CN104194732A - Preparation method of diatomite and paraffin composite phase change material - Google Patents
Preparation method of diatomite and paraffin composite phase change material Download PDFInfo
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- CN104194732A CN104194732A CN201410417511.3A CN201410417511A CN104194732A CN 104194732 A CN104194732 A CN 104194732A CN 201410417511 A CN201410417511 A CN 201410417511A CN 104194732 A CN104194732 A CN 104194732A
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Abstract
The invention relates to a preparation method of a diatomite and paraffin composite phase change material. The preparation method comprises the following steps: dissolving a phase change material paraffin in petroleum ether in a water domain at a certain temperature and stirring; then, adding a carrier diatomite with nanoscale porous structures, and continuously stirring, so that the porous structures of diatomite can be fully contacted with the phase change material to adsorb sufficient paraffin; and then, raising the temperature of the water domain to 75 DEG C, evaporating the solvent petroleum ether, then condensing and recovering the solvent petroleum ether and drying to obtain a powder composite energy storage material. The composite phase change material provided by the invention is not changed in shape in the phase change process, and paraffin is not leaked. Moreover, the composite phase change material is simple in preparation process, low in cost and energy-saving and environmentally friendly, and the solvent can be recycled.
Description
Technical field
The present invention relates to a kind of preparation method of phase change material, particularly a kind of preparation method of take the composite phase-change material that paraffin and diatomite is raw material, is the composite phase-change material that belongs to building energy saving field application.
Background technology
Utilize the latent heat of phase change material to carry out storage or the release of heat energy, be applicable to the application of utilization, waste heat recovery, intelligent automatic air-conditioning and construction, glasshouse, phase-transition heat-storage type air-conditioning, insulation macromolecular material and the special dimension of sun power, and range of application expands gradually.Building energy conservation particularly, traditional solid-liquid phase change material is in application, in order to prevent that phase change material from occurring to reveal to need container encloses before and after phase transformation, thereby increased thermal resistance, reduced heat transfer efficiency, heat transfer is the thermal resistance between phase change material and external heat transfer medium, reduced heat transfer efficiency, and cost has obviously raise.
Publication number is that CN101434832A discloses a kind of " mineral wax composite shape-setting phase-change material and preparation method thereof ", this invention be take paraffin as heat accumulating, multicomponent alcoholics compound and aromatic aldehyde compounds generation condensation reaction produce spacial framework that small molecules gelator forms and high density polyethylene(HDPE) jointly as the phase change material of the prepared setting of propping material material, this material phase transformation is functional, its weak point is to have 1% to 4% leakage, but describedly in the method utilize multicomponent alcoholics compound and aromatic aldehyde compounds generation condensation reaction to produce the leakage that spacial framework that small molecules gelator forms and high density polyethylene(HDPE) acting in conjunction prevent heat accumulating paraffin, and its polycondensation generation spacial framework is not very even, so the reactive force producing is little, and then just have a certain amount of leakage, and having spacial framework multicomponent alcoholics compound and aromatic aldehyde compounds generation condensation reaction produces acetal product and just can very easily decompose under weakly acidic condition, thereby have influence on spacial framework, and then can produce larger leakage.
Publication number is that CN1462787A Tsing-Hua University discloses a kind of " heating fixed phase change heat-storing material that building and heating is used and preparation method thereof ", adopt olefines organism and paraffin, utilize the composite phase-change material of mill, screw extrusion press and vulcanizing press preparation setting, and at the coated layer of polyethylene composite membrane in composite phase-change material surface, the Main Function of film prevents the leakage of phase change material.But this preparation technology has been applied to mill, screw extrusion press and vulcanizing press, these main equipments are many, make to increase substantially at production cost, and these equipment can be used a large amount of energy and water resources, and the coated layer of polyethylene composite membrane in phase change material surface very easily thermal ageing can have influence on work-ing life of material, the form of the fixed phase change heat-storing material of producing is fixed and then has been limited to Application Areas simultaneously.
Osmanli Sedat Karaman has shown to utilize diatomite to remove to adsorb the composite phase-change material that polyoxyethylene glycol (PEG) is prepared a kind of form stable in " Polyethylene glycol (PEG)/diatomite composite as a novel form-stable phase change material for thermal energy storage " article, the phase transition temperature interval of prepared composite phase-change material is between 27.2-32.2 ℃, and enthalpy of phase change is 87.3kJ/kg.What utilize hereinbefore is that vacuum impregnation technology is prepared diatomite adsorption liquid PEG composite phase-change material, this method is confined to diatomite adsorption liquid phase-change material, thereby due to the vacuum tightness of vacuum impregnation technology be certain to fluent material reactive force, be also uniformly to make liquid phase-change material can be adsorbed in uniformly diatomite surface, if absorption phase transformation material, because it becomes bulk or particulate state, and diatomaceous pore space structure is nano level, can not be adsorbed in diatomaceous pore space structure, so this method can not be unserviceable at diatomite adsorption phase transformation material, and prepared composite phase-change material can only be applied to build temperature adjustment, mainly because narrow phase transition temperature interval causes.
