CN103834366A - Phase change thermal storage material used at medium temperature in industries and preparation method thereof - Google Patents
Phase change thermal storage material used at medium temperature in industries and preparation method thereof Download PDFInfo
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Abstract
The invention provides a phase change thermal storage material used at medium temperature in industries and a preparation method thereof. The phase change thermal storage material is prepared from adipic acid, a copper coated carbon nanotube and a binder, wherein the mass ratio of adipic acid to the copper coated carbon nanotube is (88-98):(2-12), and the mass of the binder is 3% of the total mass of adipic acid and the copper coated carbon nanotube. The preparation method of the phase change thermal storage material comprises the steps of mechanically mixing adipic acid with the copper coated carbon nanotube according to the preset ratio, filling the mixture into a crucible after mixing adipic acid with the copper coated carbon nanotube uniformly, putting the mixture into a vacuum drying oven to undergo vacuum melting and adsorption, then doping the binder and carrying out press forming, thus obtaining the phase change thermal storage material. The thermal storage material can be applied to dewatering and drying in the industries such as solar air conditioners, floor heating, chemical printing and dyeing and the like. The preparation method is reasonable in material selection and advanced in preparation process, thus the thermal storage material used in the industrial field can be produced at low cost. The thermal storage composite material substantially improves the comprehensive properties including thermal storage, heat release efficiency and the like.
Description
Technical field
The present invention relates to the preparation of middle temperature field phase change heat storage material, provide especially a kind of take hexanodioic acid as phase change heat storage material, add carbon nanotube industrial medium temperature phase change heat storage material and preparation method thereof as enhanced thermal conduction phase.The working temperature of phase change heat storage material prepared by the method can be at 120～200 ℃.
Background technology
In industrial application, the renewable energy source take sun power as representative has contains abundant and advantages of environment protection, adheres to advancing its development and utilization significant to the Sustainable development of human society.But, heat energy shortcoming such as the otherness in the discontinuity of lifetime, space and the unstable of intensity all in utilization, this has greatly limited its large-scale application.Heat storage technology is by artificial intervention, can reasonably regulate and control to heat energy (collect, save and discharge), be the effective way that solves the uneven and raising energy use efficiency of heat energy supply and demand in time, space and intensity, be subject in recent years domestic and international investigator's extensive attention.
Heat storage technology utilizes the conversion of material internal energy, can collect heat energy, save and discharge, and then realize the Reasonable Regulation And Control to heat energy supplydemand relationship.By it, the mode of saving to heat energy can be divided into three kinds of sensible heat, chemical reaction heat and latent heat to heat storage technology.Sensible heat accumulation of heat utilizes the thermal capacitance of material to carry out accumulation of heat, realizes saving of heat energy and discharges by improving and reduce the temperature of material.When the operation of sensible heat regenerative apparatus, only have temperature to change, thereby operation and management is comparatively simple, is that current technology is the most ripe, the heat storage type being most widely used, but its thermal storage density is little, what therefore need is bulky, is difficult to realize industrialized large-scale application.Along with day by day the highlighting of global energy crisis form, just again cause investigator's extensive attention about the research of centering temperature phase change material in recent years.The main raw of research is melting salt, alloy and organic materials at present.Research shows, at lower temperature application field (<100 ℃), the water with higher sensible heat appearance and nominal price is optimum heat storage medium, and at middle high-temperature field, particularly, the research of the heat-storing material of temperature (80～250 ℃) is relatively less, a little less than heat utilization technology relative thin, lack systematic research.
Document 1 has reported that " experimental study of nano aluminium oxide and erythritol composite phase-change material " (king is, chapter is learned, Korean-Chinese, Deng .[J] chemical engineering, 2012, 40(10): 21-24.) in literary composition take erythritol as phase change material, improve the performance of erythritol phase change material as nucleator by admixture nano aluminium oxide, prepare erythritol/nano aluminium oxide composite phase-change material, test result shows, the nano aluminium oxide of admixture can be scattered in the erythritol base fluid of melted state equably, it can effectively solve the cold problem of mistake of phase change material, in the time that addition content is 0.25wt.%, the purer erythritol of thermal conductivity of composite phase-change material has improved 2 times, latent heat of phase change drops to 325.08J/g by 340.08J/g, reduce 4.41%.
