CN114890811A - 利用矿山固废制备多孔相变储能材料及方法 - Google Patents
利用矿山固废制备多孔相变储能材料及方法 Download PDFInfo
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Abstract
本发明的目的是针对相变材料传热效率低、热导率低、易泄露、化学稳定性不稳定等问题，提供一种利用矿山固废制备多孔相变储能材料及方法。本发明材料包括多孔陶瓷和位于多孔陶瓷内部的相变材料；所述多孔陶瓷由陶瓷原料铁尾矿和废石与添加剂的混合物经烧结制得；所述相变材料为石蜡、碳纳米管、交联聚乙烯和氯化钠的混合物。本发明相变储能材料的多孔陶瓷内的气泡分布排列大小均匀，相变材料不会泄露，且相变材料传热效率高、热导率高、具有良好的化学稳定性，价格成本低廉无毒性，无过冷现象发生，具有优良的储热性能。
Description
技术领域
本发明属于建筑材料技术领域，特别涉及一种利用矿山固废制备多孔相变储能材料及方法。
背景技术
在对矿石开采和分选过程中，会产生大量的废石和尾矿。尾矿的堆积不仅影响环境，还占用土地，浪费资源。有必要开发尾矿回收利用的方法以减少尾矿的堆积量。
相变储能材料是指在一定温度范围内，利用材料本身相态或结构变化，向环境自动吸收或释放潜热，从而达到调控环境温度的一类材料。当环境温度高于相变温度时，材料吸收并储存能量，以降低环境温度；当环境温度低于相变温度时，材料释放储存的能量，以提高环境的温度；相变材料可选择熔化潜热高、相变过程可逆性好、膨胀收缩性小、过冷或过热现象少、有合适的相变温度、能满足需要控制的特定温度、导热系数大且无毒的材料。相变材料为潜热储能的功能介质，其选择对储能材料的性能具有决定性的影响。近年来，随着对相变储能材料的研究，复合相变储能材料引起了广泛关注。受相变材料性能的限制，其传热效率低、热导率低、易泄露、化学稳定性差等问题仍有待解决。
现有技术中也有利用铁尾矿制备相变储能材料的技术，例如申请号201710134385.4的发明专利“一种石蜡/铁尾矿陶瓷复合相变储能材料及其熔融浸渍制备方法”，该发明制备的相变储能材料其孔隙为开孔，相变材料熔融浸渍可能会发生泄露。
发明内容
本发明的目的是针对相变材料传热效率低、热导率低、易泄露、化学稳定性不稳定等问题，提供一种利用矿山固废制备多孔相变储能材料及方法。本发明相变储能材料的多孔陶瓷内的气泡分布排列大小均匀，开孔和闭孔可随温度进行转换，相变材料不会泄露，且相变材料传热效率高、热导率高、膨胀收缩性小、相变过程可逆性好、具有良好的化学稳定性，价格成本低廉无毒性，无过冷现象发生，具备优良的储热性能。
本发明的技术方案之一为，一种利用矿山固废制备多孔相变储能材料，包括多孔陶瓷和位于多孔陶瓷内部的相变材料；
所述多孔陶瓷由陶瓷原料铁尾矿和废石与添加剂的混合物经烧结制得；所述相变材料为石蜡、碳纳米管、交联聚乙烯和氯化钠的混合物。
进一步的，所述储能材料，陶瓷原料中的铁尾矿和废石的质量比为1~2:1。
