CN101812286A - Mesoporous material-based composite phase change heat storage material and preparation method thereof - Google Patents
Mesoporous material-based composite phase change heat storage material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a mesoporous material-based composite phase change heat storage material and a preparation method thereof. The composite phase change heat storage material, which can still keep fixed shape even at the temperature higher than the melting point of phase change substance by 30 DEG C, is prepared by using mesoporous material as carrier matrix and organic substance as phase change substance according to methods of physical blending and impregnation. Compared with other technologies, reported in documents, for the preparation of shape-fixed composite phase change material, the preparation technology has the characteristics of great simplicity and saving time, and the prepared composite phase change heat storage material has high content of the phase change material, high latent heat of phase change and utilization rate of the latent heat, and obviously lowered phase change temperature.
Description
Technical field
The present invention relates to a kind of composite phase change heat-accumulation material, especially a kind of organic phase changing matter and carrier matrix compound fixed phase change heat-storing material.
Background technology
Energy dilemma and environmental pollution have caused people's showing great attention to phase-changing energy storage material research; phase change material (Phase change material; PCM) has unique latent heat performance; in the phase change process; can absorb heat or emit heat from environment to environment, thus the purpose that reaches the heat storage and discharge.Therefore, (the air-conditioning storage is cold for power peak regulation for example, the storage of sun power and heat energy to be widely used in field of thermal energy storage, industrial exhaust heat utilizes), temperature adjusting field (space flight instrument for example, constant temperature textiles, temperature adjustment building temperature control, the agricultural greenhouse aspect), and other Application Areas (for example as the camouflage material in the war industry, the optical recording material that repeatedly writes down and delete, and the controlled material of household electrical appliance, large power, electrically sub-element).
Phase change material is of a great variety, according to the character of phase change material, generally is divided into inorganic PCM, organic PCM and compound PCM three classes.Inorganic PCM mainly contains crystalline hydrate salt, melting salt, metal or alloy etc.; Organic PCM mainly comprises organism such as paraffin, resin acid class, polyoxyethylene glycol.Inorganic PCM has characteristics such as thermal conductivity height, Heat of fusion are bigger, but in use is corrosive, and " cold excessively " and " being separated " phenomenon easily take place.Compare with mineral-type, organic class PCM does not have " cold excessively " and " being separated " problem, and corrodibility is little, stable performance, but easily leak during solid-liquid phase change.Compound PCM mostly is organic and inorganic mixture, has to overcome the shortcoming that single inorganic or organic PCM exists, expanded application scope.Among the compound PCM important a kind of be shaping phase-change material, the matrix material of forming by operation material and carrier matrix, it is constant that its profile kept solid shape when operation material underwent phase transition, this characteristic has broad application prospects it, becomes the focus that people study in energy utilization and material science.
In the prior art there being preparation carrier matrix that composite phase-change material adopted: contains the graphite etc. of gypsum, cement, concrete and the netted hole shape structure of a large amount of micropores, but all exist phase change material content low (being lower than 50wt%), shortcoming such as whole latent heat of phase change is not high, latent heat utilization efficient is low.
Summary of the invention
For addressing the above problem, the object of the present invention is to provide a kind of novel composite phase-change material, it has the content height of phase change material, whole latent heat of phase change height and the high advantage of latent heat utilization efficient with respect to composite phase-change material in the prior art.
Another object of the present invention provides a kind of preparation method of this NEW TYPE OF COMPOSITE phase change material.
For achieving the above object, composite phase-change material of the present invention is composited by organic phase changing matter and carrier matrix, it is characterized in that described carrier matrix is a mesoporous material.
According to International Standards Association definition, the material of material aperture between 2-50nm is called mesoporous material, is called poromerics less than the material of 2nm.What the mesoporous material described in the present invention referred to promptly is the material of aperture between 2-50nm, and preferred aperture is at the mesoporous material of 2-10nm.
Mesoporous material as carrier matrix in the composite phase-change material of the present invention can be that inorganics also can be an organism, and is immiscible and do not react between organic phase changing matter and the carrier matrix.Described carrier matrix is preferably inorganic mesoporous material, for example: the mesoporous si molecular sieves of SBA-15, the mesoporous si molecular sieves of MCM-41, CMK-3 mesoporous carbon, activated carbon etc.
As the organic phase changing matter in the composite phase-change material of the present invention is the solid-liquid phase change material, and this class material mainly contains paraffin class, fatty acid, ester class, alcohols and high molecular polymer class etc.
