CN105349108A - Preparation method of phase-change energy-storage material - Google Patents
Preparation method of phase-change energy-storage material Download PDFInfo
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- CN105349108A CN105349108A CN201510864726.4A CN201510864726A CN105349108A CN 105349108 A CN105349108 A CN 105349108A CN 201510864726 A CN201510864726 A CN 201510864726A CN 105349108 A CN105349108 A CN 105349108A
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- 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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Abstract
The invention provides a preparation method of a phase-change energy-storage material. The preparation method comprises the steps of picking and grinding, by mass, 85-95 parts of polybasic carboxylic acid or a derivative of polybasic carboxylic acid into powder, adding, by mass, 2.50-7.50 parts of a nucleating agent and 2.50-7.50 parts of a thickener to the polybasic carboxylic acid or the derivative of the polybasic carboxylic acid, mixing the ingredients uniformly, placing the ingredients into a reactor, conducting stirring and a reaction for 30-180 minutes at the temperature of 80-150 DEG C, and obtaining a mixture; cooling the mixture to the room temperature, and obtaining the phase-change energy-storage material. The phase-change energy-storage material prepared through the preparation method is low in price and good in cyclic stability.
Description
Technical field
The application of field of material synthesis technology of the present invention, especially phase-changing energy storage material.
Background technology
Temporary transient no energy storage can be got up by phase-changing energy storage material, is discharged to during needs again, and this just can alleviate the contradiction between energy supply and demand, save energy.Utilize this characteristic of phase-changing energy storage material, the aspects such as air conditioner energy saving field, field of solar energy, aerospace field and electric power can be used in.Due to single phase change material in use unstable properties, can not meet the requirement of practical application, to the improvement of phase change material, and the research in composite phase-change energy storage material has become research emphasis in recent years.
Energy storage material is divided into substantially by the mode of energy storage: sensible heat energy storage, chemical reaction energy storage and hidden heat energy storage three major types.Sensible heat energy storage carrys out heat energy storage by the temperature variation of material, and heat-storage medium must have larger specific heat capacity.Although sensible heat energy storage material is fairly simple convenience in use, the temperature of its material self, in continuous change, cannot reach the object of control temperature, and such material energy storage density is low, thus makes corresponding device volume huge, and therefore its using value is not high.
Hidden heat energy storage utilize phase change material neither endothermic nor exothermic when phase transformation to carry out energy storage or release can, the energy density that this energy storage mode not only stores is high, and equipment therefor is simple, volume is little, flexible design, easy to use and be easy to management.Also having the advantage that very large: namely this kind of material is at phase-change accumulation energy process in which materials approximately constant temperature, therefore has most actual application prospect, is also apply maximum and most important energy storage mode at present.Phase change material has tempting prospect in field of solar energy, heat-storage and cold-storage field, air-conditioning and construction field and aerospace field.
The emphasis of current phase change material research becomes produced problem in material use to solid-liquid phase to improve.Gu the subject matter that-liquid phase becomes in material phase transformation process to be needed to solve has liquid phase to produce, must encapsulate when therefore using to it, the method for packing that oneself occurs at present has: encapsulation techniques, namely phase change material capsule body material package is got up; Utilize capillary action that phase change material is adsorbed onto in porous matrix; Shaping phase-change material is prepared with macromolecular material compound.Another problem easily occurred in mineral-type solid-liquid phase-changeable material phase transformation process is layering and surfusion, make to encounter a difficult problem to its application, for surfusion, solution has Added Nucleating Agents or adopts cold finger method (namely retain a part of cold-zone, make a part of not melting as nucleator); For demixing phenomenon, the method for solution has: a. adds thickening material; B. add crystalline structure and change agent; .c the container of splendid attire phase change material adopts laminate structure; D. rock or stir.
With reference to " Qin is apt to; Cao Chunfeng; Yang Jun; Yang Ruixiao. phase-changing energy storage material [P] .2012.CN201110283068.1. "
The Qin is kind waits a kind of phase-changing energy storage material of disclosure of the invention, and comprising: Antarctic Rock, nucleator, thickening material and thermal conducting agent, described nucleator is barium sulfate and six water strontium chlorides.Compared with prior art, this invention with barium sulfate and six water strontium chlorides for nucleator, because the aspects such as the crystal structure characteristic between this nucleator and Antarctic Rock, lattice parameter size, physical properties match, and coordinate compositions such as adding thickening material, thus solve the problem that in prior art, phase-changing energy storage material condensate depression is large.Meanwhile, because Antarctic Rock has larger latent heat of phase change, therefore, this phase-changing energy storage material also has the large feature of latent heat of phase change.Experimental result shows, phase-changing energy storage material condensate depression prepared by the present invention only has 0.4 DEG C.
