CN101805591B - Inorganic hydrated salt expanded graphite composite phase-changing heat storage material and preparation method thereof - Google Patents
Inorganic hydrated salt expanded graphite composite phase-changing heat storage material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an inorganic hydrated salt expanded graphite composite phase-changing heat storage material. In the preparation method thereof, 85-89 mass parts of inorganic hydrated salt sodium acetate trihydrate as a heat storage matrix, 5.5-6.5 mass parts of disodium hydrogenphosphate as a nucleating agent, 2.5-3.5 mass parts of carboxymethyl cellulose as a thickening agent, and 3-4.5 mass parts of expanded graphite is blended in an inorganic hydrated salt mixture as a material with a high thermal conductivity. Due to the use of the expanded graphite, the material not only maintains excellent properties of natural flake graphite such as good thermal conductivity, no toxicity and the like, but also has adsorbability which the natural flake graphite does not have. The invention solves the problems of sub-cooling degree, phase stratification and low thermal conductivity during the heat storage process. The composite phase-changing material has a low sub-cooling degree after the phase changing performance is improved, the solution thereof is uniform without sedimentation and stratification during the solid-liquid phase change, the performance is stable, the repeatability of good, and the phase-changing heat storage can be enhanced through improving the thermal conductivity of the material.
Description
One, technical field
The present invention relates to a kind of composite phase-change heat-storage material, be specifically related to inorganic hydrated salt expanded graphite composite phase-changing material and preparation method thereof.
Two, background technology
The application of phase change heat-storing material (PCM) aspect peak load shifting, novel energy-saving construction timber, waste heat recovery and the air-conditioning technical of solar heating, aerospace, thermal load more and more widely.Especially with hidden heat energy storage technology, because its equipment therefor is simple, volume is little, flexible design, easy to use and be easy to characteristics such as management and popular.In numerous latent heat storage materials, use the more materials such as paraffin, lipid acid, inorganic hydrated salt class that mainly contain.Wherein, Inorganic hydrated salt is one type of very important middle low temperature phase change heat accumulating; It can provide fusing point from several degrees centigrade to more than 100 degrees centigrade multiple phase change material, uses halogenide, vitriol, nitrate salt, phosphoric acid salt, carbonate and acetate etc. that more salt hydrate mainly contains alkali and earth alkali metal at present.This type phase change material latent heat density is very high; Volume change is little during phase transformation; And nontoxic, non-volatility, nonflammable etc., these aspects all are superior to most of paraffin and fatty acid phase change material, but the maximum shortcoming of said material was easy to generate cold-peace phase demixing phenomenon when being solid-liquid phase change.This has limited its application in reality storage thermal technology journey greatly.In numerous inorganic hydrated salt materials, Sodium acetate trihydrate (CH
3COONa3H
2O) fusing point is 58 ℃, and Heat of fusion is 265kJ/kg, the specific heat capacity of solid, liquid phase be respectively 1.97 with 3.22kJ/kg ℃; Because of its transformation temperature is suitable, latent heat density is higher, is a kind of very potential phase change material; But its condensate depression can reach tens and spend to tens degree, has seriously limited its application.At present, to salt hydrate Sodium acetate trihydrate material, the main direction of research is in such heat accumulation matrix, to add suitable reagent to solve it and cross cold-peace phase lamination problem, expands the scope and the space of its application.
In addition, the thermal conductivity of inorganic hydrated salt class heat-storing material is generally all lower, and Sodium acetate trihydrate is under solid-state and liquid two kinds of situation; Thermal conductivity is all lower, generally has only about 0.6～0.7W/m ℃, in practical application; Because the low thermal conductivity of material, phase transition heat accumulation unit is when heat accumulation and heat release, and its heat exchange efficiency is also lower; This has also limited the application of material, also is an important channel of improving its phase-change accumulation energy performance so improve the thermal conductivity of material.