Document 2 is reported take multicomponent alloy Sn-Bi-Zn-Cu-Pb as middle temperature phase change heat storage material, and its performance is studied.(Yu Tieming, warm phase-transition heat-storage performance study in Sn-Bi-Zn-Cu-Pb multicomponent alloy.[M] Wuhan University of Technology academic dissertation, 2012.) result of its research shows: Sn-Zn eutectic alloy has good heat storage performance, and its transformation temperature is 198 ℃, and latent heat of phase change is 65.8J/g, and density is 7.38g/cm
3, thermal conductivity is 53.4W/ (mK), the heat storage capacity of Sn-Zn eutectic alloy is 485.6J/cm
3.Its heat storage capacity is greater than NaNO
3/ KNO
3heat storage capacity, therefore the hot physical performance of Sn-Zn eutectic alloy has great advantage.
Document 3 is reported take NaOH/KOH binary system as heat-storing material, and NaOH/KOH binary system heat storage performance is studied.(Zhengning, the village, Cao Nian, Li Jiangrong.NaOH/KOH binary system heat storage performance research [J] XI AN JIAOTONG UNIVERSITY Subject Index, 2002,36 (11): 1133-1137.) and analyzed the phenomenons such as the melting and solidification of phase change material, obtain binary system and formed the influence curve figure to transformation temperature, result shows, the phase transformation of this binary system comprises solid-liquid phase change and solid-solid phase-change two portions; In the time that NaOH quality percentage composition is 23.4%, it is 145.6 ℃ that binary system has lowest total of the melting point, afterwards along with NaOH content increases, and binary system Melting point elevation.
Document 4 has reported that, take nitrate as heat accumulating phase change material, expanded graphite strengthens and improve heat conductivility, (Peng Guowei. the research of the preparation of expanded graphite/melting salt composite shape-setting phase change heat storage material and thermal characteristics.[M] Lanzhou University of Science & Technology academic dissertation, 2012) test and obtain equimolar eutectic nitrate and in temperature-rise period, have phase transition process twice by differential thermal analysis, Gu be once solid-transformation, its transition temperature is 117.5 ℃, phase transformation end temp is 132 ℃, latent heat of phase change is 33.34J/g, it is once solid-liquid transformation, its transition temperature is 219.5 ℃, phase transformation end temp is 227.5 ℃, and latent heat of phase change is 116.6J/g, is the salt such as molar nitric acid such as grade of 400 ℃ of preparations in working temperature, its thing phase composite is saltpetre and SODIUMNITRATE, does not have novel substance to generate.
In the research of the heat-storing material in above-mentioned middle temperature field, the problem of alloy maximum is easy oxidation, cause its work-ing life short, reliability is poor, and the cost of melting salt is low, latent heat of phase change is high, but its larger shortcoming is to exist serious mistake cold-peace to be separated, and has serious corrodibility, to having relatively high expectations of container, therefore in actual engineering, its performance degradation is larger, is difficult to guarantee its long term reliability.It is high that organic phase change material has latent heat of phase change, excessively cold little, substantially without being separated.But its thermal conductivity is little, in application, needs to add heat conduction phase medium and improve its thermal conductivity.
Summary of the invention
Technical problem to be solved by this invention is: a kind of excellent performance and lower-cost industrial medium temperature phase change heat storage material and preparation method thereof is provided.
The present invention solves its technical problem and adopts following technical scheme:
A kind of industrial medium temperature phase change heat storage material, is characterized in that, described phase change heat storage material is made up of hexanodioic acid, coppered carbon nanotube and binding agent; The mass ratio of described hexanodioic acid and coppered carbon nanotube is 88～98:2～12, and the quality of described binding agent is 3% of hexanodioic acid and both total masses of coppered carbon nanotube.
In such scheme, the use temperature scope of described phase change heat storage material is 120～200 ℃.
In such scheme, described binding agent is Xylo-Mucine.
