CN105623622A - Preparation method of gypsum-based paraffin and diatomite phase change energy storage material - Google Patents
Preparation method of gypsum-based paraffin and diatomite phase change energy storage material Download PDFInfo
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- CN105623622A CN105623622A CN201610147635.3A CN201610147635A CN105623622A CN 105623622 A CN105623622 A CN 105623622A CN 201610147635 A CN201610147635 A CN 201610147635A CN 105623622 A CN105623622 A CN 105623622A
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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
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Abstract
The invention relates to a preparation method of a gypsum-based paraffin and diatomite phase change energy storage material, and belongs to the preparation method of phase change energy storage materials. The preparation method comprises the steps that 20 g of diatomite and 20 g of paraffin are weighed according to the following proportions that for a first material, the proportion of the diatomite to the paraffin is 0.6 to 0.4, for a second material, the proportion of the diatomite to the paraffin is 0.55 to 0.45, for a third material, the proportion of the diatomite to the paraffin is 0.5 to 0.5, and for a fourth material, the proportion of the diatomite to the paraffin is 0.45 to 0.55; the diatomite and the paraffin are mixed and ground for 2 h, and at last the mixture is in a powder state; the mixture ground for 2 h is poured into a mold, and drying is conducted in a hot wind circulating oven at 80 DEG C for 4 h; the dried material is taken out of the mold, grinding is conducted for 2 h, the paraffin and the diatomite are fully fused, and the prepared composite phase change material is uniform in particle size; the composite phase change material is added into gypsum according to the mixing amounts of 10%, 20% and 30%, and the gypsum-based paraffin and diatomite phase change energy storage material is prepared. The gypsum-based paraffin and diatomite phase change energy storage material is compact in structure and uniform in particle size, the service life is prolonged, the material is used as a building thermal insulation material to adjust the indoor temperature, and the energy sources can be greatly saved.
Description
Technical field
The present invention relates to the preparation method of a kind of phase-changing energy storage material, particularly the preparation method of a kind of gypsum base paraffin/diatomite phase-changing energy storage material.
Background technology
Phase change material refers to and varies with temperature and change form and can provide the material of latent heat, utilizes heat release in its phase transition process or inhales thermal property to realize the release (or storage) of energy. Phase-changing energy storage material and gypsum are prepared gypsum-based phase change energy storage material, it is possible not only to keep the advantages such as original fire-resistant, the lightweight of gypsum building thing, and adding along with phase-changing energy storage material, the thermal storage performance of buildings can be improved, increase the thermal inertia of buildings, reduce the outer heat of Indoor environment and transmit amplitude, reduce fluctuations in indoor temperature, in maintenance human body Suitable ranges, reduce the use of building heating or air-conditioning, it is achieved that building energy conservation. Existing research display, phase change material is with a wide range of applications at building field.
Paraffin is as a kind of phase change material, and its advantage is that use temperature is extensive, and enthalpy of phase change is big, and physical and chemical performance is stablized, and cold or demixing phenomenon can not occur, and nontoxic has no irritating odor. In addition, the cheap material of construction making it be applied to large volume becomes possibility. But, it has been reported that shaping phase-change material prepare in additive mass percentage higher, paraffin class main heat accumulating percentage composition is low, and phase transformation causes enthalpy of phase change to reduce, and supports additive ratio height; Adopt the complicated preparation technologies such as microcapsule that cost can be made to increase. Being introduced by phase change material is in gypsum, and the phase-change energy-storage composite material of preparation has certain heat storage capacity, and its heat storage capacity strengthens more along with phase change material.
Summary of the invention
It is an object of the invention to be provided a kind of low preparation cost, the preparation method of gypsum base paraffin/diatomite phase-changing energy storage material that application performance is good, solves organic phase change energy storage material thermal conductivity less, and Inorganic phase change energy storage material is crossed cold and held segregative problem.