One Chinese patent application CN200810025631.3 provides organism/matter/expandable graphite composite phase change heat-storing building material and preparation method thereof; CN200310117411.0 provides the preparation method of the holder and the heat accumulating thereof of heat storage type heat pump air-conditioning plant, suppresses the combustibility of paraffin; Graphite/paraffin composite phase change heat accumulating thermal conductivity, CN200910080431.2 provides a kind of heat storage phase-changing material and method of manufacture thereof, and heat storage phase-changing material is by zeyssatite, swelling soil or expanded graphite; Urea-formaldehyde resin; Core material: heat storage phase-changing materials such as paraffin, the still unexposed Sodium acetate trihydrate of above scheme and expanded graphite bonded heat storage phase-changing material and preparation method.
Three, summary of the invention
To the problem that will solve in the above-mentioned prior art, the objective of the invention is to propose the additive formulations that a cover improves the phase transformation performance of inorganic hydrated salt Sodium acetate trihydrate, cold excessively, phase layering that solves that it exists in the storage thermal process and low thermal conductivity problem.Behind the phase transformation improved performance, composite phase-change material has less condensate depression, and solution is even during solid-liquid phase change; Do not precipitate, not stratified, stable performance, it is good to repeat performance; The thermal conductivity that improves material also is to improve its phase-change accumulation energy performance, can better application in the storage thermal technology journey of reality.
The objective of the invention is to realize: composite phase-change heat-storage material of the present invention through following technical scheme; It is characterized in that; Composition is that 85-89 part inorganic hydrated salt Sodium acetate trihydrate is as the heat accumulation matrix by quality; Quality be the disodium hydrogen phosphate of 5.5-6.5 part to make nucleator, quality be that the CMC 99.5 of 2.5-3.5 part is made thickening material, quality be the expanded graphite of 3-4.5 part as the material blending of high thermal conductivity coefficient in the inorganic hydrated salt mixture, improve its thermal conductivity.
The preparation method that the present invention proposes, its characteristic comprises following key step:
(1) with quality is the solid-state inorganic hydrated salt Sodium acetate trihydrate analytical pure particle of 85-89 part; Quality is that to make nucleator, quality be that the CMC 99.5 of 2.5-3.5 part is made thickening material (the I type CMC 99.5 that white is cotton-shaped) to the disodium hydrogen phosphate of 5.5-6.5 part; After placing the mortar porphyrize, uniform mixing;
(2) mixture that aforementioned proportion is mixed is placed in the test tube, in 80 ± 7 ℃ water-bath, is heated to complete melted state, and the back that stirs forms eutectic mixture;
(3) get the expansible black lead particle that quality is 3-4.5 part; The vacuum drying oven of putting into 65 ± 5 ℃ is after dry 15 ± 8 hours; It is retort furnace thermal treatment 60 ± 30s of 700 ± 40 ℃ that taking-up places temperature, makes the expansible black lead grain expansion, prepares to have the expanded graphite that enriches microvoid structure.
(4) above-mentioned expanded graphite is put into the inorganic hydrated salt eutectic mixture, obtain composite phase-change material behind the naturally cooling after 1 ± 0.3 hour in blended under agitation, absorption under the liquid situation.
Typical expansible black lead particulate rate of expansion 200mL/g; More than granularity 80 orders, carbon content is more than 90%, and the material of the high thermal conductivity coefficient that is used for adding adds phase change material; Can strengthen the performance of heat accumulating; But the proportion of the granulate material of often high thermal conductivity is difficult to be complementary with liquid inorganic hydrated salt solution, and like some metal-powders, density is bigger than normal; Active carbon powder, density is on the low side, in liquid solution, is not to float over solution surface, is deposited in the solution bottom exactly, can't be dispersed in the solution, is difficult to satisfy the requirement of the repeatedly solid-liquid phase change of heat accumulating in actual engineering.The expanded graphite that uses among the present invention is a kind of loose porous vermiform material that is obtained through graphite intercalation, washing and drying, high temperature puffing by natural flake graphite; Through behind the high temperature puffing; The original plane layer of graphite obviously splits and produces nonaffine deformation; And plane layer is rolled state, and the surface is netted pass structure.Advantageous properties such as the thermal conductivity that expanded graphite had both kept natural flake graphite is good, toxicological harmless have the unexistent adsorptivity of natural flake graphite again.With the inorganic hydrated salt Sodium acetate trihydrate is that phase change material (containing thickening material, nucleator), expanded graphite are supporting structure, utilizes the porous characterization of adsorption of expanded graphite, has prepared the composite phase-change material of SAT/ expanded graphite of the present invention.