This invention just using inorganic hydrated salt class as a kind of phase-changing energy storage material, obtain a kind of latent heat of phase change heat accumulating relatively preferably by different synthetic parameters methods, but this material still to there is latent heat of phase change low, the shortcomings such as cyclical stability difference.
With reference to " Wang Xiaodong; Zhang Huanzhi; The martial virtue is precious. a kind of composite phase-change energy storage material for microcapsule and preparation method thereof [P] .2011.CN201010167076.5. "
A kind of composite phase-change energy storage material for microcapsule of the disclosure of the invention such as Wang Xiaodong and preparation method thereof, its microcapsule shell material is silicon-dioxide, and microcapsule core is phase-changing energy storage material, wherein phase-changing energy storage material is the organic solid-liquid phase change energy-storage material of paraffin class.By dispersion emulsifier according to 0.2 ~ 0.5wt.%, aqueous solvent be 52.5-62.5wt.%, phase-changing energy storage material is 18.75 ~ 31.5wt.%, inorganic silicon source is 15.5 ~ 18.75wt.% proportioning, join in reaction vessel and stir 5 ~ 8h, under higher than solid-liquid phase change temperature 3 ~ 8 DEG C of conditions, make its dispersion and emulsion even; Then in emulsion, add aqueous hydrochloric acid or the pH=8.0 ~ 12.0 aqueous sodium hydroxide solution catalyzer of pH=0.93-4.07, reaction soln is naturally cooled to room temperature, be precipitated solution, the mixture of the throw out water be obtained by reacting and sherwood oil is washed, wherein the mass percentage of sherwood oil is 30wt.%, again with deionized water carry out washing, suction filtration, by products therefrom natural air drying.Invention increases phase-changing energy-storing power-saving technology, have the ability of automatic temperature-control, physical and chemical stability is good, cracking resistance, fire-retardant, wear-resisting, and thermal conductivity is high.
With reference to " Yang Zhenzhong; Jin Zhaoguo; Liu Jiguang; Qu little Zhong. microcapsule of organic phase change energy storage material and preparation method thereof [P] .2009.CN200810103749.3. "
Microcapsule of the disclosure of the invention such as Yang Zhenzhong organic phase change energy storage material and preparation method thereof.The microcapsule of this organic phase change energy storage material, are made up of core core and nucleocapsid, and the material of described core core comprises organic phase change energy storage material; Described nucleocapsid at least comprises internal layer and skin, and internal layer adopts any one method in situ aggregation method, interfacial polymerization, reacting phase partition method, complex coacervation and this Lung biopsy of sol-gel method to carry out coated; Any one method in outer these four kinds of methods of employing situ aggregation method, reacting phase partition method, sol-gel method and complex coacervation is carried out coated.The size of microcapsule of the present invention, nucleocapsid composition and shell thickness adjustable, there is good snappiness, physical strength, permeability resistance and dispersiveness, Solar use can be widely used in, industrial exhaust heat waste heat recovery, building energy conservation, constant temperature dress ornament, the fields such as cold-storage and thermal storage air-conditioning and electrical part constant temperature equal energy source, material, aerospace, weaving, electric power, medical instrument, building.
