CN109021931A - A kind of phase-change heat-storage material preparation method using unorganic glass as heat-storage medium - Google Patents
A kind of phase-change heat-storage material preparation method using unorganic glass as heat-storage medium Download PDFInfo
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- CN109021931A CN109021931A CN201810962305.9A CN201810962305A CN109021931A CN 109021931 A CN109021931 A CN 109021931A CN 201810962305 A CN201810962305 A CN 201810962305A CN 109021931 A CN109021931 A CN 109021931A
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- 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
Abstract
The phase-change heat-storage material preparation method that the invention discloses a kind of using unorganic glass as heat-storage medium, belongs to high temperature technical field of phase change heat storage.This method comprises: preparing unorganic glass;Unorganic glass is ground, is dried, dry unorganic glass powder is made;Obtained dry glass powder and basis material are prepared by phase-change heat-storage material using powder compacting sintering or high temperature infiltration method.Preparation method of the present invention is simple, and cost is relatively low, is easily mass produced, is of great significance to high-temperature phase-change heat storage material.
Description
Technical field
The present invention relates to high temperature technical field of phase change heat storage, in particular, provide a kind of using unorganic glass as storage
The phase-change heat-storage material preparation method of thermal medium.
Background technique
With the rapid economic development in our country, the demand to the energy is increasingly enhanced, but current 80% energy sources in
Non-renewable fossil energy, such as coal, petroleum, natural gas etc..Coal and petroleum not only scarcity of resources, and applying
Cheng Zhonghui causes seriously to pollute to environment.Electric heating is the heating system of a kind of cleaning, safety, by the adjusting of electrovalence policy,
Carry out resident's Peak-valley TOU power price, so that the electric heating mode with energy stores is necessary, can be further improved electricity and adopt
Warm economy, " peak load shifting " are the peak loads for reducing power grid, improve low ebb load, and smooth load curve stablizes power grid
The important means of operation.Phase-change heat-storage material be a period of time or certain space temporarily unused excess energy passes through certain
Approach is collected and is stored, and is released again in energy requirement peak period.Phase-change heat-storage material can pass through two phase transition
A large amount of thermal energy are stored or discharged, achieve the purpose that in electric heating " peak load shifting ".And with safety is good, is easy to run control
The advantages that with management.
Phase-change thermal storage medium studied both at home and abroad at present is mostly based on organic, inorganic fused salt class.Organic phase-change thermal storage
Material mainly in solid state mouldability it is preferable, be generally less prone to supercooling and phenomenon of phase separation, and the corruption to material
Corrosion is smaller, and performance is more stable, and small toxicity is at low cost.But that there are thermal coefficients is small for it, leads to the response speed to thermal change
Degree is slow, and density is lower, so that the energy storage capacity of unit volume is smaller, and the general fusing point of organic matter is lower, is unsuitable for high-temperature field
It closes, it is volatile, inflammable, easily by the slow deterioration by oxidation of oxygen in air, (cold light brightness, Lan Zhipeng, Ge Zhiwei wait heat accumulating
Progress [J] energy storage science and technology, 2015,4 (2): 119-130.);Fused salt phase-change heat-storage material is with its storage density
Height, it is at low cost the advantages that be widely applied at home and abroad phase-change thermal storage field (Zhao Qian, Wang Junbo, Song Yukuan, wait fuse salt height store up
Progress [J] inorganic chemicals industry of hot material, 2014,46 (11): 5.), and Kenisarin (Kenisarin M
M.High-temperature phase change materials forthermal energy storage[J]
.Renew.Sustain.Energy Rev., 2010,14 (3): 955-970) fused salt material to use scope at 120~1000 DEG C
Material and selection method, thermal property, compatibility and the enhancement method of hot physical property of alloy material etc. are discussed, and fluorine is related to
The mixing materials such as salt dissolving, chlorate, carbonate, nitrate, metal alloy have absolutely proved the use scope of fused salt phase-change material
Extensively, Kourkova etc. is studied (Kourkova L, Sadovska G.Heat to the thermal storage performance of Li2CO3
Capacity, enthalpy and entropy of Li2CO3 at 303,5-563.15K [J] .ThemochimActa,
2007,452:80), (Liao Min, Ding Jing, Wei little Lan wait preparation and heat transfer accumulation of heat property [J] of high temperature carbonic acid fused salt to Liao Min etc.