Four, embodiment
Composite phase-change heat-storage material; Composition is that 85-89 part transformation temperature is that inorganic hydrated salt about 58 ℃ is as the heat accumulation matrix by mass content; Quality be 5.5-6.5 part make nucleator, quality is the thickening material of doing of 2.5-3.5 part; Quality be 3-4.5 part as the material blending of high thermal conductivity coefficient in the inorganic hydrated salt mixture, improve its thermal conductivity.
Embodiment 1:
A kind of inorganic hydrated salt expanded graphite composite phase-changing heat storage material of the present invention; This phase change material mixes by following quality: Sodium acetate trihydrate analytical pure 20 grams; Disodium hydrogen phosphate 1.24g; CMC 99.5 (or CMS) 0.64g, its quality proportioning is 100: 6.2: 3.2.
During preparation, to complete melting state, the back that stirs forms mixture with the mixture heating up that mixes according to the above ratio; Get quality and be the drying expansible black lead particle later of 0.9g, placing temperature is 50 seconds of retort furnace thermal treatment of 700 ℃, takes out then; Expanded graphite is joined in the mixture; Under liquid situation, stir, adsorb after 1 hour, naturally cooling obtains inorganic hydrated salt expanded graphite composite phase-changing heat storage material.Get the sample of above-mentioned composite phase-change material, carry out the differential scanning calorimetry experiment, use the Perkin-Elmer type dsc measurement appearance of U.S. PE company to carry out rising temperature for dissolving and the experiment of lowering the temperature and solidifying, the phase transformation enthalpy that records is 254kj/kg, and the peak temperature is 58.5 ℃.
Embodiment 2:
Another kind of inorganic hydrated salt expanded graphite composite phase-changing heat storage material of the present invention; This phase change material mixes by following quality: Sodium acetate trihydrate analytical pure 20 grams; Disodium hydrogen phosphate 1.2g, CMC 99.5 0.70g, its quality proportioning is 100: 6: 3.5.
During preparation, to complete melting state, the back that stirs forms mixture with the mixture heating up that mixes according to the above ratio; Get the drying expansible black lead particle later of quality 1g, placing temperature is 50 seconds of retort furnace thermal treatment of 700 ℃, takes out then; Expanded graphite is joined in the mixture; Under liquid situation, stir, adsorb after 1 hour, naturally cooling obtains inorganic hydrated salt expanded graphite composite phase-changing heat storage material.Through measuring, its latent heat of phase change is 231.2kj/kg, and transformation temperature is 57.2 ℃.
Embodiment 3:
Another kind of inorganic hydrated salt expanded graphite composite phase-changing heat storage material of the present invention; This phase change material mixes by following quality: 5 kilograms of Sodium acetate trihydrate analytical pure; Disodium hydrogen phosphate 0.3kg, CMC 99.5 0.15kg, its quality proportioning is 100: 6: 3.During preparation, to complete melting state, the back that stirs forms mixture with the mixture heating up that mixes according to the above ratio; Get the drying expansible black lead particle later of quality 0.2kg; Placing temperature is 700 ℃ retort furnace thermal treatment 1 minute, takes out then, and expanded graphite is joined in the mixture; Under liquid situation, stir; Adsorb after 1 hour, pour the mixture of liquid state in quadrate flat plate mold naturally cooling, be pressed into the solid phase composite phase-change material of square simultaneously.Measuring its thermal conductivity through flat band method, is 2.07W/mK through its thermal conductivity of measuring.Producing the test specimen piece that the equal in quality proportioning does not contain expanded graphite, is 1.05W/mK through its thermal conductivity of measuring.Mixing expanded graphite almost doubles the thermal conductivity of inorganic hydrated salt (being typically Sodium acetate trihydrate) when phase change material is solid-state.
