CN100467565C - Method for preparing organic molecular alloy phase change energy storage material - Google Patents

Method for preparing organic molecular alloy phase change energy storage material Download PDF

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CN100467565C
CN100467565C CNB200510026226XA CN200510026226A CN100467565C CN 100467565 C CN100467565 C CN 100467565C CN B200510026226X A CNB200510026226X A CN B200510026226XA CN 200510026226 A CN200510026226 A CN 200510026226A CN 100467565 C CN100467565 C CN 100467565C
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phase change
energy storage
acid
storage material
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CN1869145A (en
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张东
田胜力
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Tongji University
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Abstract

本发明涉及相变储能材料的制备方法领域。本发明所述的有机分子合金储能材料的制备方法步骤如下:先按适当的配比间距设定一系列试配比,按设定试配比秤量有机相变材料制得试配比混合物,然后在80~100℃中恒温保持1~4小时,再将得到的产物超声波震动1~5分钟,超声波频率40~50千赫兹,温度控制在50~80℃,最后利用热分析技术测试不同试配比的有机相变材料的相变温度和相变热,取具有单相变温度和最大相变热试配比的有机分子合金相变储能材料为目标产物。利用该方法可以将多种不同的有机相变材料组合在一起,制备出自然界中没有的、相变温度可调节的、相变热较大的有机分子合金相变储能材料。

Figure 200510026226

The invention relates to the field of preparation methods of phase-change energy storage materials. The steps of the preparation method of the organic molecular alloy energy storage material according to the present invention are as follows: first, a series of trial proportions are set according to the appropriate proportioning distance, and the organic phase change material is weighed according to the set trial proportions to prepare the trial proportion mixture, Then keep the constant temperature at 80-100°C for 1-4 hours, then ultrasonically vibrate the obtained product for 1-5 minutes, the ultrasonic frequency is 40-50 kHz, the temperature is controlled at 50-80°C, and finally the thermal analysis technology is used to test different samples. The phase change temperature and phase change heat of the proportioned organic phase change material, the organic molecular alloy phase change energy storage material with a single phase change temperature and the largest phase change heat trial ratio is taken as the target product. Using this method, a variety of different organic phase change materials can be combined to prepare an organic molecular alloy phase change energy storage material that does not exist in nature, has an adjustable phase change temperature, and has a large phase change heat.

