CN104927776A - Preparation method of multilevel-structure titanium dioxide based composite phase-change material - Google Patents
Preparation method of multilevel-structure titanium dioxide based composite phase-change material Download PDFInfo
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Abstract
The invention discloses a preparation method of a multilevel-structure titanium dioxide based composite phase-change material. The method comprises the following steps of preparing monodispersed silicon dioxide microspheres; preparing composite microspheres with silicon dioxide/titanium dioxide core-shell structures; preparing multilevel-structure titanium dioxide microspheres; preparing the multilevel-structure titanium dioxide based composite phase-change material. The preparation method of the multilevel-structure titanium dioxide based composite phase-change material belongs to the technical field of energy-saving and energy-storage materials. A loading type composite phase-change material is prepared by loading a phase-change material with excellent properties of high energy-storage density, high heat conductivity and the like on a multilevel-structure titanium dioxide, and the combination properties of the solid loading ability, the cyclical stability and the like of the phase-change material are improved while the thermal properties, that the heat storage property is good, the heat efficiency is high, and the like, of the phase-change material are not influenced. The method provided by the invention is simple in reaction technique, mild in conditions and short in flow, and is applicable to industrialized production.
Description
Technical field
The invention belongs to energy-conservation energy storage material technical field, particularly the preparation method of the titania-based composite phase-change material of a kind of multilevel hierarchy.
Background technology
Phase-transition heat-storage/energy storage is the important technology improving energy utilization rate and protection of the environment, and phase change material is the key factor affecting accumulation of heat/energy storage technology development and application.Utilize the latent heat of phase change of phase change material to realize storage and the utilization of energy, contribute to improving efficiency and exploitation renewable energy source, have broad application prospects in the field such as energy-conservation of Solar use, " peak load shifting " of electric power and civil heating and air-conditioning.Phase change material, due to the excellent properties such as high energy storage density, high thermal conductivity, becomes energy-conservation energy storage material of greatest concern at present, but the problem of its easy leakage, cyclical stability difference limits its widespread use.Therefore, the research and development of phase change material become the study hotspot in energy science and material science in recent years.The problem of leak of liquid easily occurs in phase transition process for phase change material, and investigator starts the composite phase-change material that Devoting Major Efforts To Developing has higher cyclical stability.
From the patent that Related Research Domain is declared, known by by phase change material and the carrier compound with immobilized ability, be one of major way improving phase change material cyclical stability at present.CN103923614A provides a kind of preparation method of ordered porous base shaped composite phase-change material, by by phase change material and porous silicon dioxide carrier compound, improves its stability, prevents the leakage of phase change material.CN103694963A provides a kind of preparation method of composite phase-change material, by by phase change material and porous and graphited carbon microspheres compound, improves heat conductivility and the stability of phase change material.The adjustable multi-stage hollow structure carrier of micro/nano-scale is constructed by multistage assembling, phase transformation core can be encapsulated in multilevel hierarchy cavity and realize sizing, heat-transfer medium is assembled in multilevel hierarchy nano pore and improves the capacity of heat transmission, thus the heat realizing multistage assembling composite phase-change material stores and thermal conduction is strengthened, but all there is not the report to the titania-based composite phase-change material of multilevel hierarchy in existing patent.
Therefore, select a kind of phase change material carrier with multilevel hierarchy, and by suitable mode and phase change material compound, while maintenance phase change material stores the performances such as heat transfer, improve the over-all propertieies such as its immobilized ability, cyclical stability, remain a technical barrier of this area.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of loading type composite phase-change material carrier, by the effective compound with phase change material, while not affecting the performances such as phase change material accumulation of energy heat transfer, improve the over-all properties such as immobilized ability, cyclical stability of phase change material.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for the titania-based composite phase-change material of multilevel hierarchy, described method concrete steps are as follows:
Step one: prepare monodispersed silicon dioxide microsphere;
Step 2: prepare earth silicon/titanic oxide nucleocapsid structure complex microsphere, at silicon dioxide microsphere Surface coating titanium dioxide shell;
Step 3: prepare multilevel hierarchy titanium dioxide microballoon sphere, is dissolved silica template by the hydro-thermal reaction under alkaline condition, and etches the titanium dioxide microballoon sphere that titanium dioxide shell obtains multilevel hierarchy simultaneously;
Step 4: prepare the titania-based composite phase-change material of multilevel hierarchy.
