CN1465648A - Phase change energy storage composite material and preparation process thereof - Google Patents
Phase change energy storage composite material and preparation process thereof Download PDFInfo
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- CN1465648A CN1465648A CNA021121036A CN02112103A CN1465648A CN 1465648 A CN1465648 A CN 1465648A CN A021121036 A CNA021121036 A CN A021121036A CN 02112103 A CN02112103 A CN 02112103A CN 1465648 A CN1465648 A CN 1465648A
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Abstract
The composition of phase change energy-storing composite material includes 75-98% of inorganic aqueous crystal salt, 2-8% of hydrogel, the described hydrogel is selected from cross-linked starch-acrylonitrile copolymer, cross-linked sodium polyacrylate, sodium acrylate-acrylamine cross-linked copolymer, cellulose-sodium acrylate copolymer and their mixture, nd 0-20% of melting point regulating agent, and the described melting point regulating agent is selected from alkali metal halide, alkali earth metal halide and ammonium salt. Said invention also provides its preparation method.
Description
FIELD OF THE INVENTION
The present invention relates to a kind of matrix material, it has high heat storage efficiency and long repeated use life-span, also relates to the preparation method of this matrix material.
The background of invention
The energy storage material is widely used in fields such as food, medical treatment, health care.For example the energy storage material can be made the heat bag and be used for the treatment of sacroiliitis, cold compress, hot compress etc., the insulation that also can be used for medical use liquids such as medicine, blood stores.
The Chinese patent application CN 1034017A of Northwest University discloses a kind of human body temperature heat device, and its energy-storage travelling wave tube comprises basic metal and alkaline-earth metal inorganic salt and as the polyacrylic acid of thickening material.Earlier with the boiling water heating, utilize its thermal capacitance and heat of phase transformation energy storage during use; Use it for required purposes subsequently, the heat insulation that utilizes described inorganic salt phase transformation to send.This patent uses polyacrylic acid as thickening material, though the material of this patent disclosure has thermal storage and energy accumulation effect preferably, it can form supercooled liquid, influences its heating efficiency.
The Chinese patent CN1055947C of Institut Kataliza sibirskogo Otdelen. a Riossiiskei Akademit Nauk discloses a kind of heat-storing material, it comprises thermal lag matrix and thermo-sensitivity working medium, described thermal lag matrix is that particle diameter is the perforate particle of 1-5000 micron, for example silica gel.The thermo-sensitivity working medium is contained in the hole of thermal lag matrix, has eliminated working medium and has formed the defective of supercooled liquid, but improved the quality of heat-storing material.But also there are many parts that have much room for improvement in the disclosed thermal lag matrix of the document.For example silica gel is that main component is SiO
2And having a material of microvoid structure, its water-intake rate is less than 100%, thereby reduced the shared ratio of thermo-sensitivity working medium, and the energy storage effect of product is descended.In addition, silica gel has rigid-skeleton, swelling not after the absorption, and the intergranular space is big, and heat conductivility is relatively poor.
Therefore, need a kind of have thermal conductive resin and energy storage material efficiently.
The objective of the invention is to eliminate the defective of prior art, a kind of long energy storage matrix material in life-span and preparation method thereof that recycles that has is provided.
The general introduction of invention
The present invention relates to a kind of phase-change energy-storage composite material, it comprises:
The inorganic water-containing crystal salt of 75-98 weight %;
2-8 weight % hydrogel, it is 500-2 that described hydrogel is selected from water-intake rate, crosslinked starch-acrylonitrile copolymer of 000g/g, crosslinked sodium polyacrylate, sodium acrylate-acrylamide crosslinking copolymer, Mierocrystalline cellulose-sodium acrylate cross-linking copolymer, crosslinked polyacrylamide and composition thereof; With
0-20 weight % fusing point conditioning agent, described fusing point conditioning agent is selected from alkali metal halide, alkaline earth metal halide, ammonium salt.
Phase-change energy-storage composite material of the present invention also can randomly comprise the tensio-active agent of 0-5 weight % and the thermally conductive material of 0-10 weight %.