Inorganic chemicals industry, 2008,40 (10): 15-17.) use the static method melted to prepare Na2CO3-KNO3 novel molten salt, and it is right
The high-melting-point substances such as fuse salt addition sodium chloride, potassium chloride, potassium carbonate are modified;(Hu Baohua, Ding Jing, Wei are small by Hu Baohua etc.
Orchid waits the hot physical property measurement and thermal stability analysis [J] inorganic chemicals industry of high-temperature molten salt, 2010,40 (1): 22-24) with chlorine
Change sodium anhydrous calcium chloride is raw material, prepares the fused salt mixt that maximum allowable operating temperature (M.A.O.T.) is 800 DEG C.Li Yuefeng etc. (Li Yuefeng,
Eastern high temperature phase change material (pcm) Li2CO3-Na2CO3 cycle thermal stability analysis [J] energy storage science and technology, 2013,4 (2): 369)
Li2CO3-Na2CO3 Molten Binary Salts are prepared for, and its performance is studied, cold light brightness (Leng G, Qiao G, Jiang
Z,et al.Micro encapsulated&form-stable phase change materials for high
Temperature thermal energy storage [J] .Applied Energy, 2018,217:212-220.) use silicon
Diatomaceous earth prepares NaCl-KCl phase-change heat-storage material as matrix and studies its performance.But fused salt phase-change heat-storage material according to
The problems such as old that there are thermal conductivitys is low, and the coefficient of expansion is big, supercooling is serious, hygroscopicity is serious, to environmental corrosion and leakage problem (leaf
Cutting edge of a knife or a sword, the Qujiang River is blue, and Zhong Junyu waits phase-change heat-storage material progress [J] process engineering journal, 2010,10 (6): 1231-
1241.), this problem seriously limits its scope of application, therefore it is urgent, necessary for finding the new heat-storage medium of one kind.
There is softening molten condition in unorganic glass, equally equally exist under the conditions of high temperature in softening-process of setting
Heat accumulation-exothermic process, according to R. Kang Neite, (Kang Neite opens the Simple Calculation side for rushing silicate technical glass fusing institute's calorific requirement
Method [J] China glass, 1992 (5): 53-60.) research, unorganic glass can store 750J/g's or more in fusion process
Heat, and the phase-change thermal storage that experiment measures fused salt is 150J/g, thermal storage performance is far longer than fused salt, and asepsis environment-protecting, service life
Long, easily large-scale production, it is more likely that the substitute as fused salt phase-change material.Unorganic glass has the thermal cycle higher than fused salt
Performance and stable chemical property;It is not in dusting in wet environment, phenomena such as deliquescence, and according to the tune to formula
Just, change interfacial wettability and use temperature, in different environments so as to application.So in use environment application aspect, nothing
Machine glass is with greater advantage than fused salt.
Accordingly, it is intended to a kind of phase-change heat-storage material using unorganic glass as heat-storage medium be provided, to solve for existing
The problem of thering is fused salt phase-change heat-storage material to fail under humidity environment and reveal environmental corrosion and fused salt.
Summary of the invention
In order to achieve the goal above, the present invention provides a kind of phase-change heat-storage material system using unorganic glass as heat-storage medium
Preparation Method, this method are used as heat-storage medium using glass powder, carry out with structural matrix complex sintered, are prepared for a kind of with glass powder
Phase-change heat-storage material as heat-storage medium.The present invention failed under humidity environment for existing fused salt phase-change heat-storage material and
The problem of revealing environmental corrosion and fused salt, uses glass powder as heat-storage medium, and complex sintered with basis material progress
Preparation, obtains anti-moisture absorption, and thermal storage performance is good, corrosion-free and leakage high-performance phase-change heat-storage material.
