Differential Scanning Calorimetry (DSC) in examples 1-4 are shown in table 1,
| melting temperature | Melting enthalpy value | Freezing temperature | Enthalpy of solidification | |
| Example 1 | 107.04℃ | 259.28J/g | 104.67℃ | 256.31J/g |
| Example 2 | 113.32℃ | 258.27J/g | 110.30℃ | 251.12J/g |
| Example 3 | 108.71℃ | 245.36J/g | 105.04℃ | 241.88J/g |
| Example 4 | 109.25℃ | 228.31J/g | 108.47℃ | 226.56J/g |
TABLE 1
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of an intermediate-temperature phase-change heat storage material without supercooling is characterized by comprising the following steps,
step S1, preparing materials, namely preparing a first phase-change material, a second phase-change material and a nucleating agent, wherein the first phase-change material and the second phase-change material account for 80-95% by mass, and the nucleating agent accounts for 5-20% by mass;
s2, preheating the reaction kettle to 220 ℃ for 150-;
step S3, adding materials and stirring, namely adding the first phase-change material into the reaction kettle, heating until the first phase-change material is completely melted, stirring, slowly adding the second phase-change material into the reaction kettle while stirring until the second phase-change material is completely melted, slowly adding the nucleating agent into the reaction kettle while stirring, and stirring for 60-120 minutes after the nucleating agent is completely added into the reaction kettle;
step S4, pouring out and cooling, pouring out the mixture mixed in the reaction kettle, cooling to room temperature, and finishing the preparation of the heat storage material;
and step S5, testing, namely performing DSC test and step cooling experiment test on the prepared heat storage material.
2. The preparation method of a medium-temperature phase change heat storage material without supercooling according to claim 1, wherein the first phase change material is a sugar alcohol substance, and the second phase change material is a fatty acid substance or an ester substance.
3. The method for preparing a medium-temperature phase-change heat storage material without supercooling according to claim 2, wherein the first phase-change material is one or more of xylitol, sorbitol, L-arabitol, D-arabitol, ribitol, erythritol, galactitol, lactitol, D-lactitol monohydrate, maltitol, L-mannitol, D-mannitol, isomaltitol, D-threitol and mannoheptitol.
4. A method for preparing a medium-temperature phase change heat storage material without supercooling according to claim 2, wherein when the second phase change material is a fatty acid substance, the second phase change material is one or more of adipic acid, azelaic acid, polysebacic anhydride and sebacic acid.
5. The method for preparing an intermediate-temperature phase-change heat storage material without supercooling according to claim 2, wherein when the second phase-change material is an ester substance, the second phase-change material is dimethyl terephthalate.
6. The preparation method of a medium-temperature phase-change heat storage material without supercooling according to claim 1, wherein the nucleating agent is one or more of sodium pyrophosphate decahydrate, sodium sulfate decahydrate, sodium acetate trihydrate, disodium hydrogen phosphate dodecahydrate, sodium metasilicate pentahydrate and porous graphite.
7. The method for preparing an intermediate-temperature phase-change heat storage material without supercooling according to claim 1, wherein in the step S3, the stirring speed is 300-900 rpm.
8. The supercooled-free medium-temperature phase-change heat storage material prepared by the method for preparing a supercooled-free medium-temperature phase-change heat storage material according to any one of claims 1 to 7, wherein the temperature difference of the heat storage material before the melting temperature and the solidification temperature is small, only slight temperature fluctuation exists in the solidification heat release curve, and the material is noncorrosive to metals.
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