CN102888211B - A kind of composite shape-setting phase-change material and preparation method thereof - Google Patents
A kind of composite shape-setting phase-change material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of composite shape-setting phase-change material and preparation method thereof.One has certain latent heat of phase change specifically, and temperature higher than outward appearance during its transformation temperature still in the solid-state and composite shape-setting phase-change material of dimensionally stable, its framework material is polyaniline, and the phase change material playing the effect of latent heat heat accumulation is the one of n-caprylic acid, n-capric acid, positive laurostearic acid, positive TETRADECONIC ACID, n-hexadecanoic, n-octadecanoic acid, positive 20 sour, positive behenic acids, positive tetracosanoic acid or positive hydroxyhexacosanoic acid.The consumption that the latent heat of phase change of this composite shape-setting phase-change material can adjust phase change material as required makes it adjustable within the scope of 33 ~ 172J/g.Its preparation method is: 1) phase change material and aniline are distributed in water under the effect of tensio-active agent and form emulsion; 2) at 0 ~ 25 DEG C, add the polyreaction that initiator causes aniline; 3) composite shape-setting phase-change material is obtained through filtering, washing also drying after having reacted.Shaping phase-change material obtained by this method, there is preparation technology simple, cost is low, in temperature higher than still keeping solid-state during its transformation temperature and the advantage of dimensionally stable, the multiple occasions such as solar thermal utilization, intelligent automatic air-conditioning and construction thing, glasshouse, phase-change energy-storage air-conditioning, temperature control equipment can be widely used in.
Description
Technical field
The present invention relates to shaping phase-change material and preparation method thereof, one has certain latent heat of phase change specifically, and temperature below or above during its transformation temperature all in solid-state and composite shape-setting phase-change material of dimensionally stable and preparation method thereof.
Background technology
The energy is the basis of human survival and social development, and the utilizable energy of current people can be divided into two classes: fossil energy and renewable energy source.Wherein fossil energy account for the overwhelming majority of mankind's energy used.Along with the development of society, people to the demand of the energy also in quick growth.Energy dilemma has become one of main factor of restriction social development.So people invest energy-conservation and field of renewable energy sight one after another.In the productive life activity of people, the final utilization form overwhelming majority of energy is heat energy.Therefore, the storage of heat energy just becomes an important research field that is energy-conservation and exploitation renewable energy source.Phase change material is undergone phase transition between the two phases by material and absorbs or discharge a large amount of heat energy, thus plays the effect of heat energy storage.Therefore, phase change material causes the broad interest of people as the basic substance of thermal energy storage.In addition, the many energy forms in actual production and life, as the valley period power energy etc. of sun power, industrial exhaust heat, used heat and electrical network, all also exist the time difference between a supply and demand.If these energy storage can not be got up to cause great waste.And use phase change material these energy first can be stored with the form of heat energy, and then the supply people stable when needing use, for energy-conservation and exploitation renewable energy source provide an approach easily.Phase change material is absorbing or release heat energy and in the process that undergoes phase transition, and itself temperature is almost constant or change is very little, and therefore phase change material can also by temperature control devices field.
Most study in phase change material, source is the widest, price is the most cheap, most actual application prospect be solid-liquid phase change material, it changes by material the storage realizing heat energy between solid, liquid two-phase.But solid-liquid phase change material also exists serious problems, and namely material in use can repeatedly exist in fluid form, so the encapsulation problem of material must be solved, cause the practical application of material very inconvenient.For this reason, investigators propose the way being made into shaping phase-change material.When temperature is higher than its transformation temperature, shaping phase-change material is macroscopically still showing as solid-state and dimensionally stable, thus solves an encapsulation difficult problem for phase change material.In addition, carry out will adding various filler when modification is entered to solid-liquid phase change material, and the existence in fluid form that phase change material in use repeats can inevitably cause filler be separated with phase change material and lose the effect of modification.Propping material network in shaping phase-change material can stop filler to be separated with phase change material, plays the effect of stable material performance.Therefore, shaping phase-change material has become the study hotspot of phase-change heat-storage material.
The research of shaping phase-change material has the history of recent two decades.People use various method, utilize multiple starting material, prepare multiple shaping phase-change material, two classes are summed up: the first kind is adsorbed in the solid, porous material such as polynite by solid-liquid phase change material and obtains, there is not pressure-bearing in this type of shaping phase-change material, easily leaks, and propping material range of choice is narrow, hole utilization ratio is low, the deficiencies such as anisotropic heat conductivity; Equations of The Second Kind is encapsulated in polymer propping material by method that is coated or soft or hard block by solid-liquid phase change material and obtains, these type of shaping phase-change material wide material sources, and not easily leak, volume energy storage density is high, heat conductivility isotropy, is convenient to application.
