基于热力学模型的新型无机熔盐水化物相变储能材料的研究
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摘要
经济的快速发展使世界能源危机日益加重,如何提高能源利用效率、实现节能减排已受到普遍关注。相变储能材料(Phase change material,即PCM)因其在相变过程中储存或释放潜热,从而有效缓解能源紧张所带来的供求失衡的矛盾,已成为当前各国研究的热点。国际上普通采用“配方法”寻找新型储能材料,耗时耗材且不易找到真正的共晶点。本文从我国储量丰富的镁锂资源入手,选择合适的热力学模型对储能密度大的多元盐水体系的相图进行计算,以期寻找到温度适宜的相变储能材料。主要研究内容及创新性结果如下：
1.简要评述了国际上常用的几种热力学模型,并用Pitzer-Simonson-Clegg (PSC)模型和BET模型对七种三元盐水体系(CaCl2-LiCl-H2O、LiCl-LiNO3-H2O、LiNO3-Mg(NO3)2-H2O、NaNO3-Mg(NO3)2-H2O、KNO3-LiNO3-H2O、KNO3-Mg(NO3)2-H2O和CuCl2-LiCl-H2O)的溶解度进行计算,与实验值进行对照,用以比较这两种热力学模型的预测能力。相图计算结果表明,若三元体系中所含两种盐的溶解性均较高,BET模型的计算值与实验值十分吻合,预测能力明显优于PSC模型；若三元体系中同时包含溶解性高和溶解性较低的电解质,PSC模型既考虑长程静电作用,又添加溶剂与离子相互作用,所以在结合二元及三元体系实验数据的情况下可较为准确的计算体系相图,而BET模型的计算结果不尽如人意。
2.选择合适的热力学模型对若干含锂(镁)的盐水体系相图进行计算,寻找温度适宜的共晶材料。(1)由于LiNO3-KNO3-M(NO3)n-H2O (M=Na (n=1), Mg (n=2))体系中包含低温时溶解性较低的KNO3和高溶解性的LiNO3,选择PSC模型,结合相关二元及三元体系的实验数据,拟合模型参数,计算这两个四元体系及其所包含的二元及三元子体系的相图,并从中找到三个二元共晶占:KNO3-LiNO3-3H2O、NaNO3-LiNO3-3H2O, LiNO3-3H2O-Mg(NO3)2-6H2O,及五个三元共晶点：KNO3-LiNO3-3H2O-LiNO3. NaNO3-LiNO3-3H2O-LiNO3LiNO3-3H2O-LiNO3-Mg(NO3)2-6H2O、LiNO3-3H2O-NaNO3-KNO3> KN03-LiNO3-3H20-Mg(NO3)2-6H20,它们的熔点在294K-301K之间。(2)对于各盐溶解性均较高的LiNO3-NaNO3-NH4NO3-H2O体系和Mg(NO3)2-MgCl2-H2O体系,选择BET模型,结合实验数据获得二元参数及三元盐盐相互作用参数,计算这两个体系及其子体系的相图。从中找到三个二元共晶点：NaNO3-LiNO3-3H2O、NH4NO3-LiNO3·3H2O、Mg(NO3)2·6H2O-MgCl2·6H2O和四个三元共晶点：NaNO3-LiN3-·3H2O-LiNO3·NH4NO3-LiNO3-3H2O-LiNO3、 Mg(NO3)2·6H2O-Mg(NO3)2·2H2O-MgCl2·6H2O、LiNO3·3H2O-NaNO3-NH4NO3。
3.用等温溶解度法测定KNO3-LiNO3-H2O体系283.15K的溶解度,用固相消失法测定KNO3-LiNO3-NaNO3-H2O体系298.1K和308.5K的溶解度,及其子体系LiNO3-NaNO3-H2O在323.1K的溶解度。所有实验值均与本文PSC模型预测值吻合。
4.对本文用热力学模型预测的部分共晶材料的储能性能进行熔化结晶行为测试,并用DSC或DTA测定材料的熔点及熔化热。结果表明：(1)二元共晶材料KNO3(17.5%)-LiNO3-3H2O (82.5%)和三元共晶材料KNO3(20.9%)-LiNO3-3H2O (64.4%)-LiNO3(14.7%). LiNO3-3H2O (76.2%)-NaNO3(5.9%)-KNO3(17.9%),具有较好的储能效果,它们的熔点与模型预测值相差小于±1K,且均在室温范围(293±5K),可用作潜在的室温相变储能材料。(2)BET模型预测的三元共晶点LiNO3-3H2O (63.4%)-NaNO3(5.5%)-NH4NO3(31.3%),其熔点为287.1K,与模型预测值基本一致,熔化结晶行为曲线表明吸放热性能良好,可用作潜在的低温相变储能材料。(3)二元共晶材料Mg(NO3)2-6H2O (61.6%)-MgCl2-6H2O (38.4%)的熔点为333.5K,比BET模型的预测值高2K,熔化热约为137J·g-1,可用作潜在的相变储能材料。而三元共晶材料Mg(NO3)2-6H2O (45.6%)-Mg(NO3)2-2H2O (29.6%)-MgCl2-6H2O (24.8%)的储能效果较差,不适用于潜在的相变储能材料。
The present energy crisis caused by economic development is more and more serious. How to increase utilization ratio of energy and save energy attracts worldwide attentions. Phase change material (PCM), which can store or release latent heat during phase change process and solve the unbalance between supply and demand of energy shortage, has become hot topic in the research. Conventionally, a formula method is used widely for looking for PCM, which is difficult to find real eutectic points. In this paper, thermodynamic model has been chosen for calculating the phase diagrams of lithium and magnesium hydrated salt systems and finding phase change materials with suitable temperature. The main research contents and results are:
