CN108504330A - The preparation method of polyethylene glycol/titanium dioxide composite phase-change energy storage material - Google Patents
The preparation method of polyethylene glycol/titanium dioxide composite phase-change energy storage material Download PDFInfo
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- CN108504330A CN108504330A CN201810287417.9A CN201810287417A CN108504330A CN 108504330 A CN108504330 A CN 108504330A CN 201810287417 A CN201810287417 A CN 201810287417A CN 108504330 A CN108504330 A CN 108504330A
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- C—CHEMISTRY; METALLURGY
- 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
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention discloses the preparation methods of polyethylene glycol/titanium dioxide composite phase-change energy storage material, including：At room temperature so that polyethylene glycol dissolves in the mixed liquor of deionized water and organic solvent, then titanium source is added into the mixed solution and is obtained by the reaction.The method of the present invention is simple for process, it is whole to carry out at room temperature, polyethylene glycol produced by the present invention/titanium dioxide composite phase-change energy storage material enthalpy of phase change is high, with good packaging effect and the capacity of heat transmission, Product transport is simple, effectively solves the problems, such as the liquid phase leakage that material occurs in use.
Description
Technical field
The invention belongs to phase-change accumulation energy fields, and in particular to the system of polyethylene glycol/titanium dioxide composite phase-change energy storage material
Preparation Method.
Background technology
From the 1970s, energy problem and environmental problem gradually cause the extensive concern of people, thus people open
How energy saving beginning research is and improves energy utilization rate.Currently, the use of phase-changing energy storage material is to improve energy utilization rate
Effective way.Polyethylene glycol (PEG) is a kind of up-and-coming phase-changing energy storage material, it has suitable phase transition temperature and dives
Heat, the high advantage of memory capacity, and nontoxic have good biocompatibility, biological degradability, hydrophily, are easy to chemistry and change
The characteristics of property.But polyethylene glycol has liquid phase generation in phase transition process, has certain mobility.Therefore it is made generally at present poly-
Ethylene glycol shaping phase-change material is combined, in phase transformation using polyethylene glycol as heat accumulating with encapsulating material (i.e. carrier matrix)
The former solid shape of front and back maintenance, does not flow.With going deep into for research, it has been found that shaping phase-change material, which removes, has phase transformation object
Outside the heat storage function of matter, the specific physical chemical efficiency of encapsulating material is also worth deeply developing, to which exploitation is with difunctional
Composite phase-change energy storage material.Titanium dioxide is with nontoxic, chemical stabilization photoelectric conversion efficiency is high, photocatalytic activity is strong, sterilization
Performance waits well many special materialization effects, and purposes is very extensive, the phase-change accumulation energy prepared using titanium dioxide as carrier matrix
Material has huge potential using value in the energy and environment etc..
The master of entitled " preparation of polyethylene glycol composite phase-change material and the performance study " of Changchun Polytechnic Univ.'s health sea poplar
Academic dissertation (2012) discloses a kind of PEG/TiO2The preparation method of composite phase-change material, detailed process are：It weighs
3.0gPEG is dissolved in the ethyl alcohol of 20ml；The another Butyl Phthalate for weighing 8.5g, is dissolved in 10ml ethyl alcohol；Two kinds of solution are merged,
It is ultrasonically treated 3min, it is made uniformly to mix, 3h is persistently stirred to 2.0 with the salt acid for adjusting pH of 2mol/L in high-speed stirred, is added dropwise
Ammonium hydroxide stands 18h, and colloidal sol becomes pale yellow transparent gel, and vacuum drying for 24 hours, obtains faint yellow solid.The PEG/ being prepared
TiO2The enthalpy of phase change of composite phase-change material is respectively：47.92J/g, 59.65J/g, 70.07J/g, 72.39J/g, with individual phase
It answers the enthalpy of phase change of the PEG of molecular weight to compare, reduces 69.97J/g, 59.78J/g, 56.89J/g, 63.33J/g respectively.As it can be seen that
The PEG/TiO prepared by this method2It is many that composite phase-change material causes heat content to reduce.To find out its cause, mainly titanium source hydrolyzes too
Caused by fast extremely difficult control.