Polyaniline is a class conducting polymer composite, and it has excellent environmental stability and thermostability, and its preparation process is simple, can be used as a kind of excellent framework material and is applied to shaping phase-change material field.But have not yet to see the report of polyaniline involved in the present invention/fatty acid shaping phase-change material.
Summary of the invention
The invention provides a kind of pulverous composite shape-setting phase-change material newly and preparation method thereof.This composite shape-setting phase-change material take polyaniline as framework material, with the one of n-caprylic acid, n-capric acid, positive laurostearic acid, positive TETRADECONIC ACID, n-hexadecanoic, n-octadecanoic acid, positive 20 sour, positive behenic acids, positive tetracosanoic acid or positive hydroxyhexacosanoic acid for phase-change heat-storage material, the consumption of phase-change heat-storage material can be adjusted as required to adjust its phase-change thermal storage ability.The preparation method of this composite shape-setting phase-change material is simple, and raw material is easy to get, and is a kind of excellent shaping phase-change material.
For achieving the above object, the present invention takes following technical scheme.
A kind of pulverous composite shape-setting phase-change material, it is characterized in that: its framework material is polyaniline, the phase change material playing the effect of latent heat heat accumulation is the one of n-caprylic acid, n-capric acid, positive laurostearic acid, positive TETRADECONIC ACID, n-hexadecanoic, n-octadecanoic acid, positive 20 sour, positive behenic acids, positive tetracosanoic acid or positive hydroxyhexacosanoic acid; When the fusing point of temperature higher than phase change material, this composite shape-setting phase-change material outward appearance is still in solid-state and dimensionally stable; The consumption that the latent heat of phase change of this composite shape-setting phase-change material can adjust phase change material as required makes it adjustable within the scope of 33 ~ 172J/g.
Described composite shape-setting phase-change material prepares as follows: higher than at the fusing point 5 ~ 20 DEG C of phase change material, first dispersed with stirring after the mixing of a certain amount of phase change material, tensio-active agent and water is formed emulsion in 1 ~ 2 hour, add a certain amount of aniline and concentrated hydrochloric acid again or only add a certain amount of aniline, continuing dispersed with stirring and obtain stable emulsion in 0.5 ~ 1 hour; The water at low temperature of 0 ~ 20 DEG C or mixture of ice and water is adopted to cool aforementioned stable emulsion and Keep agitation emulsion again; After aforementioned stable emulsion is cooled to 0 ~ 25 DEG C, then keep this temperature, under agitation add the polyreaction that a certain amount of ammonium persulfate aqueous solution causes aniline, the ammonium persulfate aqueous solution concentration added is 0.075 ~ 0.59g/mL; Add-on is 7.8 ~ 12% of preparation emulsion time institute water consumption volume; Composite shape-setting phase-change material is obtained through filtering, washing also drying after reacting 2 ~ 12 hours again.
Described tensio-active agent is Sodium dodecylbenzene sulfonate or cetyl trimethylammonium bromide.
In described stable emulsion, the content of water is 30 ~ 35 times of phase change material and aniline quality sum, the content of phase change material is 20 ~ 90% of phase change material and aniline quality sum, the consumption of tensio-active agent is 0.06 ~ 0.5% of the quality of water used, the consumption of concentrated hydrochloric acid is institute's water consumption volume 0.8 ~ 1.2% or without concentrated hydrochloric acid.
Tool of the present invention has the following advantages.
The invention provides a kind of pulverous shaping phase-change material newly, different shape can be pressed into as required, its latent heat of phase change can be changed by the consumption of adjustment phase change material as required, environmental stability is good, can according to the different phase change material of the different choice of use temperature as phase-change heat-storage material, and the preparation method of this shaping phase-change material is simple, cost is lower, raw materials used all cheap and easy to get, utilize the present invention effectively can improve the performance of organic phase change material, expand its range of application.
Embodiment
Embodiment 1.
1) prepare emulsion: the palmitic acid getting 2.6g, the cetyl trimethylammonium bromide of 0.08g mixes with 90mL water, puts into the water-bath of 68 DEG C, stirs and adds 0.4g aniline and 1mL concentrated hydrochloric acid after 1 hour, then stirs and obtain stable emulsion in 1 hour.
2) cooling of emulsion: keep stirring velocity constant, change the hot water bath of 68 DEG C into ice-water bath, until emulsion temperature drops to 0 ~ 5 DEG C.