Further, described step one is specially: in the mixed solution of tetraethoxy, dehydrated alcohol and deionized water, under 20 DEG C of-30 DEG C of conditions, magnetic agitation, add the ammoniacal liquor that volumetric concentration is 25%-28%, reaction 3-8 hour, collect pressed powder, washing, oven dry, obtain the silicon dioxide microsphere of diameter within the scope of 50-500nm.
Further, described tetraethoxy: ammoniacal liquor: water: the mol ratio of dehydrated alcohol is 1:(2 ~ 20): (20 ~ 140): (50 ~ 100).
Further, described step 2 is specially: mixed with lower alcohol and ammoniacal liquor (25% ~ 28%) by silicon dioxide microsphere obtained in step one, after ultrasonic disperse, 40 ~ 60 DEG C of water-baths and magnetic agitation, slowly add the mixed type low-alcohol solution configured by titanium source again, react 12 ~ 24 hours, centrifugal, alcohol wash, washing, oven dry, obtain the hud typed complex microsphere of earth silicon/titanic oxide.
Further, the mol ratio of described silicon dioxide microsphere, ammoniacal liquor, titanium source, lower alcohol is 1:(2 ~ 20): (1 ~ 30): (200 ~ 1000).
Further, described titanium source comprises: one or more in tetrabutyl titanate, isopropyl titanate, and described lower alcohol comprises: one or more in methyl alcohol, ethanol.
Further, described step 3 is specially: by earth silicon/titanic oxide nucleocapsid structure complex microsphere ultrasonic disperse obtained for step 2 in concentration be 0.1 ~ 10 molL
-1sodium hydroxide solution in, the mass ratio of described earth silicon/titanic oxide nucleocapsid structure complex microsphere, sodium hydroxide is 1:20 ~ 40, react 2 hours ~ 10 hours under 90 ~ 200 DEG C of conditions in encloses container, be cooled to room temperature, collect white precipitate washing, dry, product being soaked in concentration is 0.1 ~ 5 molL
-1in hydrochloric acid soln, washing, oven dry; Then 300 ~ 500 DEG C of high-temperature calcinations 1 ~ 7 hour, obtain multilevel hierarchy titanium dioxide microballoon sphere.
Further, described step 4 is specially: the multilevel hierarchy titanium dioxide microballoon sphere obtained in step 3, phase change material, ethanol are mixed, 50 ~ 90 DEG C of water-baths and magnetic agitation 3 ~ 5 hours, dry 24 ~ 72 hours in 70 ~ 100 DEG C of baking ovens, then in retort furnace 250 ~ 300 DEG C calcining 1 ~ 3 hour, obtain loading type composite phase-change material.
Further, the mass ratio of described multilevel hierarchy titanium dioxide microballoon sphere, phase change material, ethanol is 1:1 ~ 20:30 ~ 100.
Further, described phase change material comprises: one or more of lithium nitrate, SODIUMNITRATE, polyoxyethylene glycol, Octadecane, paraffin.
Beneficial effect of the present invention is: prepared the titania-based composite phase-change material of multilevel hierarchy by load phase change material on multilevel hierarchy titania support, phase transformation core is encapsulated in multilevel hierarchy cavity and realizes sizing, heat-transfer medium is assembled in multilevel hierarchy nano pore and improves the capacity of heat transmission, the heat achieving multilevel hierarchy composite phase-change material stores the lifting with the over-all properties such as thermal conduction, and simple with method reaction process provided by the invention, mild condition, flow process are short, are applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the multilevel hierarchy titanium dioxide/lithium nitrate composite phase-change material adopting the inventive method to prepare.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is explained in further detail.Should be appreciated that specific embodiment described herein only for explaining the present invention, being not intended to limit the present invention.
On the contrary, the present invention is contained any by the substituting of making on marrow of the present invention and scope of defining of claim, amendment, equivalent method and scheme.Further, in order to make the public have a better understanding to the present invention, in hereafter details of the present invention being described, detailedly describe some specific detail sections.Do not have the description of these detail sections can understand the present invention completely for a person skilled in the art yet.
