相变蓄热材料研发及在日光温室中的应用
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摘要
为解决北方日光温室安全过冬保证率低、冬季生产成本高和生产效率低的问题，本文对相变蓄热技术应用于温室墙体的基本理论和关键技术进行了系统的研究。根据北方的气候特点、日光温室的生产特点、种植作物的生长生产条件等要求，以相变温度和材料的潜热值为主要依据，通过对有研究基础相变材料的重点筛选，优选出了适合日光温室的无机和有机蓄热相变材料。对无机相变材料存在的过冷和相分离弊端，做了大量的相变材料改性试验研究，得到了高低两个温级的温室用蓄热材料体系；采用封装法将选出的蓄热材料应用于温室墙板，测试的温室内温度、湿度和地温等环境因子的改变，验证了相变温室蓄热性能的改善。针对一种有机相变材料相变温度无法满足温室生产要求和固液相变材料在相变过程中的泄漏问题，着重研究了相变材料的复合、定形等方法、原材料配比及复合、定形后的力学和热学特性，得到了适于日光温室的、相变潜热大小不同的两种相变定形材料蓄热体系。采用将定形相变材料直接掺入建筑墙体材料的方法，设计了相变砌块的制备方法和生产工艺，将其用于温室墙体中。温室内环境参数和种植物生长特性的实测结果证明了相变温室蓄热调温功能良好。本研究的主要结论有：
（1）研发了两温级无机相变蓄热材料体系。针对优选出的适用北方日光温室的无机相变蓄热材料Na2HPO4·12H_2O，通过优选成核剂和增稠剂、对进行改性（消除过冷度和相分离）实验研究，得到相变温度在33℃左右的温室用蓄热材料体系的质量比为Na2HPO4·12H_2O：硅酸钠：石墨=100:3:3的混合物。对上述高温级蓄热材料体系加质量比为8%的KCl降低相变温度，可获得低温级（25～26℃）的温室用蓄热材料体系，但引起了过冷度增加和相分离现象加剧。对其开展进一步的改性实验研究，得到相变温度为25～26℃左右的温室用最优蓄热材料体系为质量比Na2HPO4·12H_2O：KCl：硅酸钠：石墨=50:4:3:1的混合物。两温级最优蓄热材料体系按不同的比例组合应用于温室，能更好适应于不同气候、不同作物的日光温室中。
（2）无机相变蓄热板墙的应用具有改善温室的作物生产环境、提高温室过冬安全性和生产效益的效果。采用特殊塑料袋封装Na2HPO4·12H_2O相变材料体系，将其镶嵌于温室墙板中形成相变蓄热板墙。典型日和最冷月的连续气温、低温、湿度实测数据显示，相变板墙温室具有提高室内最低温度达2.7℃和平均温度1.5℃，降低室内最高温度1.2℃的明显效果；也有提高室内最低地温0.6℃和平均地温，降低室内最高地温0.7℃的作用；与对室内温度影响相对应，同时也能降低室内最小湿度8%和平均湿度0.5%。相变墙温室与当地的灰砂砖夹沙温室相比，经济性更好。
（3）研发了两种温室用有机蓄热相变材料体系。利用石蜡（PW）和硬脂酸正丁酯（BS）热性能互补性、化学相容性及稳定性，研究不同配比的复合相变材料的热性能，得到最佳温室用蓄热复合材料配比为石蜡：硬脂酸正丁酯热=1：1。以此为复合相变材料，用真空吸附法将其与稻壳制成BS/PW/稻壳定形相变材料。用差式扫描量热法测定相变蓄热材料的相变热流密度峰值位置分别出现在50.49℃和49.54℃，熔解潜热和凝固潜热分别为63.32J/g和59.82J/g。3000次的熔解/凝固循环后，BS/PW/稻壳具有良好的热稳定性。红外光谱扫描表明，各组分有良好的相容性和化学稳定性；扫描电镜微观结构图证明硬脂酸正丁酯和石蜡复合材料多数被吸附进稻壳内部，致密性良好。用聚苯乙烯颗粒代替稻壳用真空吸附法制成的BS/PW/聚苯乙烯颗粒定形相变材料有更大潜热值，其熔解潜热和凝固潜热分别为93.61J/g和95.58J/g。热稳定性、相容性和化学稳定性具佳，扫描电镜表明其致密性优于BS/PW/稻壳定形相变材料。综合考虑相变温度和潜热值两方面，BS/PW/聚苯乙烯颗粒定形相变材料是更优的温室用蓄热相变材料体系。
（4）设计了相变混凝土砌块的制备方法，测试了其热学力学性能。对混凝土弱碱化后与有机定形相变材料直接混合即可制备相变混凝土砌块。实验优化出砌块混凝土的质量配合比为水泥:粉煤灰:细沙:砾石:陶粒:石灰:石膏=20:25:17:10:25:1:2。通过对稻壳相变砌块和聚苯乙烯颗粒相变砌块的力学指标（最低抗压强度、最低干密度、最大吸水率、最大软化系数）和砌块的热学指标（最大导热系数、最大比热容、蓄热系数、相变潜热值）的测试结果分析可知，相变聚苯颗粒砌块蓄热性能优于相变稻壳砌块的蓄热性能，相变聚苯颗粒砌块力学性能却劣于相变稻壳砌块的力学性能。但相变材料的最大掺加量受力学性能的低限值的制约，研究建议相变稻壳掺量不大于5%，聚苯乙烯颗粒掺量不大于12%。
