CN113651634B - 一种防泄漏的复合储热材料的制备方法 - Google Patents

一种防泄漏的复合储热材料的制备方法 Download PDF

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CN113651634B
CN113651634B CN202110918131.8A CN202110918131A CN113651634B CN 113651634 B CN113651634 B CN 113651634B CN 202110918131 A CN202110918131 A CN 202110918131A CN 113651634 B CN113651634 B CN 113651634B
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田丽梅
李子源
王养俊
王欢
商震
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Weihai Institute Of Bionics Jilin University
Jilin University
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Abstract

本发明公开了一种防泄漏的复合储热材料的制备方法，属于储热材料技术领域，针对现有相变储热材料的防泄漏方案所存在缺陷，本发明以聚氨酯海绵为模板依次使用两种不同固含量、粒径与粘度的不同的固含量、粒径与粘度的陶瓷浆料分别浸入内部孔丝和表皮，最后高温烧结并去除模板后，在真空度为‑0.1MPa～‑0.7MPa环境中吸附熔融的相变储热材料的到所述防泄漏的复合储热材料。复合储热材料的芯材填充率经过100小时，相较于初始状态下降了7％，说明具有良好的防泄漏性能，该材料还具有相变储热密度高的特点。

Description

一种防泄漏的复合储热材料的制备方法
技术领域
本发明属于储热材料技术领域。
背景技术
相变储热材料在融化时受热融化时会发生泄漏，通常，为了防止泄露，一是使用其他材料进行封装，如环氧树脂与聚酰胺树脂、金属容器或管道等，缺点是工序复杂，使用温度受限，金属容器易被腐蚀，二是相变材料与多孔材料复合，在依靠微纳级空隙的束缚作用壁面融化的相变材料流出，但此方法限制了相变材料的流动，削弱了热对流强度，并且孔隙率低，储热密度也较低。
发明内容
为了避免相变材料在使用过程中的泄露，本发明提出了一种防泄漏的复合储热材料及其制备方法。
本发明提出的防泄漏的复合储热材料由陶瓷骨架和相变芯材复合而成。
所述陶瓷骨架由内部大孔和表面微孔构成，内部大孔的孔径为0.8-3mm，表面微孔的孔径为1-20微米，微孔层的厚度为0.5-2mm。
一种防泄漏的复合储热材料的制备方法如下：
1)先将孔径为0.8-3mm的聚氨酯海绵用浓度为10-25wt％NaOH溶液浸泡1.5-3小时；
2)将聚氨酯海绵浸入陶瓷浆料A，使浆料完全充满聚氨酯海绵内部，并将多余的浆料挤出，海绵丝网表面附着的浆料厚度在0.2-0.5mm，之后静止干燥24小时定型，获得骨架一。
3)将步骤2)中获得的骨架一的各个面分别浸入陶瓷浆料B中0.5-2mm。
4)将定型后的聚氨酯海绵置入高温炉中，在500-600摄氏度保温2小时，将聚氨酯烧除，之后继续升温至1600度并保温一定时间，获得陶瓷骨架。
5)将相变芯材放入容器中置于真空高温炉中，加热至熔融后，将陶瓷骨架浸入芯材液体中，在真空度为-0.1MPa～-0.7MPa环境中吸附30分钟以上，直至陶瓷骨架内部空隙完全充满相变芯材。
其中，陶瓷浆料A与陶瓷浆料B具有不同的固含量、粒径与粘度。
陶瓷浆料A的组分为：陶瓷粉末50-75wt％，粒径为1000目～3000目，助烧剂5-10wt％，粘接剂2-8wt％，分散剂0.5-2wt％,去离子水10-46wt％。
陶瓷浆料B的组分为：陶瓷粉末45-65wt％，粒径为3500目～5000目，助烧剂5-10wt％，粘接剂4-10wt％，分散剂0.5-2wt％，去离子水10-46wt％
陶瓷浆料A和陶瓷浆料B选自碳化硅、氧化铝、氮化铝和氮化硅中的一种；
助烧剂为氧化铝和/或高岭土；粘接剂为羧甲基纤维素钠，分散剂为聚丙烯酸钠。
相变芯材包括但不限于硝酸钠、硝酸钾等硝酸盐或亚硝酸盐，氯化钠、氯化钾等氯盐，碳酸钠、碳酸钾等碳酸盐以及氟盐。
本发明的有益效果：
本发明所提供的防泄漏的复合储热材料内部为相互连通的大孔，具有较高的负载率，储热密度高，200度温差下储热密度能够达到237W/m*K，且不会限制芯材的流动，表皮为微孔，使用时芯材不易泄露。复合储热材料的芯材填充率经过100小时，相较于初始状态仅下降了7％，说明具有良好的防泄漏性能。
附图说明
图1为本发明方法步骤流程示意图。
图2陶瓷骨架内部结构照片
图3陶瓷骨架照片
图4表皮扫面电镜照片
图5复合储热材料芯材填充率随时间变化曲线
具体实施方式
实施例1
1)先将孔径为0.8-3mm的聚氨酯海绵用NaOH进行预处理。
2)将聚氨酯海绵浸入陶瓷浆料A，使浆料完全充满聚氨酯海绵内部，并将多余的浆料挤出，海绵丝网表面附着的浆料厚度在0.2-0.5mm，之后静止干燥24小时定型，获得骨架一。
3)将步骤2)中获得的骨架一的各个面分别浸入陶瓷浆料B中0.5-2mm。
4)将定型后的泡沫置入高温炉中，在500-600摄氏度保温2小时，将聚氨酯烧除，之后继续升温至1600度并保温一定时间，获得陶瓷骨架。
5)将相变芯材放入容器中置于真空高温炉中，加热至熔融后，将陶瓷骨架浸入芯材液体中，在真空度为-0.1MPa～-0.7MPa环境中吸附30分钟以上，直至陶瓷骨架内部空隙完全充满相变芯材。
陶瓷浆料A的组分为：碳化硅粉末60wt％，粒径为2000目，氧化铝和高岭土各6wt％，羧甲基纤维素钠1.5wt％，聚丙烯酸钠0.5wt％,去离子水26wt％。
陶瓷浆料B的组分为：碳化硅粉末56wt％，粒径为3000目与5000目各50％，氧化铝8wt％，高岭土6wt％，羧甲基纤维素钠5wt％，聚丙烯酸钠0.5wt％,去离子水24.5wt％.
由于表面微孔层的空隙是由陶瓷粉末颗粒之间的间隙形成的，粒径越大，空隙越大，利于真空吸附过程中相变芯材的吸附，但在常压环境工作芯材容易泄露，反之粒径越小，空隙越小，芯材不容易泄露，但会影响芯材的吸附，为了兼顾吸附过程与防止泄露，所以陶瓷浆料B中粉末粒径为3000目与5000目各50％。陶瓷浆料B中粘接剂含量高于浆料A是为了提高浆料粘度，避免浆料浸入大孔空隙过多，并提高表皮与大孔区域的连接强度。
性能测试：
以太阳盐(40wt％硝酸钾+60wt％硝酸钠)作为芯材，对制得得复合储热材料进行测试.导热率为2.1W/m*K高于纯太阳盐0.59W/m*K，200度温差下储热密度为237W/m*K。为了评估其防泄漏性能，将获得的复合相变材料样品置于鼓风高温箱内，升温至熔点以上，并开启鼓风机，使热气流流过样品表面，每隔1小时对样品重量进行称重，并计算填充率，填充率通过芯材重量除以芯材密度再除以材料体积计算得到。复合储热材料的芯材填充率经过100小时，相较于初始状态下降了7％，说明具有良好的防泄漏性能。
以上实施例仅作为本发明的优选方式，在以下范围内均可实现本发明方法：
陶瓷浆料A的组分为：陶瓷粉末50-75wt％，粒径为1000目～3000目，助烧剂5-10wt％，粘接剂2-8wt％，分散剂0.5-2wt％,去离子水10-30wt％。
陶瓷浆料B的组分为：陶瓷粉末45-65wt％，粒径为3500目～5000目，助烧剂5-10wt％，粘接剂4-10wt％，分散剂0.5-2wt％，去离子水10-33wt％。
陶瓷浆料A和陶瓷浆料B选自碳化硅、氧化铝、氮化铝和氮化硅中的一种。
所述的相变芯材包括但不限于硝酸钠、硝酸钾等硝酸盐或亚硝酸盐，氯化钠、氯化钾等氯盐，碳酸钠、碳酸钾等碳酸盐以及氟盐。