Phase-change heat-storage material preparation method according to the present invention using unorganic glass as heat-storage medium, including following step
It is rapid:
(1) unorganic glass is prepared;
(2) unorganic glass ground, dried, dry unorganic glass powder is made;
(3) use powder compacting sintering or high temperature infiltration method by the unorganic glass powder and basis material of obtained drying
It is prepared into phase-change heat-storage material.
Further, described the step of preparing unorganic glass include: according to use temperature deploy glass formula, according to formula
Glass after melting is quenched by smelting glass.Use unorganic glass as heat-storage medium, environmental corrosion is influenced
It is weak, and hygroscopic effect will not be generated in wet condition;Thermal storage performance is good, heating conduction is better than fused salt.
Further, described to grind unorganic glass, dry, the step of dry unorganic glass powder is made, wraps
It includes: quenched glass being mixed into after dehydrated alcohol carries out wet-milling with the ratio of grinding media to material of 2:1-4:1 and is dried, dry nothing is prepared
Machine glass powder.
Further, the main chemical compositions of unorganic glass include: (1) SiO2: as the skeleton structure of glass, add ratio
For example between 30%-80%, raw material is quartz sand, sandstone, quartzite and quartz;(2)Al2O3: it is steady to improve chemical stability, heat
Qualitative, mechanical strength and hardness, for adding proportion between 0%-30%, raw material is feldspar, clay, aluminium oxide, aluminium hydroxide, wax
Stone;(3)Na2O: cosolvent, for adding proportion between 0%-20%, raw material is sodium carbonate, sodium hydroxide, sodium nitrate, saltcake;
(4)B2O3: reduce thermal expansion coefficient, improve chemical stability, thermal stability, mechanical strength, adding proportion 0%-15% it
Between, raw material be boric acid, borax and contain boron mineral;(5)Li2O: cosolvent reduces softening temperature, and adding proportion is in 0.1%-1%
Between, primary raw material is lithium carbonate and matter containing lithium minerals, and (6) CaO: improving chemical stability and mechanical strength, adds ratio
For example between 0%-13%, primary raw material is calcite, lime stone, winnofil;(7) MgO: increase high temperature viscosity, improve
Chemical stability and mechanical strength, for adding proportion in 0-13.5%, primary raw material is dolomite and magnesite;(8) it ZnO: improves
Chemical stability and thermal stability, for adding proportion between 0%-6%, primary raw material has Zinc Oxide and Ling Xinkuang;(9)ZrO2:
Thermal stability, fire resistance, mechanical property and chemical stability are improved, reduces the coefficient of expansion, adding proportion is in 30%-80%
Between, primary raw material has: baddeleyite and zircon.
Further, basis material include: ceramic powders, it is metal powder, porous ceramic film material, porous metal material, more
Hole carbon material.
Further, the powder compacting sintering method include: by dry unorganic glass powder and basis material powder with
Certain proportion mixing, mold are suppressed and are sintered under conditions of being higher than unorganic glass softening temperature, and heat accumulating is made.
Further, the method for impregnation preparation method includes: that dry unorganic glass powder is pressed into block, is placed in
Porous matrix material surface is infiltrated using the temperature higher than 50 DEG C -70 DEG C of unorganic glass softening temperature, and the infiltration time is that 2-8 is small
When, heat accumulating is made.
Further, the use temperature range of unorganic glass heat-storage medium is at 550 DEG C -1200 DEG C, according to the adjustment of formula
It can be applied under different use environments;
Beneficial effects of the present invention:
The present invention uses a kind of phase-change heat-storage material preparation method using unorganic glass as heat-storage medium, using glass powder
The method being sintered in conjunction with basis material prepares unorganic glass phase-change heat-storage material, can provide in molten condition and be higher than fused salt three
Times or so thermal storage performance and the problem of there is no leakages, the failure of burn into humidity environment, in conjunction with basis material after can be
There is certain mechanical property under hot conditions.Preparation method of the present invention is simple, and cost is relatively low, is easily mass produced, to high temperature
Phase-change heat-storage material is of great significance.