3) initiated polymerization: keep the temperature of emulsion at 0 ~ 5 DEG C, under vigorous stirring, the 7mL aqueous solution containing 0.98g ammonium persulphate is slowly added drop-wise in emulsion, adds in 20 minutes, Keep agitation, react 12 hours.
4) separation and purification product: the mixture after having reacted is filtered, filter cake is washed with water, then filter cake is dried in 60 DEG C and obtained composite shape-setting phase-change material.
5) heat accumulation test: the Q2000 type differential scanning calorimeter (DSC) that the thermal energy storage performance test of described composite shape-setting phase-change material is produced in TA company of the U.S. is carried out, specific operation process is: the composite shape-setting phase-change material taking 1.5 ~ 4mg puts into sample crucible, in the temperature range of 20 ~ 100 DEG C, scan with the temperature rise rate of 10 DEG C/min; Then the program using instrument to carry processes experimental result, and the start-up phase temperature recording composite shape-setting phase-change material is 61.47 DEG C, and phase transformation peak temperature is 64.89 DEG C, and latent heat of phase change is 172.3J/g.
6) stability test: composite shape-setting phase-change material tabletting machine is made a right cylinder at the pressure of 1MPa, puts into the thermostat container of 70 DEG C, observes cylindrical shape and does not change and do not have liquid remittance to leak after 12 hours.
Embodiment 2.
1) prepare emulsion: the palmitic acid getting 1.8g, the cetyl trimethylammonium bromide of 0.054g mixes with 90mL water, puts into the water-bath of 70 DEG C, stirs and adds 1.2g aniline and 1.1mL concentrated hydrochloric acid after 1 hour, then stirs and obtain stable emulsion in 1 hour.
2) cooling of emulsion: keep stirring velocity constant, change the hot water bath of 70 DEG C into ice-water bath, until emulsion temperature drops to 0 ~ 5 DEG C.
3) initiated polymerization: keep the temperature of emulsion at 0 ~ 5 DEG C, under vigorous stirring, the 10mL aqueous solution containing 2.91g ammonium persulphate is slowly added drop-wise in emulsion, adds in 20 minutes, Keep agitation, react 2 hours.
4) separation and purification product: the mixture after having reacted is filtered, filter cake is washed with water, then filter cake is dried in 60 DEG C and obtained composite shape-setting phase-change material.
5) heat accumulation test: the Q2000 type differential scanning calorimeter (DSC) that the thermal energy storage performance test of described composite shape-setting phase-change material is produced in TA company of the U.S. is carried out, specific operation process is: the composite shape-setting phase-change material taking 1.5 ~ 4mg puts into sample crucible, in the temperature range of 20 ~ 100 DEG C, scan with the temperature rise rate of 10 DEG C/min; Then the program using instrument to carry processes experimental result, and the start-up phase temperature recording composite shape-setting phase-change material is 60.38 DEG C, and phase transformation peak temperature is 62.71 DEG C, and latent heat of phase change is 102.8J/g.
5) stability test: composite shape-setting phase-change material tabletting machine is made a right cylinder at the pressure of 1MPa, puts into the thermostat container of 70 DEG C, observes cylindrical shape and does not change and do not have liquid remittance to leak after 12 hours.
Embodiment 3.
1) emulsion is prepared: 20 acid of getting 1.6g, the cetyl trimethylammonium bromide of 0.08g mixes with 70mL water, puts into the water-bath of 80 DEG C, stirs and adds 0.4g aniline and 0.56mL concentrated hydrochloric acid after 2 hours, then stirs and obtain stable emulsion in 1 hour.
2) cooling of emulsion: keep stirring velocity constant, the hot water bath of 80 DEG C is changed into the cooling bath of 15 ~ 20 DEG C, until emulsion temperature drops to 20 ~ 25 DEG C.
3) initiated polymerization: keep the temperature of emulsion at 20 ~ 25 DEG C, under vigorous stirring, the 10mL aqueous solution containing 0.98g ammonium persulphate is slowly added drop-wise in emulsion, adds in 20 minutes, Keep agitation, react 12 hours.
4) separation and purification product: the mixture after having reacted is filtered, filter cake is washed with water, then filter cake is dried in 60 DEG C and obtained composite shape-setting phase-change material.