CMC 99.5 can replace with CMS.
Other embodiment is following:
| Material weight part scheme number | Expanded graphite | Sodium acetate trihydrate | Disodium hydrogen phosphate | CMC 99.5 |
| 1 | 3 | 85 | 6 | 3.5 |
| 2 | 4.5 | 88 | 6.5 | 2.5 |
| 3 | 4 | 89 | 5.5 | 3 |
| 4 | 4.5 | 85 | 6.5 | 2.5 |
| 5 | 4 | 88 | 6.5 | 3 |
| 6 | 4 | 89 | 6 | 3.5 |
| 7 | 4.5 | 86 | 5.5 | 3 |
| 8 | 4 | 88 | 6 | 3 |
| 9 | 3 | 89 | 6 | 3 |
The material prescription of above composition all can reach effect of the present invention.
Claims (2)
1. inorganic hydrated salt expanded graphite composite phase-changing heat storage material; It is characterized in that; Composition and quality that composite phase-change storage material is formed are following: by quality is that 85-89 part inorganic hydrated salt Sodium acetate trihydrate is as the heat accumulation matrix; Quality be the disodium hydrogen phosphate of 5.5-6.5 part to make nucleator, quality be that the CMC 99.5 of 2.5-3.5 part is made thickening material, and the expanded graphite that enriches microvoid structure for 3-4.5 part with the quality as the material blending of high thermal conductivity coefficient in the inorganic hydrated salt mixture; The said expanded graphite that enriches microvoid structure is: the rate of expansion 200mL/g of expanded graphite particles; More than granularity 80 orders; Carbon content is more than 90%, and expanded graphite particles is put into 65 ± 5 ℃ vacuum drying oven after dry 15 ± 8 hours, and taking out and placing temperature is retort furnace thermal treatment 60 ± 30s of 700 ± 40 ℃; Expanded graphite particles is expanded, prepare and have the expanded graphite that enriches microvoid structure.
2. the preparation method of inorganic hydrated salt expanded graphite composite phase-changing heat storage material, its characteristic may further comprise the steps:
(1) with quality is the solid-state inorganic hydrated salt Sodium acetate trihydrate analytical pure particle of 85-89 part; Quality is that to make nucleator, quality be that the CMC 99.5 of 2.5-3.5 part is made thickening material to the disodium hydrogen phosphate of 5.5-6.5 part; After placing the mortar porphyrize, uniform mixing;
(2) mixture that aforementioned proportion is mixed is placed in the test tube, in 80 ± 7 ℃ water-bath, is heated to complete melted state, and the back that stirs forms eutectic mixture;
(3) get the expanded graphite particles that quality is 3-4.5 part, the rate of expansion 200mL/g of expanded graphite particles, more than granularity 80 orders, carbon content is more than 90%; The vacuum drying oven of putting into 65 ± 5 ℃ is after dry 15 ± 8 hours, and taking out and placing temperature is retort furnace thermal treatment 60 ± 30s of 700 ± 40 ℃, and expanded graphite particles is expanded, and prepares to have the expanded graphite that enriches microvoid structure;
(4) above-mentioned expanded graphite is put into the inorganic hydrated salt eutectic mixture, obtain composite phase-change material behind the naturally cooling after 1 ± 0.3 hour in blended under agitation, absorption under the liquid situation.
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