The invention still further relates to a kind of preparation method of described phase-change energy-storage composite material, it comprises the following steps:
1) the described inorganic water-containing crystal salt of heat fused;
2) add described hydrogel; With
3) ultrasonic dispersing it.
When matrix material of the present invention contains optional fusing point conditioning agent, tensio-active agent or thermal conducting agent, these additives can be added in the inorganic water-containing crystal salt of heat fused, make it homodisperse with ultrasonic wave, in this dispersion, add described hydrogel again.
The detailed description of invention
The present invention relates to a kind of phase-change energy-storage composite material that comprises inorganic water-containing crystal salt, hydrogel.
Inorganic water-containing crystal salt as the thermo-sensitivity working medium in the matrix material of the present invention is without particular limitation, as long as it can be by phase transformation absorption or release of heat.Be applicable to that inorganic water-containing crystal salt of the present invention is well-known in the art, inorganic preferably water-containing crystal salt be noncorrosive, do not pollute the environment and have high heat of phase transformation.The example of inorganic water-containing crystal salt commonly used has Na
2SO
410H
2O, Na
2CO
310H
2O, CaCl
26H
2O, ZnCl
22.5H
2O, KF4H
2O, LiNO
3/ Mg (NO
3)
26H
2O, Na
3PO
412H
2O, Na
2B
4O
710H
2O, MgAc
24H
2O, NaAC3H
2O, Mg (NO
3) 4H
2O, MgI
28H
2O, KF4H
2O, NaClNa
2SO
410H
2O, NH
4ClNa
2SO
410H
2O, Ca (NO
3)
24H
2O, Na (NO
3)
26H
2O, Al (NO
3)
39H
2O, NaAl (SO
4)
212H
2O, Zn (NO
3)
24H
2O, Zn (NO
3)
26H
2O, Mn (NO
3)
24H
2O, Mn (NO
3)
26H
2O, K
3PO
47H
2O and K
2HPO
43H
2O etc.
In the matrix material of the present invention, the content of inorganic water-containing crystal salt is without particular limitation, and it depends on required purposes.If but content is too low, then the energy storage DeGrain if content is too high, then is difficult to whole crystal are contained in the copolymer networks.The content of inorganic water-containing crystal salt is preferably 75-98 weight % in matrix material of the present invention; 80-95 weight % more preferably; Be preferably 88-92 weight %.
Use hydrogel as thermal lag matrix in the matrix material of the present invention.Be meant in water can swelling and keep large quantity of moisture and don't dissolved cross-linked polymer compound for term " hydrogel " in this article, and this hydrogel has network structure.
Be applicable to that hydrogel of the present invention is without particular limitation, as long as its water-intake rate greater than 500g/g, is preferably 500-2,000g/g gets final product.
Water-intake rate is the yardstick of hydrogel adsorptive capacity, and in general, water-intake rate is high more, and then adsorptive capacity is big more.The water-intake rate of resin is measured with methods known in the art.This measuring method can be referring to Yan Hui, Zhang Lihua, Zhou Xiumiao. use chemical industry, 30 (2) 2001:38.
Water-intake rate is 500-2, thereby this hydrogel of 000g/g has enough big hole hydrophilic small molecules can be spread therein.The illustrative example of described hydrogel comprises crosslinked starch-acrylonitrile copolymer, crosslinked sodium polyacrylate, sodium acrylate-acrylamide crosslinking copolymer, Mierocrystalline cellulose-sodium acrylate cross-linking copolymer, crosslinked polyacrylamide and composition thereof.
In matrix material of the present invention, the consumption of hydrogel is without particular limitation, depends on the consumption of described temperature-sensitive working medium.In general, the content of hydrogel is 2-8 weight %, is preferably 3-6 weight %, more preferably 4-5 weight %.
