CN103834366B - A kind of industrial medium temperature phase change heat storage material and preparation method thereof - Google Patents
A kind of industrial medium temperature phase change heat storage material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of industrial medium temperature phase change heat storage material and preparation method thereof.This phase change heat storage material is made up of adipic acid, coppered carbon nanotube and binding agent；Described adipic acid is 88～98:2～12 with the mass ratio of coppered carbon nanotube, and the quality of described binding agent is the 3% of both adipic acid and coppered carbon nanotube gross mass.The preparation method of this phase change heat storage material is: by preset blending ratio, adipic acid and coppered carbon nanotube are carried out mechanical mixture, loads in crucible after mix homogeneously, puts into the absorption of vacuum drying oven vacuum fusion, then mixes binding agent compression molding and get final product.This heat-storing material can apply to the dehydrate of the industries such as solar airconditioning, floor heating, chemical industry printing and dyeing.Selection of the present invention is reasonable, and preparation technology is advanced such that it is able to low-cost production goes out a kind of industrial circle heat-storing material, and the application of this heat storage composite material makes accumulation of heat, exothermal efficiency etc. be greatly improved in interior combination property.
Description
Technical field
The present invention relates to the preparation of middle temperature field phase change heat storage material, specifically provide a kind of with adipic acid as phase change heat storage material,
Add the CNT industrial medium temperature phase change heat storage material and preparation method thereof as enhanced thermal conduction phase.Phase transformation prepared by the method
The operating temperature of heat-storing material can be at 120～200 DEG C.
Background technology
In commercial Application, the regenerative resource with solar energy as representative has contains abundant and advantages of environment protection, adheres to pushing away
Enter its development and utilization significant to the sustainable development of human society.But, in utilization, all there is the time in heat energy
The shortcomings such as the unstability of discontinuity, the diversity in space and intensity, this greatly limits the application of its large-scale.Accumulation of heat skill
Art, by artificial intervention, can reasonably regulate and control (collect, save and discharge) to heat energy, be solve heat energy supply and demand the time,
Imbalance on space and intensity and improve the effective way of energy use efficiency, the most wide by domestic and international researcher
General attention.
Heat storage technology utilizes the conversion of material internal energy, can be collected heat energy, saves and discharge, and then realizes heat energy
The Reasonable Regulation And Control of supply-demand relationship.Heat energy is saved mode by it by heat storage technology can be divided into sensible heat, chemical reaction heat and latent heat three
Kind.Sensible heat accumulation of heat utilizes the thermal capacitance of material to carry out accumulation of heat, realizes saving and releasing of heat energy by the temperature improving and reducing material
Put.Sensible heat regenerative apparatus only has temperature to change when running, thus runs and manage relatively simple, is that current technology is the most ripe,
The heat storage type being most widely used, but its thermal storage density is little, it is therefore desirable to bulky, be difficulty with industrialized greatly
Sizable application.Recently as day by day highlighting of global energy crisis form, the research about centering temperature phase-change material is drawn the most again
Play the extensive attention of researcher.The main material of research is fuse salt, alloy and organic material at present.Research shows, at low temperature
Application (< 100 DEG C), have higher sensible heat holding the water with low price is optimum heat storage medium, and at middle high-temperature field,
The research of the heat-storing material of middle temperature (80～250 DEG C) is relatively fewer, and heat utilization technology is the weakest, lacks systematic research.
Document 1 report the experimentation of erythritol composite phase-change material " nano aluminium oxide with " (king is, chapter is come, Korean-Chinese,
Deng. [J] Chemical Engineering, 2012,40(10): 21-24.) with erythritol as phase-change material in literary composition, made by admixture nano aluminium oxide
Improve the performance of erythritol phase-change material for nucleator, prepared erythritol/nano aluminium oxide composite phase-change material, survey
Test result shows, the nano aluminium oxide of admixture can be homogeneously dispersed in the erythritol base fluid of molten state, and it can be effective
Solving the supercool problem of phase-change material, when addition content is 0.25wt.%, the red algae that the heat conductivity of composite phase-change material is purer is sugared
Alcohol improves 2 times, and latent heat of phase change is dropped to 325.08J/g by 340.08J/g, decreases 4.41%.