With reference to " Ji Junling; Wang Yuan; He Yeli; Wang Wei. heat storing and heat preserving microcapsule and its preparation method and application [P] .2011, CN201010514415.2. "
The invention such as Ji Junling relates to a kind of microcapsules of storing energy through phase change and its preparation method and application, and particularly relating to a kind of core core material is heat storing and heat preserving microcapsule of phase-changing energy storage material and its preparation method and application.These microcapsule are made up of core core, internal layer nucleocapsid and outer nucleocapsid, and core core material is organic phase change material; Internal layer nucleocapsid take vinyl monomer as polymerization single polymerization monomer, by interfacial polymerization parcel core core; Outer nucleocapsid with etherification melamine resin performed polymer for polymerization single polymerization monomer, by in-situ polymerization wrapping inner layer nucleocapsid.Heat storing and heat preserving microcapsule of the present invention, capsule wall has thermoset nature, and degrading resistance property is better, wear resistance and good endurance.Can be used for textiles heat preserving finishing and building thermal insulation material, it can ensure that the organic phase change material of the core core of heat storing and heat preserving microcapsule has larger phase-change energy, and organic phase change material mobility and migration can not occur after undergoing phase transition, thus temp. control function can be kept enduringly.
Several example above, mainly describe preparation method and some application prospects of microcapsule phase-change energy storage material, current existing phase-changing energy storage material comprises: hydration salt is as Na
2sO
410H
2o, MgCl
26H
2o etc., organic compound class is as low in the phase change material such as paraffin, polyalcohols all exists storage density, the problems such as expensive, cyclical stability is poor.
But although can be obtained the microencapsulated phase change material of salt hydrate-organic composite by modification, the mistake cold-peace that salt hydrate itself exists is separated and the problem of cyclical stability difference still cannot solve.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of preparation method of phase-changing energy storage material, comprising the steps:
The polycarboxylic acid or derivatives thereof getting 85 ~ 95 parts according to mass ratio is pulverized last, in described polycarboxylic acid or derivatives thereof, add the nucleator of 2.50 ~ 7.50 parts according to mass ratio, the thickening material mixing of 2.50 ~ 7.50 parts is placed in reactor, at 80 ~ 150 DEG C of stirring reaction 30 ~ 180min, obtain mixture; And be cooled to room temperature, obtain described phase-changing energy storage material.
Further, described tensio-active agent is one or more in cetyl trimethylammonium bromide, cetyldimethylethylambromide bromide ammonium, palmityl trimethyl ammonium chloride, polyoxyethylenated alcohol sodium sulfate and sodium lauryl sulphate.
Further, described polycarboxylic acid or derivatives thereof is selected from one or more in oxalic acid, propanedioic acid, the third three acid, succinic acid, hexanodioic acid.
Further, described nucleator is borax, water glass, calcium sulfate at least one.
Further, described thickening material is polyacrylamide or polyvinyl alcohol.
Beneficial effect:
The present invention has synthesized a kind of new phase change materials for heat energy storage.First, the transformation temperature of this phase change material is at 90 ~ 120 DEG C; Secondly the latent heat of phase change of this phase-changing energy storage material reaches 300 ~ 400Jg
-1, compare existing phase change material, the storage density of this phase change material improves 2 ~ 3.5 times, and this is the maximum advantage of this phase change material;
Again, the shortcoming of existing phase-changing energy storage material ubiquity cyclicity poor stability, this shortcoming is that material itself causes on the one hand, as: the mistake cold-peace of inorganic hydrated salt is separated, and being that phase change material working cycle is irreversible on the other hand causes.The present invention has taken into full account the demand of cyclical stability in the preparation process of phase-changing energy storage material, finally makes this novel phase-change material circulate after 500 times latent heat of phase change without obviously weakening.
Finally, this phase-changing energy storage material low in raw material price, preparation cost is lower.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of phase-changing energy storage material of the present invention.
Fig. 2 is that the embodiment of the present invention 1 phase-changing energy storage material circulates 100 thickness means of differential scanning calorimetry (DSC) graphic representations.
Fig. 3 is that the embodiment of the present invention 4 phase-changing energy storage material circulates 500 thickness means of differential scanning calorimetry (DSC) graphic representations.
Fig. 4 is that the embodiment of the present invention 5 phase-changing energy storage material circulates 500 thickness means of differential scanning calorimetry (DSC) graphic representations.
Embodiment
Below, will be described in detail the embodiment of the present invention by reference to the accompanying drawings.
Step one: prepare starting material.Starting material of the present invention comprise:
1, tensio-active agent: cetyl trimethylammonium bromide (being called for short CTAB), cetyldimethylethylambromide bromide ammonium (being called for short EHDAB), palmityl trimethyl ammonium chloride (being called for short CTAC), polyoxyethylenated alcohol sodium sulfate (being called for short AES) and sodium lauryl sulphate (being called for short AS) etc. can be selected from.