Figure 200510026226

Description

The method for preparing organic molecular alloy phase change energy storage material
Technical field
The invention belongs to the thermal energy storage technical field, particularly the preparation method field of phase-changing energy storage material.
Background technology
Phase-changing energy storage material utilizes material neither endothermic nor exothermic in phase transition process to come storage power or releases energy, and has characteristics such as the approximate isothermal of storage density height, heat accumulation heat release, process be easy to control.The kind of phase-changing energy storage material is a lot, can be divided into by the mode of phase transformation that solid-solid phase transition material, solid-liquid phase change material, solid-gas phase become material, liquid-gas phase becomes material etc.; Moiety by material can be divided into mineral-type and organic class (comprising the high score subclass) phase-changing energy storage material.
Organic class phase change material is commonly used paraffin, lipid acid or its ester class, alcohols, arene, fragrant ketone, amides etc.The advantage of organic class phase change material is that formability better, generally is not easy to occur surfusion and is separated when solid state, and the corrodibility of material is less, and performance is more stable, and toxicity is little, cost is low; Energy storage capacity little, the less unit volume of density is less thereby shortcoming is a thermal conductivity, and fusing point is lower, be unsuitable for using in the high temperature occasion, and volatile, easy firing even blast or worn out by airborne oxygen slow oxidation.
Summary of the invention
The objective of the invention is to propose the preparation method of a kind of transformation temperature organic molecular alloy phase change energy storage material adjustable, that heat of phase transformation is bigger.
Because the phase transformation performance of organic molecule alloy is different with the phase transformation performance of single component, therefore, can be by regulating different components and proportioning to obtain the phase change material of a series of different transformation temperatures and heat of phase transformation.The method that the present invention adopts soak to combine with vibration of ultrasonic wave, and utilize modern thermoanalysis technology, by a series of examination proportioning mixtures are carried out hot analytical test, study the thermal characteristics of different proportioning organic molecular alloy phase change materials, get examination proportioning, thereby prepare the satisfactory organic molecular alloy phase change energy storage material of performance with single-phase alternating temperature degree and maximal phase heating.
The preparation method of organic molecular alloy phase change energy storage material of the present invention, its step is as follows:
A, the preparation of examination proportioning mixture: set a series of examination proportionings by suitable proportioning spacing,, make examination proportioning mixture by setting examination proportioning weighing organic phase change material;
B, soak: the examination proportioning mixture that step a is obtained kept 1~4 hour in 80~100 ℃ of constant temperature;
C, vibration of ultrasonic wave: the product vibration of ultrasonic wave that step b is obtained 1~5 minute, ultrasonic frequency 40~50 kilohertzs, temperature is controlled at 50~80 ℃;
D, utilize the transformation temperature and the heat of phase transformation of the organic phase change material of the different examination of thermoanalysis technology test proportionings, getting the organic molecular alloy phase change energy storage material with single-phase alternating temperature degree and maximal phase heating examination proportioning is target product.
The preparation method of organic molecular alloy phase change energy storage material of the present invention, wherein the described thermoanalysis technology of step a is meant differential scanning calorimetric (DSC) analytical technology; Organic phase change material can be two or more the material in alkane, lipid acid and the derivative thereof, as tetradecanoic acid, palmitinic acid, stearic acid, butyl stearate, lauryl alcohol, and tetradecyl alcohol, hexadecanol, docosane, hexacosane etc.
Beneficial effect of the present invention: the preparation method who utilizes organic molecular alloy phase change energy storage material of the present invention, multiple different organic phase change material can be combined, the different proportionings of regulating the different components of molecular alloy and identical component by modern thermoanalysis technology can obtain the phase change material of different transformation temperatures, the method that adopts soak to combine with vibration of ultrasonic wave is again prepared organic molecular alloy phase change energy storage material that occurring in nature does not have, that transformation temperature is adjustable, heat of phase transformation is bigger.
Description of drawings
Fig. 1 is the DSC curve of the machine molecular alloy phase-changing energy storage material that makes of embodiment 1.
Fig. 2 is the DSC curve of the machine molecular alloy phase-changing energy storage material that makes of embodiment 2.
Fig. 3 is the DSC curve of the machine molecular alloy phase-changing energy storage material that makes of embodiment 3.
Embodiment
Embodiment 1
With chemical pure n-caprylic acid, lauric acid as raw material.Setting examination proportioning (mol ratio) series is n-caprylic acid: lauric acid=5:95,10:90,15:85,20:80,25:75,30:70,35:65,40:60,45:55,50:50,55:45,60:40,65:35,70:30,75:25,80:20,85:15,90:10,95:5.Examination proportioning mixture is incubated 4 hours in 80 ℃ constant temperature insulating container, the water-bath of then test tube being put into ultrasonic generator, the temperature of control water-bath is 60 ℃, and the ultrasonic vibration time is 3 minutes, and ultrasonic frequency is 40~50 kilohertzs.Through above-mentioned series examination proportioning mixture is carried out hot analytical test, get examination proportioning with single-phase alternating temperature degree and maximal phase heating, determine that the target proportioning is n-caprylic acid: lauric acid=80:20 (mol ratio), the DSC test result of this molecular alloy is seen Fig. 1.
Embodiment 2
With chemical pure n-caprylic acid, palmitinic acid as raw material.Setting examination proportioning (mol ratio) series is n-caprylic acid: palmitinic acid=5:95,10:90,15:85,20:80,25:75,30:70,35; 65,40:60,45:55,50:50,55:45,60:40,65:35,70:30,75:25,80:20,85:15,90:10,95:5.Examination proportioning mixture is incubated 2.5 hours in 90 ℃ constant temperature insulating container, the water-bath of then test tube being put into ultrasonic generator, the temperature of control water-bath is 50 ℃, and the ultrasonic vibration time is 5 minutes, and ultrasonic frequency is 40~50 kilohertzs.Through above-mentioned series examination proportioning mixture is carried out hot analytical test, get examination proportioning with single-phase alternating temperature degree and maximal phase heating, determine that the target proportioning is n-caprylic acid: palmitinic acid=95:5 (mol ratio), the DSC test result of this molecular alloy is seen Fig. 2.
Embodiment 3
With chemical pure capric acid, tetradecanoic acid as raw material.Setting examination proportioning (mol ratio) series is capric acid: tetradecanoic acid=5:95,10:90,15:85,20:80,25:75,30:70,35:65,40:60,45:55,50:50,55:45,60:40,65:35,70:30,75:25,80:20,85:15,90:10,95:5.Examination proportioning mixture is incubated 1 hour in 100 ℃ constant temperature insulating container, the water-bath of then test tube being put into ultrasonic generator, the temperature of control water-bath is 80 ℃, and the ultrasonic vibration time is 1 minute, and ultrasonic frequency is 40~50 kilohertzs.Through above-mentioned series examination proportioning mixture is carried out hot analytical test, get examination proportioning with single-phase alternating temperature degree and maximal phase heating, determine that the target proportioning is capric acid: tetradecanoic acid=75:25 (mol ratio), the DSC test result of this molecular alloy is seen Fig. 3.
By the DSC test result of above embodiment and organic molecule alloy as seen, utilize the preparation method of organic molecular alloy phase change energy storage material of the present invention can obtain the original non-existent phase change material of occurring in nature, and can obtain the phase change material of needed specified temp in the practical application, also guarantee to have higher heat of phase transformation simultaneously.