FOR ALL WE KNOW, butyl titanate easily hydrolyzes, or even opens the bottle of butyl titanate, can be observed in bottleneck
White cigarette, this is that it hydrolyzes generation with water vapor in air.Titanium source hydrolysis can cause very much precipitation to quickly form soon, to be unable to shape
At good colloidal sol, you can't get favorable sealing properties and the suitable PEG/TiO of heat content2Composite phase-change material.This is also exactly
PEG/TiO2Still unsolved difficulties in the preparation method of composite phase-change material.
Invention content
The purpose of the present invention is to provide a kind of preparation method of polyethylene glycol/titanium dioxide composite phase-change energy storage material,
The preparation method realizes controlled hydrolysis and the polycondensation of titanium source by the control to preparation parameter, has higher phase to obtain
Become polyethylene glycol/titanium dioxide composite phase-change energy storage material of enthalpy, there is good packaging effect and the capacity of heat transmission, effectively solve
The problem of liquid phase leakage that material occurs in use.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of preparation method of polyethylene glycol/titanium dioxide composite phase-change energy storage material, includes the following steps：
(1) after mixing deionized water, n,N-Dimethylformamide and isopropanol, the equal relative molecular weight of number is added thereto
For 6000 polyethylene glycol, uniform stirring 0.5~10 hour under the rotating speed of 350~1200r/min；
(2) butyl titanate is added thereto again, uniform stirring 0.5~10 is small under the rotating speed of 350~1200r/min
When, obtain clear solution；
(3) then, the clear solution is centrifuged, centrifugation gained supernatant is discarded, takes centrifugation gained heavy
Shallow lake is washed, and then in 40~80 DEG C of dryings, obtains polyethylene glycol/titanium dioxide composite phase-change energy storage material；
Wherein, the mass ratio of deionized water, n,N-Dimethylformamide, isopropanol, polyethylene glycol and butyl titanate is
(0.80~1.75)：(0.30~0.65)：(0.30~0.65)：(0.7~2.2)：1.
In some specific examples of the present invention, in step (1), rotating speed 750r/min.
In some specific examples of the present invention, in step (2), rotating speed 750r/min.
In some specific examples of the present invention, in step (3), drying time is 24~96 hours.
In the present invention, whole preparation process (in addition to drying) carries out at ambient temperature, and room temperature typically refers to 10~
40℃。
The present invention also provides the polyethylene glycol being prepared by the above method/titanium dioxide composite phase-change energy storage materials.
In the present invention, the polyethylene glycol that the equal relative molecular weight of the number of appropriate dosage is 6000 is added to deionized water, N,
In dinethylformamide and isopropanol solvent, there is the PEG of long zigzag chain structures to become the poly- of loop network structure
Object is closed, solution viscosity increases, since, there is intermolecular hydrogen bonding effect, so, water is at molten between water and solvent alcohol
Among the encirclement of agent molecule.After the butyl titanate of appropriate dosage is added thereto, reactant molecule needs to break through solvent molecule
Encirclement mutually collide, and the steric hindrance that isopropanol solvent and PEG are formed has delayed tetrabutyl titanate hydrolysis to be formed micro- significantly
The process of core, and slow down the diffusion velocity of reactant molecule；In another aspect, aprotic solvent n,N-Dimethylformamide
In the presence of stable effect being played to deionized water, to slow down the dissociation of deionized water and be reacted with butyl titanate.Cause
This, the fast hydrolyzing of butyl titanate is effectively avoided, on the other hand, since the site hydrolyzed is dispersed in loop network
In structure, so that its polycondensation controllable-rate, and then the titanium colloidal sol of three-dimensional net structure is formed in loop network structure, two
Person is uniformly dispersed in a network, and after dry, titanium colloidal sol becomes nano-titanium dioxide.Due to the hair between nano-titanium dioxide gap
Thin suction-operated, nano-titanium dioxide encapsulate PEG inside it；Due to the network confinement of network structure, PEG molecules or part
Sub-chain motion is restricted, and limits the macroscopic view flowing of PEG；Due to bonding action and the titanium hydroxyl (Ti- of titanium dioxide surface
OH) with polyethylene glycol terminal hydroxy group (CH2- OH) between hydrogen bond action, polyethylene glycol is firmly embedded into the netted of titanium dioxide
In porous structure.So when more than PEG melting temperatures, the entire strands of PEG can not free movement lead to material macroscopically
Still solid-state is presented, shows as solid-solid phase-change process, polyethylene glycol liquid will not leak out.