Document 2 reports that with multicomponent alloy Sn-Bi-Zn-Cu-Pb be middle temperature phase change heat storage material, and studies its performance.(Yu
Ferrum is engraved, the middle temperature phase-transition heat-storage performance study of Sn-Bi-Zn-Cu-Pb multicomponent alloy.[M] Wuhan University of Technology academic dissertation, 2012.)
The result of its research shows: Sn-Zn eutectic alloy has good heat storage performance, and its phase transition temperature is 198 DEG C, and latent heat of phase change is
65.8J/g, density is 7.38g/cm3, thermal conductivity is 53.4W/ (m K), and the heat storage capacity of Sn-Zn eutectic alloy is 485.6J/cm3。
Its heat storage capacity is more than NaNO3/KNO3Heat storage capacity, therefore the hot physical performance of Sn-Zn eutectic alloy has great advantage.
Document 3 is reported with NaOH/KOH binary system as heat-storing material, carries out NaOH/KOH binary system heat storage performance
Research.(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 analyze the phenomenon such as melting and solidification of phase-change material, it is thus achieved that binary system forms phase
The influence curve figure of height, result shows, the phase transformation of this binary system includes solid-liquid phase change and solid-solid phase-change two parts；At NaOH
When weight/mass percentage composition is 23.4%, binary system has lowest total of the melting point to be 145.6 DEG C, increases along with NaOH content afterwards, two
Unit's system fusing point raises.
Document 4 reports with nitrate as heat accumulating phase change material, and expanded graphite strengthens and improves heat conductivility, (Peng Guowei. swollen
Swollen graphite/fuse salt composite shape-setting phase change heat storage material preparation and the research of hot property.[M] Lanzhou University of Science & Technology academic dissertation, 2012)
Obtain equimolar eutectic nitrate by differential thermal analysis test in temperature-rise period, have twice phase transition process, be once solid-
Gu change, its transition temperature is 117.5 DEG C, and phase transformation end temp is 132 DEG C, and latent heat of phase change is 33.34J/g, is once solid-liquid
Changing, its transition temperature is 219.5 DEG C, and phase transformation end temp is 227.5 DEG C, and latent heat of phase change is 116.6J/g, in operating temperature is
The equimolar nitrate of 400 DEG C of preparations, its thing phase composition is potassium nitrate and sodium nitrate, does not has novel substance to generate.
In the research of the heat-storing material in above-mentioned middle temperature field, the problem of alloy maximum is easily oxidation, causes its service life short,
Reliability is poor, and the low cost of fuse salt, and latent heat of phase change is high, but its bigger shortcoming be exist serious supercool and separated,
And there is serious corrosivity, the requirement to container is higher, and therefore in actual engineering, its performance degradation is relatively big, is difficult to protect
Demonstrate,prove its long term reliability.It is high that organic phase change material then has latent heat of phase change, supercool little, substantially without being separated.But its
Heat conductivity is little, needs in the application to add heat conduction phase medium to improve its heat conductivity.
Summary of the invention
The technical problem to be solved is: provide a kind of excellent performance and lower-cost industrial medium temperature phase-transition heat-storage material
Material and preparation method thereof.
The present invention solves its technical problem and uses following technical scheme:
A kind of industrial medium temperature phase change heat storage material, it is characterised in that described phase change heat storage material is by adipic acid, coppered carbon nanometer
Pipe and binding agent composition；Described adipic acid is 88～98:2～12 with the mass ratio of coppered carbon nanotube, the matter of described binding agent
Measure as the 3% of both adipic acid and coppered carbon nanotube gross mass.
In such scheme, the use temperature range of described phase change heat storage material is 120～200 DEG C.
In such scheme, described binding agent is sodium carboxymethyl cellulose.