The preparation method of the titania-based composite phase-change material of a kind of multilevel hierarchy, described method is passed through load phase change material on titania support thus is obtained loading type composite phase-change material, do not affecting while phase change material stores the performances such as heat transfer, improve the over-all propertieies such as its immobilized ability, cyclical stability, the preparation method of described composite phase-change material specifically comprises the steps:
Step one: prepare monodispersed silicon dioxide microsphere, in the mixed solution of tetraethoxy, dehydrated alcohol and deionized water, under 20 DEG C of-30 DEG C of conditions, magnetic agitation, add the ammoniacal liquor that volumetric concentration is 25%-28%, reaction 3-8 hour, collect pressed powder, washing, oven dry, obtain the silicon dioxide microsphere of diameter within the scope of 50-500nm.Each molar ratio of material is: tetraethoxy: ammoniacal liquor: water: dehydrated alcohol=1:(2 ~ 20): (20 ~ 140): (50 ~ 100);
Step 2: prepare earth silicon/titanic oxide nucleocapsid structure complex microsphere, at silicon dioxide microsphere Surface coating titanium dioxide shell, silicon dioxide microsphere, lower alcohol and ammoniacal liquor (25% ~ 28%) are mixed with certain weight ratio, after ultrasonic disperse, 40 ~ 60 DEG C of water-baths and magnetic agitation, more slowly add the mixed type low-alcohol solution configured by titanium source, react 12 ~ 24 hours, centrifugal, alcohol wash, washing, oven dry, obtain the hud typed complex microsphere of earth silicon/titanic oxide.Wherein the mol ratio of silicon dioxide microsphere, ammoniacal liquor, titanium source, lower alcohol is: 1:(2 ~ 20): (1 ~ 30): (200 ~ 1000);
Described titanium source comprises: one or more in tetrabutyl titanate, isopropyl titanate, wherein preferred tetrabutyl titanate;
Described lower alcohol comprises: one or more in methyl alcohol, ethanol, wherein preferred alcohol;
Step 3: prepare multilevel hierarchy titanium dioxide microballoon sphere, by the hydro-thermal reaction under alkaline condition, silica template is dissolved, and etch the titanium dioxide microballoon sphere that titanium dioxide shell obtains multilevel hierarchy simultaneously, by earth silicon/titanic oxide nucleocapsid structure complex microsphere ultrasonic disperse obtained for step 2 in concentration be 0.1 ~ 10 molL
-1sodium hydroxide solution in, in encloses container under 90 ~ 200 DEG C of conditions react 2 hours ~ 10 hours, be cooled to room temperature, collect white precipitate washing, dry.Product being soaked in concentration is 0.1 ~ 5 molL
-1in hydrochloric acid soln, washing, oven dry; Then 300 ~ 500 DEG C of high-temperature calcinations 1 ~ 7 hour, obtain multilevel hierarchy titanium dioxide microballoon sphere.Wherein, the mass ratio of earth silicon/titanic oxide nucleocapsid structure complex microsphere, sodium hydroxide is 1:20 ~ 40;
Step 4: prepare the titania-based composite phase-change material of multilevel hierarchy, multilevel hierarchy titanium dioxide microballoon sphere, phase change material, ethanol are mixed by certain weight ratio, 50 ~ 90 DEG C of water-baths and magnetic agitation 3 ~ 5 hours, dry 24 ~ 72 hours in 70 ~ 100 DEG C of baking ovens, then in retort furnace 250 ~ 300 DEG C calcining 1 ~ 3 hour, obtain loading type composite phase-change material.Wherein, the mass ratio of multilevel hierarchy titanium dioxide microballoon sphere, phase change material, ethanol is 1:1 ~ 20:30 ~ 100.
Described phase change material comprises: one or more of lithium nitrate, SODIUMNITRATE, polyoxyethylene glycol, Octadecane, paraffin.