A preparation method for phase change heat storage material for industrial medium temperature, is characterized in that, it comprises the following steps:
1) get the raw materials ready: choose hexanodioic acid, coppered carbon nanotube and binding agent, the mass ratio of described hexanodioic acid and coppered carbon nanotube is 88～98:2～12, the quality of described binding agent is 3% of hexanodioic acid and both total masses of coppered carbon nanotube;
2) by hexanodioic acid, coppered carbon nanotube drying treatment 24 hours, hexanodioic acid grinding is crossed after 100 mesh sieves, carried out mechanically mixing 15 minutes with coppered carbon nanotube by preset blending ratio, after mixing, pack in crucible, put into vacuum drying oven, melting absorption 6 hours at 150～160 ℃ of temperature;
3) mix binding agent and carry out compression molding, obtain described industrial medium temperature phase change heat storage material.
In such scheme, described coppered carbon nanotube is to adopt following method to obtain:
1) first carbon nanotube is processed 30 minutes at 400 ℃ of temperature, after then mixing with ethanol, carried out again ultrasonication 40 minutes;
2) in the carbon nano tube surface copper facing of treated mistake, the processing parameter adopting when copper facing is: bath temperature: 80 ± 1 ℃, and pH value: 12 ± 0.1, plating time: 0.5～5h.
In such scheme, the electroplate liquid formulation adopting when copper facing is: the stablizer of the copper sulfate of 1～10wt%, the complexing agent of 1～5wt%, 1～3wt%, pH value conditioning agent, the reductive agent of 2～8wt% and the water of 75～94wt% of 1～8wt%.
In such scheme, described complexing agent is sodium hypophosphite.
In such scheme, described stablizer is DMF.
In such scheme, described reductive agent is that volumetric concentration is 36% formaldehyde.
In such scheme, described binding agent is Xylo-Mucine.
In the present invention: the effect of copper sulfate is to provide cupric ion, in chemical bronze plating liquid, mantoquita content is higher, and plating speed is also faster; In actual plating process, when content is increased to after certain certain amount, plate fast increase not obvious.The effect of reductive agent formaldehyde is to provide electronics and deposits copper to cupric ion, so reductive agent provides the capacity of water of electronics to have conclusive effect to whole plating process.In general, the higher plating of the content of formaldehyde speed is just faster, but is increased to certain degree when the concentration of formaldehyde, plates fast increase no longer obvious.But the too high motivating force providing of formaldehyde content is excessive, can accelerate the self-decomposition of plating solution, plating excessive velocities can affect quality of coating.Complexing agent is that sodium hypophosphite is mainly for controlling copper-plated speed, and the effect DMF of stablizer is exactly the generation that stops solution self-decomposition, makes plating have the carrying out of control.Stablizer is generally very effective to the stability of raising plating solution, but most stable agent plays a part to strangle to the catalytic effect of electroless copper reaction again, even can make to react completely to stop.The amount of general stablizer is controlled at the scope of 10mg/L left and right.Stablizer has a great impact plating speed.From above-mentioned, can find out, in copper facing process, every kind of material has feature and the effect of self, is interact and restrict, and final copper-plated performance is had to important impact.
The present invention compared with prior art has advantages of following main:
One, innovation of the present invention are that adopting the hexanodioic acid that latent heat of phase change is high, thermal characteristics is excellent is phase change material, utilize the heat conductivility of the strongthener of coppered carbon nano-tube material simultaneously, adopt the method for vacuum fusion absorption to form phase change material.
Two, the invention provides a kind of heat-storing material with high latent heat of phase change, high heat conductance, the composition of this heat-storing material is optimized to design, realize the significantly raising of its over-all properties.Wherein, introduce coppered carbon nano-tube material, itself has excellent performance, and as excellent conduction, thermal conductivity, itself also has abundant pore structure, has good characterization of adsorption.