The preparation method of a kind of industrial medium temperature phase change heat storage material, it is characterised in that it comprises the following steps:
1) getting the raw materials ready: choose adipic acid, coppered carbon nanotube and binding agent, described adipic acid with the mass ratio of coppered carbon nanotube is
88～98:2～12, the quality of described binding agent is the 3% of both adipic acid and coppered carbon nanotube gross mass；
2) by adipic acid, coppered carbon nanotube dried 24 hours, after adipic acid grinding is crossed 100 mesh sieves, with coppered carbon
Nanotube carries out mechanical mixture 15 minutes by preset blending ratio, loads in crucible, put into vacuum drying oven after mix homogeneously,
Melted absorption 6 hours at a temperature of 150～160 DEG C；
3) mix binding agent and carry out compression molding, i.e. obtain described industrial medium temperature phase change heat storage material.
In such scheme, described coppered carbon nanotube is to use following method to obtain:
1) first CNT is processed 30 minutes at a temperature of 400 DEG C, after then mixing with ethanol, carry out ultrasonic Treatment again
40 minutes；
2) in processed carbon nano tube surface copper facing, the technological parameter used during copper facing is: bath temperature: 80 ± 1 DEG C,
PH value: 12 ± 0.1, plating time: 0.5～5h.
In such scheme, the electroplate liquid formulation used during copper facing is: the chelating agent of copper sulfate, 1～5wt%, 1～the 3wt% of 1～10wt%
The reducing agent of the pH value regulator of stabilizer, 1～8wt%, 2～8wt% and the water of 75～94wt%.
In such scheme, described chelating agent is sodium hypophosphite.
In such scheme, described stabilizer is DMF.
In such scheme, described reducing agent be volumetric concentration be the formaldehyde of 36%.
In such scheme, described binding agent is sodium carboxymethyl cellulose.
In the present invention: the effect of copper sulfate is to provide copper ion, in chemical bronze plating liquid, mantoquita content is the highest, and plating speed is the fastest；?
During actual plating, after content increases to certain a certain amount, the increase of plating speed is inconspicuous.The effect of reducing agent formaldehyde is to carry
Supplied for electronic deposits copper to copper ion, so the capacity of water that reducing agent provides electronics has conclusive work to whole plating process
With.In general, the content the highest plating speed of formaldehyde is the fastest, but when the concentration of formaldehyde increases to certain degree, plating speed
Increase the most obvious.But the driving force of the too high offer of content of formaldehyde is excessive, can accelerate the selfdecomposition of plating solution, and plating rate is too fast,
Quality of coating can be affected.Chelating agent is that sodium hypophosphite is primarily used to control copper-plated speed, effect N, the N-diformazan of stabilizer
Base Methanamide is exactly the generation stoping solution selfdecomposition so that plating has the carrying out of control.The stabilizer stability to improving plating solution
General very effective, but the catalytic effect of electroless copper reaction is acted the effect strangled again by most stable agent, even can make reaction
Stop completely.The amount of general stabilizer controls the scope at about 10mg/L.Plating speed is had a great impact by stabilizer.
From above-mentioned it can be seen that during copper facing, every kind of material has feature and the effect of self, is to interact and restriction,
Final copper-plated performance is suffered from important impact.
The present invention compared with prior art has a following main advantage:
One, the innovation of the present invention are that using the adipic acid that latent heat of phase change is high, hot property is excellent is phase-change material, simultaneously
Utilize the heat conductivility of the reinforcing material of coppered carbon nano-tube material, use the method for vacuum fusion absorption to form phase-change material.
Two, the present invention provides a kind of heat-storing material with high latent heat of phase change, high heat conductance, enters the composition of this heat-storing material
Row optimizes design, it is achieved being greatly improved of its combination property.Wherein, introducing coppered carbon nano-tube material, itself has excellence
Performance, such as excellent conduction, heat conductivity, itself also there is abundant pore structure, there is good characterization of adsorption.