In the polyethylene glycol being prepared by the method for the present invention/titanium dioxide phase-changing energy storage material, polyethylene glycol is as storage
Energy material, is at normal temperatures crystalline state；Titanium dioxide is not undergone phase transition as inorganic matrix carrier in test scope.It is described
The enthalpy of phase change of polyethylene glycol/titanium dioxide phase-changing energy storage material can be higher than 120J/g, have good packaging effect, do not occur
Polyethylene glycol permeates.
Compared with prior art, the present invention has technique effect beneficial below：
(1) preparation method of the present invention is simple for process, and raw material is simple to operation, whole almost to carry out at room temperature, fits
Close industrial production.
(2) composite phase-change energy storage material obtained by the method for the present invention, while ensureing high energy-storage property, and to work
Medium polyethylene glycol carries out well packaged, shape of the energy storage material in macroscopically presentation solid while making polyethylene glycol undergo phase transition
State effectively prevents the leakage of polyethylene glycol, performance from stablizing.
Description of the drawings
Fig. 1 is that the EDX for polyethylene glycol/titanium dioxide composite phase-change energy storage material that the embodiment of the present invention 1 is prepared is bent
Line chart.
Fig. 2 is that the XRD for polyethylene glycol/titanium dioxide composite phase-change energy storage material that the embodiment of the present invention 1 is prepared is bent
Line chart.
Fig. 3 a and 3b are that polyethylene glycol/titanium dioxide composite phase-change energy storage material that the embodiment of the present invention 1 is prepared exists
Stereoscan photograph under different amplification.
Fig. 4 is the transmission electricity for polyethylene glycol/titanium dioxide composite phase-change energy storage material that the embodiment of the present invention 1 is prepared
Mirror photo.
Fig. 5 is that the DSC for polyethylene glycol/titanium dioxide composite phase-change energy storage material that the embodiment of the present invention 1 is prepared is bent
Line chart.
Fig. 6 is the DSC curve figure for polyethylene glycol/composite titania material that comparative example 1 is prepared.
Fig. 7 is the DSC curve figure for polyethylene glycol/composite titania material that comparative example 2 is prepared.
Specific implementation mode
In order to better illustrate the present invention, it is easy to understand technical scheme of the present invention, below in conjunction with the accompanying drawings and is embodied
Example, invention is further described in detail.It should be understood that following embodiments is merely to illustrate the present invention, do not represent or
The scope of the present invention is limited, protection scope of the present invention is subject to claims.
Reagents or instruments used without specified manufacturer in following embodiment is the routine that can be commercially available
Product.
Embodiment 1
8.64 grams of deionized waters, 3.02 grams of n,N-Dimethylformamide and 3.02 grams of isopropanols are weighed respectively, are sequentially added
In the round-bottomed flask of 250mL, mixed solution is formed；The poly- second two that the equal relative molecular mass of number for weighing 10.60 grams again is 6000
Alcohol is added directly into above-mentioned mixed solution, and uniform stirring 30min, obtains clear solution under the rotating speed of 750r/min；By 5.0g
Butyl titanate is added in above-mentioned clear solution, and uniform stirring 1 hour under the rotating speed of 750r/min is then centrifuged for detaching,
Centrifugation gained supernatant is discarded, takes centrifugation gained precipitation to be washed, washs 3 times respectively with absolute ethyl alcohol and deionized water, so
It is 24 hours dry at 40~80 DEG C afterwards, obtain final product.Process (in addition to drying) made above carries out at room temperature.
EDX tests are carried out to final product, EDX curves are as shown in Figure 1.By in Fig. 1 it is found that the element group of the final product
As C, O, Ti, wherein O:The atomic percent of Ti is 76.21:10.93, so that it is determined that there is TiO in final product2In the presence of.
XRD tests are carried out to final product, XRD curves are as shown in Figure 2.From Figure 2 it can be seen that the standard card of each peak value and PEG
Piece corresponds to, and illustrates in final product there are PEG and without chemically reacting.