Claims (5)

1、一种有机分子合金相变储能材料的制备方法,其步骤如下:1. A method for preparing an organic molecular alloy phase-change energy storage material, the steps of which are as follows: a、试配比混合物制备:设定一系列试配比,按设定试配比秤量有机相变材料,制得试配比混合物,其中,有机相变材料选自肉豆蔻酸、棕榈酸、癸酸、正辛酸或月桂酸中的两种;a. Preparation of test proportion mixture: set a series of test proportions, weigh the organic phase change material according to the set test proportion, and prepare the test proportion mixture, wherein the organic phase change material is selected from myristic acid, palmitic acid, Two of capric, n-caprylic, or lauric acid; b、高温保温:将步骤a得到的试配比混合物在恒温80~100℃中保持1~4小时;b. High temperature insulation: keep the trial proportion mixture obtained in step a at a constant temperature of 80-100°C for 1-4 hours; c、超声波震动:将步骤b得到的产物超声波震动1~5分钟,超声波频率40~50千赫兹,温度控制在50~80℃;c, ultrasonic vibration: ultrasonically vibrate the product obtained in step b for 1 to 5 minutes, the ultrasonic frequency is 40 to 50 kHz, and the temperature is controlled at 50 to 80°C; d、利用热分析技术测试不同试配比的有机相变材料的相变温度和相变热,取具有单相变温度和最大相变热试配比的有机分子合金相变储能材料为目标产物。d. Use thermal analysis technology to test the phase change temperature and heat of phase change of organic phase change materials with different trial ratios, and take organic molecular alloy phase change energy storage materials with single phase transition temperature and maximum phase change heat trial ratio as the target product. 2、如权利要求1所述的有机分子合金相变储能材料的制备方法,其特征在于步骤d所说的热分析技术是指差示扫描量热分析技术。2. The method for preparing an organic molecular alloy phase change energy storage material as claimed in claim 1, characterized in that the thermal analysis technique mentioned in step d refers to differential scanning calorimetry analysis technique. 3、按权利要求1所述制备方法制得的有机分子合金相变储能材料,由正辛酸和月桂酸组成,其中,正辛酸:月桂酸的摩尔比为80:20。3. The organic molecular alloy phase change energy storage material prepared according to the preparation method of claim 1 is composed of n-octanoic acid and lauric acid, wherein the molar ratio of n-octanoic acid: lauric acid is 80:20. 4、按权利要求1所述制备方法制得的有机分子合金相变储能材料,由正辛酸和棕榈酸组成,其中,正辛酸:棕榈酸的摩尔比为95:5。4. The organic molecular alloy phase-change energy storage material prepared according to the preparation method of claim 1 is composed of n-octanoic acid and palmitic acid, wherein the molar ratio of n-octanoic acid: palmitic acid is 95:5. 5、按权利要求1所述制备方法制得的有机分子合金相变储能材料,由癸酸和肉豆蔻酸组成,其中,癸酸:肉豆蔻酸的摩尔比为75:25。5. The organic molecular alloy phase change energy storage material prepared according to the preparation method of claim 1, which is composed of capric acid and myristic acid, wherein the molar ratio of capric acid:myristic acid is 75:25.
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DE19813562A1 (en) * 1997-05-21 1998-11-26 Schuemann Sasol Gmbh & Co Kg Latent heat body
CN1429261A (en) * 2000-05-19 2003-07-09 法国石油研究所 Method for making quasi-incompressible phase-change material with low thermal conductivity, and resulting product
CN1594192A (en) * 2004-07-15 2005-03-16 南京大学 Energy storage building material and preparing method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19813562A1 (en) * 1997-05-21 1998-11-26 Schuemann Sasol Gmbh & Co Kg Latent heat body
CN1429261A (en) * 2000-05-19 2003-07-09 法国石油研究所 Method for making quasi-incompressible phase-change material with low thermal conductivity, and resulting product
CN1594192A (en) * 2004-07-15 2005-03-16 南京大学 Energy storage building material and preparing method thereof

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