Three, and the conventional chelating agent (disodiumedetate (Na of current industrial copper facing2) and stabilizer (2,2 ' EDTA)
-bipyridyl) to compare, chelating agent and stabilizer employed in the present invention are the most cheap, as a example by stabilizer, 2,2 '-
The price existing market of bipyridyl is at 200,000/ton, and the market price of DMF is at 8000 yuan/ton, and several
Nontoxic, environmental pollution is little.Copper plate sedimentation rate prepared by the present invention is fast, and adhesive force is strong.
Four, at the copper coating of CNT, significantly improve the shortcoming of poor compatibility between material with carbon element and adipic acid material,
Improve their bond strength, thus improve heat conduction and heat transfer property.On the other hand CNT has stronger absorbability,
When heat-storing material generation solid-liquid phase change as the carrier of phase-change material, it is possible to effectively overcome the liquid phase substance in phase transition process to reveal
Problem.
Five, technique is simple, and the raw material that whole preparation process is selected is simple, takes full advantage of the feature of material, it is not necessary to too much
Change existing equipment just can be with Fast back-projection algorithm excellent performance and lower-cost modified heat-storing material.
In a word, present invention process is simple, easy to operate, it is not necessary to too much to change existing equipment, and prepared coppered carbon
The more unmodified material of performance of nano-tube material modification adipic acid heat-storing material greatly improves, and preparation cost is relatively low.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of coppered carbon nanotube.From the figure, it can be seen that the caliber of CNT is at about 40nm,
The thickness of copper plate is between 10～20nm, and copper plate is firmly attached to the surface of CNT.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
Embodiment 1
Adipic acid is chosen: 90%, coppered carbon nanotube 10% according to mass percent.Wherein adipic acid can directly be dried place
Managing 24 hours, first CNT processes 30 minutes at a temperature of 400 DEG C, carries out ultrasonic after then mixing with ethanol again
Ripple processes 40 minutes, then carries out copper coating, and after copper facing completes, dried i.e. obtained coppered carbon nanotube after 10 hours.
Technological parameter during copper facing is as follows:
Bath temperature: 80 ± 1 DEG C
PH value: 12 ± 0.1, adjusts with NaOH
Alr mode: magnetic agitation
Plating time: 0.5h.
Fig. 1 is the stereoscan photograph of coppered carbon nanotube.It will be noted from fig. 1 that the copper plate of carbon nano tube surface is tightly
It is attached to the surface of CNT.
Then, after adipic acid grinding is crossed 100 mesh sieves, carry out mechanical mixture 15 minutes with coppered carbon nanotube by preset blending ratio,
Load in crucible after mix homogeneously, put into vacuum drying oven, melted absorption 6 hours at a temperature of 150～160 DEG C.Become at tabletting
During type, mix outward the binding agent of 3%CMC.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 237.6J/g, and solidification heat release enthalpy is
220.5J/g, records at Hot Disc company 2500S type thermal constant analyser, and the thermal conductivity of composite phase change heat-accumulation material is 2.02
W/mK, specific heat capacity is 1.14J/gK.
It should be noted that the preset blending ratio of adipic acid and coppered carbon nanotube is mainly according to client heat storage performance and heat conductivity
The requirement of the comprehensive consideration of energy determines, by client root border requirements set factually.
Embodiment 2
Adipic acid is chosen: 92%, coppered carbon nanotube 8% according to mass percent.Wherein adipic acid can directly be dried process
24 hours, first CNT processed 30 minutes at a temperature of 400 DEG C, carries out at ultrasound wave after then mixing with ethanol again
Managing 40 minutes, then carry out copper coating (method same as in Example 1), after copper facing completes, dried after 10 hours and get final product
Coppered carbon nanotube.
Technological parameter during copper facing is as follows:
Bath temperature: 80 ± 1 DEG C
PH value: 12 ± 0.1, adjusts with NaOH
Alr mode: magnetic agitation
Plating time: 5h.