The object of the present invention is achieved like this: this preparation method, take paraffin as heat accumulating, with the propping material of diatomite as paraffin, paraffin is embedded in diatomite pore texture the phase change material made and adds in gypsum, be prepared into gypsum base paraffin/diatomite phase-changing energy storage material; Concrete steps are as follows:
(1) respectively diatomite and paraffin are taken 20g in following ratio; It is respectively: 1# material, 2# material, 3# material and 4# material; Wherein, 1# material is diatomite: paraffin=0.6:0.4,2# material is diatomite: paraffin=0.55:0.45,3# material is diatomite: paraffin=0.5:0.5,4# material is diatomite: paraffin=0.45:0.55;
(2) grinding 2 hours after diatomite and paraffin being mixed, finally in pulverulence;
(3) the grinding mixing material of 2 hours is poured in mould, dry 4 hours in 80 DEG C of Hotaircirculatingovens;
(4) being taken out from mould by the material after oven dry, then grind 2 hours, paraffin and diatomite are fully merged, the composite phase-change material particle diameter of preparation is even;
(5) finally phase-changing energy storage material is added in gypsum according to the volume of 10%, 20% and 30% respectively, it is prepared into gypsum base paraffin/diatomite phase-changing energy storage material.
Described paraffin is solid paraffin, and purity is 90%-99%.
Described diatomite is solid, and purity is 90%-99%.
The useful effect of the present invention: adopt mixed mill-heating process, olefin material is embedded in the three-dimensional pore space of diatomite, take paraffin as energy storage material, it is prepared into phase-change energy-storage composite material, again phase change material is added and gypsum is made gypsum base composite phase-change energy storage material, adopt diatomite as the propping material of paraffin, obtain high enthalpy of phase change, low preparation cost, the gypsum base composite phase-change energy storage material that endurance quality is good.
(1) adopting phase-changing energy storage material prepared by mixed mill-heating process, the method easily operates, and the experiment condition without harshness, and starting material also easily obtain.
(2) solving organic phase change energy storage material thermal conductivity less, Inorganic phase change energy storage material is crossed cold and is held segregative problem. Reach the object of the present invention.
(3) present invention obtains high enthalpy of phase change, low preparation cost, apply shaping phase-change material of good performance.
The phase-changing energy storage material of the present invention is used as the lagging material of buildings, can effectively reduce the outer heat of Indoor environment and transmit amplitude, reduce fluctuations in indoor temperature, in maintenance human body Suitable ranges, reduce the use of building heating or air-conditioning, it is achieved that building energy conservation.
Accompanying drawing illustrates:
Fig. 1 a is the starting material olefin material micro-structure diagram of the present invention.
Fig. 1 b is the starting material diatomite material micro-structure diagram of the present invention.
Fig. 1 c is the gypsum base phase change composite material 1# material microstructure figure of the present invention.
Fig. 1 d is the gypsum base phase change composite material 4# material microstructure figure of the present invention.
Fig. 2 is the starting material of the present invention and the specific surface area figure of gypsum base phase change composite material.
Fig. 3 a is the starting material diatom grogs footpath distribution plan of the present invention.
Fig. 3 b is the starting material paraffin size distribution figure of the present invention.
Fig. 3 c is the gypsum base phase change composite material 1# material of the present invention, 2# material, 3# material, 4# material particle size distribution plan.
Fig. 4 a is the gypsum base phase change composite material 3# material XRD figure of the present invention.
Fig. 4 b is the gypsum base phase change composite material 4# material XRD figure of the present invention.
Fig. 5 a is the starting material paraffin FT-IR analysis chart of the present invention.
Fig. 5 b is the starting material diatomite FT-IR analysis chart of the present invention.
Fig. 5 c is the gypsum base phase change composite material 3# material FT-IR analysis chart of the present invention.
Fig. 5 d is the gypsum base phase transformation compound 4# material FT-IR analysis chart of the present invention.
The starting material olefin material TG that Fig. 6 a is the present invention schemes.
The starting material diatomite material TG that Fig. 6 b is the present invention schemes.
The gypsum base phase change composite material 3# material TG that Fig. 6 c is the present invention schemes.
The gypsum base phase change composite material 4# material TG that Fig. 6 d is the present invention schemes.
The starting material olefin material DSC that Fig. 7 a is the present invention schemes.
Fig. 7 b is the starting material diatomite material DSC test pattern of the present invention.
Fig. 7 c is the gypsum base phase change composite material 3# material DSC test pattern of the present invention.
Fig. 7 d is the gypsum base phase change composite material 4# material DSC test pattern of the present invention.
Fig. 8 a is the starting material olefin material DSC loop test figure of the present invention.
Fig. 8 b is the gypsum base phase change composite material 1# material DSC loop test figure of the present invention.
Fig. 8 c is the gypsum base phase change composite material 4# material DSC loop test figure of the present invention.