（5）相变混凝土砌块用于日光温室墙体对改善温室生产环境效果明显。将以BP/BS/稻壳为定型相变材料生产的相变混凝土砌块，实测室内的气温发现，该温室的典型日室内气温变化幅度比对照砖温室的小3.5℃，最低温度提高1.7℃和最高温度降低2.4%，北墙内外的温差的变化范围减小3.1℃。温室内种植的金鹏1号番茄，生长初期株高、茎粗、干重、鲜重和生长后期的株高、根长、茎粗、叶数、花序数、结果数、果重、植株总重量等，相变温室较对照温室的状态均有明显优势。
（6）研究得到的无机相变材料墙体和有机相变材料墙体在北方日光温室中的应用效果表明，相变温室具有良好的蓄热性和对温度的“削峰填谷”的调温性能。对改善温室作物的生产环境，提高温室生产效益，均有明显的积极影响。该研究成果有生产实用性和推广应用价值。
Current greenhouses in Northwest China have low thermal effectiveness, and high costsand low efficiency in production. The phase change heat storage technique was used as thebasis for greenhouse wall design to resolve those issues. We identified optimal inorganic andorganic phase change heat storage materials, based on the characteristics of Northern Chinaclimate, solar greenhouse production, and requirements of growth of plants, with respect tothe phase change temperature and latent heat values. Inorganic phase change materials havelow phase change temperature and phase separation. We carried out various experiments withmodified materials, and two types of materials for high and low temperatures were identified.Encapsulated heat storage materials were used as greenhouse wallboards. Based onmeasurements of internal air temperature, humidity and ground temperature in the greenhouse,improvement in greenhouse characteristics was verified. A single kind of organic phasechange material cannot meet the requirements of all greenhouse productions, and solid-liquidmaterials have leakage problems during phase change. We studied compositions and shapingmethods for composite phase change materials, and the mechanical and thermalcharacteristics of the materials, and two different kinds of phase change material for heatstorage system suitable for solar greenhouses were identified, with different latent heat.Phase change blocks were produced by mixing these materials with wall building materials.Greenhouse environmental parameters and plant growth characteristics show that thegreenhouse based on phase change heat storage materials has excellent temperatureadjustment performance.
The major conclusions of this thesis are as follows.