Paraffin is mainly mixed by straight-chain paraffin, and in general, its fusing point and Heat of fusion increase with the growth of carbochain, can obtain the heat-storing material of series of phase transitions temperature like this, but along with the growth of carbochain, the increased value of fusing point reduces gradually, is tending towards certain value the most at last.Paraffin has lot of advantages as the phase changing energy storage material, as the Heat of fusion height, steam forces down when undergoing phase transition, spontaneous nucleation does not have separating out, do not have surfusion during crystallization, chemical property stablely, nontoxic has no irritating odor, price is low etc., but also has problems such as heat conductivility is relatively poor.
The fatty acid material is commonly used capric acid, tetradecanoic acid, palmitinic acid, stearic acid etc.As the energy storage phase change material, fatty acid shows the thermal characteristics of good circulation fusion/crystallization-stable, and not having cold-peace, to separate out phenomenon, fusing point moderate etc., but price is higher.
The phase changing energy storage material of high molecular polymer class, as high density polyethylene(HDPE), polyoxyethylene glycol etc., they had both had the advantage of small molecules organic phase change material, had the macromolecular material characteristic again, were that Recent study gets a more class phase changing energy storage material.Preferred molecular weight of the present invention is that the polyoxyethylene glycol of 1500-10000 is as the organic phase changing matter in the composite phase-change material.
Preferably, the content of described organic phase change material in composite phase-change material is 30～90wt%, and is preferred, and the content of described organic phase change material in matrix material is 50～70wt%.
Composite phase-change material described in the present invention can adopt carrier matrix and organic phase change material blend, dipping, absorption to be prepared from.
More specifically, the preparation method of the composite phase-change material described in the present invention comprises the steps:
(1) organic phase change material is dissolved in the organic solvent;
(2) in the solution that step (1) obtains, add mesoporous material and dispersed with stirring;
(3) the mesoporous material drying that is adsorbed with organic phase change material that step (2) is obtained is removed organic solvent.
Preferably, the churning time in the described step (2) is 0.5～5.0 hour, organic phase change material is fully contacted with the pore surface of mesoporous material and adsorbs on it.
The middle drying temperature of described step (3) generally is higher than the fusing point of organic phase change material but is lower than its decomposition temperature, to investigate the setting situation of organic phase change material in mesoporous material, the situation that organic phase change material leaks out can not occur.Preferably, drying temperature is higher than 30 ℃ of organic phase change material fusing points.
Described organic solvent is selected according to the solvability of organic phase change material and the volatility of organic solvent self, can be dehydrated alcohol, Virahol, dimethyl formamide etc.
It is operation material that the present invention selects organic phase change material, and the mesoporous material in different apertures is a carrier matrix, utilizes the method for blend, dipping to prepare mesoporous material-based composite shape-setting phase-change material.And in the prior art there be preparation composite phase-change material selected carrier matrix: contain the graphite of gypsum, cement, concrete and the netted hole shape structure of a large amount of micropores, shortcoming such as have phase change material content low (being lower than 50wt%), whole latent heat of phase change is not high, latent heat utilization efficient is low.Adopting mesoporous material among the present invention is carrier matrix, the mesoporous material carrier matrix aperture of being adopted can be in the 2-50nm scope flexible, utilize its porous absorption and mesoporous confinement effect to efficiently solve the phase transformation leakage problem of organic phase change material, and the content height of phase change material (can reach 80wt%) in the composite shape-setting phase-change material that obtains, latent heat of phase change and latent heat utilization rate are all higher, and transformation temperature significantly reduces.And preparation technology of the present invention is simple, and is time saving and energy saving, and cost is low, is suitable for applying.
Description of drawings
Fig. 1 is according to the XRD spectra of the sample of embodiments of the invention 1 acquisition;
Fig. 2 is according to the DSC curve of the sample of embodiments of the invention 1 acquisition;
Fig. 3 is according to the XRD spectra of the sample of embodiments of the invention 2 acquisitions;
Fig. 4 is according to the DSC curve of the sample of embodiments of the invention 2 acquisitions;
Fig. 5 is according to the XRD spectra of the sample of embodiments of the invention 3 acquisitions;
Fig. 6 is according to the DSC curve of the sample of embodiments of the invention 3 acquisitions.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
The invention relates to a kind of mesoporous material-based composite shape-setting phase change heat storage material, organic phase change material is dissolved in the organic solvent, under strong stirring, add mesoporous material, stir, treat organic phase change material the absorption on the mesoporous material, dipping fully after, place dry 3 days of the baking oven that is higher than 30 ℃ of organic phase change material fusing points.
Used organic phase change material is that molecular weight is 1500～10000 polyoxyethylene glycol among the following embodiment; Used organic solvent is a dehydrated alcohol; Used mesoporous material is the mesoporous si molecular sieves of SBA-15, the mesoporous si molecular sieves of MCM-41 or activated carbon.