Three, with the conventional complexing agent (disodium ethylene diamine tetraacetate (Na of current industrial copper facing
2) and stablizer (2 EDTA), 2 '-dipyridyl) compare, the complexing agent adopting in the present invention and stablizer are not only cheap, take stablizer as example, 2, the price existing market of 2 '-dipyridyl is at 200,000/ton, and N, the market value of dinethylformamide is at 8000 yuan/ton, and almost non-toxic, and environmental pollution is little.Copper plate sedimentation rate prepared by the present invention is fast, strong adhesion.
Four, at the copper coating of carbon nanotube, greatly improve the poor shortcoming of consistency between carbon material and hexanodioic acid material, improve their bonding strength, thereby improved heat conduction and heat transfer property.Carbon nanotube has stronger adsorptive power on the other hand, in the time of heat-storing material generation solid-liquid phase change, as the carrier of phase change material, can effectively overcome the liquid phase substance leakage problem in phase transition process.
Five, technique is simple, and the starting material that whole preparation process is selected are simple, takes full advantage of the feature of material, just can synthesize fast excellent performance and lower-cost modification heat-storing material without too much changing existing equipment.
In a word, technique of the present invention is simple, easy to operate, and without too much changing existing equipment, and the more unmodified material of performance of prepared coppered carbon nano-tube material modification hexanodioic acid heat-storing material greatly improves, and preparation cost is lower.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of coppered carbon nanotube.As we can see from the figure, the caliber of carbon nanotube is in 40nm left and right, and the thickness of copper plate is between 10～20nm, and copper plate is tightly attached to the surface of carbon nanotube.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
Embodiment 1
Choose hexanodioic acid according to mass percent: 90%, coppered carbon nanotube 10%.Wherein hexanodioic acid can directly carry out drying treatment 24 hours, first carbon nanotube is processed 30 minutes at 400 ℃ of temperature, then after mixing with ethanol, carry out ultrasonication 40 minutes again, then carry out copper coating, after copper facing completes, drying treatment obtains coppered carbon nanotube after 10 hours.
Processing parameter when copper facing is as follows:
Bath temperature: 80 ± 1 ℃
PH value: 12 ± 0.1, adjust with NaOH
Alr mode: magnetic agitation
Plating time: 0.5h.
Fig. 1 is the stereoscan photograph of coppered carbon nanotube.As can see from Figure 1, the copper plate of carbon nano tube surface is tightly attached to the surface of carbon nanotube.
Then, hexanodioic acid grinding is crossed after 100 mesh sieves, carried out mechanically mixing 15 minutes with coppered carbon nanotube by preset blending ratio, after mixing, pack in crucible, put into vacuum drying oven, melting absorption 6 hours at 150～160 ℃ of temperature.In the time of compression molding, mix the binding agent of 3%CMC outward.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 237.6J/g, and solidifying heat release enthalpy is 220.5J/g, records at the Hot Disc 2500S of company type thermal constant analyser, and the thermal conductivity of composite phase change heat-accumulation material is 2.02W/mK, and specific heat capacity is 1.14J/gK.
It should be noted that, the preset blending ratio of hexanodioic acid and coppered carbon nanotube is mainly that the requirement of the comprehensive consideration to heat storage performance and heat conductivility according to client is determined, is set according to the actual requirements by client.
Embodiment 2
Choose hexanodioic acid according to mass percent: 92%, coppered carbon nanotube 8%.Wherein hexanodioic acid can directly carry out drying treatment 24 hours, first carbon nanotube is processed 30 minutes at 400 ℃ of temperature, then after mixing with ethanol, carry out again ultrasonication 40 minutes, carry out copper coating (with embodiment 1 same procedure), after copper facing completes, drying treatment obtains coppered carbon nanotube after 10 hours again.
Processing parameter when copper facing is as follows:
Bath temperature: 80 ± 1 ℃
PH value: 12 ± 0.1, adjust with NaOH
Alr mode: magnetic agitation
Plating time: 5h.
Then, hexanodioic acid grinding is crossed after 100 mesh sieves, carried out mechanically mixing 15 minutes with coppered carbon nanotube by preset blending ratio, after mixing, pack in crucible, put into vacuum drying oven, melting absorption 6 hours at 150～160 ℃ of temperature.In the time of compression molding, mix the binding agent of 3%CMC outward.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 239.6J/g, and solidifying heat release enthalpy is 225.5J/g, records at the Hot Disc 2500S of company type thermal constant analyser, and the thermal conductivity of composite phase change heat-accumulation material is 1.91W/mK, and specific heat capacity is 1.21J/gK.