(1) Na2HPO4· H_2O is a phase change heat storage material optimal for solargreenhouses in the north, but its low temperature and phase separation characteristics affectits performance stability. With identified nucleating and thickening agents frommodification experiments, the composition for phase change materials at about33℃isidentified as a mixture with mass ratio of Na2HPO4· H_2O: sodium silicate: graphite=100:3:3.Adding to this high temperature heat storage material system with mass ratio8%KCl toreduce the phase transition temperature, a low temperature (25~26℃) material can beobtained, but this causes over cooling and phase separation. Further modification experiments show that an optimal material with mass ratio of Na2HPO4· H_2O: KCl: sodium silicate:graphite=50:4:3:1has phase transition temperature of25~26℃as well. Heat storagematerials of the two temperatures can be used in solar greenhouses for different crops.
(2) Special plastic packaging was used for the Na2HPO4·12H_2O phase change materialsystem, for embedding in greenhouse wall to form a phase change heat storage wall. Airtemperature, humidity, and low temperature data for typical days and continuousmeasurements for the coldest month show that the greenhouse built with the phase changematerial clearly increased the lowest and average indoor temperatures, reduces the highestindoor temperature. The materials also improved minimum and lowest indoor soiltemperatures, reduced highest indoor soil temperature. Corresponding to the indoortemperatures, the materials can reduce the minimum and average indoor humidity. Comparedwith control greenhouses with lime-sand bricks, phase change wall greenhouses haveimproved performance. This indicates that the phase transition materials have improved cropgrowth environment, winter performance and production efficiency of greenhouses.
(3) Paraffin wax (PW) and n-butyl stearate (BS) have complementary thermalperformances, and good chemical compatibility and stability. The optimal ratio of compositeheat storage material is identified for paraffin wax: n-butyl stearate=1:1, based onexperiments on their thermal properties. A composite phase change material is made byvacuum adsorption by rice husk as BS/PW/rice husk phase change material. Differentialscanning calorimetry is used to determine the phase change heat transfer of phase change heatstorage materials, and the density peaks appeared at50.49C and49.54C, respectively; themelting and solidification latent heats, are63.32J/g and59.82J/g, respectively. After3000melting and solidification cycles, BS/PW/rice husk still showed good thermal stability, andinfrared spectral scanning showed that the components were in good compatibility andchemical stability. Scanning electron microscopy showed that most n-butyl stearate andparaffin composites were absorbed inside the rice husk, having good compactness. Withpolystyrene particles replacing rice husk with vacuum adsorption to form BS/PW/polystyreneparticle, a phase change material of higher latent heat value is realized, with its melting andsolidification latent heat of93.61J/g and95.58J/g, respectively. The thermal and chemicalstabilities and compatibility are good. Scanning electron microscopy showed that its densitywas better than the BS/PW/rice husk phase change material. Considering the phase changetemperature and latent heat value, the BS/PW/polystyrene phase change material is a goodheat storage phase change material.
(4) Weak-alkalinized cement can be mixed directly with organic phase changematerials to make concrete blocks. Experiments show that the optimized mixing ratio of cement, fly ash, sand, gravel, ceramsite: lime, gypsum=20:25:17:10:25:1:2. Based on themechanical characteristics (minimum compressive strength and dry density, maximum waterabsorption and softening coefficients) and thermal indexes (maximum thermal conductivity,specific heat, coefficient of heat storage, phase change latent heat value), polystyrene particlephase change blocks have better heat storage capacity, but the rice husk phase change blockshave better mechanical characteristics. The maximum mixture ratio of phase change materialsis restricted by the lower threshold of mechanical properties. We suggest that phase changerice husk content is not more than5%, and polystyrene particles content is not more than12%.