进一步的，所述储能材料，所述添加剂包括粘结剂、流变剂、分散剂、消泡剂、润滑剂、基体改性剂，加入量依次为陶瓷原料质量的0.3~0.6wt%，0.3~0.6wt%，1.7~2.2wt%，0.3~0.6wt%，0.1~0.3wt%，0.8~1.2wt%；粘结剂为聚乙烯醇PVA和硅溶胶，二者质量比例为1~3:1；流变剂为高岭土和聚酰胺蜡，二者质量比例为0.5~1:1；分散剂为聚乙二醇；消泡剂为乙醇；润滑剂为氧化蜡；基体改性剂Gemini。
进一步的，所述储能材料，所述石蜡、碳纳米管、交联聚乙烯和氯化钠的质量份比例为：65~85份：1.5~3.6份：3.0~5.7份：1.6~2.7份。
进一步的，所述储能材料，多孔陶瓷孔隙率﹥75%。
进一步的，所述储能材料，导热系数为0.4~0.5W/m•K，相变潜热为99~111J/g，石蜡填充率为91.2~98.1％。
作为优选，所述储能材料，润滑剂聚乙烯蜡为氧化聚乙烯蜡，长链分子上有一定量的羰基和羟基，可提高有机物的相溶性，起到润滑作用。
本发明的技术方案之二为，一种利用矿山固废制备多孔相变储能材料方法，包括如下步骤：
1）按比例取石蜡、碳纳米管、交联聚乙烯和氯化钠，将石蜡和NaCl混合，加热到熔融状态；
2）再将交联聚乙烯和碳纳米管分别加入，混合均匀，制备成相变材料；
2）将利用废石和铁尾矿制备的多孔陶瓷在130~150 ℃下预热10~15 min，与相变材料进行浸渍处理，既得多孔相变储能材料。
进一步的，上述利用矿山固废制备多孔相变储能材料方法，所述利用废石和铁尾矿制备的多孔陶瓷的制备方法为：
1）将铁尾矿与废石经过球磨制成过200目筛的粉末，以水为溶剂，制成料浆，且在浆料中按比例加入依次加入粘结剂、流变剂、分散剂、消泡剂、润滑剂，搅拌均匀，制备成浆料；
2）对有机泡沫体进行预处理，即是将有机泡沫体浸入质量浓度10-20%NaOH溶液中，40-60 ℃下处理2-6h，再反复揉搓3~5min，并用清水洗干净后晾干；将有机泡沫体与浆料混合，进行浸渍处理，即进行挂浆，挂浆过程中反复挤压有机泡沫体，使浆料充分的挂在有机泡沫体上，然后去除多余浆料，在室温的条件下干燥18~24 h，再在70~90℃的干燥箱中干燥14~18h，得到胚体；
3）对胚体进行烧结，烧成多孔陶瓷。
进一步的，所述有机泡沫体为聚氨酯泡沫体。
进一步的，烧结过程是先升温至180~200℃，升温速率为2~2.5℃/min并保温45~90min，排除有机泡沫体，再升温至750~800℃，升温速率为3~4℃/min并保温1.5~2.5h，然后以5~6℃/min的升温速率烧至1100~1200℃并保温1.5~2.5h。
进一步的，在浸渍处理后，对聚氨酯泡沫进行低温处理，将聚氨酯泡沫在3-8℃左右保持1.5～2.5h。
作为优选，交联聚乙烯具有典型网状空间结构，能够有效的提升材料化学稳定性，改善复合材料的力学性能。
作为优选，熔融状态下相变材料中加入NaCl能够使其储热性能增强，储能密度变高。
作为优选，相变材料中加入碳纳米管能提高其热导性，一定程度上弥补了石蜡导热率低的缺点，使其性能更加优良。
作为优选，制备多孔陶瓷的原料铁尾矿和废石中含有金属物质，如铜等，一定程度上亦能增加相变材料的导热率。
作为优选，在进行浸渍处理时，加入Gemini作为基体改性剂，用于水性体系，一是能够减少聚氨酯的水敏性问题，改善其黏附力，促进浆料附着厚度的均匀性，二是在弱碱性条件下（氢氧化钠和硅溶胶为碱性）能够与聚乙二醇、聚酰胺蜡交联，在孔隙内形成一层“隔膜”，该“隔膜”随温度（>130℃）升高会发生破裂，随着温度的降低（<60℃）会再次形成。