2, emulsifying agent, optional in poly(oxyethylene glycol) 400 list olein (be called for short PEG400MO) or the two olein (PEG400DO) of poly(oxyethylene glycol) 400 to polyethylene glycol 6000 list olein (being called for short PEG6000MO) or the two olein (PEG6000DO) of polyethylene glycol 6000 any one.
Above-mentioned tensio-active agent and emulsifying agent are as the core of phase-changing energy storage material.
3, polycarboxylic acid or derivatives thereof, can be selected from oxalic acid, propanedioic acid, the third three acid, succinic acid, hexanodioic acids etc. as the main material of phase-changing energy storage material.
4, nucleator, can be selected from borax Na
2b
4o
710H
2o, water glass Na
2siO
39H
2o, calcium sulfate CaSO
4deng.
5, thickening material, optional from polyacrylamide, polyvinyl alcohol etc.
Above-mentioned starting material are ready, then estimate the phase-changing energy storage material total mass M that need prepare, then account for the mass percent of described total mass M according to each starting material, calculate the quality m of each starting material actual needs
x.
Shown in composition graphs 1, in implementation and operation, each raw-material proportion relation operates as follows:
According to mass ratio, the emulsifying agent of the tensio-active agent of 8.25 ~ 16.75 parts with 8.25 ~ 16.75 parts is mixed, heated and stirred, obtain the first mixture.
Step 2: the polycarboxylic acid or derivatives thereof getting 58.75 ~ 78.50 parts according to mass ratio is pulverized last, mix with described first mixture and be placed in reactor, at 80 ~ 150 DEG C of stirring reaction 30 ~ 180min, make described first mixture and described polycarboxylic acid or derivatives thereof emulsion dispersion near transformation temperature even, obtain the second mixture.
Step 3: add the nucleator of 2.50 ~ 6.50 parts according to mass ratio in described second mixture, the thickening material of 2.50 ~ 6.50 parts mixes and be cooled to room temperature (naturally cooling solidification about need 1 ~ 3h), obtain the 3rd mixture of solid phase.Then affiliated 3rd mixture is ground or cut, obtain different shape (as: Powdered, sheet and bar-shaped etc.), described phase-changing energy storage material can be obtained.
The inventive method is introduced below in conjunction with embodiment 1 ~ 4.Reaction parameter and the phase-changing energy storage material parameter of each embodiment are as shown in table 1.
The reaction parameter of table 1 embodiment 1 ~ 4 and phase-changing energy storage material parameter
As known from Table 1, the new phase change materials for heat energy storage of the present invention's synthesis, by the ratio of allocation of raw materials, makes its transition temperature range be fixed on 90 ~ 120 DEG C; Using appropriate tensio-active agent, emulsifying agent, polycarboxylic acid as the base material of phase-changing energy storage material, be convenient to the phase change material deep processing of synthesis and transhipment; Add appropriate nucleator and thickening material raising latent heat of phase change density simultaneously, make the more existing raising of its latent heat of phase change 2 ~ 3.5 times.
Again shown in composition graphs 2, to the performance test experiment of the phase-changing energy storage material of embodiment 1 carry out circulation 100 times and 500 times, found that, circulate the latent heat of phase change density 365/Jg after 100 times
-1, transformation temperature is 101 DEG C; Circulate the latent heat of phase change density measurement result after 500 times without obviously weakening, and transformation temperature is 101 DEG C; Illustrate this novel phase-change material circulation 100 ~ 500 times after latent heat of phase change without obviously weakening.
Again shown in composition graphs 3, the phase-changing energy storage material of embodiment 4 is carried out to the performance test experiment of circulation 500 times, found that, the latent heat of phase change density measurement result after 500 times that circulates is still 230.74/Jg
-1, transformation temperature is 150 DEG C; Illustrate that this novel phase-change material to circulate after 500 times latent heat of phase change without obviously weakening.
The present invention also provides the preparation method of another kind of phase-changing energy storage material, and each raw-material proportion relation operates as follows:
The polycarboxylic acid or derivatives thereof getting 85 ~ 95 parts according to mass ratio is pulverized last, in described polycarboxylic acid or derivatives thereof, add the nucleator of 2.50 ~ 7.50 parts according to mass ratio, the thickening material mixing of 2.50 ~ 7.50 parts is placed in reactor, at 80 ~ 150 DEG C of stirring reaction 30 ~ 180min, obtain mixture; And be cooled to room temperature (naturally cooling solidification about needs 1 ~ 3h), obtain solid-phase mixture.