(5) In the solar greenhouse built with concrete blocks of BP/BS/rice husk phase changematerial, we found that the measured indoor air temperature, variations in the typical indoortemperature were lower than the control greenhouse of common bricks, the minimumtemperature and average temperature increased, and the temperature difference betweeninside and outside the north wall is reduced. Jinpeng No.1tomatoes grown in theexperimental greenhouse have better early stage plant height, stem diameter, dry weight, freshweight, and later growth stage plant height, root length, stem diameter, leaf number andflower number, fruit number, weight, plant total weight, etc. The phase transition material hasa clear advantage for the experiment greenhouse than the control one.
(6) Our experiments of inorganic and organic phase change material walls in solargreenhouses show that the new materials have good thermal effects for "cutting peaks andvalleys" in temperature control. The materials can improve the production environment andproduction efficiency of greenhouses. The results of our studies have great practicalapplication values.
（1）研发了两温级无机相变蓄热材料体系。针对优选出的适用北方日光温室的无机相变蓄热材料Na2HPO4·12H_2O，通过优选成核剂和增稠剂、对进行改性（消除过冷度和相分离）实验研究，得到相变温度在33℃左右的温室用蓄热材料体系的质量比为Na2HPO4·12H_2O：硅酸钠：石墨=100:3:3的混合物。对上述高温级蓄热材料体系加质量比为8%的KCl降低相变温度，可获得低温级（25～26℃）的温室用蓄热材料体系，但引起了过冷度增加和相分离现象加剧。对其开展进一步的改性实验研究，得到相变温度为25～26℃左右的温室用最优蓄热材料体系为质量比Na2HPO4·12H_2O：KCl：硅酸钠：石墨=50:4:3:1的混合物。两温级最优蓄热材料体系按不同的比例组合应用于温室，能更好适应于不同气候、不同作物的日光温室中。
（2）无机相变蓄热板墙的应用具有改善温室的作物生产环境、提高温室过冬安全性和生产效益的效果。采用特殊塑料袋封装Na2HPO4·12H_2O相变材料体系，将其镶嵌于温室墙板中形成相变蓄热板墙。典型日和最冷月的连续气温、低温、湿度实测数据显示，相变板墙温室具有提高室内最低温度达2.7℃和平均温度1.5℃，降低室内最高温度1.2℃的明显效果；也有提高室内最低地温0.6℃和平均地温，降低室内最高地温0.7℃的作用；与对室内温度影响相对应，同时也能降低室内最小湿度8%和平均湿度0.5%。相变墙温室与当地的灰砂砖夹沙温室相比，经济性更好。
（3）研发了两种温室用有机蓄热相变材料体系。利用石蜡（PW）和硬脂酸正丁酯（BS）热性能互补性、化学相容性及稳定性，研究不同配比的复合相变材料的热性能，得到最佳温室用蓄热复合材料配比为石蜡：硬脂酸正丁酯热=1：1。以此为复合相变材料，用真空吸附法将其与稻壳制成BS/PW/稻壳定形相变材料。用差式扫描量热法测定相变蓄热材料的相变热流密度峰值位置分别出现在50.49℃和49.54℃，熔解潜热和凝固潜热分别为63.32J/g和59.82J/g。3000次的熔解/凝固循环后，BS/PW/稻壳具有良好的热稳定性。红外光谱扫描表明，各组分有良好的相容性和化学稳定性；扫描电镜微观结构图证明硬脂酸正丁酯和石蜡复合材料多数被吸附进稻壳内部，致密性良好。用聚苯乙烯颗粒代替稻壳用真空吸附法制成的BS/PW/聚苯乙烯颗粒定形相变材料有更大潜热值，其熔解潜热和凝固潜热分别为93.61J/g和95.58J/g。热稳定性、相容性和化学稳定性具佳，扫描电镜表明其致密性优于BS/PW/稻壳定形相变材料。综合考虑相变温度和潜热值两方面，BS/PW/聚苯乙烯颗粒定形相变材料是更优的温室用蓄热相变材料体系。
（4）设计了相变混凝土砌块的制备方法，测试了其热学力学性能。对混凝土弱碱化后与有机定形相变材料直接混合即可制备相变混凝土砌块。实验优化出砌块混凝土的质量配合比为水泥:粉煤灰:细沙:砾石:陶粒:石灰:石膏=20:25:17:10:25:1:2。通过对稻壳相变砌块和聚苯乙烯颗粒相变砌块的力学指标（最低抗压强度、最低干密度、最大吸水率、最大软化系数）和砌块的热学指标（最大导热系数、最大比热容、蓄热系数、相变潜热值）的测试结果分析可知，相变聚苯颗粒砌块蓄热性能优于相变稻壳砌块的蓄热性能，相变聚苯颗粒砌块力学性能却劣于相变稻壳砌块的力学性能。但相变材料的最大掺加量受力学性能的低限值的制约，研究建议相变稻壳掺量不大于5%，聚苯乙烯颗粒掺量不大于12%。
（5）相变混凝土砌块用于日光温室墙体对改善温室生产环境效果明显。将以BP/BS/稻壳为定型相变材料生产的相变混凝土砌块，实测室内的气温发现，该温室的典型日室内气温变化幅度比对照砖温室的小3.5℃，最低温度提高1.7℃和最高温度降低2.4%，北墙内外的温差的变化范围减小3.1℃。温室内种植的金鹏1号番茄，生长初期株高、茎粗、干重、鲜重和生长后期的株高、根长、茎粗、叶数、花序数、结果数、果重、植株总重量等，相变温室较对照温室的状态均有明显优势。