Fig. 9 a is the starting material gypsum test specimen thermal conductivity figure of the present invention.
Fig. 9 b is that the gypsum base phase change composite material 1# material of the present invention, 2# material, 3# material, 4# material add in gypsum, and phase change material content is the thermal conductivity of 10%.
Figure 10 is the gypsum base phase change composite material 3# material thermal conductivity energy analysis chart of the present invention.
Embodiment
This preparation method take paraffin as heat accumulating, with the propping material of diatomite as paraffin, paraffin embeds the phase change material made in diatomite and adds in gypsum, be prepared into gypsum base paraffin/diatomite phase-changing energy storage material; Concrete steps are as follows:
(1) respectively diatomite and paraffin are taken 20g in following ratio; It is respectively: 1# material, 2# material, 3# material and 4# material; Wherein, 1# material is diatomite: paraffin=0.6:0.4,2# material is diatomite: paraffin=0.55:0.45,3# material is diatomite: paraffin=0.5:0.5,4# material is diatomite: paraffin=0.45:0.55;
(2) grinding 2 hours after diatomite and paraffin being mixed, finally in pulverulence;
(3) the grinding mixing material of 2 hours is poured in mould, dry 4 hours in 80 DEG C of Hotaircirculatingovens;
(4) being taken out from mould by the material after oven dry, then grind 2 hours, paraffin and diatomite are fully merged, the composite phase-change material particle diameter of preparation is even;
(5) finally phase-changing energy storage material is added in gypsum according to the volume of 10%, 20% and 30% respectively, it is prepared into gypsum base paraffin/diatomite phase-changing energy storage material.
Described paraffin is solid paraffin, and purity is 90%-99%.
Described diatomite is solid, and purity is 90%-99%.
Fig. 1 is the configuration of surface stereoscan photograph of starting material paraffin, diatomite and embodiment one, four gypsum base phase transformation composite phase-change material. Being all cake shape structure from the known starting material of micro-structure diagram and gypsum base phase change composite material, and diatomite is porous cake shape structure, paraffin surface is comparatively level and smooth, and degree of compactness is good, and after paraffin is embedded diatomite, the hole of diatomite becomes few. From 1# material and 4# material figure it may be seen that increasing along with paraffin amount, the surface of 4# material is more more smooth than 1# material.
Fig. 2 is the specific surface area figure of starting material diatomite, paraffin and gypsum base phase change composite material 1# material, 2# material, 3# material, 4# material. Can finding out that the specific surface area of paraffin is relatively big from data, diatomite is less, and along with the increase of paraffin amount, the specific surface area of phase change composite material is more and more close to paraffin.
Fig. 3 is starting material paraffin, diatomite and embodiment one, two, three, four gypsum base phase change composite material size distribution figure. can find out that the particle diameter of paraffin is bigger from analytical data, the particle diameter of diatomite is smaller, gypsum base phase change composite material is increasing to the particle diameter of 4# material from 1# material, more and more close with the size distribution figure of paraffin, this ratio shared in phase change material to paraffin is relevant, owing to diatomite inside has a large amount of unique network-like microvoid structure, and still keep original loose porous shape form after absorption paraffin, along with the increase diatomite adsorption amount of paraffin amount reaches capacity state substantially, paraffin covers diatomite surface gradually, therefore its median size increases gradually.
Fig. 4 is embodiment three, embodiment four XRD test pattern. As seen from the figure, the intensity at the peak of gypsum base phase change composite material is different, is caused owing to paraffin in matrix material is different with the content of diatomite.
Fig. 5 is starting material paraffin, diatomite and embodiment three, four FT-IR analysis chart. Therefrom can obtain this figure just diatomite obtain with superposing of paraffin, can also see that any new peak shape does not occur by figure simultaneously, therefore embedding in diatomite at paraffin and do not generate new material, structure still remains unchanged, and gypsum base phase change composite material is stablized.
Fig. 6 is that starting material paraffin, diatomite and embodiment three, four TG scheme. Entirety, gypsum base phase change composite material better heat stability at normal temperatures, it is possible to be prepared into long-life energy-storage materials of construction.