The hydrogel that uses in the matrix material of the present invention is commercially available.For example; described crosslinked starch-acrylonitrile copolymer can be available from Shanghai Ritz-Carlton chemical industry company limited (water-intake rate be 600g/g); described crosslinked sodium polyacrylate can be available from the lucky first chemical industry company limited (water-intake rate is 500g/g) in Shanghai; described sodium acrylate-acrylamide crosslinking copolymer can fly clean scientific ﹠ technical corporation (water-intake rate is 800g/g) available from Jiangxi; described Mierocrystalline cellulose-sodium acrylate cross-linking copolymer can be available from Shanghai Ritz-Carlton chemical industry company limited (water-intake rate be 600g/g), and described crosslinked polyacrylamide can be available from Hufeng Biological Science and Technology Co., Ltd., Shanghai (water-intake rate be 800g/g).
Also can contain the fusing point conditioning agent so that regulate the transformation temperature of material as required in the matrix material of the present invention.The consumption of this fusing point conditioning agent is generally 0-20 weight %, is preferably 5-15 weight %, more preferably 8-12 weight %.
The illustrative example of fusing point conditioning agent comprises alkali metal halide, as Potassium monofluoride, Sodium Fluoride, Repone K, sodium-chlor, Potassium Bromide, Sodium Bromide; Alkaline earth metal halide is as magnesium chloride, magnesium bromide, calcium chloride, Calcium Bromide etc.; Ammonium salt such as Neutral ammonium fluoride, ammonium chloride, brometo de amonio, ammonium sulfate, ammonium nitrate etc.
Phase-change energy-storage composite material of the present invention also can randomly contain conventional additives, and for example tensio-active agent, thermally conductive material etc. are so that further improve described performance of composites.
The effect of tensio-active agent is to prevent that inorganic water-containing crystal salt from luming in accumulation of heat-heat release working cycle.The tensio-active agent that is applicable to matrix material of the present invention is this area tensio-active agent commonly used, and its illustrative example comprises alkyl trimethyl ammonium salt, thanomin, lignin carbonate, silicone surfactant etc.The consumption of tensio-active agent is without particular limitation, is generally 0-5 weight %.
Also can use thermally conductive material to improve the heat conductivility of material in the matrix material of the present invention, improve the accumulation of heat effect.The example of suitable thermally conductive material has metal-powder, as silver powder, copper powder, aluminium powder, expanded graphite powder etc.For the consideration of controlling cost, aluminium powder is preferably.The particle diameter of thermally conductive material is generally less than 0.5 micron.The content of thermally conductive material is without particular limitation in the matrix material of the present invention, as long as can reach the purpose that improves heat conduction efficiency.The content of thermally conductive material is generally 0-10 weight %.
The invention still further relates to a kind of preparation method of described phase-change energy-storage composite material, it comprises the following steps:
1) the described inorganic water-containing crystal salt of heat fused;
2) add described hydrogel; With
3) ultrasonic dispersing it.
At one preferably in the example of the present invention, earlier a certain amount of inorganic water-containing crystal salt is placed container, slowly heating makes it whole fusings, in the inorganic salt of this fusing, add fusing point conditioning agent, tensio-active agent and thermally conductive material powder, make it to be evenly dispersed in the described inorganic salt melt with ultrasonic wave, add hydrogel subsequently while stirring, after reinforced the finishing, constant temperature stirred one hour under the inorganic salt temperature of fusion.
During use, can earlier phase-change energy-storage composite material be placed container, utilize resistance wire or external heat source heating phase-change energy-storage composite material, make it temperature and be higher than 1～5 ℃ of transformation temperature, inorganic water-containing crystal salt absorbs heat energy and all fusings.Then this container is placed the system that needs insulation, when the temperature of system reached or is lower than phase point temperature, inorganic salt crystallization (solidifying) discharged heat energy, and system temperature was remained within the scope of requirement in the long time.Repeat aforesaid operations, phase-change energy-storage composite material can be recycled.
Further specify the present invention below by embodiment.
Test method
Stability test
500 gram samples are placed reaction vessel, melt-solidify round-robin test, circulate after 100 times, with following its thermo-efficiency of thermo-efficiency determination of test method, greater than 95%, it is qualified then to be considered as stability test as if the thermo-efficiency conservation rate.
