CN102531550B - Poly fatty acid shape-stabilized phase change material and preparation method thereof - Google Patents
Poly fatty acid shape-stabilized phase change material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a poly fatty acid shape-stabilized phase change material and a preparation method thereof. The shape-stabilized phase change material is composited with the following raw materials: 30-60% of poly fatty acid eutectic mixture and 40-70% of mud ceramsite. The preparation method comprises the following steps: vaccumizing the mud ceramsite for 30-100 minutes at a temperature higher than the phase change point of the poly fatty acid eutectic mixture, and adding melted poly fatty acid; increasing the pressure to the normal pressure to allow the liquid poly fatty acid to gradually permeate into the mud ceramsite, and cooling to obtain the poly fatty acid/mud ceramsite shape-stabilized phase change material. The preparation method is simple, and the obtained phase change material has relatively low phase change temperature, and is suitable for room temperature conditioning of civil buildings.
Description
Technical field
The present invention relates to a kind of polyhydric aliphatic acid cut shape phase change material and preparation method thereof, belong to building energy conservation and heat accumulating field.
Background technology
Along with increasingly sharpening of world energy sources crisis, people more and more pay close attention to effective utilization of the energy.Phase change material is a kind of material that can change its physical condition and absorption or discharge large energy in certain temperature range.Solid-liquid phase change material for example, when envrionment temperature is higher than its transformation temperature, it will be liquid from solid state transformation, absorb simultaneously and store a large amount of latent heat; And when envrionment temperature reduced again, phase change material carried out again from liquid state to solid-state reverse transformation, and the heat that stores is discharged in the environment again went.When the physical condition variation occured so repeatedly, the phase change material self-characteristic was almost constant, but envrionment temperature can be maintained in certain scope, reduced calorific loss, the utilization ratio of the Effective Raise energy.
Lipid acid is as non-paraffin class organic phase change material, because it has the advantages such as high melting enthalpy, nonflammable, thermostability that the phase transition process cubical expansivity is little and good and chemical stability, is being used widely aspect building energy conservation and the daily life.But the fusing point of most of lipid acid is higher than the temperature requirement scope of applied environment, therefore usually needs to replace single lipid acid to satisfy the applied environment requirement with binary or Diversity lipid acid.Schroeder's formula is the effective ways commonly used of determining the minimum eutectic proportioning of binary compound fat acid, but the above compound fat acid of ternary and ternary proportioning really rule needs a large amount of experiments, filters out suitable polyhydric aliphatic acid phase change material by the character of measuring product under the different proportionings.
Shaping phase-change material is normally combined by phase change material and various porous material, utilize the fine porosity of porous medium inside that phase change material is dispersed into small-particle to store, improve the stability that phase change material stores by capillary effect in porous medium, and then can keep certain shape when phase change material is undergone phase transition, leakage phenomenon can not appear.Utilize simultaneously the high characteristics of Heat Conduction in Porous Media rate can also improve the heat exchange efficiency of phase change material.Compare with common phase change material, shaping phase-change material has the advantages such as packaging cost is low, and heat transfer resistance is little, is difficult for leaking, and use is safe.
Chinese patent file CN101838521A (application number 201010169075.4) discloses a kind of take bentonite as matrix, take the preparation method of binary of fatty acids as the composite phase-change energy storage material of phase-change accumulation energy main body, the method is at first carried out modification to bentonite, then prepare the binary of fatty acids eutectic mixture with myristic acid and palmitinic acid or with lauric acid and myristic acid, at last modified montmorillonite, binary of fatty acids and dehydrated alcohol are mixed, heat, stir, are dried to constant weight, namely get binary of fatty acids/bentonite composite phase-change material.The transformation temperature of this composite phase-change material is higher, when especially preparing the binary of fatty acids eutectic system with lauric acid and myristic acid, the transformation temperature of final gained composite phase-change material is restricted the application of binary of fatty acids/bentonite composite phase-change material up to 36 ℃.
Summary of the invention
For the deficiencies in the prior art, the invention provides lower polyhydric aliphatic acid cut shape phase change material of a kind of transformation temperature and preparation method thereof.
Technical scheme of the present invention is as follows:
A kind of shaping phase-change material is composited by following weight percent by polyhydric aliphatic acid and sludge ceramsite: polyhydric aliphatic acid eutectic mixture 30%~60%; Sludge ceramsite 40%~70%;
Described polyhydric aliphatic acid eutectic mixture is the eutectic mixture more than three kinds or three kinds in capric acid, lauric acid, myristic acid, palmitinic acid, the stearic acid; Described sludge ceramsite be mud after clay and the sewage work's mummification as raw material, by clay: the mud after the mummification=(8.8~9.2): (1.2~0.8) mass ratio mixing, granulation, under 920~970 ℃, fire and form.