Detailed description of the invention
Fig. 1 is the phase-change heat-storage material preparation method flow chart according to the present invention using unorganic glass as heat-storage medium;
Fig. 2 is to prepare unorganic glass phase-change heat-storage material schematic diagram using powder compacting sintering method;
Fig. 3 is to prepare unorganic glass phase-change heat-storage material schematic diagram using infiltration method.
Specific embodiment
Below in conjunction with specific attached drawing the present invention is described in detail specific embodiment.It should be noted that in following embodiments
The combination of the technical characteristic or technical characteristic of description is not construed as isolated, they can be combined with each other to reaching
To superior technique effect.In the drawings of the following embodiments, the identical label that each attached drawing occurs represent identical feature or
Person's component, can be apply to different embodiments.
As shown in Figure 1, the phase-change heat-storage material preparation method packet according to the present invention using unorganic glass as heat-storage medium
Include following steps:
In a step 102, according to using temperature to deploy glass formula, according to formula smelting glass, by the glass after melting
It is quenched;
At step 104, quenched glass is mixed into after dehydrated alcohol carries out wet-milling with certain ratio of grinding media to material and is dried, made
It is standby to obtain dry glass powder;
In step 106, using powder compacting sintering or high temperature infiltration method by obtained dry glass powder and matrix material
Material is prepared into phase-change heat-storage material.
Fig. 2 shows prepare unorganic glass phase-change heat-storage material schematic diagram using powder compacting sintering method.Utilize powder pressure
The phase-change heat-storage material preparation method of sintering process preparation processed is simple, even particle distribution;More existing material, phase-change material and ring
Border contact area is big, can achieve better heat transfer effect, and unorganic glass has many advantages, such as non-hygroscopic, and corrosivity is small, can
To supplement the short slab of existing fused salt heat accumulating.
Fig. 3, which is shown, prepares unorganic glass phase-change heat-storage material schematic diagram using infiltration method.The phase prepared using infiltration method
Change heat storage material prepares phase-change material and is evenly distributed, and more existing material, phase-change material and environment contact area are big, and skeleton
Material is more powder sintered, and the preparation method is more solid, can achieve better heat transfer effect, and unorganic glass has non-hygroscopic, corrosion
The advantages that property is small, can supplement the short slab of existing fused salt heat accumulating.
Example 1:
1. glass formula of the fusion temperature at 650 DEG C is mixed according to using temperature to deploy glass formula, it is molten according to formula
Glass is refined, the glass after melting is quenched.
2. quenched glass is put into planetary ball mill, with the ratio of grinding media to material of 3:1, it is wet to be mixed into dehydrated alcohol progress
Mill, the speed of rotation are 80 turns/min, and runing time is 48 hours.
It is dried 12 hours 3. the powder after ball milling is put under 80 DEG C of environment, prepares dry glass powder, partial size exists
Between 4-6 microns.
4. basis material accounting 45%, example uses MgO powder for basis material, sample mass 50g, so weighing
The MgO powder of 22.5g and the glass powder of 27.5g are put into mortar and are fully ground, and prepare uniformly mixed powder.
5. uniformly mixed powder is put into the mold that diameter is 50mm, is suppressed, prepared with the pressure of 30Mpa
Unsintered sample.
6. being sintered using Muffle furnace to sample, sintering process is to be warming up within room temperature 60 minutes 100 DEG C then 90 minutes
120 minutes are kept the temperature to 410 DEG C, furnace cooling after 650 DEG C of heat preservations 120 minutes was then warming up at 120 minutes.
Example 2:
1. glass formula of the fusion temperature at 650 DEG C is mixed according to using temperature to deploy glass formula, it is molten according to formula
Glass is refined, the glass after melting is quenched.
2. quenched glass is put into planetary ball mill, with the ratio of grinding media to material of 3:1, it is wet to be mixed into dehydrated alcohol progress
Mill, the speed of rotation are 80 turns/min, and runing time is 48 hours.
It is dried 12 hours 3. the powder after ball milling is put under 80 DEG C of environment, prepares dry glass powder, partial size exists
Between 4-6 microns.