Fig. 7 is that starting material paraffin, diatomite and embodiment three, four DSC scheme. From DSC figure it can be seen that in the process of rise in temperature, the differential thermal curve of diatomite is a level and smooth exotherm substantially; There are two endotherm(ic)peaks in paraffin near 70 DEG C and near 450 DEG C, this is because paraffin melting point is lower, starts when about 70 DEG C to melt, peak value occur when about 450 DEG C, be because paraffin starts material decomposition when this temperature. Transformation temperature and the wax phase change temperature of gypsum base phase change composite material (1# material, 2# material, 3# material, 4# material) are basically identical, also near 70 DEG C, there is a mild endotherm(ic)peak, have endotherm(ic)peak just slightly to raise near 400 500 DEG C equally.
Fig. 8 is starting material paraffin, diatomite and embodiment one, four circulation DSC test pattern. The quality change scope that can find out paraffin from cyclic curve is+2.593%, the quality change scope of gypsum is-18.59897%, and prepare gypsum base phase change composite material experience thermal cycling after quality change scope be about �� 1%, quality change amount is comparatively stable, illustrate that paraffin and diatomite mix even, the latent heat stable performance of gypsum base composite phase-change material.
Fig. 9 is gypsum, embodiment one, two, three, four heat conductivility analysis chart. By the contrast of two graphic representations, can find out on the whole, after gypsum test specimen adds phase change material, no matter it is all obviously reduce to its thermal conductivity when constant weight when wet curing or in oven dry, illustrates and add the heat-insulating property that phase change material can obviously promote gypsum. Thermal conductivity presents decline trend from gypsum base phase change composite material 1# to gypsum base phase change composite material 4#, but the amplitude reduced is different.
Figure 10 is the gypsum base phase change composite material 3# heat conductivility analysis chart that the content added is respectively 10%, 20%, 30% phase change material. Can be drawn by above-mentioned experimental result, gypsum base phase change composite material thermal conductivity ratio pure gypsum thermal conductivity is little, same gypsum, along with the increase adding phase change material amount, thermal conductivity also diminishes gradually, and this is mainly because pure gypsum sample thermal capacitance is less, and the heat energy that itself can discharge and store is less, therefore temperature variation is very fast, can reach envrionment temperature soon.
The present invention is set forth further below in conjunction with specific embodiments, transformation temperature and the enthalpy of phase change measuring tempeature scope of shaping phase-change material of the present invention are 30��1000 DEG C, the temperature recording the summit of main absorption corresponding is transformation temperature, between the starting temperature and final temperature at peak, the heat that the area that absorption peak surrounds with baseline is corresponding is enthalpy of phase change. The microtexture of paraffin, diatomite and gypsum base phase change composite material with scanning electron microscope analysis. By measuring the specific surface area of starting material and gypsum base phase change composite material, observe the stability at high operating temperatures of gypsum base phase change composite material. Adopting laser particle analyzer to analyze starting material diatomite, paraffin and gypsum base phase change composite material size, phase change material and non-phase change material heat conductivility are analyzed by DRE-2C unstable state thermal technology's sensor. Result shows, in phase change material, the content of paraffin becomes positive correlation with size, roughly presents negative correlativing relation with the thermal conductivity of phase-change energy-storage composite material. The experiment of infrared spectra, X-ray fluorescence spectra is finally used gypsum base phase change material chemical composition to be researched and analysed.
Embodiment 1:
Paraffin/diatomite phase-changing energy storage material, it obtains from the raw material of following weight percent: phase change composite material 1# material is diatomite: paraffin=0.6:0.4.
Embodiment 2:
Paraffin/diatomite phase-changing energy storage material, it obtains from the raw material of following weight percent: phase change composite material 2# material is diatomite: paraffin=0.55:0.45.
Embodiment 3:
Paraffin/diatomite phase-changing energy storage material, it obtains from the raw material of following weight percent: phase change composite material 3# material is diatomite: paraffin=0.5:0.5.
Embodiment 4:
Paraffin/diatomite phase-changing energy storage material, it obtains from the raw material of following weight percent: phase change composite material 4# material is diatomite: paraffin=0.45:0.55.