Preferred according to the present invention, described polyhydric aliphatic acid is capric acid/lauric acid/myristic acid ternary eutectic mixture, or lauric acid/myristic acid/stearic acid ternary eutectic mixture, or capric acid/lauric acid/stearic acid ternary eutectic mixture, lauric acid/myristic acid/palmitinic acid/stearic acid quaternary eutectic mixture.
The preparation method of shaping phase-change material of the present invention, step is as follows:
Sludge ceramsite is vacuumized 30~100 minutes under the temperature that is higher than 10~20 ℃ of polyhydric aliphatic acid eutectic mixture transformation temperatures, vacuum tightness is 0.08~0.10MPa; The polyhydric aliphatic acid eutectic mixture that adds fusing; Rise to normal pressure, liquid polyhydric aliphatic acid eutectic mixture is infiltrated in the sludge ceramsite gradually, the absorption infiltration time is 60~150 minutes; Cooling namely gets polyhydric aliphatic acid/sludge ceramsite shaping phase-change material.
Polyhydric aliphatic acid eutectic mixture and sludge ceramsite all can prepare by prior art in the above-mentioned raw materials.The preferred following preparation method of the present invention:
(1) preparation of polyhydric aliphatic acid:
A. according to by Schroeder's formula
The proportioning of the binary of fatty acids eutectic mixture that calculates is the optional two kinds of mixing in capric acid, lauric acid, myristic acid, palmitinic acid, the stearic acid, and fusing point higher in both is as benchmark T
0, at T
0+ 10 ℃~T
0Mixture heating up with these two kinds of lipid acid under+20 ℃ the water bath condition stirred 30~60 minutes, obtained the binary of fatty acids eutectic mixture after ultrasonic 2~5 minutes;
B. measure transformation temperature and the corresponding enthalpy of gained binary of fatty acids eutectic mixture, and calculate its theoretical molecular mass according to mixing match; This binary of fatty acids eutectic mixture is mixed with the third lipid acid according to Schroeder's formula as single fat acid, and method obtains ternary aliphatic acid eutectic mixture as described in the step a; By that analogy, mixed by ternary aliphatic acid eutectic mixture and the 4th kind of lipid acid, can obtain quaternary lipid acid eutectic mixture, by that analogy, and then get polyhydric aliphatic acid eutectic mixture.
First number of polyhydric aliphatic acid is more, and gained eutectic mixture fusing point is lower, decides according to the environment for use temperature; Consider preparation technology's complicacy and the suitability of eutectic mixture fusing point, generally be preferably binary, ternary, quaternary lipid acid eutectic mixture.Ternary aliphatic acid eutectic mixture particularly preferably.
[2] preparation of sludge ceramsite: the clay after will drying and the mud after the mummification are by (8.8~9.2): (1.2~0.8) mass ratio mixes mixing, by the prior art granulation, at 920~970 ℃ of lower sintering, sieve, make the sludge ceramsite that particle diameter is 5~8mm.
According to the present invention, preferred scheme is as follows:
Preferred scheme one,
(1) the best mixing quality ratio that calculates myristic acid and stearic acid binary of fatty acids according to Schroeder's formula is 72.66% and 27.34%, myristic acid and stearic acid are mixed by this proportioning, mixture heating up with these two kinds of lipid acid under 85 ℃ of water bath condition stirred 50 minutes, after ultrasonic 3 minutes myristic acid/stearic acid binary eutectic mixture; Measuring myristic acid/stearic binary eutectic mixture transformation temperature is 47.55 ℃, and latent heat of phase change is 182.3J/g, and calculating its theoretical molecular mass is 241.39; Regard this binary of fatty acids eutectic mixture as single lipid acid, then carry out compoundly with lauric acid that calculate as can be known according to Schroeder's formula, binary of fatty acids eutectic mixture and lauric best mixing quality ratio are 49% and 51%; After this proportioning mixing, be heated under 65 ℃ of water bath condition and stirred 50 minutes, get lauric acid/myristic acid/stearic acid ternary eutectic mixture after ultrasonic 3 minutes.
(2) with clay: the sludge ceramsite of mud=9: 1 mass ratio vacuumizes 40 minutes under 50 ℃, vacuum tightness is 0.098MPa; Lauric acid/myristic acid that adding has been melted/stearic acid ternary eutectic mixture; Rise to normal pressure, the ternary eutectic mixture infiltrated sludge ceramsite 120 minutes; Cooling namely gets ternary aliphatic acid/sludge ceramsite shaping phase-change material.