5) heat accumulation test: the Q2000 type differential scanning calorimeter (DSC) that the thermal energy storage performance test of described composite shape-setting phase-change material is produced in TA company of the U.S. is carried out, specific operation process is: the composite shape-setting phase-change material taking 1.5 ~ 4mg puts into sample crucible, in the temperature range of 20 ~ 100 DEG C, scan with the temperature rise rate of 10 DEG C/min; Then the program using instrument to carry processes experimental result, and the start-up phase temperature recording composite shape-setting phase-change material is 73.92 DEG C, and phase transformation peak temperature is 76.03 DEG C, and latent heat of phase change is 163.3J/g.
6) stability test: composite shape-setting phase-change material tabletting machine is made a right cylinder at the pressure of 1MPa, puts into the thermostat container of 80 DEG C, observes cylindrical shape and does not change and do not have liquid remittance to leak after 12 hours.
Embodiment 4.
1) prepare emulsion: the TETRADECONIC ACID of getting 2.7g, the Sodium dodecylbenzene sulfonate of 0.5g mixes with 100mL water, puts into the water-bath of 74 DEG C, stirs and adds 0.3g aniline after 1 hour, then stirs and obtain stable emulsion in 0.5 hour.
2) cooling of emulsion: keep stirring velocity constant, change the hot water bath of 74 DEG C into ice-water bath, until emulsion temperature drops to 0 ~ 5 DEG C.
3) initiated polymerization: keep the temperature of emulsion at 0 ~ 5 DEG C, under vigorous stirring, the 10mL aqueous solution containing 0.75g ammonium persulphate is slowly added drop-wise in emulsion, adds in 20 minutes, Keep agitation, react 12 hours.
4) separation and purification product: the mixture after having reacted is filtered, filter cake is washed with water, then filter cake is dried in 50 DEG C and obtained composite shape-setting phase-change material.
5) heat accumulation test: the Q2000 type differential scanning calorimeter (DSC) that the thermal energy storage performance test of described composite shape-setting phase-change material is produced in TA company of the U.S. is carried out, specific operation process is: the composite shape-setting phase-change material taking 1.5 ~ 4mg puts into sample crucible, in the temperature range of 10 ~ 90 DEG C, scan with the temperature rise rate of 10 DEG C/min; Then the program using instrument to carry processes experimental result, and the start-up phase temperature recording composite shape-setting phase-change material is 53.04 DEG C, and phase transformation peak temperature is 58.52 DEG C, and latent heat of phase change is 168.5J/g.
6) stability test: composite shape-setting phase-change material tabletting machine is made a right cylinder at the pressure of 1MPa, puts into the thermostat container of 65 DEG C, observes cylindrical shape and does not change and do not have liquid remittance to leak after 12 hours.
Embodiment 5.
1) prepare emulsion: the TETRADECONIC ACID of getting 0.6g, the Sodium dodecylbenzene sulfonate of 0.5g mixes with 100mL water, puts into the water-bath of 60 DEG C, stirs and adds 2.4g aniline after 2 hours, then stirs and obtain stable emulsion in 0.5 hour.
2) cooling of emulsion: keep stirring velocity constant, change the hot water bath of 60 DEG C into ice-water bath, until emulsion temperature drops to 0 ~ 5 DEG C.
3) initiated polymerization: keep the temperature of emulsion at 0 ~ 5 DEG C, under vigorous stirring, the 12mL aqueous solution containing 5.89g ammonium persulphate is slowly added drop-wise in emulsion, adds in 20 minutes, Keep agitation, react 12 hours.
4) separation and purification product: the mixture after having reacted is filtered, filter cake is washed with water, then filter cake is dried in 50 DEG C and obtained composite shape-setting phase-change material.
5) heat accumulation test: the Q2000 type differential scanning calorimeter (DSC) that the thermal energy storage performance test of described composite shape-setting phase-change material is produced in TA company of the U.S. is carried out, specific operation process is: the composite shape-setting phase-change material taking 1.5 ~ 4mg puts into sample crucible, in the temperature range of 10 ~ 90 DEG C, scan with the temperature rise rate of 10 DEG C/min; Then the program using instrument to carry processes experimental result, and the start-up phase temperature recording composite shape-setting phase-change material is 52.91 DEG C, and phase transformation peak temperature is 57.29 DEG C, and latent heat of phase change is 33.2J/g.
6) stability test: composite shape-setting phase-change material tabletting machine is made a right cylinder at the pressure of 1MPa, puts into the thermostat container of 65 DEG C, observes cylindrical shape and does not change and do not have liquid remittance to leak after 12 hours.