Summary of the invention
The concrete technical problems that the present invention will solve is that the problem of revealing occurs phase transition process, and preparation technology is loaded down with trivial details, the problem that production cost is high, and object is to provide the preparation method of a kind of diatomite and paraffin composite phase change material.
To achieve these goals, the present invention takes following technical scheme.
A preparation method for diatomite and paraffin composite phase change material, described in it, method follows these steps to carry out:
(1) by the phase change material paraffin of 30-50wt%, in temperature is the waters of 55 ℃, stir 1 hour, paraffin is fully dissolved in enough sherwood oils;
(2) in step (1), add the carrier 50-70wt% diatomite with nano level hole structure, fully stir, make the paraffin that diatomite pore space structure can be enough with the abundant Contact-sorption of phase change material paraffin;
(3) after the abundant Adsorption Paraffin of diatomite, rising waters temperature is 75 ℃, evaporating solvent sherwood oil, and solvent sherwood oil is reclaimed in rear condensation,, and be dried, obtain powder composite energy-storage material.
Further, supplementary technology scheme is as follows.
Described paraffin is that n-dodecane mixes arbitrarily to positive octacosane.
The boiling range of described sherwood oil is 60-90 ℃.
The evaporative condenser recovered temperature of described sherwood oil is 75 ℃.
Realize a kind of diatomite that the present invention is above-mentioned provided and the preparation method of paraffin composite phase change material, compared with prior art, its advantage and positively effect are as follows.
Present method adopts nano level hole structure diatomite to adsorb phase change material paraffin, because diatomite has uniform nano level hole structure, this special structure can produce surface tension and capillary force, paraffin can be adsorbed in pore space structure within the scope of certain proportion.
The porous material diatomite phase change material paraffin that present method adopts all has chemical 'inertia', can not react and reduce its chemical stability, thereby can not affect its transformation temperature and enthalpy of phase change yet, and with respect to other solid support materials and phase change material contrast, there is good stability in application, can not decompose, not perishable and aging, can repeated multiple timesly apply.
Present method adopts diatomite surface to form certain capillary force and surface tension with phase change material paraffin, impels a certain amount of paraffin of absorption that diatomite can be stable, on its surface, any leakage does not occur.
Present method is compared with existing phase change material preparation method, as container encloses, microcapsulary.This preparation method is easy, avoids utilizing large-scale instrument and equipment, and low production cost only need to be used mechanical stirring device, electric heater unit and a condensate recycling device.
It is because he has very wide phase transition temperature interval and high enthalpy of phase change as phase change material that present method is selected paraffin, it is the mixture to positive octacosane by n-dodecane, phase transition temperature interval is between 0-60 ℃, enthalpy of phase change is all higher than 100kJ/kg, and has good chemical stability, acidproof, alkaline-resisting, also can under rugged environment, use, and have good thermostability, heat decomposition temperature is more than 240 ℃.
Present method, owing to adopting sherwood oil to make solvent, can be dissolved paraffin well, has further reduced production cost, not destroyed by visible its chemical structure of infrared spectrogram, and energy cycling and reutilization, has realized the object of low energy expenditure and recycle.
Present method does not need directly to use by container encloses, and preparation technology is simple, with low cost, energy-conserving and environment-protective, solvent can cycling and reutilization.
Accompanying drawing explanation
Fig. 1 is the SEM figure of diatomite of the present invention and diatomite adsorption paraffin.
In figure: visible diatomite nano level pore space structure.
Fig. 2 is the SEM figure of diatomite adsorption paraffin of the present invention.
In figure: visible diatomite nano level pore space structure be can't see, with and adsorbed equably a large amount of paraffin.
Fig. 3 is the DSC test pattern of compound 42% paraffin wax of diatomite of the present invention.
Fig. 4 is the morphological stability figure of compound 42% paraffin wax of diatomite of the present invention.
In figure: at the variation diagram higher than its its form of phase transition temperature interval (80 ℃), form is not any change, without any leakage.
Fig. 5 is the DSC test pattern of compound 38% Octadecane of diatomite of the present invention.
Fig. 6 is the morphological stability figure of compound 38% Octadecane of diatomite of the present invention.
In figure: at the variation diagram higher than its its form of phase transition temperature interval (80 ℃), form is not any change, without any leakage.
Fig. 7 is the DSC test pattern of compound 35% n-dodecane of diatomite of the present invention.
Fig. 8 is the morphological stability figure of compound 35% n-dodecane of diatomite of the present invention.
In figure: at the variation diagram higher than its its form of phase transition temperature interval (80 ℃), form is not any change, without any leakage.