Then, after adipic acid grinding is crossed 100 mesh sieves, carry out mechanical mixture 15 minutes with coppered carbon nanotube by preset blending ratio,
Load in crucible after mix homogeneously, put into vacuum drying oven, melted absorption 6 hours at a temperature of 150～160 DEG C.Become at tabletting
During type, mix outward the binding agent of 3%CMC.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 239.6J/g, and solidification heat release enthalpy is
225.5J/g, records at Hot Disc company 2500S type thermal constant analyser, and the thermal conductivity of composite phase change heat-accumulation material is 1.91
W/mK, specific heat capacity is 1.21J/gK.
Embodiment 3
Adipic acid is chosen: 94%, coppered carbon nanotube 6% according to mass percent.Wherein adipic acid can directly be dried process
24 hours, first CNT processed 30 minutes at a temperature of 400 DEG C, carries out at ultrasound wave after then mixing with ethanol again
Managing 40 minutes, then carry out copper coating, after copper facing completes, dried i.e. obtained coppered carbon nanotube after 10 hours.
Technological parameter during copper facing is as follows:
Bath temperature: 80 ± 1 DEG C
PH value: 12 ± 0.1, adjusts with NaOH
Alr mode: magnetic agitation
Plating time: 3h.
Then, after adipic acid grinding is crossed 100 mesh sieves, carry out mechanical mixture 15 minutes with coppered carbon nanotube by preset blending ratio,
Load in crucible after mix homogeneously, put into vacuum drying oven, melted absorption 6 hours at a temperature of 150～160 DEG C.Become at tabletting
During type, mix outward the binding agent of 3%CMC.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 241.6J/g, and solidification heat release enthalpy is
229.5J/g, records at Hot Disc company 2500S type thermal constant analyser, and the thermal conductivity of composite phase change heat-accumulation material is 1.83
W/mK, specific heat capacity is 1.24J/gK.
Embodiment 4
Adipic acid is chosen: 96%, coppered carbon nanotube 4% according to mass percent.Wherein adipic acid can directly be dried process
24 hours, first CNT processed 30 minutes at a temperature of 400 DEG C, carries out at ultrasound wave after then mixing with ethanol again
Managing 40 minutes, then carry out copper coating (copper-plating technique same as in Example 1), after copper facing completes, dried 10 is little
Obtain coppered carbon nanotube time after, after adipic acid grinding is crossed 100 mesh sieves, carry out machinery with coppered carbon nanotube by preset blending ratio
Mixing 15 minutes, load in crucible, put into vacuum drying oven after mix homogeneously, at a temperature of 150～160 DEG C, melted absorption 6 is little
Time.When compression molding, mix outward the binding agent of 3%CMC.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 249.6J/g,
Solidification heat release enthalpy is 235.5J/g, records at Hot Disc company 2500S type thermal constant analyser, composite phase change heat-accumulation material
Thermal conductivity is 1.35W/mK, and specific heat capacity is 1.29J/gK.
Embodiment 5
Adipic acid is chosen: 98%, coppered carbon nanotube 2% according to mass percent.Wherein adipic acid can directly be dried process
24 hours, first CNT processed 30 minutes at a temperature of 400 DEG C, carries out at ultrasound wave after then mixing with ethanol again
Manage 40 minutes, then carry out copper coating (copper-plating technique same as in Example 2), copper facing complete after dried 10 hours
After i.e. obtain coppered carbon nanotube, after adipic acid grinding is crossed 100 mesh sieves, to carry out machinery by preset blending ratio mixed with coppered carbon nanotube
Close 15 minutes, load in crucible after mix homogeneously, put into vacuum drying oven, melted absorption 6 hours at a temperature of 150～160 DEG C.
When compression molding, mix outward the binding agent of 3%CMC.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 253.2J/g, solidification
Heat release enthalpy is 241.6J/g, records at Hot Disc company 2500S type thermal constant analyser, the thermal conductance of composite phase change heat-accumulation material
Rate is 0.85W/mK, and specific heat capacity is 1.31J/gK.