Embodiment 3
Choose hexanodioic acid according to mass percent: 94%, coppered carbon nanotube 6%.Wherein hexanodioic acid can directly carry out drying treatment 24 hours, first carbon nanotube is processed 30 minutes at 400 ℃ of temperature, then after mixing with ethanol, carry out ultrasonication 40 minutes again, then carry out copper coating, after copper facing completes, drying treatment obtains coppered carbon nanotube after 10 hours.
Processing parameter when copper facing is as follows:
Bath temperature: 80 ± 1 ℃
PH value: 12 ± 0.1, adjust with NaOH
Alr mode: magnetic agitation
Plating time: 3h.
Then, hexanodioic acid grinding is crossed after 100 mesh sieves, carried out mechanically mixing 15 minutes with coppered carbon nanotube by preset blending ratio, after mixing, pack in crucible, put into vacuum drying oven, melting absorption 6 hours at 150～160 ℃ of temperature.In the time of compression molding, mix the binding agent of 3%CMC outward.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 241.6J/g, and solidifying heat release enthalpy is 229.5J/g, records at the Hot Disc 2500S of company type thermal constant analyser, and the thermal conductivity of composite phase change heat-accumulation material is 1.83W/mK, and specific heat capacity is 1.24J/gK.
Embodiment 4
Choose hexanodioic acid according to mass percent: 96%, coppered carbon nanotube 4%.Wherein hexanodioic acid can directly carry out drying treatment 24 hours, first carbon nanotube is processed 30 minutes at 400 ℃ of temperature, then after mixing with ethanol, carry out again ultrasonication 40 minutes, carry out again copper coating (copper-plating technique identical with embodiment 1), after copper facing completes, drying treatment obtains coppered carbon nanotube after 10 hours, hexanodioic acid grinding is crossed after 100 mesh sieves, carry out mechanically mixing 15 minutes with coppered carbon nanotube by preset blending ratio, after mixing, pack in crucible, put into vacuum drying oven, melting absorption 6 hours at 150～160 ℃ of temperature.In the time of compression molding, mix the binding agent of 3%CMC outward.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 249.6J/g, and solidifying heat release enthalpy is 235.5J/g, records at the Hot Disc 2500S of company type thermal constant analyser, and the thermal conductivity of composite phase change heat-accumulation material is 1.35W/mK, and specific heat capacity is 1.29J/gK.
Embodiment 5
Choose hexanodioic acid according to mass percent: 98%, coppered carbon nanotube 2%.Wherein hexanodioic acid can directly carry out drying treatment 24 hours, first carbon nanotube is processed 30 minutes at 400 ℃ of temperature, then after mixing with ethanol, carry out again ultrasonication 40 minutes, carry out again copper coating (copper-plating technique identical with embodiment 2), after copper facing completes, drying treatment obtains coppered carbon nanotube after 10 hours, hexanodioic acid grinding is crossed after 100 mesh sieves, carry out mechanically mixing 15 minutes with coppered carbon nanotube by preset blending ratio, after mixing, pack in crucible, put into vacuum drying oven, melting absorption 6 hours at 150～160 ℃ of temperature.In the time of compression molding, mix the binding agent of 3%CMC outward.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 253.2J/g, and solidifying heat release enthalpy is 241.6J/g, records at the Hot Disc 2500S of company type thermal constant analyser, and the thermal conductivity of composite phase change heat-accumulation material is 0.85W/mK, and specific heat capacity is 1.31J/gK.