SEM tests are carried out to final product, stereoscan photograph is as shown in Figure 3a and Figure 3b shows.TEM is carried out to final product
Test, transmission electron microscope photo are as shown in Figure 4.In terms of the stereoscan photograph of Fig. 3 a and Fig. 3 b, material is in bulk；From the saturating of Fig. 4
It penetrates electromicroscopic photograph and can see apparent lattice (polyethylene glycol) and exist, poly- second two can be seen that according to the distribution situation of lattice
Alcohol is wrapping in titanium dioxide granule, in conjunction with Fig. 3 a and Fig. 3 b, and then can be inferred that bulk material is accumulated by little particle
It is formed.Can see material surface substantially from Fig. 3 a and Fig. 3 b is in opposite continuous phase, can't see apparent pore structure, explanation
PEG is embedded in TiO substantially2In three-dimensional net structure, and it is existing not generate reunion in nanometer range for composite material granular size
As uniformity is good, illustrates that polyethylene glycol is distributed to well in titanium dioxide spatial network, and titanium dioxide plays matrix work
With.This discrete form provides good mechanical strength for entire compound.Therefore, can ensure in phase transition process compound
The problem of material keeps solid shape, the polyethylene glycol leakage that will not have melted.
Dsc analysis is carried out to final product according to the following steps：
Under high pure nitrogen atmosphere, 5~10mg of sample size, heating rate 10 DEG C/min, throughput 50mL/min, scanning temperature
Range is spent from -10 DEG C~110 DEG C.Using the Q-1000 differential scanning calorimeters (DSC) of TA companies of the U.S., test sample heating-
Phase transition temperature in temperature-fall period and enthalpy of phase change.First with 10 DEG C/min from -10 DEG C~110 DEG C, constant temperature 3min is kept, heat is eliminated and goes through
History；Then -10 DEG C (temperature-fall periods) are cooled to from 110 DEG C with 10 DEG C/min；110 DEG C are warming up to from -10 DEG C with 10 DEG C/min again
(temperature-rise period), the phase transition temperature and enthalpy of phase change of analysis test temperature-fall period and temperature-rise period.DSC curve as shown in figure 5, from
The phase transformation enthalpy that product can be calculated in DSC curve is 127.5J/g, and carrier matrix titanium dioxide is not sent out in test scope
Raw phase transformation.
Performance evaluation is packaged to final product according to the following steps：
Final product made from 5g is weighed, is laid in clean surface plate, a thin layer sample powder is formed, at 100 DEG C
Middle placement 1h, polyethylene glycol adherency has not been observed on surface in surface plate after taking-up, illustrates do not have polyethylene glycol to permeate,
Titanium dioxide plays the role of good setting to polyethylene glycol, and composite phase-change material has shape retentivity, reaches setting
Purpose to get to final product be PEG/TiO2Shaping phase-change material.
As a result, according to the above test result, it can be found that：The final product that embodiment 1 is prepared is polyethylene glycol/bis-
Titanium oxide composite material, phase transformation enthalpy are 127.5J/g, and nano-titanium dioxide plays the role of good setting to polyethylene glycol,
So that composite material has excellent encapsulation performance.
Comparative example 1
8.64 grams of deionized waters, 3.02 grams of n,N-Dimethylformamide and 3.02 grams of isopropanols are weighed respectively, are sequentially added
In the round-bottomed flask of 250mL, mixed solution is formed；The poly- second two that the equal relative molecular mass of number for weighing 10.60 grams again is 6000
Alcohol is added directly into above-mentioned mixed solution, and uniform stirring 30min, obtains clear solution under the rotating speed of 750r/min；By 25g titaniums
Sour four butyl esters are added in above-mentioned clear solution, and uniform stirring 1 hour under the rotating speed of 750r/min is then centrifuged for detaching, abandon
Centrifugation gained supernatant is removed, takes centrifugation gained precipitation to be washed, washs 3 times respectively with absolute ethyl alcohol and deionized water, then
It is 24 hours dry at 40~80 DEG C, obtain final product.Process (in addition to drying) made above carries out at room temperature.