Fig. 9 be before the sherwood oil massfraction table recycled of the present invention and preparation with the infrared spectra comparison diagram of the sherwood oil of collecting.
In figure: contrast infrared spectrogram can find out that it does not have the generation of new functional group and the functional group of sherwood oil all, illustrates that the present invention does not destroy the chemical structure of sherwood oil in preparation process, can repeat to recycle.
Figure 10 is different types of Thermal Performance of Paraffin Wax that can relate in the present invention.
In figure: know paraffin by n-dodecane to positive octacosane arbitrarily than mixing, and its phase transition temperature interval is within the scope of 0-60 ℃, its enthalpy of phase change has very high enthalpy of phase change between 140-260kJ/kg.
Figure 11 is the TG I figure of partial phase change material paraffin involved in the present invention.
Figure 12 is the TG II figure of partial phase change material paraffin involved in the present invention.
Figure 13 is the particle diameter table with test results of composite phase-change material involved in the present invention.
In figure: adopt Bettersize2000 Intelligent Laser particle size analyzer, adopt the particle size distribution test of rewet test method to matrix material, test specification is between 0.02-2000 μ m, this figure mainly illustrates that the prepared composite phase-change material powder diameter of the present invention can reach micron order, afterwards can be with other material of construction well in conjunction with application.
Embodiment
In order to understand better the present invention, below in conjunction with embodiment, further illustrate the specific embodiment of the present invention, but embodiment of the present invention is not only confined to the following examples.
Implement the preparation method of a kind of diatomite and paraffin composite phase change material, present method is 42% in maximum that paraffin wax adsorbs, after higher than transformation temperature, it has stable thermal characteristics without any leakage, can repeatedly use, and its enthalpy of phase change can reach 108kJ/kg; Maximum that Octadecane adsorbs is 38%, and after higher than transformation temperature, it has stable thermal characteristics without any leakage, and repeatedly use properties is still stable, and its enthalpy of phase change can reach 126kJ/kg; Maximum that n-dodecane adsorbs is 35%, after higher than transformation temperature, it has stable thermal characteristics without any leakage, and repeatedly use properties is still stable, and its enthalpy of phase change can reach 113kJ/kg, compared with prior art, obtained unforeseeable effect.
Embodiment 1
Implement the preparation method of a kind of diatomite and paraffinic base composite phase-change material, this preparation method's step is as follows.
(1) in temperature is the waters of 50 ℃, by the phase change material paraffin (section) of 42wt%, be dissolved in sherwood oil, utilize magnetic stirrer to stir 1 hour, make its be fully dissolved in sherwood oil (sherwood oil institute consumption be paraffin and diatomite volume and 2 times).
(2) in above-mentioned steps (1), add solid support material 58wt% diatomite (Jilin Province, natural mineral, large at China's wide reserves that distribute, and cheap easy acquisition), continue fully to stir, diatomite pore space structure can fully be contacted with phase change material paraffin, its surface tension and physical force can all be brought into play the enough paraffin of absorption.
(3) after the abundant Adsorption Paraffin of diatomite, improving waters temperature to 75 ℃ can evaporate as the sherwood oil of solvent completely for making, and adding circulated water condensing works condensation recovered solvent sherwood oil (more than the sherwood oil of being recycled in this preparation process can reach 60wt%, and its can recycling to reduce production costs and to reach the preparation process of no waste discharge).
(4) products therefrom is put into loft drier and it is fully dried (by above-mentioned actually operating, just can acquire the uniform and stable product of form, and above-mentioned steps only need to be used a magnetic stirring apparatus and an electric heating waters pot, so preparation process requires the low wide popularization and application of being convenient to).
Diatomite cavity structure is filled completely after testing, detection knows that (seeing accompanying drawing 3) its phase transition temperature interval is 42-57 ℃, enthalpy of phase change can reach 108kJ/kg, mean particle size can reach 20um with interior (seeing accompanying drawing table 13), 1000 times repeatedly heating/cooling after, composite phase-change material is without any leakage (accompanying drawing 4: can find out that cylinder shape material is in the drawings heated to 80 ℃ of (far above its transformation temperature) its forms any variation does not occur, and leak without any material around).
Embodiment 2
Implement the preparation method of a kind of diatomite and paraffinic base composite phase-change material, this preparation method's step is as follows.
(1) at room temperature, by the phase change material paraffin of 38wt% (this is Octadecane), be dissolved in sherwood oil, utilize magnetic stirrer to stir 1 hour, make its be fully dissolved in sherwood oil (sherwood oil institute consumption be paraffin and diatomite volume and 2 times).
(2) in above-mentioned steps (1), add solid support material 62wt% diatomite (as in Example 1), continue fully to stir, diatomite pore space structure can fully be contacted with phase change material paraffin, its surface tension and physical force can all be brought into play the enough paraffin of absorption.