Embodiment 6
Choose hexanodioic acid according to mass percent: 88%, coppered carbon nanotube 12%.Wherein hexanodioic acid can directly carry out drying treatment 24 hours, first carbon nanotube is processed 30 minutes at 400 ℃ of temperature, then after mixing with ethanol, carry out again ultrasonication 40 minutes, carry out again copper coating (copper-plating technique identical with embodiment 3), after copper facing completes, drying treatment obtains coppered carbon nanotube after 10 hours, hexanodioic acid grinding is crossed after 100 mesh sieves, carry out mechanically mixing 15 minutes with coppered carbon nanotube by preset blending ratio, after mixing, pack in crucible, put into vacuum drying oven, melting absorption 6 hours at 150～160 ℃ of temperature.In the time of compression molding, mix the binding agent of 3%CMC outward.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 220.4J/g, and solidifying heat release enthalpy is 213.7J/g, records at the Hot Disc 2500S of company type thermal constant analyser, and the thermal conductivity of composite phase change heat-accumulation material is 2.23W/mK, and specific heat capacity is 1.05J/gK.
Claims (10)
1. an industrial medium temperature phase change heat storage material, is characterized in that, described phase change heat storage material is made up of hexanodioic acid, coppered carbon nanotube and binding agent; The mass ratio of described hexanodioic acid and coppered carbon nanotube is 88～98:2～12, and the quality of described binding agent is 3% of hexanodioic acid and both total masses of coppered carbon nanotube.
2. industrial medium temperature phase change heat storage material as claimed in claim 1, is characterized in that, the use temperature scope of described phase change heat storage material is 120～200 ℃.
3. industrial medium temperature phase change heat storage material as claimed in claim 1, is characterized in that, described binding agent is Xylo-Mucine.
4. a preparation method for phase change heat storage material for industrial medium temperature, is characterized in that, it comprises the following steps:
1) get the raw materials ready: choose hexanodioic acid, coppered carbon nanotube and binding agent, the mass ratio of described hexanodioic acid and coppered carbon nanotube is 88～98:2～12, the quality of described binding agent is 3% of hexanodioic acid and both total masses of coppered carbon nanotube;
2) by hexanodioic acid, coppered carbon nanotube drying treatment, after hexanodioic acid grinding is sieved, carry out mechanically mixing with coppered carbon nanotube by preset blending ratio, after mixing, pack in crucible, put into vacuum drying oven, melting absorption 6 hours at 150～160 ℃ of temperature;
3) mix binding agent and carry out compression molding, obtain described industrial medium temperature phase change heat storage material.
5. preparation method as claimed in claim 4, is characterized in that, described coppered carbon nanotube is to adopt following method to obtain: 1) first carbon nanotube is processed 30 minutes at 400 ℃ of temperature, after then mixing with ethanol, carried out ultrasonication 40 minutes again; 2) in the carbon nano tube surface copper facing of treated mistake, the processing parameter adopting when copper facing is: bath temperature: 80 ± 1 ℃, and pH value: 12 ± 0.1, plating time: 0.5～5h.
6. preparation method as claimed in claim 4, it is characterized in that, the electroplate liquid formulation adopting when copper facing is: the stablizer of the copper sulfate of 1～10wt%, the complexing agent of 1～5wt%, 1～3wt%, pH value conditioning agent, the reductive agent of 2～8wt% and the water of 75～94wt% of 1～8wt%.
7. preparation method as claimed in claim 6, is characterized in that, described complexing agent is sodium hypophosphite.
8. preparation method as claimed in claim 6, is characterized in that, described stablizer is DMF.
9. preparation method as claimed in claim 6, is characterized in that, described reductive agent is that volumetric concentration is 36% formaldehyde.
10. preparation method as claimed in claim 4, is characterized in that, described binding agent is Xylo-Mucine.
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| CN106762418A (en) * | 2017-01-19 | 2017-05-31 | 上海交通大学 | Isolated island energy resource system based on the adjustable electric power storage accumulation of heat of wind-power electricity generation |
| CN110872486A (en) * | 2018-08-31 | 2020-03-10 | 青海大学 | Method for simultaneously inhibiting supercooling of hydrous salt phase change material and enhancing heat transfer performance |
| CN111826128A (en) * | 2020-07-13 | 2020-10-27 | 黄冈师范学院 | Modified diatomite/adipic acid phase change heat storage material and preparation method thereof |
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