EDX, XRD and DSC test are carried out according to the method for embodiment 1, DSC curve is as shown in Figure 6.Test result shows：
The final product that comparative example 1 is prepared is also polyethylene glycol/composite titania material, and phase transformation enthalpy is 50.0J/g.Claim
Polyethylene glycol made from 5g/titanium dioxide composite phase-change energy storage material powder is taken, is laid in clean surface plate, it is thin to form one
Layer sample powder, places 1h in 100 DEG C, has observed a small amount of polyethylene glycol adherency after taking-up in surface plate, has illustrated poly- second
Glycol is permeated.
It can be seen that using 5g titanium sources different from embodiment 1,25g titanium sources have been used in comparative example 1, it is obtained
The enthalpy of phase change of polyethylene glycol/composite titania material is significantly lower than 1 products therefrom of embodiment of similarity condition, moreover, comparison
The packaging effect of 1 gained composite material of example is also obviously not so good as 1 products therefrom of embodiment.
Comparative example 2
8.64 grams of deionized waters, 3.02 grams of n,N-Dimethylformamide and 3.02 grams of isopropanols are weighed respectively, are sequentially added
In the round-bottomed flask of 250mL, mixed solution is formed；5.0g butyl titanates are add to the above mixed solution, in 750r/
Uniform stirring 1 hour under the rotating speed of min；The polyethylene glycol that the equal relative molecular mass of number for weighing 10.60 grams again is 6000 is direct
It is added thereto, uniform stirring 30min under the rotating speed of 750r/min；Be then centrifuged for detaching, will centrifugation gained supernatant discard, take from
Precipitation obtained by the heart is washed, and is washed respectively 3 times with absolute ethyl alcohol and deionized water, then 24 hours dry at 40~80 DEG C,
Obtain final product.Process (in addition to drying) made above carries out at room temperature.
EDX, XRD and DSC test are carried out according to the method for embodiment 1, DSC curve is as shown in Figure 7.Test result shows：
The final product that comparative example 2 is prepared is also polyethylene glycol/composite titania material, and phase transformation enthalpy is 21.6J/g.
It can be seen that it is different from the step of polyethylene glycol is eventually adding titanium source is first added in embodiment 1, in comparative example 2 first
Titanium source is added and is eventually adding polyethylene glycol, the phase transformation enthalpy of obtained polyethylene glycol/composite titania material is very low, shows
Write 1 products therefrom of embodiment less than similarity condition.
Embodiment 2
8.64 grams of deionized waters, 3.02 grams of n,N-Dimethylformamide and 3.02 grams of isopropanols are weighed respectively, are sequentially added
In the round-bottomed flask of 250mL, mixed solution is formed；The poly- second two that the equal relative molecular mass of number for weighing 10.60 grams again is 6000
Alcohol is added directly into above-mentioned mixed solution, and uniform stirring 30min, obtains clear solution under the rotating speed of 750r/min；By 10g titaniums
Sour four butyl esters are added in above-mentioned clear solution, and uniform stirring 1 hour under the rotating speed of 750r/min is then centrifuged for detaching, abandon
Centrifugation gained supernatant is removed, takes centrifugation gained precipitation to be washed, washs 3 times respectively with absolute ethyl alcohol and deionized water, then
It is 24 hours dry at 40~80 DEG C, obtain final product.Process (in addition to drying) made above carries out at room temperature.
Test shows：The final product that embodiment 2 is prepared is also polyethylene glycol/composite titania material, phase transformation
Enthalpy is 110.0J/g, and does not have polyethylene glycol to permeate.
Embodiment 3
8.64 grams of deionized waters, 3.02 grams of n,N-Dimethylformamide and 3.02 grams of isopropanols are weighed respectively, are sequentially added
In the round-bottomed flask of 250mL, mixed solution is formed；The polyethylene glycol that the equal relative molecular mass of number for weighing 8.83 grams again is 6000
It is added directly into above-mentioned mixed solution, uniform stirring 30min, obtains clear solution under the rotating speed of 750r/min；By 10g metatitanic acids
Four butyl esters are added in above-mentioned clear solution, and uniform stirring 1 hour under the rotating speed of 750r/min is then centrifuged for detaching, discard
Centrifugation gained supernatant takes centrifugation gained precipitation to be washed, is washed 3 times with absolute ethyl alcohol and deionized water, then existed respectively
40~80 DEG C of dryings 96 hours, obtain final product.Process (in addition to drying) made above carries out at room temperature.