1. Several thermodynamic models commonly used were evaluated, and a Pitzer-Simonson-Clegg model (PSC model) and a BET model were chosen for calculating phase diagrams of seven ternary systems including CaCl2-LiCl-H2O, LiCl-LiNO3-H2O, LiNO3-Mg(NO3)2-H2O, NaNO3-Mg(NO3)2-H2O, KNO3-LiNO3-H2O, KNO3-Mg(NO3)2-H2O and CuCl2-LiCl-H2O, and the calculated values are compared with experimental data. The results show that the BET model is more appropriate than the PSC model to predict the properties of highly soluble hydrated salt systems. For salt-water systems consisting of lowly soluble salt and highly soluble salt, the PSC model, which includes long range electrostatic terms and interaction between solvent water and ions, is more suitable than the BET model.
2. Suitable model was applied to calculate phase diagrams of salt-water systems containing lithium (magnesium), and then eutectic points with appropriate temperature were found.(1) For LiNO3-KNO3-M(NO3)n-H2O (M=Na (n=1), Mg (n=2)) systems containing lowly soluble salt KNO3and highly soluble salt LiNO3, combining with experimental data of its binary and ternary systems, the PSC model was used to calculate phase diagrams of quaternary systems and their sub-systems. In these phase diagrams, we have found three binary eutectic points:KNO3-LiNO3-3H2O, NaNO3-LiNO3-3H2O, LiNO3-3H2O-Mg(NO3)2-6H2O, and five ternary eutectic points:KNO3-LiNO3-3H2O-LiNO3, NaNO3-LiNO3-3H2O-LiNO3, LiNO3·3H2O-LiNO3-Mg(NO3)2-6H2O, LiNO3·3H2O-NaNO3-KNO3, KNO3-LiNO3-3H2O-Mg(NO3)2-6H2O, with melting temperature range from294K to301K.(2) The BET model is applied to calculate phase diagrams of systems LiNO3-NaNO3-NH4NO3-H2O, Mg(NO3)2-MgCl2-H2O and their sub-systems, and then three binary eutectic points including NaNO3-LiNO3-3H2O, NH4NO3-LiNO3-3H2O, Mg(NO3)2-6H2O-MgCl2-6H2O, and four ternary eutectic points including NaNO3-LiNO3·3H2O-LiNO3, NH4NO3-LiNO3·3H2O-LiNO3, Mg(NO3)2-6H2O-Mg(NO3)2-2H2O-MgCl2-6H2O and LiNO3·3H2O-NaNO3-NH4NO3were found.
3. The solubility isotherm of the KNO3-LiNO3-H2O system at283.1K has been determined using method of isothermal solution, and the solubilities of the KNO3-LiNO3-NaNO3-H2O system at298.1K and308.5K as well as its sub-system LiNO3-NaNO3-H2O at323.1K have been measured by means of isothermal solid-disappearance method. The experimental solubility data are in excellent agreement with the calculated values.
4. Melting and crystallization behavior of the aforementioned predicted eutectic points have been measured using our device, and DSC or DTA was used to measure the fusion heat and fusion temperature. The results show that:(1) The binary eutectic points KNO3(17.5%)-LiNO3·3H2O (82.5%) and the ternary eutectic point KNO3(20.9%)-LiNO3·3H2O (64.4%)-LiNO3(14.7%), LiNO3·3H2O (76.2%)-NaNO3(5.9%)-KNO3(17.9%) can be taken as potential room temperature PCM with high stored energy effect, and the differences of melting temperature between experimental data and predicted ones are less than±1K.(2) The ternary eutectic point LiNO3·3H2O (63.4%)-NaNO3(5.5%)-NH4NO3(31.3%) which has excellent heat storage behavior, could be used as potential low temperature PCM.(3) The binary eutectic point Mg(NO3)2·6H2O (61.6%)-MgCl2·6H2O (38.4%) whose melting point is333.5K and phase change heat is137J·g-1, could be regarded as potential PCM. However, ternary eutectic point Mg(NO3)2-6H2O (45.6%)-Mg(NO3)2·2H2O (29.6%)-MgCl2·6H2O (24.8%) possesses less storage energy ability.