Endurance test
500 gram samples are placed reaction vessel, melt-solidify round-robin test, circulate after 200 times, the sample that detects by an unaided eye has or not separates out phenomenon and produces, and nothing is separated out phenomenon, and then to be considered as endurance test qualified.
The thermo-efficiency test
Utilize differential thermal analyzer (CDR-1 type, Shanghai balance equipment factory system) to measure the heat of phase transformation (Δ H) of sample, melt-solidify circulation primary after, its thermo-efficiency conservation rate is: (Δ H
1/ Δ H
0) * 100%, Δ H
0For melting-solidify the heat of phase transformation of sample after the circulation primary, Δ H
0For there not being the heat of phase transformation of circulation time sample.
Embodiment 1
With 75 gram Na
2CO
310H
2O (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai) places reaction vessel, slowly is heated to 32 ℃ with hot plate and makes it whole fusings.Slowly add 10 gram sodium-chlor subsequently, 3 gram silicone surfactants (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai), 4 gram particles directly are the copper powder of 50nm.The ultrasonic wave (frequency 40KHz) that produces with KQ-1500B ultrasonic generator (available from Kunshan Ultrasonic Instruments Co., Ltd.) made it homodisperse 30 minutes.Add 8 gram cross-linking starch-acrylonitrile copolymers (available from Shanghai Ritz-Carlton chemical industry company limited, water-intake rate is 600g/g) subsequently while stirring, stirred 1 hour at 30 ℃ of constant temperature after reinforced the finishing, obtain cotton-shaped matrix material.
With above-mentioned test method the matrix material that makes is tested, be the results are shown in table 1.
Comparative example 1
Repeat the step of embodiment 1, but replace cross-linking starch-acrylonitrile copolymer with silica gel.With above-mentioned test method the matrix material that makes is tested, be the results are shown in table 1.
By test-results as seen, sample can not all adsorb, be filled in the hole of silica gel, and the inside and outside residing environment difference of sample of hole after 100 circulations, produces and separates out phenomenon, and the thermo-efficiency conservation rate is lower than 90%.
Embodiment 2
With 98 gram Na
2SO
410H
2O (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai) places reaction vessel, slowly is heated to 32 ℃ with hot plate and makes it whole fusings.Add the crosslinked sodium polyacrylate of 2 grams (available from the Shanghai first chemical industry of Ji company limited, water-intake rate is 500g/g) subsequently while stirring, stirred 1 hour at 32 ℃ of constant temperature after reinforced the finishing, obtain cotton-shaped matrix material.
With above-mentioned test method the matrix material that makes is tested, be the results are shown in table 1.
Embodiment 3
With 80 gram CaCl
26H
2O (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai) places reaction vessel, slowly is heated to 30 ℃ with gaslight and makes it whole fusings.Slowly add 5 gram magnesium bromides subsequently, 5 gram silicone surfactants, 4 gram particles directly are the aluminium powder of 53nm.The ultrasonic wave (frequency 40KHz) that produces with the KQ-1500B ultrasonic generator made it homodisperse 30 minutes.Add the crosslinked polyacrylamide (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai, water-intake rate is 800g/g) of 6 grams subsequently while stirring, stirred 1 hour at 30 ℃ of constant temperature after reinforced the finishing, obtain cotton-shaped matrix material.
With above-mentioned test method the matrix material that makes is tested, be the results are shown in table 1.
Embodiment 4
With 95 gram KF
44H
2O (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai) places reaction vessel, slowly is heated to 19 ℃ with hot plate and makes it whole fusings.Slowly add 1 gram Repone K, 1 gram particle subsequently and directly be the expanded graphite powder of 53nm.The ultrasonic wave (frequency 40KHz) that produces with the KQ-1500B ultrasonic generator made it homodisperse 30 minutes.Add 3 gram sodium acrylate-acrylamide crosslinking copolymers (fly clean scientific ﹠ technical corporation available from Jiangxi, water-intake rate is 800g/g) subsequently while stirring, stirred 1 hour at 19 ℃ of constant temperature after reinforced the finishing, obtain cotton-shaped matrix material.