BET specific surface area, pore volume and the mean pore size of the mesoporous si molecular sieves of used SBA-15 is respectively 556.26m
2/ g0.738cm
3/ g and 5.233nm; BET specific surface area, pore volume and the mean pore size of the mesoporous si molecular sieves of used MCM-41 is respectively 758.31m
2/ g, 0.655cm
3/ g and 4.357nm; BET specific surface area, pore volume and the mean pore size of used activated carbon is respectively 1197.69m
2/ g, 0.440cm
3/ g and 3.916nm.
The content of described organic phase change material in composite phase change heat-accumulation material is in 30～90wt% scope.
Described churning time is 0.5～5.0 hour.
Prepared mesoporous material-based inorganic-organic composite phase change heat-accumulation material is carried out structure (X-ray diffraction (XRD), infrared spectra (FTIR), N
2Absorption specific surface and pore size distribution are measured (BET)) and thermal properties (differential scanning calorimetric (DSC), thermogravimetric (TG)) sign.The composite phase change heat-accumulation material that confirmation obtains has and wherein the identical crystalline phase of organic phase change material; Through measuring, when organic phase change material content is 40～80wt% in the composite phase change heat-accumulation material, more than the organic phase change material fusing point 30～40 ℃ its still can keep setting; The transformation temperature of composite phase change heat-accumulation material is than 2～10 ℃ of the reductions of organic phase change material, and the latent heat of phase change of composite phase change heat-accumulation material is 10～100J/g, and the latent heat utilization rate is 30～95%; Has good thermostability below 250 ℃.
Embodiment 1
Polyoxyethylene glycol (the PEG of dissolving 4g in the 40ml dehydrated alcohol, molecular weight 1500), under the strong stirring, in above-mentioned solution, add the mesoporous si molecular sieves of 1g SBA-15 or mesoporous si molecular sieves of MCM-41 or activated carbon (AC), stir 1.0h under the room temperature, mixed back 80 ℃ of dryings 3 days.
Result of implementation: as shown in Figure 1, different mesoporous material-based composite phase change heat storage materials have and wherein the identical crystalline phase of organic phase change material (PEG); Fig. 2 is the DSC curve of composite phase change heat-accumulation material, and the transformation temperature of different mesoporous material-based composite phase change heat storage materials is starkly lower than the transformation temperature of pure organic phase change material PEG.As shown in table 1, when the content of organic phase change material is 80wt% in the different mesoporous material-based composite phase change heat storage materials, the transformation temperature of composite phase change heat-accumulation material reduces with the increase of mesoporous material pore volume and mean pore size wherein, the transformation temperature of composite phase change heat-accumulation material (temperature of fusion) has reduced by 1.4～6.2 ℃ than pure organic phase change material PEG, enthalpy of phase change is 78.94～101.8J/g, and the latent heat utilization rate is between 92.87～95.29%.
The thermal characteristics result of the sample that table 1: embodiment 1 obtains
| Sample | ??PEG1500/??SBA-15 | ??PEG1500/??MCM-41 | ??PEG1500/AC | ??PEG1500 |
| Temperature of fusion (℃) | ??43.90 | ??46.60 | ??48.25 | ??49.68 |
| Melting heat (J/g) | ??82.14 | ??78.94 | ??101.8 | ??148.20 |
| Heat of solidification (J/g) | ??76.28 | ??75.22 | ??96.25 | ??141.36 |
| Latent heat utilization rate (%) | ??92.87 | ??95.29 | ??94.55 | ??95.38 |
Embodiment 2
Dissolving a certain amount of polyoxyethylene glycol (PEG, molecular weight 1500) in dehydrated alcohol under the strong stirring, adds a certain amount of activated carbon (AC) in above-mentioned solution, stir under the room temperature, mixes back 80 ℃ of dryings 3 days.
Table 2: the consumption of raw material in embodiment 2
| PEG1500 content (wt%) | Dehydrated alcohol (ml) | ??PEG1500(g) | ??AC(g) | Churning time (h) |
| ?30 | ??15 | ??1.5 | ??3.5 | ?3.5 |
| ?40 | ??20 | ??2.0 | ??3.0 | ?3.0 |
| ?50 | ??25 | ??2.5 | ??2.5 | ?2.5 |
| ?60 | ??30 | ??3.0 | ??2.0 | ?2.0 |
| ?70 | ??35 | ??3.5 | ??1.5 | ?1.5 |
Result of implementation: as shown in Figure 3, the composite phase change heat-accumulation material of different PEG content has and wherein the identical crystalline phase of organic phase change material (PEG); Fig. 4 is the DSC curve of the composite phase change heat-accumulation material of different PEG content, and the transformation temperature of the composite phase change heat-accumulation material of different PEG content is lower than the transformation temperature of pure organic phase change material PEG.As shown in table 3, the transformation temperature of composite phase change heat-accumulation material and enthalpy of phase change increase with the increase of organic phase change material content wherein, the transformation temperature of composite phase change heat-accumulation material has reduced by 1.1～3.1 ℃ than pure organic phase change material PEG, enthalpy of phase change is 8.18～81.29J/g, the latent heat utilization rate of 40wt%PEG/AC composite phase change heat-accumulation material has only 29.34%, and the latent heat utilization rate of the composite phase change heat-accumulation material of all the other content is between 91.24～95.12%.