[case study on implementation 1]
Silicon dioxide microsphere, ethanol and ammoniacal liquor (25% ~ 28%) are mixed with certain weight ratio, after ultrasonic disperse, 45 DEG C of water-baths and magnetic agitation, slowly add the ethanolic soln configured by tetrabutyl titanate again, react 24 hours, centrifugal, alcohol wash, washing, oven dry, obtain the hud typed complex microsphere of earth silicon/titanic oxide; Wherein the mass ratio of silicon dioxide microsphere, ammoniacal liquor, tetrabutyl titanate, ethanol is: 1:5:17:790.By the earth silicon/titanic oxide nucleocapsid structure complex microsphere ultrasonic disperse that obtains in concentration be 1 molL
-1sodium hydroxide solution in, in encloses container under 120 DEG C of conditions react 2 hours, be cooled to room temperature, collect white precipitate washing, dry.Product being soaked in concentration is 0.1 molL
-1in hydrochloric acid soln, washing, oven dry; Then 450 DEG C of high-temperature calcinations 4 hours, obtain multilevel hierarchy titanium dioxide microballoon sphere.Wherein, the mass ratio of earth silicon/titanic oxide nucleocapsid structure complex microsphere, sodium hydroxide is 1:27;
Multilevel hierarchy titanium dioxide microballoon sphere, lithium nitrate, ethanol are mixed by certain weight ratio, 70 DEG C of water-baths and magnetic agitation 4 hours, dries 24 hours in 80 DEG C of baking ovens.Then in retort furnace 280 DEG C calcining 2 hours, obtain loading type composite phase-change material.Wherein, the mass ratio of multilevel hierarchy titanium dioxide microballoon sphere, lithium nitrate, ethanol is 1:1.5:60.
[case study on implementation 2]
Silicon dioxide microsphere, ethanol and ammoniacal liquor (25% ~ 28%) are mixed with certain weight ratio, after ultrasonic disperse, 45 DEG C of water-baths and magnetic agitation, slowly add the ethanolic soln configured by isopropyl titanate again, react 24 hours, centrifugal, alcohol wash, washing, oven dry, obtain the hud typed complex microsphere of earth silicon/titanic oxide; Wherein the mass ratio of silicon dioxide microsphere, ammoniacal liquor, isopropyl titanate, ethanol is: 1:5:16:790.By the earth silicon/titanic oxide nucleocapsid structure complex microsphere ultrasonic disperse that obtains in concentration be 1 molL
-1sodium hydroxide solution in, in encloses container under 150 DEG C of conditions react 4 hours, be cooled to room temperature, collect white precipitate washing, dry.Product being soaked in concentration is 0.1 molL
-1in hydrochloric acid soln, washing, oven dry; Then 450 DEG C of high-temperature calcinations 4 hours, obtain multilevel hierarchy titanium dioxide microballoon sphere.Wherein, the mass ratio of earth silicon/titanic oxide nucleocapsid structure complex microsphere, sodium hydroxide is 1:27;
Multilevel hierarchy titanium dioxide microballoon sphere, polyoxyethylene glycol, ethanol are mixed by certain weight ratio, 80 DEG C of water-baths and magnetic agitation 4 hours, dries 24 hours in 80 DEG C of baking ovens.Then in retort furnace 280 DEG C calcining 2 hours, obtain loading type composite phase-change material.Wherein, the mass ratio of multilevel hierarchy titanium dioxide microballoon sphere, polyoxyethylene glycol, ethanol is 1:10:60.
The above is only the preferred embodiment for the present invention; it should be pointed out that the member of ordinary skill for the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Beneficial effect of the present invention is: prepared the titania-based composite phase-change material of multilevel hierarchy by load phase change material on multilevel hierarchy titania support, phase transformation core is encapsulated in multilevel hierarchy cavity and realizes sizing, heat-transfer medium is assembled in multilevel hierarchy nano pore and improves the capacity of heat transmission, the heat achieving multilevel hierarchy composite phase-change material stores the lifting with the over-all properties such as thermal conduction, and simple with method reaction process provided by the invention, mild condition, flow process are short, are applicable to suitability for industrialized production.
Claims (10)
1. a preparation method for the titania-based composite phase-change material of multilevel hierarchy, is characterized in that, described method concrete steps are as follows:
Step one: prepare monodispersed silicon dioxide microsphere;
Step 2: prepare earth silicon/titanic oxide nucleocapsid structure complex microsphere, at silicon dioxide microsphere Surface coating titanium dioxide shell;
Step 3: prepare multilevel hierarchy titanium dioxide microballoon sphere, is dissolved silica template by the hydro-thermal reaction under alkaline condition, and etches the titanium dioxide microballoon sphere that titanium dioxide shell obtains multilevel hierarchy simultaneously;
Step 4: prepare the titania-based composite phase-change material of multilevel hierarchy.
2. the preparation method of titania-based composite phase-change material according to claim 1, it is characterized in that, described step one is specially: in the mixed solution of tetraethoxy, dehydrated alcohol and deionized water, under 20 DEG C of-30 DEG C of conditions, magnetic agitation, add the ammoniacal liquor that volumetric concentration is 25%-28%, reaction 3-8 hour, collects pressed powder, washing, oven dry, obtains the silicon dioxide microsphere of diameter within the scope of 50-500nm.