With above-mentioned test method the matrix material that makes is tested, be the results are shown in table 1.
Embodiment 5
With 1: 1 LiNO of 75 grams
3/ Mg (NO
3)
26H
2O (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai) places reaction vessel, slowly is heated to 30 ℃ with hot plate and makes it whole fusings.Slowly add 17 gram magnesium bromides subsequently, 1 gram silicone surfactant, 1 gram particle directly is the aluminium powder of 53nm.The ultrasonic wave (frequency 40KHz) that produces with the KQ-1500B ultrasonic generator made it homodisperse 30 minutes.Add the crosslinked polyacrylamide (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai, water-intake rate is 800g/g) of 6 grams subsequently while stirring, stirred 1 hour at 30 ℃ of constant temperature after reinforced the finishing, obtain cotton-shaped matrix material.
With above-mentioned test method the matrix material that makes is tested, be the results are shown in table 1.
Embodiment 6
With 88 gram ZnCl
22.5H
2O (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai) places reaction vessel, slowly is heated to 13 ℃ with hot plate and makes it whole fusings.Slowly add 4 gram ammonium sulfate, 3 gram thanomin tensio-active agents subsequently.The ultrasonic wave (frequency 40KHz) that produces with the KQ-1500B ultrasonic generator made it homodisperse 30 minutes.Add the crosslinked polyacrylamide (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai, water-intake rate is 800g/g) of 5 grams subsequently while stirring, stirred 1 hour at 13 ℃ of constant temperature after reinforced the finishing, obtain cotton-shaped matrix material.
With above-mentioned test method the matrix material that makes is tested, be the results are shown in table 1.
Embodiment 7
With 92 gram Na
2HPO
412H
2O (available from Hufeng Biological Science and Technology Co., Ltd., Shanghai) places reaction vessel, slowly is heated to 40 ℃ with hot plate and makes it whole fusings.Slowly add 2 gram Calcium Bromides, 1 gram chlorination oxypropyl trimethyl ammonium surfactant, 1 gram particle subsequently and directly be the silver powder of 53nm.The ultrasonic wave (frequency 40KHz) that produces with the KQ-1500B ultrasonic generator made it homodisperse 30 minutes.Add 4 gram Mierocrystalline cellulose-sodium acrylate cross-linking copolymers (available from Shanghai Ritz-Carlton chemical industry company limited, water-intake rate is 600g/g) subsequently while stirring, stirred 1 hour at 40 ℃ of constant temperature after reinforced the finishing, obtain cotton-shaped matrix material.
With above-mentioned test method the matrix material that makes is tested, be the results are shown in table 1.
Table 1
| Stability test n=100 | Endurance test n=200 | Thermo-efficiency n=1 | |
| Embodiment 1 | Qualified | Nothing is separated out | ????100％ |
| Comparative example 1 | Defective | Separate out | ????99.2％ |
| Embodiment 2 | Qualified | Nothing is separated out | ????100％ |
| Embodiment 3 | Qualified | Nothing is separated out | ????100％ |
| Embodiment 4 | Qualified | Nothing is separated out | ????100％ |
| Embodiment 5 | Qualified | Nothing is separated out | ????100％ |
| Embodiment 6 | Qualified | Nothing is separated out | ????100％ |
| Embodiment 7 | Qualified | Nothing is separated out | ????100％ |
By last table result as seen, energy storage matrix material of the present invention has the long life-span that recycles.Compare with the matrix material of existing silica matrix, stability and thermo-efficiency conservation rate height, long service life circulates 200 times the time, and sample does not still have the phenomenon of separating out and produces.