（6）研究得到的无机相变材料墙体和有机相变材料墙体在北方日光温室中的应用效果表明，相变温室具有良好的蓄热性和对温度的“削峰填谷”的调温性能。对改善温室作物的生产环境，提高温室生产效益，均有明显的积极影响。该研究成果有生产实用性和推广应用价值。
Current greenhouses in Northwest China have low thermal effectiveness, and high costsand low efficiency in production. The phase change heat storage technique was used as thebasis for greenhouse wall design to resolve those issues. We identified optimal inorganic andorganic phase change heat storage materials, based on the characteristics of Northern Chinaclimate, solar greenhouse production, and requirements of growth of plants, with respect tothe phase change temperature and latent heat values. Inorganic phase change materials havelow phase change temperature and phase separation. We carried out various experiments withmodified materials, and two types of materials for high and low temperatures were identified.Encapsulated heat storage materials were used as greenhouse wallboards. Based onmeasurements of internal air temperature, humidity and ground temperature in the greenhouse,improvement in greenhouse characteristics was verified. A single kind of organic phasechange material cannot meet the requirements of all greenhouse productions, and solid-liquidmaterials have leakage problems during phase change. We studied compositions and shapingmethods for composite phase change materials, and the mechanical and thermalcharacteristics of the materials, and two different kinds of phase change material for heatstorage system suitable for solar greenhouses were identified, with different latent heat.Phase change blocks were produced by mixing these materials with wall building materials.Greenhouse environmental parameters and plant growth characteristics show that thegreenhouse based on phase change heat storage materials has excellent temperatureadjustment performance.
The major conclusions of this thesis are as follows.
(1) Na2HPO4· H_2O is a phase change heat storage material optimal for solargreenhouses in the north, but its low temperature and phase separation characteristics affectits performance stability. With identified nucleating and thickening agents frommodification experiments, the composition for phase change materials at about33℃isidentified as a mixture with mass ratio of Na2HPO4· H_2O: sodium silicate: graphite=100:3:3.Adding to this high temperature heat storage material system with mass ratio8%KCl toreduce the phase transition temperature, a low temperature (25~26℃) material can beobtained, but this causes over cooling and phase separation. Further modification experiments show that an optimal material with mass ratio of Na2HPO4· H_2O: KCl: sodium silicate:graphite=50:4:3:1has phase transition temperature of25~26℃as well. Heat storagematerials of the two temperatures can be used in solar greenhouses for different crops.