(3), after the abundant Adsorption Paraffin of diatomite, improve waters temperature to 75 ℃ and can evaporate completely as the sherwood oil of solvent for making, and adding circulated water condensing works condensation recovered solvent sherwood oil.
(4) products therefrom is put into loft drier it is fully dried.
By above-mentioned actually operating, just can acquire the uniform and stable product of form, and above-mentioned steps only need to use a magnetic stirring apparatus and an electric heating waters pot, so preparation process requires the low wide popularization and application of being convenient to.
Diatomite cavity structure is filled completely after testing, (accompanying drawing 5) its phase transition temperature interval 27-32 ℃ is known in detection, enthalpy of phase change can reach 126kJ/kg, mean particle size can reach 20um with interior (accompanying drawing table 13), 1000 times repeatedly heating/cooling after, composite phase-change material is without any leakage (accompanying drawing 6: can find out that cylinder shape material is in the drawings heated to 80 ℃ of (far above its transformation temperature) its forms any variation does not occur, and leak without any material around).
Embodiment 3
Implement the preparation method of a kind of diatomite and paraffinic base composite phase-change material, this preparation method's step is as follows.
(1) at room temperature, by the phase change material paraffin of 35wt% (this is n-dodecane), be dissolved in sherwood oil, utilize magnetic stirrer to stir 1 hour, make its be fully dissolved in sherwood oil (sherwood oil institute consumption be paraffin and diatomite volume and 2 times).
(2) in above-mentioned steps (1), add solid support material 65wt% diatomite (as in Example 1), continue fully to stir, diatomite pore space structure can fully be contacted with phase change material paraffin, its surface tension and physical force can all be brought into play the enough paraffin of absorption.
(3), after the abundant Adsorption Paraffin of diatomite, improve waters temperature to 75 ℃ and can evaporate completely as the sherwood oil of solvent for making, and adding circulated water condensing works condensation recovered solvent sherwood oil.
(4) products therefrom is put into loft drier it is fully dried.(by above-mentioned actually operating, just can acquire the uniform and stable product of form, and above-mentioned steps only need to use a magnetic stirring apparatus and an electric heating waters pot, so preparation process requiring the low wide popularization and application of being convenient to).
Diatomite cavity structure is filled completely after testing, (accompanying drawing 7) its phase transition temperature interval 12-19 ℃ is known in detection, and enthalpy of phase change can reach 113kJ/kg, and mean particle size can reach 20um, (accompanying drawing table 13, D10: corresponding particle diameter when size-grade distribution number reaches 10%; D50: corresponding particle diameter when size-grade distribution number reaches 50%; D90: corresponding particle diameter when size-grade distribution number reaches 90%) 1000 times repeatedly heating/cooling after, composite phase-change material is without any leakage (accompanying drawing 8: can find out that cylinder shape material is in the drawings heated to 80 ℃ of (far above its transformation temperature) its forms any variation does not occur, and leak without any material around).
Claims (4)
1. a preparation method for diatomite and paraffin composite phase change material, described in it, method follows these steps to carry out:
(1) by the phase change material paraffin of 30-50wt%, in temperature is the waters of 55 ℃, stir 1 hour, paraffin is fully dissolved in enough sherwood oils;
(2) in step (1), add the carrier 50-70wt% diatomite with nano level hole structure, fully stir, make the paraffin that diatomite pore space structure can be enough with the abundant Contact-sorption of phase change material paraffin;
(3) after the abundant Adsorption Paraffin of diatomite, rising waters temperature is 75 ℃, evaporating solvent sherwood oil, and solvent sherwood oil is reclaimed in rear condensation, and is dried, and obtains powder composite energy-storage material.
2. the method for claim 1, described paraffin is any mixing that n-dodecane arrives positive octacosane.
3. the method for claim 1, described sherwood oil boiling range is 60-90 ℃.
4. the method as described in claim 1 or 3, the evaporative condenser recovered temperature of described sherwood oil is 75 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107867809A (en) * | 2017-11-29 | 2018-04-03 | 安徽元通采暖科技有限公司 | A kind of processing method of heating equipment insulation Heat Conduction Material |
| CN111233367A (en) * | 2020-01-20 | 2020-06-05 | 东南大学 | Preparation method of liquid paraffin/diatomite capsule phase change material and obtained material |
| CN111718691A (en) * | 2020-07-01 | 2020-09-29 | 南方科技大学 | Diatom-based phase change energy storage material and preparation method and application thereof |
| CN113249096A (en) * | 2021-05-17 | 2021-08-13 | 河北科技大学 | Porous medium composite phase change material and preparation method and application thereof |
| CN115353866A (en) * | 2022-08-18 | 2022-11-18 | 中国地质大学（武汉） | Mineral-based heat storage microsphere and preparation method thereof |
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