Embodiment 6
Adipic acid is chosen: 88%, coppered carbon nanotube 12% according to mass percent.Wherein adipic acid can directly be dried place
Managing 24 hours, first CNT processes 30 minutes at a temperature of 400 DEG C, carries out ultrasonic after then mixing with ethanol again
Ripple processes 40 minutes, then carries out copper coating (copper-plating technique same as in Example 3), copper facing complete after dried 10
I.e. obtain coppered carbon nanotube after hour, after adipic acid grinding is crossed 100 mesh sieves, carry out machine with coppered carbon nanotube by preset blending ratio
Tool mixes 15 minutes, loads in crucible, put into vacuum drying oven after mix homogeneously, melted absorption 6 at a temperature of 150～160 DEG C
Hour.When compression molding, mix outward the binding agent of 3%CMC.The fusing heat absorption enthalpy of composite phase change heat-accumulation material is 220.4J/g,
Solidification heat release enthalpy is 213.7J/g, records at Hot Disc company 2500S type thermal constant analyser, composite phase change heat-accumulation material
Thermal conductivity is 2.23W/mK, and specific heat capacity is 1.05J/gK.
Claims (7)
1. the preparation method of an industrial medium temperature phase change heat storage material, it is characterised in that it comprises the following steps:
1) getting the raw materials ready: choose adipic acid, coppered carbon nanotube and binding agent, described adipic acid is 88～98:2～12 with the mass ratio of coppered carbon nanotube, and the quality of described binding agent is the 3% of both adipic acid and coppered carbon nanotube gross mass；
2) by adipic acid, coppered carbon nanotube dried, after being sieved by adipic acid grinding, carry out mechanical mixture with coppered carbon nanotube by preset blending ratio, load in crucible after mix homogeneously, put into vacuum drying oven, melted absorption 6 hours at a temperature of 150 ~ 160 DEG C；
3) mix binding agent and carry out compression molding, i.e. obtain described industrial medium temperature phase change heat storage material.
2. preparation method as claimed in claim 1, it is characterised in that described coppered carbon nanotube is to use following method to obtain: 1) first CNT is processed 30 minutes at a temperature of 400 DEG C, carry out ultrasonic Treatment again 40 minutes after then mixing with ethanol；2) in processed carbon nano tube surface copper facing, the technological parameter used during copper facing is: bath temperature: 80 ± 1 DEG C, pH value: 12 ± 0.1, plating time: 0.5 ~ 5h.
3. preparation method as claimed in claim 2, it is characterized in that, the electroplate liquid formulation used during copper facing is: the copper sulfate of 1 ~ 10wt%, the chelating agent of 1 ~ 5wt%, the stabilizer of 1 ~ 3wt%, the pH value regulator of 1 ~ 8wt%, the reducing agent of 2 ~ 8wt% and the water of 75 ~ 94wt%.
4. preparation method as claimed in claim 3, it is characterised in that described chelating agent is sodium hypophosphite.
5. preparation method as claimed in claim 3, it is characterised in that described stabilizer is DMF.
6. preparation method as claimed in claim 3, it is characterised in that described reducing agent be volumetric concentration be the formaldehyde of 36%.
7. preparation method as claimed in claim 1, it is characterised in that described binding agent is sodium carboxymethyl cellulose.
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| CN104371664A (en) * | 2014-11-04 | 2015-02-25 | 镇江新梦溪能源科技有限公司 | Novel composite organic phase-change heat storage material and preparation method thereof |
| CN104559936B (en) * | 2014-12-19 | 2017-12-29 | 武汉理工大学 | A kind of medium temperature phase change heat storage material and preparation method thereof |
| CN106634856A (en) * | 2016-12-02 | 2017-05-10 | 中节能六合天融环保科技有限公司 | Two-gradient phase-change thermal storage material and preparation method thereof |
| 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 |
| CN111826128B (en) * | 2020-07-13 | 2021-10-22 | 黄冈师范学院 | Modified diatomite/adipic acid phase change heat storage material and preparation method thereof |
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