与现有技术相比，本发明的有益效果为：
1.本发明所提供的一种铁尾矿与废石多孔相变储能材料及其制备方法的有益效果是通过在孔隙率高（高达75%以上）的多孔陶瓷内浸渍相变材料。
2.多孔陶瓷内的气泡分布排列大小均匀，对相变材料而言，多孔陶瓷相当于多孔骨架，可通过毛细管力的作用使相变材料不会泄露，且相变材料传热效率高、热导率高、具有良好的化学稳定性，价格成本低廉无毒性，无过冷现象发生，具有优良的储热性能。
具体实施方式
以下通过具体的实施方式对本发明作进一步说明。
实施例1
一种利用矿山固废制备多孔相变储能材料，包括多孔陶瓷和位于多孔陶瓷内部的相变材料；
所述多孔陶瓷由陶瓷原料铁尾矿和废石与添加剂的混合物经烧结制得，铁尾矿与废石的质量比为1:1；所述相变材料为石蜡、碳纳米管、交联聚乙烯和氯化钠的混合物，质量份数比为80份：3份：5.2份：2.2份。
所述添加剂包括粘结剂（聚乙烯醇PVA和硅溶胶，二者质量比例为2:1）、流变剂（高岭土和聚酰胺蜡，二者质量比例为2:3）、分散剂（聚乙二醇）、消泡剂（乙醇）、润滑剂（氧化聚乙烯蜡）、基体改性剂（Gemin），加入量依次为陶瓷原料质量的0.5wt%，0.5wt%，2.0wt%，0.5wt%，0.1wt%，1.0wt%。
制备方法为：
1）取200目的陶瓷粉料120 g、100目陶瓷粉料的120 g、60目陶瓷粉料的60 g，以水为溶剂，制成料浆，浆料固含量为60 %，分散剂、流变剂、粘结剂、消泡剂、润滑剂、基体改性剂分别为1.51 g、1.51g、6.12 g、1.51 g、0.30 g、3. 03g，将配料倒入烧杯内，进行搅拌；
2）将有机泡沫体预处理，即浸入质量浓度15%NaOH溶液中，50℃下处理4h，再反复揉搓4min，并用清水洗干净后晾干；将预处理厚度有机泡沫体与浆料混合，浸渍处理，即进行挂浆，挂浆过程中反复挤压有机泡沫体，使浆料充分的挂在有机泡沫体上，然后去除多余浆料，在室温的条件下干燥24h，再在90℃的干燥箱中干燥14h，得到胚体；
3）将胚体脱模放入马弗炉中，先升温至200℃，升温速率为2.5℃/min，并保温1h，排除有机泡沫体，再升温至800℃，升温速率为4℃/min并保温2h，后以6℃/min的升温速率烧至1200℃，并保温1.5h，既得多孔陶瓷；
4）将80g石蜡在100℃下熔融，事先在石蜡中加入2.2g熔融无机盐NaCl，加入5.2g交联聚乙烯，再加入3.0g的碳纳米管，制备成相变材料；
5）将多孔陶瓷在200 ℃下预热20 min，浸渍相变材料，即得多孔相变储能材料。
所制备的复合相变储能材料其导热系数为0.47W/m•K，相变潜热为101J/g，石蜡填充率为97.5％。
实施例2
一种利用矿山固废制备多孔相变储能材料，包括多孔陶瓷和位于多孔陶瓷内部的相变材料；
所述多孔陶瓷由陶瓷原料铁尾矿和废石与添加剂的混合物经烧结制得，铁尾矿与废石的质量比为1:1；所述相变材料为石蜡、碳纳米管、交联聚乙烯和氯化钠的混合物，占相变材料质量的80wt%，3.0wt%，5.2wt%，2.2wt%。