1.简要评述了国际上常用的几种热力学模型,并用Pitzer-Simonson-Clegg (PSC)模型和BET模型对七种三元盐水体系(CaCl2-LiCl-H2O、LiCl-LiNO3-H2O、LiNO3-Mg(NO3)2-H2O、NaNO3-Mg(NO3)2-H2O、KNO3-LiNO3-H2O、KNO3-Mg(NO3)2-H2O和CuCl2-LiCl-H2O)的溶解度进行计算,与实验值进行对照,用以比较这两种热力学模型的预测能力。相图计算结果表明,若三元体系中所含两种盐的溶解性均较高,BET模型的计算值与实验值十分吻合,预测能力明显优于PSC模型；若三元体系中同时包含溶解性高和溶解性较低的电解质,PSC模型既考虑长程静电作用,又添加溶剂与离子相互作用,所以在结合二元及三元体系实验数据的情况下可较为准确的计算体系相图,而BET模型的计算结果不尽如人意。
2.选择合适的热力学模型对若干含锂(镁)的盐水体系相图进行计算,寻找温度适宜的共晶材料。(1)由于LiNO3-KNO3-M(NO3)n-H2O (M=Na (n=1), Mg (n=2))体系中包含低温时溶解性较低的KNO3和高溶解性的LiNO3,选择PSC模型,结合相关二元及三元体系的实验数据,拟合模型参数,计算这两个四元体系及其所包含的二元及三元子体系的相图,并从中找到三个二元共晶占:KNO3-LiNO3-3H2O、NaNO3-LiNO3-3H2O, LiNO3-3H2O-Mg(NO3)2-6H2O,及五个三元共晶点：KNO3-LiNO3-3H2O-LiNO3. NaNO3-LiNO3-3H2O-LiNO3LiNO3-3H2O-LiNO3-Mg(NO3)2-6H2O、LiNO3-3H2O-NaNO3-KNO3> KN03-LiNO3-3H20-Mg(NO3)2-6H20,它们的熔点在294K-301K之间。(2)对于各盐溶解性均较高的LiNO3-NaNO3-NH4NO3-H2O体系和Mg(NO3)2-MgCl2-H2O体系,选择BET模型,结合实验数据获得二元参数及三元盐盐相互作用参数,计算这两个体系及其子体系的相图。从中找到三个二元共晶点：NaNO3-LiNO3-3H2O、NH4NO3-LiNO3·3H2O、Mg(NO3)2·6H2O-MgCl2·6H2O和四个三元共晶点：NaNO3-LiN3-·3H2O-LiNO3·NH4NO3-LiNO3-3H2O-LiNO3、 Mg(NO3)2·6H2O-Mg(NO3)2·2H2O-MgCl2·6H2O、LiNO3·3H2O-NaNO3-NH4NO3。
3.用等温溶解度法测定KNO3-LiNO3-H2O体系283.15K的溶解度,用固相消失法测定KNO3-LiNO3-NaNO3-H2O体系298.1K和308.5K的溶解度,及其子体系LiNO3-NaNO3-H2O在323.1K的溶解度。所有实验值均与本文PSC模型预测值吻合。
4.对本文用热力学模型预测的部分共晶材料的储能性能进行熔化结晶行为测试,并用DSC或DTA测定材料的熔点及熔化热。结果表明：(1)二元共晶材料KNO3(17.5%)-LiNO3-3H2O (82.5%)和三元共晶材料KNO3(20.9%)-LiNO3-3H2O (64.4%)-LiNO3(14.7%). LiNO3-3H2O (76.2%)-NaNO3(5.9%)-KNO3(17.9%),具有较好的储能效果,它们的熔点与模型预测值相差小于±1K,且均在室温范围(293±5K),可用作潜在的室温相变储能材料。(2)BET模型预测的三元共晶点LiNO3-3H2O (63.4%)-NaNO3(5.5%)-NH4NO3(31.3%),其熔点为287.1K,与模型预测值基本一致,熔化结晶行为曲线表明吸放热性能良好,可用作潜在的低温相变储能材料。(3)二元共晶材料Mg(NO3)2-6H2O (61.6%)-MgCl2-6H2O (38.4%)的熔点为333.5K,比BET模型的预测值高2K,熔化热约为137J·g-1,可用作潜在的相变储能材料。而三元共晶材料Mg(NO3)2-6H2O (45.6%)-Mg(NO3)2-2H2O (29.6%)-MgCl2-6H2O (24.8%)的储能效果较差,不适用于潜在的相变储能材料。
The present energy crisis caused by economic development is more and more serious. How to increase utilization ratio of energy and save energy attracts worldwide attentions. Phase change material (PCM), which can store or release latent heat during phase change process and solve the unbalance between supply and demand of energy shortage, has become hot topic in the research. Conventionally, a formula method is used widely for looking for PCM, which is difficult to find real eutectic points. In this paper, thermodynamic model has been chosen for calculating the phase diagrams of lithium and magnesium hydrated salt systems and finding phase change materials with suitable temperature. The main research contents and results are:
1. Several thermodynamic models commonly used were evaluated, and a Pitzer-Simonson-Clegg model (PSC model) and a BET model were chosen for calculating phase diagrams of seven ternary systems including CaCl2-LiCl-H2O, LiCl-LiNO3-H2O, LiNO3-Mg(NO3)2-H2O, NaNO3-Mg(NO3)2-H2O, KNO3-LiNO3-H2O, KNO3-Mg(NO3)2-H2O and CuCl2-LiCl-H2O, and the calculated values are compared with experimental data. The results show that the BET model is more appropriate than the PSC model to predict the properties of highly soluble hydrated salt systems. For salt-water systems consisting of lowly soluble salt and highly soluble salt, the PSC model, which includes long range electrostatic terms and interaction between solvent water and ions, is more suitable than the BET model.