Then described solid-phase mixture is ground or cut, obtain different shape (as: Powdered, sheet and bar-shaped etc.), described phase-changing energy storage material can be obtained.
The inventive method is introduced below in conjunction with embodiment 5 ~ 6.Reaction parameter and the phase-changing energy storage material parameter of each embodiment are as shown in table 2.
The reaction parameter of table 2 embodiment 5 ~ 6 and phase-changing energy storage material parameter
As known from Table 2, the new phase change materials for heat energy storage adopting the another kind of synthetic method of the present invention to obtain, by the ratio of allocation of raw materials, makes its transition temperature range be fixed on 90 ~ 120 DEG C; Using polycarboxylic acid as the base material of phase-changing energy storage material, be convenient to the phase change material deep processing of synthesis and transhipment; Add appropriate nucleator and thickening material raising latent heat of phase change density simultaneously, make the more existing raising of its latent heat of phase change 2 ~ 3.5 times.
Shown in composition graphs 4, the phase-changing energy storage material of embodiment 5 is carried out to the performance test experiment of circulation 500 times, found that, the latent heat of phase change density survey after 500 times that circulate still has 210.72/Jg
-1, transformation temperature is 114 DEG C; Illustrate that this novel phase-change material to circulate after 500 times latent heat of phase change without obviously weakening.
Claims (4)
1. a preparation method for phase-changing energy storage material, is characterized in that, comprises the steps:
The polycarboxylic acid or derivatives thereof getting 85 ~ 95 parts according to mass ratio is pulverized last, in described polycarboxylic acid or derivatives thereof, add the nucleator of 2.50 ~ 7.50 parts according to mass ratio, the thickening material mixing of 2.50 ~ 7.50 parts is placed in reactor, at 80 ~ 150 DEG C of stirring reaction 30 ~ 180min, obtain mixture; And be cooled to room temperature, obtain described phase-changing energy storage material.
2. the preparation method of phase-changing energy storage material according to claim 1, is characterized in that, described polycarboxylic acid or derivatives thereof be selected from oxalic acid, propanedioic acid, the third three acid, succinic acid, hexanodioic acid one or more.
3. the preparation method of phase-changing energy storage material according to claim 1, it is characterized in that, described nucleator is borax, water glass, calcium sulfate at least one.
4. the preparation method of phase-changing energy storage material according to claim 1, it is characterized in that, described thickening material is polyacrylamide or polyvinyl alcohol.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105950118A (en) * | 2016-05-23 | 2016-09-21 | 中国科学院青海盐湖研究所 | Phase-change energy storage material and method for preparing same |
| WO2019109571A1 (en) * | 2017-12-07 | 2019-06-13 | 洛阳尖端技术研究院 | Temperature-regulating lining and manufacturing method and use thereof |
| CN112175582A (en) * | 2020-09-29 | 2021-01-05 | 华南理工大学 | Oxalic acid dihydrate/alum salt eutectic phase-change material and preparation method thereof |
| CN114305852A (en) * | 2022-03-10 | 2022-04-12 | 北京科技大学 | Phase change material cold compress paste |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105950118A (en) * | 2016-05-23 | 2016-09-21 | 中国科学院青海盐湖研究所 | Phase-change energy storage material and method for preparing same |
| CN105950118B (en) * | 2016-05-23 | 2019-03-19 | 中国科学院青海盐湖研究所 | Phase-changing energy storage material and preparation method thereof |
| WO2019109571A1 (en) * | 2017-12-07 | 2019-06-13 | 洛阳尖端技术研究院 | Temperature-regulating lining and manufacturing method and use thereof |
| CN112175582A (en) * | 2020-09-29 | 2021-01-05 | 华南理工大学 | Oxalic acid dihydrate/alum salt eutectic phase-change material and preparation method thereof |
| CN114305852A (en) * | 2022-03-10 | 2022-04-12 | 北京科技大学 | Phase change material cold compress paste |
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Application publication date: 20160224 |