所述添加剂包括粘结剂（聚乙烯醇PVA和硅溶胶，二者质量比例为2:1）、流变剂（高岭土和聚酰胺蜡，二者质量比例为2:3）、分散剂（聚乙二醇）、消泡剂（乙醇）、润滑剂（氧化聚乙烯蜡）、基体改性剂（Gemin），加入量依次为陶瓷原料质量的0.5wt%，0.5wt%，2.0wt%，0.5wt%，0.1wt%，1.0wt%。
制备方法为：
1）同实施例1步骤1）；
2）同实施例1步骤2）；
3）将胚体脱模放入马弗炉中，先升温至180℃，升温速率为28℃/min，并保温45min，排除有机泡沫体，再升温至750℃，升温速率为3℃/min并保温1.5h，后以6℃/min的升温速率烧至1100℃，并保温2h，既得多孔陶瓷；
4）将80g石蜡在100℃下熔融，事先在石蜡中加入2.2g熔融无机盐NaCl，加入2.6g交联聚乙烯，再加入1.5g的碳纳米管，制备成相变材料；
5）将多孔陶瓷在150 ℃下预热15min，浸渍相变材料，即得多孔相变储能材料。
所制备的复合相变储能材料其导热系数为0.40W/m•K，相变潜热为111J/g，石蜡填充率为91.2％。
实施例3
一种利用矿山固废制备多孔相变储能材料，原料同实施例1。
区别在于制备方法中的步骤5）为将多孔陶瓷在2000 ℃下预热30min，浸渍相变材料，即得多孔相变储能材料。
所制备的复合相变储能材料其导热系数为0.50W/m•K，相变潜热为99J/g，石蜡填充率为98.1％。
实施例4
一种利用矿山固废制备多孔相变储能材料，包括多孔陶瓷和位于多孔陶瓷内部的相变材料；
所述多孔陶瓷由陶瓷原料铁尾矿和废石与添加剂的混合物经烧结制得，铁尾矿与废石的质量比为2:1；所述相变材料为石蜡、碳纳米管、交联聚乙烯和氯化钠的混合物，质量份数比为85份：2.5份：3.0份：1.6份。
所述添加剂包括粘结剂（聚乙烯醇PVA和硅溶胶，二者质量比例为1:1）、流变剂（高岭土和聚酰胺蜡，二者质量比例为1:1）、分散剂（聚乙二醇）、消泡剂（乙醇）、润滑剂（氧化聚乙烯蜡）、基体改性剂（Gemin），加入量依次为陶瓷原料质量的0.3wt%，0.3wt%，1.7wt%，0.3wt%，0.2wt%，0.8wt%。
制备方法同实施例2。
实施例5
一种利用矿山固废制备多孔相变储能材料，包括多孔陶瓷和位于多孔陶瓷内部的相变材料；
所述多孔陶瓷由陶瓷原料铁尾矿和废石与添加剂的混合物经烧结制得，铁尾矿与废石的质量比为2:1；所述相变材料为石蜡、碳纳米管、交联聚乙烯和氯化钠的混合物，质量份数比为65份：3.份：5.7份：2.7份。
所述添加剂包括粘结剂（聚乙烯醇PVA和硅溶胶，二者质量比例为3:1）、流变剂（高岭土和聚酰胺蜡，二者质量比例为1:2）、分散剂（聚乙二醇）、消泡剂（乙醇）、润滑剂（氧化聚乙烯蜡）、基体改性剂（Gemin），加入量依次为陶瓷原料质量的0.6wt%，0.6wt%，2.2wt%，0.6wt%，0.3wt%，1.2wt%。
制备方法同实施例2。
Claims (10)
1.一种利用矿山固废制备多孔相变储能材料，其特征在于，包括多孔陶瓷和位于多孔陶瓷内部的相变材料；
所述多孔陶瓷由陶瓷原料铁尾矿和废石与添加剂的混合物经烧结制得；所述相变材料为石蜡、碳纳米管、交联聚乙烯和氯化钠的混合物；所述添加剂包括粘结剂、流变剂、分散剂、消泡剂、润滑剂、基体改性剂。