Preferred scheme two,
(1) the best mixing quality ratio that calculates lauric acid and myristic acid according to Schroeder's formula is 65.08%: 34.92%, lauric acid and myristic acid are mixed by this proportioning, mixture heating up with these two kinds of lipid acid under 65 ℃ of water bath condition stirred 60 minutes, after ultrasonic 2 minutes lauric acid/myristic acid binary eutectic mixture; The binary eutectic mixture transformation temperature of measuring lauric acid/myristic acid is 35.10 ℃, and latent heat of phase change is 210.2J/g, and calculating its theoretical molecular mass is 209.30; Regard this binary of fatty acids eutectic mixture as single lipid acid, then carry out compoundly with capric acid that calculate as can be known according to Schroeder's formula, the best mixing quality ratio of binary of fatty acids eutectic mixture and capric acid is 47.6%: 52.4%; After this proportioning mixing, be heated under 50 ℃ of water bath condition and stirred 60 minutes, get capric acid/lauric acid/myristic acid ternary eutectic mixture after ultrasonic 2 minutes.
(2) with clay: the sludge ceramsite of mud=8.9: 1.1 mass ratio vacuumizes 50 minutes under 40 ℃, vacuum tightness is 0.095MPa; Capric acid/lauric acid that adding has been melted/myristic acid ternary eutectic mixture; Rise to normal pressure, the ternary eutectic mixture infiltrated sludge ceramsite 100 minutes; Cooling namely gets ternary aliphatic acid/sludge ceramsite shaping phase-change material.
Compare with technology with currently available products, advantage of the present invention is:
1, the present invention is take sludge ceramsite as porous matrix, prepare shaping phase-change material take polyhydric aliphatic acid eutectic as the phase-change accumulation energy main body, the phase change material that provides, its transformation temperature scope is at 15~34 ℃, concrete transformation temperature can be controlled by kind and the proportioning of lipid acid, and the room temperature that is applicable to covil construction is regulated.Can reduce the air-conditioning power consumption summer, stores the sunlight heat daytime in winter, discharges the heat that stores evening, saves the heating system energy consumption.
2, the proportioning of polyhydric aliphatic acid eutectic mixture provided by the present invention is determined method, easily and effectively, need not to carry out great many of experiments and screens one by one, saves production cost.According to the synthetic binary of fatty acids eutectic of Schroeder's formula, measure its transformation temperature and latent heat of phase change first, calculate its theoretical molecular mass; Then the binary of fatty acids eutectic is regarded as single fat acid, with the third lipid acid according to Schroeder's formula synthesis of ternary lipid acid eutectic, and then polyhydric aliphatic acid eutectic.
3, the present invention is take sludge ceramsite as porous matrix, can utilize in a large number mud, promoted on the one hand the changing waste into resources of sludge of sewage treatment plant, the ingenious high porosity characteristic of having utilized sludge ceramsite on the other hand, increase the adsorptive capacity of phase change material in porous matrix, improved the energy-saving efficiency of unit volume shaping phase-change material.
Embodiment
The present invention will be further described below in conjunction with embodiment.Used sludge ceramsite is clay among the embodiment: mud=(8.8~9.2): (1.2~0.8) quality makes at 970 ℃ of lower sintering than mixing granulation, and particle diameter is 5~8mm.
The compound proportioning of the binary of lipid acid can directly be determined according to Schroeder's formula among the embodiment, and concrete equation is as follows:
X
A+X
B=1
Δ H wherein
AWith Δ H
BBe respectively the mole melting enthalpy of A, two kinds of lipid acid of B; T
AAnd T
BBe respectively the fusing point of A, two kinds of lipid acid of B; T is the eutectic point of A, two kinds of lipid acid of B; X
AAnd X
BWhen being respectively A, two kinds of lipid acid congruent meltings of B in mixture shared mol ratio.
Embodiment 1,
(1) calculates myristic acid according to Schroeder's formula and stearic best mixing quality ratio is 72.66%: 27.34%, myristic acid and stearic acid are mixed by this proportioning, mixture heating up with these two kinds of lipid acid under 85 ℃ of water bath condition stirred 50 minutes, after ultrasonic 3 minutes myristic acid/stearic acid binary eutectic mixture.