Claims (10)
1. phase-change energy-storage composite material, it comprises:
The inorganic water-containing crystal salt of 75-98 weight %;
2-8 weight % hydrogel, it is 500-2 that described hydrogel is selected from water-intake rate, crosslinked starch-acrylonitrile copolymer of 000g/g, crosslinked sodium polyacrylate, sodium acrylate-acrylamide crosslinking copolymer, Mierocrystalline cellulose-sodium acrylate cross-linking copolymer, crosslinked polyacrylamide and composition thereof; With
0-20 weight % fusing point conditioning agent, described fusing point conditioning agent is selected from alkali metal halide, alkaline earth metal halide, ammonium salt.
2. matrix material as claimed in claim 1 is characterized in that it also comprises the tensio-active agent of 0-5 weight % and the thermally conductive material of 0-10 weight %.
3. as any one described matrix material among the claim 1-2, it is characterized in that described inorganic water-containing crystal salt is selected from Na
2SO
410H
2O, Na
2CO
310H
2O, CaCl
26H
2O, ZnCl
22.5H
2O, KF4H
2O, LiNO
3/ Mg (NO
3)
26H
2O, Na
3PO
412H
2O, Na
2B
4O
710H
2O, MgAc
24H
2O, NaAC3H
2O, Mg (NO
3) 4H
2O, MgI
28H
2O, KF4H
2O, NaClNa
2SO
410H
2O, NH
4ClNa
2SO
410H
2O, Ca (NO
3)
24H
2O, Na (NO
3)
26H
2O, Al (NO
3)
39H
2O, NaAl (SO
4)
212H
2O, Zn (NO
3)
24H
2O, Zn (NO
3)
26H
2O, Mn (NO
3)
24H
2O, Mn (NO
3)
26H
2O, K
3PO
47H
2O and K
2HPO
43H
2O.
4. as any one described matrix material among the claim 1-2, the content that it is characterized in that described inorganic water-containing crystal salt is 80-95 weight %, is preferably 88-92 weight %.
5. as any one described matrix material among the claim 1-2, the content that it is characterized in that described hydrogel is 3-6 weight %, is preferably 4-5 weight %.
6. as any one described matrix material among the claim 1-2, the content that it is characterized in that described fusing point conditioning agent is 5-15 weight %, is preferably 8-12 weight %.
7. one kind as the preparation method of phase-change energy-storage composite material as described in any one among the claim 1-6, and it comprises the following steps:
1) the inorganic water-containing crystal salt of heat fused;
2) add hydrogel, it is 500-2 that described hydrogel is selected from water-intake rate, crosslinked starch-acrylonitrile copolymer of 000g/g, crosslinked sodium polyacrylate, sodium acrylate-acrylamide crosslinking copolymer, Mierocrystalline cellulose-sodium acrylate cross-linking copolymer, crosslinked polyacrylamide and composition thereof.
8. method as claimed in claim 7, it is characterized in that still it also comprises adding fusing point conditioning agent before in step (2) afterwards in step (1), and the fusing point conditioning agent being dispersed in step in the inorganic water-containing crystal salt of fusing with ultrasonic wave, described fusing point conditioning agent is selected from alkali metal halide, alkaline earth metal halide, ammonium salt.
9. method as claimed in claim 8 is characterized in that also adding tensio-active agent and thermal conducting agent when adding the fusing point conditioning agent.
10. as any one described method among the claim 7-9, it is characterized in that described inorganic water-containing crystal salt is selected from Na
2SO
410H
2O, Na
2CO
310H
2O, CaCl
26H
2O, ZnCl
22.5H
2O, KF4H
2O, LiNO
3/ Mg (NO
3)
26H
2O, Na
3PO
412H
2O, Na
2B
4O
7L0H
2O, MgAc
24H
2O, NaAC3H
2O, Mg (NO
3) 4H
2O, MgI
28H
2O, KF4H
2O, NaClNa
2SO
410H
2O, NH
4ClNa
2SO
410H
2O, Ca (NO
3)
24H
2O, Na (NO
3)
26H
2O, Al (NO
3)
39H
2O, NaAl (SO
4)
212H
2O, Zn (NO
3)
24H
2O, Zn (NO
3)
26H
2O, Mn (NO
3)
24H
2O, Mn (NO
3)
26H
2O, K
3PO
47H
2O and K
2HPO
43H
2O.
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