4. basis material accounting 45%, example uses Al2O3Powder is basis material, sample mass 50g, so weighing
22.5g Al2O3The glass powder of powder and 27.5g, which are put into mortar, to be fully ground, and uniformly mixed powder is prepared
5. uniformly mixed powder is put into the mold that diameter is 50mm, is suppressed, prepared with the pressure of 30Mpa
Unsintered sample
6. being sintered using Muffle furnace to sample, sintering process is to be warming up within room temperature 60 minutes 100 DEG C then 90 minutes
120 minutes are kept the temperature to 410 DEG C, furnace cooling after 650 DEG C of heat preservations 120 minutes was then warming up at 120 minutes.
Example 3:
1. glass formula of the fusion temperature at 650 DEG C is mixed according to using temperature to deploy glass formula, it is molten according to formula
Glass is refined, the glass after melting is quenched.
2. quenched glass is put into planetary ball mill, with the ratio of grinding media to material of 3:1, it is wet to be mixed into dehydrated alcohol progress
Mill, the speed of rotation are 80 turns/min, and runing time is 48 hours.
It is dried 12 hours 3. the powder after ball milling is put under 80 DEG C of environment, prepares dry glass powder, partial size exists
Between 4-6 microns.
4. basis material uses MgO foamed ceramics, the porosity of foamed ceramics is 80%~90%, bulk density 0.5
~0.7g/cm3, aperture 10-60PPI, with a thickness of 13mm, diameter 50mm, quality 18g, matrix accounting is 45%, so
Weigh the glass powder of 22g.
5. it is to be pressed into the cylinder that diameter is 50mm to be placed in above foamed ceramics that glass powder, which is placed on diameter,.
6. being infiltrated using Muffle furnace to sample, Infiltration Technics are to be warming up within room temperature 60 minutes 100 DEG C then 90 minutes
120 minutes are kept the temperature to 410 DEG C, 680 DEG C of heat preservation furnace coolings after sixty minutes were then warming up at 120 minutes.
Example 4:
1. glass formula of the fusion temperature at 650 DEG C is mixed according to using temperature to deploy glass formula, it is molten according to formula
Glass is refined, the glass after melting is quenched.
2. quenched glass is put into planetary ball mill, with the ratio of grinding media to material of 3:1, it is wet to be mixed into dehydrated alcohol progress
Mill, the speed of rotation are 80 turns/min, and runing time is 48 hours.
It is dried 12 hours 3. the powder after ball milling is put under 80 DEG C of environment, prepares dry glass powder, partial size exists
Between 4-6 microns.
4. basis material uses Al2O3The porosity of foamed ceramics, foamed ceramics is 80%~90%, and bulk density is
0.36~0.5g/cm3, aperture 10,20,30,60PPI, with a thickness of 13mm, diameter 50mm, quality 18g, matrix accounting
It is 45%, so weighing the glass powder of 22g.
5. it is to be pressed into the cylinder that diameter is 50mm to be placed in above foamed ceramics that glass powder, which is placed on diameter,.
6. being infiltrated using Muffle furnace to sample, Infiltration Technics are to be warming up within room temperature 60 minutes 100 DEG C then 90 minutes
120 minutes are kept the temperature to 410 DEG C, 680 DEG C of heat preservation furnace coolings after sixty minutes were then warming up at 120 minutes.
Example 5:
1. glass formula of the fusion temperature at 650 DEG C is mixed according to using temperature to deploy glass formula, it is molten according to formula
Glass is refined, the glass after melting is quenched.
2. quenched glass is put into planetary ball mill, with the ratio of grinding media to material of 3:1, it is wet to be mixed into dehydrated alcohol progress
Mill, the speed of rotation are 80 turns/min, and runing time is 48 hours.
It is dried 12 hours 3. the powder after ball milling is put under 80 DEG C of environment, prepares dry glass powder, partial size exists
Between 4-6 microns.
4. basis material uses foam copper, the porosity of foam copper is 95%~98%, and bulk density is 0.1~0.8g/
cm3, aperture 5-130PPI, with a thickness of 10mm, diameter 50mm, quality 20g, matrix accounting is 45%, so weighing 24g
Glass powder.