Claims (5)

1.一种防泄漏的复合储热材料的制备方法，其特征在于，该方法的步骤如下：
1）先将孔径为0.8-3mm的聚氨酯海绵用浓度为10-25wt%的NaOH溶液浸泡1.5-3小时；
2）将聚氨酯海绵浸入陶瓷浆料A，使浆料完全充满聚氨酯海绵内部，并将多余的浆料挤出，海绵丝网表面附着的浆料厚度在0.2-0.5mm，之后静止干燥24小时定型，获得骨架一；
3）将步骤2）中获得的骨架一的各个面分别浸入陶瓷浆料B中0.5-2mm；
4）将定型后的聚氨酯海绵置入高温炉中，在500-600摄氏度保温2小时，将聚氨酯烧除，之后继续升温至1600度并保温一定时间，获得陶瓷骨架；所述陶瓷骨架由内部大孔和表面微孔构成，内部大孔的孔径为0.8-3mm，表面微孔的孔径为1-20微米，微孔层的厚度为0.5-2mm；
5）将相变芯材放入容器中置于真空高温炉中，加热至熔融后，将陶瓷骨架浸入芯材液体中，在真空度为-0.1MPa~ -0.7MPa环境中吸附30分钟以上，直至陶瓷骨架内部空隙完全充满相变芯材；
其中，陶瓷浆料A与陶瓷浆料B具有不同的固含量、粒径与粘度，陶瓷浆料A的固含量>陶瓷浆料B的固含量，陶瓷浆料A的粒径>陶瓷浆料B的粒径，陶瓷浆料A的粘度＜陶瓷浆料B的粘度。
2.根据权利要求1所述的防泄漏的复合储热材料的制备方法，其特征在于，
陶瓷浆料A的组分为：陶瓷粉末50-75wt%，粒径为1000目~3000目，助烧剂5-10wt%，粘接剂2-8wt%，分散剂0.5-2 wt%,去离子水10-30wt%；
陶瓷浆料B的组分为：陶瓷粉末45-65wt%，粒径为3500目~5000目，助烧剂5-10wt%，粘接剂4-10wt%，分散剂0.5-2 wt%，去离子水10-46wt%，陶瓷浆料B各组分之和为100wt%。
3.根据权利要求2所述的防泄漏的复合储热材料的制备方法，其特征在于，陶瓷浆料A和陶瓷浆料B中的陶瓷粉末选自碳化硅、氧化铝、氮化铝和氮化硅中的一种；助烧剂为氧化铝和/或高岭土；粘接剂为羧甲基纤维素钠；分散剂为聚丙烯酸钠。
4.根据权利要求1所述的防泄漏的复合储热材料的制备方法，其特征在于，相变芯材为硝酸盐、亚硝酸盐、氯盐、碳酸盐或氟盐。
5.一种根据权利要求1所述的防泄漏的复合储热材料的制备方法得到的防泄漏的复合储热材料。
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