Claims (3)
1. a pulverous composite shape-setting phase-change material, it is characterized in that: its framework material is polyaniline, the phase change material playing the effect of latent heat heat accumulation is the one of n-caprylic acid, n-capric acid, positive laurostearic acid, positive TETRADECONIC ACID, n-hexadecanoic, n-octadecanoic acid, positive 20 sour, positive behenic acids, positive tetracosanoic acid or positive hydroxyhexacosanoic acid; This composite shape-setting phase-change material is prepared as follows: higher than at the fusing point 5 ~ 20 DEG C of phase change material, first dispersed with stirring after the mixing of a certain amount of phase change material, tensio-active agent and water is formed emulsion in 1 ~ 2 hour, add a certain amount of aniline and concentrated hydrochloric acid again or only add a certain amount of aniline, continuing dispersed with stirring and obtain stable emulsion in 0.5 ~ 1 hour; Then the water at low temperature of 0 ~ 20 DEG C or mixture of ice and water is adopted to cool aforementioned stable emulsion and Keep agitation emulsion; After aforementioned stable emulsion is cooled to 0 ~ 25 DEG C, keep this temperature, under agitation add the polyreaction that a certain amount of ammonium persulfate aqueous solution causes aniline, then obtain composite shape-setting phase-change material through filtering, washing also drying after reacting 2 ~ 12 hours; When the fusing point of temperature higher than phase change material, this composite shape-setting phase-change material outward appearance is still in solid-state and dimensionally stable; The consumption that the latent heat of phase change of this composite shape-setting phase-change material can adjust phase change material as required makes it adjustable within the scope of 33 ~ 172J/g.
2. according to composite shape-setting phase-change material according to claim 1, it is characterized in that: in described preparation method: in stable emulsion, the content of water is 30 ~ 35 times of phase change material and aniline quality sum, the content of phase change material is 20 ~ 90% of phase change material and aniline quality sum, the content of tensio-active agent is 0.06 ~ 0.5% of the quality of water used, the content of concentrated hydrochloric acid is institute's water consumption volume 0.8 ~ 1.2% or not containing concentrated hydrochloric acid; The ammonium persulfate aqueous solution concentration added is 0.075 ~ 0.59g/mL; Add-on is 7.8 ~ 12% of preparation emulsion time institute water consumption volume.
3. according to composite shape-setting phase-change material according to claim 1, it is characterized in that: in described preparation method, tensio-active agent is Sodium dodecylbenzene sulfonate or cetyl trimethylammonium bromide.
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| CN103146351B (en) * | 2013-03-20 | 2015-07-08 | 长沙理工大学 | Shaped phase-change material with high heat-conducting property and preparation method thereof |
| CN104830281B (en) * | 2015-05-07 | 2017-12-05 | 长沙理工大学 | A kind of medium temperature composite shape-setting phase-change heat-storage material and preparation method thereof |
| CN104845592B (en) * | 2015-05-07 | 2017-12-29 | 长沙理工大学 | A kind of high heat conduction medium temperature shaping phase-change material and preparation method thereof |
| CN104830280B (en) * | 2015-05-07 | 2017-11-10 | 长沙理工大学 | A kind of shaping phase-change material for passive type Thermal protection and preparation method thereof |
| CN106753265B (en) * | 2017-01-12 | 2019-04-05 | 合肥工业大学 | A kind of raising CH3NH3PbI3The method of phase transition temperature |
| CN109082266B (en) * | 2018-08-27 | 2021-02-12 | 西南科技大学 | High-thermal-conductivity and high-heat-storage-coefficient foam carbon-based phase-change energy storage sensing material |
| TWI695918B (en) * | 2019-08-27 | 2020-06-11 | 財團法人紡織產業綜合研究所 | Fabric |
| CN110684510B (en) * | 2019-10-23 | 2021-10-26 | 广东工业大学 | Heat-conduction-enhanced heat-energy-storage shape-stabilized phase-change composite material and preparation method thereof |
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| CN101845293A (en) * | 2010-05-25 | 2010-09-29 | 北京交通大学 | Infrared phase-changing material and preparation method thereof |
| CN102605463A (en) * | 2011-12-15 | 2012-07-25 | 江南大学 | Preparation method and application for fatty acid/polymer shaped phase-change superfine complex fiber |
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| CN102407088A (en) * | 2010-09-21 | 2012-04-11 | 中国科学院化学研究所 | Preparation method for phase-change energy-storage microcapsule and phase-change energy-storage microcapsule |
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| CN101845293A (en) * | 2010-05-25 | 2010-09-29 | 北京交通大学 | Infrared phase-changing material and preparation method thereof |
| CN102605463A (en) * | 2011-12-15 | 2012-07-25 | 江南大学 | Preparation method and application for fatty acid/polymer shaped phase-change superfine complex fiber |
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