(2) Special plastic packaging was used for the Na2HPO4·12H_2O phase change materialsystem, for embedding in greenhouse wall to form a phase change heat storage wall. Airtemperature, humidity, and low temperature data for typical days and continuousmeasurements for the coldest month show that the greenhouse built with the phase changematerial clearly increased the lowest and average indoor temperatures, reduces the highestindoor temperature. The materials also improved minimum and lowest indoor soiltemperatures, reduced highest indoor soil temperature. Corresponding to the indoortemperatures, the materials can reduce the minimum and average indoor humidity. Comparedwith control greenhouses with lime-sand bricks, phase change wall greenhouses haveimproved performance. This indicates that the phase transition materials have improved cropgrowth environment, winter performance and production efficiency of greenhouses.
(3) Paraffin wax (PW) and n-butyl stearate (BS) have complementary thermalperformances, and good chemical compatibility and stability. The optimal ratio of compositeheat storage material is identified for paraffin wax: n-butyl stearate=1:1, based onexperiments on their thermal properties. A composite phase change material is made byvacuum adsorption by rice husk as BS/PW/rice husk phase change material. Differentialscanning calorimetry is used to determine the phase change heat transfer of phase change heatstorage materials, and the density peaks appeared at50.49C and49.54C, respectively; themelting and solidification latent heats, are63.32J/g and59.82J/g, respectively. After3000melting and solidification cycles, BS/PW/rice husk still showed good thermal stability, andinfrared spectral scanning showed that the components were in good compatibility andchemical stability. Scanning electron microscopy showed that most n-butyl stearate andparaffin composites were absorbed inside the rice husk, having good compactness. Withpolystyrene particles replacing rice husk with vacuum adsorption to form BS/PW/polystyreneparticle, a phase change material of higher latent heat value is realized, with its melting andsolidification latent heat of93.61J/g and95.58J/g, respectively. The thermal and chemicalstabilities and compatibility are good. Scanning electron microscopy showed that its densitywas better than the BS/PW/rice husk phase change material. Considering the phase changetemperature and latent heat value, the BS/PW/polystyrene phase change material is a goodheat storage phase change material.
(4) Weak-alkalinized cement can be mixed directly with organic phase changematerials to make concrete blocks. Experiments show that the optimized mixing ratio of cement, fly ash, sand, gravel, ceramsite: lime, gypsum=20:25:17:10:25:1:2. Based on themechanical characteristics (minimum compressive strength and dry density, maximum waterabsorption and softening coefficients) and thermal indexes (maximum thermal conductivity,specific heat, coefficient of heat storage, phase change latent heat value), polystyrene particlephase change blocks have better heat storage capacity, but the rice husk phase change blockshave better mechanical characteristics. The maximum mixture ratio of phase change materialsis restricted by the lower threshold of mechanical properties. We suggest that phase changerice husk content is not more than5%, and polystyrene particles content is not more than12%.
(5) In the solar greenhouse built with concrete blocks of BP/BS/rice husk phase changematerial, we found that the measured indoor air temperature, variations in the typical indoortemperature were lower than the control greenhouse of common bricks, the minimumtemperature and average temperature increased, and the temperature difference betweeninside and outside the north wall is reduced. Jinpeng No.1tomatoes grown in theexperimental greenhouse have better early stage plant height, stem diameter, dry weight, freshweight, and later growth stage plant height, root length, stem diameter, leaf number andflower number, fruit number, weight, plant total weight, etc. The phase transition material hasa clear advantage for the experiment greenhouse than the control one.
(6) Our experiments of inorganic and organic phase change material walls in solargreenhouses show that the new materials have good thermal effects for "cutting peaks andvalleys" in temperature control. The materials can improve the production environment andproduction efficiency of greenhouses. The results of our studies have great practicalapplication values.
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