3. the preparation method of titania-based composite phase-change material according to claim 2, is characterized in that, described tetraethoxy: ammoniacal liquor: water: the mol ratio of dehydrated alcohol is 1:(2 ~ 20): (20 ~ 140): (50 ~ 100).
4. the preparation method of titania-based composite phase-change material according to claim 1, it is characterized in that, described step 2 is specially: mixed with lower alcohol and ammoniacal liquor (25% ~ 28%) by silicon dioxide microsphere obtained in step one, after ultrasonic disperse, 40 ~ 60 DEG C of water-baths and magnetic agitation, more slowly add the mixed type low-alcohol solution configured by titanium source, react 12 ~ 24 hours, centrifugal, alcohol wash, washing, oven dry, obtain the hud typed complex microsphere of earth silicon/titanic oxide.
5. the preparation method of titania-based composite phase-change material according to claim 4, is characterized in that, the mol ratio of described silicon dioxide microsphere, ammoniacal liquor, titanium source, lower alcohol is 1:(2 ~ 20): (1 ~ 30): (200 ~ 1000).
6. the preparation method of titania-based composite phase-change material according to claim 5, it is characterized in that, described titanium source comprises: one or more in tetrabutyl titanate, isopropyl titanate, and described lower alcohol comprises: one or more in methyl alcohol, ethanol.
7. the preparation method of titania-based composite phase-change material according to claim 1, is characterized in that, described step 3 is specially: by earth silicon/titanic oxide nucleocapsid structure complex microsphere ultrasonic disperse obtained for step 2 in concentration be 0.1 ~ 10 molL
-1sodium hydroxide solution in, the mass ratio of described earth silicon/titanic oxide nucleocapsid structure complex microsphere, sodium hydroxide is 1:20 ~ 40, react 2 hours ~ 10 hours under 90 ~ 200 DEG C of conditions in encloses container, be cooled to room temperature, collect white precipitate washing, dry, product being soaked in concentration is 0.1 ~ 5 molL
-1in hydrochloric acid soln, washing, oven dry; Then 300 ~ 500 DEG C of high-temperature calcinations 1 ~ 7 hour, obtain multilevel hierarchy titanium dioxide microballoon sphere.
8. the preparation method of titania-based composite phase-change material according to claim 1, it is characterized in that, described step 4 is specially: the multilevel hierarchy titanium dioxide microballoon sphere obtained in step 3, phase change material, ethanol are mixed, 50 ~ 90 DEG C of water-baths and magnetic agitation 3 ~ 5 hours, dry 24 ~ 72 hours in 70 ~ 100 DEG C of baking ovens, then in retort furnace 250 ~ 300 DEG C calcining 1 ~ 3 hour, obtain loading type composite phase-change material.
9. the preparation method of titania-based composite phase-change material according to claim 8, is characterized in that, the mass ratio of described multilevel hierarchy titanium dioxide microballoon sphere, phase change material, ethanol is 1:1 ~ 20:30 ~ 100.
10. the preparation method of titania-based composite phase-change material according to claim 9, is characterized in that, described phase change material comprises: one or more of lithium nitrate, SODIUMNITRATE, polyoxyethylene glycol, Octadecane, paraffin.
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| CN106318338A (en) * | 2016-08-19 | 2017-01-11 | 武汉科技大学 | In-situ alloy-oxide complex-phase heat-storage refractory material and preparation method thereof |
| CN107936931A (en) * | 2017-12-11 | 2018-04-20 | 大连理工大学 | A kind of magnetic thermal energy conversion and thermal energy storage stable phase change composite material and preparation method thereof |
| CN109468122A (en) * | 2018-12-18 | 2019-03-15 | 北京化工大学 | One kind " core-shell structure copolymer " type mesoporous silicon oxide/organic phase change material composite Nano capsule and preparation method thereof |
| CN115286983A (en) * | 2022-09-14 | 2022-11-04 | 台州邦博装饰材料有限公司 | Heat-insulating coating for building exterior wall |
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| CN115491112B (en) * | 2022-11-01 | 2023-07-11 | 广东万联新材料有限公司 | Coating for building outer wall |
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