5. it is to be pressed into the cylinder that diameter is 50mm to be placed in above foamed ceramics that glass powder, which is placed on diameter,.
6. being infiltrated using Muffle furnace to sample, Infiltration Technics are to be warming up within room temperature 60 minutes 100 DEG C then 90 minutes
120 minutes are kept the temperature to 410 DEG C, 680 DEG C of heat preservation furnace coolings after sixty minutes were then warming up at 120 minutes.
Although the embodiment of the present invention is had been presented for herein, it will be appreciated by those of skill in the art that not taking off
In the case where from spirit of that invention, the embodiments herein can be changed.Above-described embodiment is only exemplary, should not be with
Restriction of the embodiments herein as interest field of the present invention.
Claims (8)
1. a kind of phase-change heat-storage material preparation method using unorganic glass as heat-storage medium, which is characterized in that including following step
It is rapid:
(1) unorganic glass is prepared;
(2) unorganic glass ground, dried, dry unorganic glass powder is made;
(3) it using powder compacting sintering or high temperature infiltration method prepared by the unorganic glass powder of obtained drying and basis material
At phase-change heat-storage material.
2. according to the method described in claim 1, it is characterized by: described the step of preparing unorganic glass includes: according to using
Temperature deploys glass formula, and according to formula smelting glass, the glass after melting is quenched.
3. according to the method described in claim 2, drying is made it is characterized by: described ground unorganic glass, dried
Unorganic glass powder the step of include: by quenched glass with the ratio of grinding media to material of 2:1-4:1 be mixed into dehydrated alcohol carry out wet-milling
After dry, dry unorganic glass powder is prepared.
4. according to the method described in claim 1, it is characterized by: the main chemical compositions of unorganic glass include: SiO2: ratio
Between 30%-80%;Al2O3: ratio is between 0%-30%;Na2O: ratio is between 0%-20%;B2O3: ratio 0%-15% it
Between;Li2O: ratio is between 0.1%-1%;CaO: ratio is between 0%-13%;MgO: ratio is in 0-13.5%;ZnO: ratio exists
Between 0%-6%;ZrO2: ratio is between 30%-80%.
5. according to the method described in claim 1, it is characterized by: described matrix material include: ceramic powders, metal powder,
Porous ceramic film material, porous metal material, porous carbon materials.
6. according to the method described in claim 5, it is characterized by: the powder compacting sintering method are as follows: by dry inorganic glass
Glass powder is mixed in a certain proportion with basis material powder, and mold is suppressed and under conditions of being higher than unorganic glass softening temperature
It is sintered, heat accumulating is made.
7. according to the method described in claim 5, it is characterized by: the method for impregnation is the preparation method comprises the following steps: by dry inorganic glass
Glass powder is pressed into block, is placed in porous matrix material surface, using the temperature for being higher than 50 DEG C -70 DEG C of unorganic glass softening temperature
Degree infiltration, infiltration time are 2-8 hours, and heat accumulating is made.
8. according to the method described in claim 1, it is characterized by: the use temperature range of unorganic glass heat-storage medium is 550
It DEG C -1200 DEG C, can be applied under different use environments according to the adjustment of formula.
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CN110408368A (en) * | 2019-07-24 | 2019-11-05 | 长安大学 | A kind of storage salt material preparation method |
CN113675285A (en) * | 2021-06-29 | 2021-11-19 | 国网天津市电力公司电力科学研究院 | Double-glass double-sided PV/T assembly |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110408368A (en) * | 2019-07-24 | 2019-11-05 | 长安大学 | A kind of storage salt material preparation method |
CN110358506A (en) * | 2019-08-26 | 2019-10-22 | 中国科学院过程工程研究所 | A method of heat accumulating is prepared using incineration of refuse flyash |
CN113675285A (en) * | 2021-06-29 | 2021-11-19 | 国网天津市电力公司电力科学研究院 | Double-glass double-sided PV/T assembly |
CN113675285B (en) * | 2021-06-29 | 2023-09-29 | 国网天津市电力公司电力科学研究院 | Double-sided PV/T subassembly of dual glass |
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Application publication date: 20181218 |