The thermal characteristics result of the sample that table 3: embodiment 2 obtains
| PEG1500 content | Temperature of fusion (℃) | Melting heat (J/g) | Heat of solidification (J/g) | Latent heat utilization rate (%) |
| ?40wt％ | ??47.05 | ??8.18 | ??2.40 | ??29.34 |
| ?50wt％ | ??48.20 | ??23.17 | ??21.14 | ??91.24 |
| ?60wt％ | ??48.90 | ??49.67 | ??45.91 | ??92.43 |
| ?70wt％ | ??49.02 | ??81.29 | ??77.32 | ??95.12 |
Embodiment 3
The polyoxyethylene glycol (PEG, molecular weight 1500,4000,6000,10000) of dissolving 3.5g in the 35ml dehydrated alcohol under the strong stirring, adds the activated carbon (AC) of 1.5g in above-mentioned solution, stir 1.5h under the room temperature, mixes back 80 ℃ of dryings 3 days.
Result of implementation: as shown in Figure 5, the composite phase change heat-accumulation material of different PEG molecular weight has and wherein the identical crystalline phase of organic phase change material (PEG); Fig. 6 is the DSC curve of the composite phase change heat-accumulation material of different PEG molecular weight, and the transformation temperature of the composite phase change heat-accumulation material of different PEG molecular weight is starkly lower than the transformation temperature of the pure organic phase change material PEG of corresponding molecular weight.As shown in table 4, PEG content is that the transformation temperature of the PEG/AC composite phase change heat-accumulation material of 70wt% increases with the increase of organic phase change material molecular weight wherein, the transformation temperature of composite phase change heat-accumulation material than the reduction of the pure organic phase change material PEG of corresponding molecular weight 1.1～5 ℃, enthalpy of phase change is 8.18～81.29J/g, and the latent heat utilization rate of composite phase change heat-accumulation material is between 91.13～95.40%.
The thermal characteristics result of the sample that table 4: embodiment 3 obtains
| The PEG molecular weight | Temperature of fusion (℃) | Melting heat (J/g) | Heat of solidification (J/g) | Latent heat utilization rate (%) |
| ?1500 | ??49.02 | ??81.29 | ??77.32 | ??95.12 |
| ?4000 | ??57.69 | ??83.09 | ??75.72 | ??91.13 |
| ?6000 | ??62.80 | ??90.22 | ??85.22 | ??94.46 |
| ?10000 | ??63.96 | ??85.12 | ??81.38 | ??95.40 |
Claims (10)
1. a composite phase-change material is composited by organic phase changing matter and carrier matrix, it is characterized in that, described carrier matrix is a mesoporous material.
2. composite phase-change material according to claim 1 is characterized in that the aperture of described mesoporous material is at 2-10nm.
3. composite phase-change material according to claim 1 is characterized in that, described mesoporous material is inorganic mesoporous material.
4. composite phase-change material according to claim 3 is characterized in that, described mesoporous material is the mesoporous si molecular sieves of SBA-15, the mesoporous si molecular sieves of MCM-41, CMK-3 mesoporous carbon or activated carbon.
5. composite phase-change material according to claim 1 is characterized in that, described organic phase changing matter is selected from one or more in the solid-liquid phase change material of paraffin class, fatty acid, ester class, alcohols and high molecular polymer class.
6. composite phase-change material according to claim 5 is characterized in that, described organic phase changing matter is that molecular weight is the polyoxyethylene glycol of 1500-10000.
7. composite phase-change material according to claim 1 is characterized in that, the content of described organic phase changing matter in composite phase-change material is 30～90wt%.
8. the preparation method of arbitrary described composite phase-change material among the claim 1-7 comprises the steps:
(1) organic phase changing matter is dissolved in the organic solvent;
(2) in the solution that step (1) obtains, add mesoporous material and dispersed with stirring;
(3) the mesoporous material drying that is adsorbed with organic phase changing matter that step (2) is obtained is removed organic solvent.
9. preparation method according to claim 8 is characterized in that, the churning time in the step (2) is 0.5～5.0 hour.
10. preparation method according to claim 9 is characterized in that, drying temperature is higher than 30 ℃ of organic phase changing matter fusing points in the described step (3).
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Application publication date: 20100825 |