By composition, being mixed in proportion by starting material, become phase transformation mixing material, case study on implementation one, 23, four is all prepared according to following step:
(1) respectively diatomite and paraffin are taken in following ratio. It is respectively: 1# material is: diatomite: paraffin=0.6:0.4,2# material is: diatomite: paraffin=0.55:0.45,3# material is: diatomite: paraffin=0.5:0.5,4# material is: diatomite: paraffin=0.45:0.55;
(2) grinding 2 hours after diatomite and paraffin being mixed, finally in pulverulence;
(3) the grinding mixing material of 2 hours is poured in mould, dry 4 hours in 80 DEG C of Hotaircirculatingovens;
(4) being taken out from mould by the material after oven dry, then grind 2 hours, paraffin and diatomite are fully merged, the composite phase-change material particle diameter of preparation is even;
(5) finally phase-changing energy storage material is added in gypsum according to the volume of 10%, 20% and 30% respectively, it is prepared into gypsum base paraffin/diatomite phase-changing energy storage material.
The gypsum-based phase change energy storage material made according to above-mentioned formula and technique presents micro-yellow, and this gypsum base phase change composite material measures through circulation, repeatedly tests, this strong mechanical property, preparation method's technique of phase-changing energy storage material of the present invention is simple simultaneously, easy to operate, is easy to suitability for industrialized production. The packaging that the material that the present embodiment adopts adopts when dispatching from the factory all can meet seal request. After measured, the transformation temperature of this phase-changing energy storage material is about 70 DEG C.
Embodiment above describes the ultimate principle of the present invention; the advantage of main characteristic sum the present invention; industry technician should understand; the present invention is not by the restriction of above-mentioned case study on implementation; the principle that the present invention is only described described in above embodiment and specification sheets; without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications and will enter in the claimed scope of the invention. In the claimed scope of the present invention, appending claims defines with equivalent.
Claims (3)
1. the preparation method of gypsum base paraffin/diatomite phase-changing energy storage material, it is characterized in that: this preparation method take paraffin as heat accumulating, with the propping material of diatomite as paraffin, paraffin embeds diatomite make phase change material and add again in gypsum, it is prepared into gypsum base paraffin/diatomite phase-changing energy storage material; Concrete steps are as follows:
(1) respectively diatomite and paraffin are taken 20g in following ratio; It is respectively: 1# material, 2# material, 3# material and 4# material; Wherein, 1# material is diatomite: paraffin=0.6:0.4,2# material is diatomite: paraffin=0.55:0.45,3# material is diatomite: paraffin=0.5:0.5,4# material is diatomite: paraffin=0.45:0.55;
(2) grinding 2 hours after diatomite and paraffin being mixed, finally in pulverulence;
(3) the grinding mixing material of 2 hours is poured in mould, dry 4 hours in 80 DEG C of Hotaircirculatingovens;
(4) being taken out from mould by the material after oven dry, then grind 2 hours, paraffin and diatomite are fully merged, the composite phase-change material particle diameter of preparation is even;
(5) finally phase change material is added in gypsum according to the volume of 10%, 20% and 30% respectively, it is prepared into gypsum base paraffin/diatomite phase-changing energy storage material.
2. the preparation method of a kind of gypsum base paraffin/diatomite phase-changing energy storage material according to claim 1, is characterized in that: described paraffin is solid paraffin, and purity is 90%-99%.
3. the preparation method of a kind of gypsum base paraffin/diatomite phase-changing energy storage material according to claim 1, is characterized in that: described diatomite is solid, and purity is 90%-99%.
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Cited By (5)
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| CN107286913A (en) * | 2017-06-27 | 2017-10-24 | 中国矿业大学 | Red mud paraffin composite phase change energy storage material and its mix grinding method preparation method |
| 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 |
| CN109837069A (en) * | 2019-03-11 | 2019-06-04 | 河北地质大学 | A kind of multi-phase matrix composite phase-change energy storage material and preparation method 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 |
| CN115353866B (en) * | 2022-08-18 | 2024-06-28 | 中国地质大学（武汉） | Mineral-based heat storage microsphere and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286913A (en) * | 2017-06-27 | 2017-10-24 | 中国矿业大学 | Red mud paraffin composite phase change energy storage material and its mix grinding method preparation method |
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| CN109837069A (en) * | 2019-03-11 | 2019-06-04 | 河北地质大学 | A kind of multi-phase matrix composite phase-change energy storage material and preparation method thereof |
| CN109837069B (en) * | 2019-03-11 | 2021-03-16 | 河北地质大学 | Multi-element matrix composite phase change energy storage material and preparation method 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 |
| CN115353866B (en) * | 2022-08-18 | 2024-06-28 | 中国地质大学（武汉） | Mineral-based heat storage microsphere and preparation method thereof |
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