Test shows：The final product that embodiment 3 is prepared is also polyethylene glycol/composite titania material, phase transformation
Enthalpy is 102.8J/g, and does not have polyethylene glycol to permeate.
Embodiment 4
8.64 grams of deionized waters, 3.02 grams of n,N-Dimethylformamide and 3.02 grams of isopropanols are weighed respectively, are sequentially added
In the round-bottomed flask of 250mL, mixed solution is formed；The polyethylene glycol that the equal relative molecular mass of number for weighing 7.06 grams again is 6000
It is added directly into above-mentioned mixed solution, uniform stirring 30min, obtains clear solution under the rotating speed of 750r/min；By 10g metatitanic acids
Four butyl esters are added in above-mentioned clear solution, and uniform stirring 1 hour under the rotating speed of 750r/min is then centrifuged for detaching, discard
Centrifugation gained supernatant takes centrifugation gained precipitation to be washed, is washed 3 times with absolute ethyl alcohol and deionized water, then existed respectively
40~80 DEG C of dryings 48 hours, obtain final product.Process (in addition to drying) made above carries out at room temperature.
Test shows：The final product that embodiment 4 is prepared is also polyethylene glycol/composite titania material, phase transformation
Enthalpy is 93.0J/g, and does not have polyethylene glycol to permeate.
The performance data of above-described embodiment 1~4 and the composite material of comparative example 1 and 2 is summarized and compared, it is as follows
Shown in table 1.
Table 1：Polyethylene glycol/composite titania material performance data
As it can be seen from table 1 polyethylene glycol/titanium dioxide the composite phase change energy-storing prepared using method provided by the invention
Material (Examples 1 to 4), enthalpy of phase change are apparently higher than comparative example 1 and comparative example 2.The enthalpy of phase change of comparative example 2 is very low, can not
It is used as energy storage material.Meanwhile polyethylene glycol/titanium dioxide the composite phase change energy-storing prepared using method provided by the invention
Material (Examples 1 to 4) all shows transformation of the solid to solid during phase transition, and no liquid occurs, and encapsulation performance is bright
It is aobvious to be better than comparative example 1.
It should be noted that embodiment described above is only used for explaining the present invention, do not constitute to any of the present invention
Limitation, by referring to exemplary embodiments, invention has been described, it should be appreciated that word used in it is descriptive
With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation
Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to
And specific method, material and embodiment, it is not intended that the present invention is limited to particular case disclosed in it, on the contrary, this hair
It is bright to can be extended to other all methods and applications with the same function.
Claims (5)
1. the preparation method of polyethylene glycol/titanium dioxide composite phase-change energy storage material, includes the following steps：
(1) after mixing deionized water, n,N-Dimethylformamide and isopropanol, the equal relative molecular weight of number is added thereto is
6000 polyethylene glycol, uniform stirring 0.5~10 hour under the rotating speed of 350~1200r/min；
(2) butyl titanate is added thereto again, uniform stirring 0.5~10 hour, obtains under the rotating speed of 350~1200r/min
To clear solution；
(3) then, the clear solution is centrifuged, will centrifugation gained supernatant discard, take centrifugation gained precipitate into
Row washing, then in 40~80 DEG C of dryings, obtains polyethylene glycol/titanium dioxide composite phase-change energy storage material；
Wherein, the mass ratio of deionized water, n,N-Dimethylformamide, isopropanol, polyethylene glycol and butyl titanate is (0.80
~1.75)：(0.30~0.65)：(0.30~0.65)：(0.7~2.2)：1.
2. preparation method as described in claim 1, which is characterized in that in step (1), rotating speed 750r/min.
3. preparation method as described in claim 1, which is characterized in that in step (2), rotating speed 750r/min.
4. preparation method as described in claim 1, which is characterized in that in step (3), drying time is 24~96 hours.
5. the polyethylene glycol obtained by preparation method as described in any one of claims 1 to 4/titanium dioxide composite phase-change storage
It can material.
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| 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 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN109468122B (en) * | 2018-12-18 | 2020-07-24 | 北京化工大学 | Core-shell type mesoporous silica/organic phase change material composite nanocapsule and preparation method thereof |
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