2. Suitable model was applied to calculate phase diagrams of salt-water systems containing lithium (magnesium), and then eutectic points with appropriate temperature were found.(1) For LiNO3-KNO3-M(NO3)n-H2O (M=Na (n=1), Mg (n=2)) systems containing lowly soluble salt KNO3and highly soluble salt LiNO3, combining with experimental data of its binary and ternary systems, the PSC model was used to calculate phase diagrams of quaternary systems and their sub-systems. In these phase diagrams, we have found three binary eutectic points:KNO3-LiNO3-3H2O, NaNO3-LiNO3-3H2O, LiNO3-3H2O-Mg(NO3)2-6H2O, and five ternary eutectic points:KNO3-LiNO3-3H2O-LiNO3, NaNO3-LiNO3-3H2O-LiNO3, LiNO3·3H2O-LiNO3-Mg(NO3)2-6H2O, LiNO3·3H2O-NaNO3-KNO3, KNO3-LiNO3-3H2O-Mg(NO3)2-6H2O, with melting temperature range from294K to301K.(2) The BET model is applied to calculate phase diagrams of systems LiNO3-NaNO3-NH4NO3-H2O, Mg(NO3)2-MgCl2-H2O and their sub-systems, and then three binary eutectic points including NaNO3-LiNO3-3H2O, NH4NO3-LiNO3-3H2O, Mg(NO3)2-6H2O-MgCl2-6H2O, and four ternary eutectic points including NaNO3-LiNO3·3H2O-LiNO3, NH4NO3-LiNO3·3H2O-LiNO3, Mg(NO3)2-6H2O-Mg(NO3)2-2H2O-MgCl2-6H2O and LiNO3·3H2O-NaNO3-NH4NO3were found.
3. The solubility isotherm of the KNO3-LiNO3-H2O system at283.1K has been determined using method of isothermal solution, and the solubilities of the KNO3-LiNO3-NaNO3-H2O system at298.1K and308.5K as well as its sub-system LiNO3-NaNO3-H2O at323.1K have been measured by means of isothermal solid-disappearance method. The experimental solubility data are in excellent agreement with the calculated values.
4. Melting and crystallization behavior of the aforementioned predicted eutectic points have been measured using our device, and DSC or DTA was used to measure the fusion heat and fusion temperature. The results show that:(1) The binary eutectic points KNO3(17.5%)-LiNO3·3H2O (82.5%) and the ternary eutectic point KNO3(20.9%)-LiNO3·3H2O (64.4%)-LiNO3(14.7%), LiNO3·3H2O (76.2%)-NaNO3(5.9%)-KNO3(17.9%) can be taken as potential room temperature PCM with high stored energy effect, and the differences of melting temperature between experimental data and predicted ones are less than±1K.(2) The ternary eutectic point LiNO3·3H2O (63.4%)-NaNO3(5.5%)-NH4NO3(31.3%) which has excellent heat storage behavior, could be used as potential low temperature PCM.(3) The binary eutectic point Mg(NO3)2·6H2O (61.6%)-MgCl2·6H2O (38.4%) whose melting point is333.5K and phase change heat is137J·g-1, could be regarded as potential PCM. However, ternary eutectic point Mg(NO3)2-6H2O (45.6%)-Mg(NO3)2·2H2O (29.6%)-MgCl2·6H2O (24.8%) possesses less storage energy ability.
引文
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