(2) with determine with dsc method myristic acid/stearic binary eutectic mixture, transformation temperature is 47.55 ℃, and latent heat of phase change is 182.3J/g, and calculating its theoretical molecular mass is 241.39; Regard this binary of fatty acids eutectic mixture as single lipid acid, then carry out compoundly with lauric acid that calculate as can be known according to Schroeder's formula, binary of fatty acids eutectic mixture and lauric best mixing quality ratio are 49%/51%; After this proportioning mixing, be heated under 65 ℃ of water bath condition and stirred 50 minutes, get lauric acid/myristic acid/stearic acid ternary eutectic mixture after ultrasonic 3 minutes, its transformation temperature is 31.47 ℃, latent heat of phase change is 171.2J/g.
(3) with clay: the sludge ceramsite of mud=9: 1 mass ratio vacuumizes 40 minutes under 50 ℃, vacuum tightness is 0.098MPa; Lauric acid/myristic acid that adding has been melted/stearic acid ternary eutectic mixture; System is risen to normal pressure, and the ternary eutectic mixture infiltrated sludge ceramsite 120 minutes; Cooling namely gets ternary aliphatic acid/sludge ceramsite shaping phase-change material.Use determine with dsc method, its transformation temperature is 31.53 ℃, and latent heat of phase change is 59.05J/g.
Embodiment 2,
(1) the mixing quality ratio that calculates lauric acid and myristic acid according to Schroeder's formula is 65.08%: 34.92%, lauric acid and myristic acid are mixed by this proportioning, mixture heating up with these two kinds of lipid acid under 65 ℃ of water bath condition stirred 60 minutes, after ultrasonic 2 minutes lauric acid/myristic acid binary eutectic mixture.
(2) with the binary eutectic mixture of determine with dsc method lauric acid/myristic acid, transformation temperature is 35.10 ℃, and latent heat of phase change is 210.2J/g, and calculating its theoretical molecular mass is 209.30; Regard this binary of fatty acids eutectic mixture as single lipid acid, then carry out compoundly with capric acid that calculate as can be known according to Schroeder's formula, the best mixing quality ratio of binary of fatty acids eutectic mixture and capric acid is 47.6%/52.4%; After this proportioning mixing, be heated under 50 ℃ of water bath condition and stirred 60 minutes, get capric acid/lauric acid/myristic acid ternary eutectic mixture after ultrasonic 2 minutes, its transformation temperature is 17.05 ℃, latent heat of phase change is 203.7J/g.
(3) with clay: the sludge ceramsite of mud=8.9: 1.1 mass ratio vacuumizes 50 minutes under 40 ℃, vacuum tightness is 0.095MPa; Capric acid/lauric acid that adding has been melted/myristic acid ternary eutectic mixture; System is risen to normal pressure, and the ternary eutectic mixture infiltrated sludge ceramsite 100 minutes; Cooling namely gets ternary aliphatic acid/sludge ceramsite shaping phase-change material.Use determine with dsc method, its transformation temperature is 17.10 ℃, and latent heat of phase change is 68.0J/g.
Claims (4)
1. the preparation method of a shaping phase-change material is compound by following weight percent by polyhydric aliphatic acid eutectic mixture and sludge ceramsite: polyhydric aliphatic acid eutectic mixture 30% ~ 60%, sludge ceramsite 40% ~ 70%;
Sludge ceramsite is vacuumized 30 ~ 100 minutes under the temperature that is higher than 10 ~ 20 ℃ of polyhydric aliphatic acid eutectic mixture transformation temperatures, vacuum tightness 0.08~0.10MPa adds the polyhydric aliphatic acid eutectic mixture that melts; Rise to normal pressure, liquid polyhydric aliphatic acid eutectic mixture is infiltrated in the sludge ceramsite gradually, the absorption infiltration time is 60 ~ 150 minutes; Cooling gets polyhydric aliphatic acid/sludge ceramsite shaping phase-change material;
Described polyhydric aliphatic acid eutectic mixture is the eutectic mixture more than three kinds or three kinds in capric acid, lauric acid, myristic acid, palmitinic acid, the stearic acid; Described sludge ceramsite be mud after clay and the sewage work's mummification as raw material, press clay: the mud after the mummification=(8.8 ~ 9.2): (1.2~0.8) mass ratio mixes, granulation, fires to form under 920 ~ 970 ℃;
Wherein, described polyhydric aliphatic acid eutectic mixture prepares according to the following steps:
A. according to the proportioning of the binary of fatty acids eutectic mixture that is calculated by Schroeder's formula:
X
A+X
B=1
△ H wherein
AWith △ H
BBe respectively the mole melting enthalpy of A, two kinds of lipid acid of B; T
AAnd T
BBe respectively the fusing point of A, two kinds of lipid acid of B; T is the eutectic point of A, two kinds of lipid acid of B; X
AAnd X
BWhen being respectively A, two kinds of lipid acid congruent meltings of B in mixture shared mol ratio;
With the optional two kinds of mixing in capric acid, lauric acid, myristic acid, palmitinic acid, the stearic acid, fusing point higher in both is as benchmark T
0, at T
0+ 10 ℃ ~ T
0Mixture heating up with these two kinds of lipid acid under+20 ℃ the water bath condition stirred 30 ~ 60 minutes, obtained the binary of fatty acids eutectic mixture after ultrasonic 2 ~ 5 minutes;
B. measure transformation temperature and the corresponding enthalpy of gained binary of fatty acids eutectic mixture, and calculate its theoretical molecular mass according to mixing match; This binary of fatty acids eutectic mixture is mixed with the third lipid acid according to Schroeder's formula as single fat acid, and method obtains ternary aliphatic acid eutectic mixture as described in the step a; By that analogy, mixed by ternary aliphatic acid eutectic mixture and the 4th kind of lipid acid, can obtain quaternary lipid acid eutectic mixture, by that analogy, and then get polyhydric aliphatic acid eutectic mixture.