2.根据权利要求1所述的利用矿山固废制备多孔相变储能材料，其特征在于，陶瓷原料中的铁尾矿和废石的质量比为1~2:1。
3.根据权利要求1所述的利用矿山固废制备多孔相变储能材料，其特征在于，所述粘结剂、流变剂、分散剂、消泡剂、润滑剂、基体改性剂，加入量依次为陶瓷原料质量的0.3~0.6wt%，0.3~0.6wt%，1.7~2.2wt%，0.3~0.6wt%，0.1~0.3wt%，0.8~1.2wt%；粘结剂为聚乙烯醇PVA和硅溶胶，二者质量比例为1~3:1；流变剂为高岭土和聚酰胺蜡，二者质量比例为0.5~1:1；分散剂为聚乙二醇；消泡剂为乙醇；润滑剂为氧化蜡；基体改性剂Gemini。
4.根据权利要求1所述的利用矿山固废制备多孔相变储能材料，其特征在于，所述石蜡、碳纳米管、交联聚乙烯和氯化钠的质量份比例为：65~85份：1.5~3.6份：3.0~5.7份：1.6~2.7份。
5.根据权利要求1所述的利用矿山固废制备多孔相变储能材料，其特征在于，多孔陶瓷孔隙率﹥75%。
6.根据权利要求1所述的利用矿山固废制备多孔相变储能材料，其特征在于，导热系数为0.4~0.5W/m•K，相变潜热为99~111J/g，石蜡填充率为91.2~98.1％。
7.一种利用矿山固废制备多孔相变储能材料方法，其特征在于，包括如下步骤：
1）按比例取石蜡、碳纳米管、交联聚乙烯和氯化钠，将石蜡和NaCl混合，加热到熔融状态；
2）再将交联聚乙烯和碳纳米管分别加入，混合均匀，制备成相变材料；
2）将利用废石和铁尾矿制备的多孔陶瓷在130~150 ℃下预热10~15 min，与相变材料进行浸渍处理，既得多孔相变储能材料。
8.根据权利要求7所述的利用矿山固废制备多孔相变储能材料方法，其特征在于，所述利用废石和铁尾矿制备的多孔陶瓷的制备方法为：
1）将铁尾矿与废石经过球磨制成过200目筛的粉末，以水为溶剂，制成料浆，且在浆料中按比例加入依次加入粘结剂、流变剂、分散剂、消泡剂、润滑剂，搅拌均匀，制备成浆料；
2）对有机泡沫体进行预处理，即是将有机泡沫体浸入质量浓度10-20%NaOH溶液中，40-60 ℃下处理2-6h，再反复揉搓3~5min，并用清水洗干净后晾干；将有机泡沫体与浆料混合，进行浸渍处理，即进行挂浆，挂浆过程中反复挤压有机泡沫体，使浆料充分的挂在有机泡沫体上，然后去除多余浆料，在室温的条件下干燥18~24 h，再在70~90℃的干燥箱中干燥14~18h，得到胚体；
3）对胚体进行烧结，烧成多孔陶瓷。
9.根据权利要求7所述的利用矿山固废制备多孔相变储能材料方法，其特征在于，所述有机泡沫体为聚氨酯泡沫体；在浸渍处理后，对聚氨酯泡沫进行低温处理，将聚氨酯泡沫在3-8℃左右保持1.5～2.5h。
10.根据权利要求7所述的利用矿山固废制备多孔相变储能材料方法，其特征在于，烧结过程是先升温至180~200℃，升温速率为2~2.5℃/min并保温45~90min，排除有机泡沫体，再升温至750~800℃，升温速率为3~4℃/min并保温1.5~2.5h，然后以5~6℃/min的升温速率烧至1100~1200℃并保温1.5~2.5h。
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