2. the preparation method of shaping phase-change material as claimed in claim 1, it is characterized in that, described polyhydric aliphatic acid is capric acid/lauric acid/myristic acid ternary eutectic mixture, lauric acid/myristic acid/stearic acid ternary eutectic mixture, capric acid/lauric acid/stearic acid ternary eutectic mixture or lauric acid/myristic acid/palmitinic acid/stearic acid quaternary eutectic mixture.
3. the preparation method of shaping phase-change material as claimed in claim 1 is characterized in that, step is as follows:
(1) the mixing quality ratio that calculates myristic acid and stearic acid binary of fatty acids according to Schroeder's formula is 72.66% and 27.34%, myristic acid and stearic acid are mixed by this proportioning, mixture heating up with these two kinds of lipid acid under 85 ℃ of water bath condition stirred 50 minutes, after ultrasonic 3 minutes myristic acid/stearic acid binary eutectic mixture; Measuring myristic acid/stearic binary eutectic mixture transformation temperature is 47.55 ℃, and latent heat of phase change is 182.3J/g, and calculating its theoretical molecular mass is 241.39; Regard this binary of fatty acids eutectic mixture as single lipid acid, then carry out compoundly with lauric acid that calculate as can be known according to Schroeder's formula, binary of fatty acids eutectic mixture and lauric mixing quality ratio are 49% and 51%; After this proportioning mixing, be heated under 65 ℃ of water bath condition and stirred 50 minutes, get lauric acid/myristic acid/stearic acid ternary eutectic mixture after ultrasonic 3 minutes;
(2) with clay: the sludge ceramsite of mud=9:1 mass ratio vacuumizes 40 minutes under 50 ℃, and vacuum tightness is 0.098MPa; Lauric acid/myristic acid that adding has been melted/stearic acid ternary eutectic mixture; Rise to normal pressure, the ternary eutectic mixture infiltrated sludge ceramsite 120 minutes; Cooling namely gets ternary aliphatic acid/sludge ceramsite shaping phase-change material.
4. the preparation method of shaping phase-change material as claimed in claim 1 is characterized in that, step is as follows:
(1) the mixing quality ratio that calculates lauric acid and myristic acid according to Schroeder's formula is 65.08%: 34.92%, lauric acid and myristic acid are mixed by this proportioning, mixture heating up with these two kinds of lipid acid under 65 ℃ of water bath condition stirred 60 minutes, after ultrasonic 2 minutes lauric acid/myristic acid binary eutectic mixture; Measure the binary eutectic mixture of lauric acid/myristic acid, transformation temperature is 35.10 ℃, and latent heat of phase change is 210.2J/g, and calculating its theoretical molecular mass is 209.30; Regard this binary of fatty acids eutectic mixture as single lipid acid, then carry out compoundly with capric acid that the mixing quality that calculates binary of fatty acids eutectic mixture and capric acid according to Schroeder's formula is than being 47.6%:52.4%; After this proportioning mixing, be heated under 50 ℃ of water bath condition and stirred 60 minutes, get capric acid/lauric acid/myristic acid ternary eutectic mixture after ultrasonic 2 minutes;
(2) with clay: the sludge ceramsite of mud=8.9:1.1 mass ratio vacuumizes 50 minutes under 40 ℃, and vacuum tightness is 0.095MPa; Capric acid/lauric acid that adding has been melted/myristic acid ternary eutectic mixture; Rise to normal pressure, the ternary eutectic mixture infiltrated sludge ceramsite 100 minutes; Cooling namely gets ternary aliphatic acid/sludge ceramsite shaping phase-change material.
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