CN106187293B - 一种莫来石碳化硅微孔骨料及其制备方法 - Google Patents

一种莫来石碳化硅微孔骨料及其制备方法 Download PDF

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CN106187293B
CN106187293B CN201610588254.9A CN201610588254A CN106187293B CN 106187293 B CN106187293 B CN 106187293B CN 201610588254 A CN201610588254 A CN 201610588254A CN 106187293 B CN106187293 B CN 106187293B
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silicon carbide
micropore
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mullite
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桑绍柏
任博
李亚伟
徐义彪
王庆虎
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Wuhan University of Science and Engineering WUSE
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Abstract

本发明涉及一种莫来石碳化硅微孔骨料及其制备方法。其技术方案是：先以45~70wt%的矾土生料和30~55wt%的晶体硅切割废液为原料，外加所述原料0.5~5.0wt%的造孔剂，混合均匀，于20~50MPa条件下压制成型，自然干燥，在60~110℃条件下烘烤12~24h；然后升温至1350~1550℃，保温1~12h，再自然冷却至室温，破碎，制得莫来石碳化硅微孔骨料。所述晶体硅切割废液的化学成分是：SiC含量≥35wt%，Si含量≥15wt%，C含量≥4wt%；所述矾土生料的Al2O3含量≥60wt%；矾土生料粒径＜0.074mm。本发明具有生产成本低，工艺简单，节约资源和保护环境的特点；所制备的莫来石碳化硅微孔骨料导热系数低、强度高、耐磨性能好和侵蚀能力强。

Description

一种莫来石碳化硅微孔骨料及其制备方法
技术领域
本发明属于微孔骨料技术领域。尤其涉及一种莫来石碳化硅微孔骨料及其制备方法。
背景技术
近年来，随着高温窑炉的飞速发展及节能减排的迫切需要，窑炉工作衬用耐火材料朝低导热化发展成为一种趋势，而实现低导热化目标的主要方法是开发轻量化微孔骨料。
矾土基耐火材料具有较为优异的化学稳定性能以及高温性能，常作为工作衬广泛应用于炼铁、水泥和化工等高能耗行业，该类耐火材料低导热化的实现对于工业能耗的降低起着举足轻重的作用。“一种微孔轻量矾土耐火骨料及其制备方法”(CN104177107A)专利技术，该技术以70~95wt%的矾土生料和5~30wt%的有机聚合物为原料，外加原料30~60wt%的水，经湿磨、自然干燥和烧成，制得容重为2.5~3.1g/cm3和显气孔率为6~16%的微孔轻量矾土骨料。该微孔轻量矾土骨料利用有机聚合物烧失的过程得到部分微孔，不仅成本高，而且所得原料开口气孔偏高和强度偏低，对用该原料制得的耐火材料抗侵蚀性能不利。
近些年，光伏产业在我国也得到了蓬勃发展。其中，在工业生产太阳能电池基板时会不断排放出大量晶体硅切割废液，这些废液中通常含有聚乙二醇、碳化硅以及硅屑粉。据不完全统计，我国每年被当作废液排放掉的晶体硅切割液达到上万吨。目前切割废液的回收大多以回收聚乙二醇为主，因而导致大量固体废弃物排出，不仅造成了资源的大量浪费，也对环境带来了严重的污染。近年来依靠物理方法实现切割废液中碳化硅粉和单质硅的回收也有相关的专利技术报道，但由于该种回收工艺不够成熟，不仅对设备要求极高，还会带来巨大能耗，经济效益较差。除了以上提纯工艺之外，目前并未有晶体硅切割废液高效综合利用的相关报道。
发明内容
本发明旨在克服现有技术缺陷，目的在于提供一种生产成本低、工艺简单、节约资源和保护环境的莫来石碳化硅微孔骨料的制备方法，用该方法制备的莫来石碳化硅微孔骨料导热系数低、强度高、耐磨性能好和抗侵蚀能力强。
为实现上述目的，本发明所采用的技术方案是：先以45~70wt%的矾土生料和30~55wt%的晶体硅切割废液为原料，外加所述原料0.5~5.0wt%的造孔剂，混合均匀，于20~50MPa条件下压制成型，自然干燥，在60~110℃条件下烘烤12~24h；然后升温至1350~1550℃，保温1~12h，再自然冷却至室温，破碎，制得莫来石碳化硅微孔骨料。
所述矾土生料的Al2O3含量≥60wt%；矾土生料粒径＜0.074mm。
所述晶体硅切割废液的化学成分是：SiC含量≥35wt%，Si含量≥15wt%，C含量≥4wt%。
所述的造孔剂为无烟煤、竹炭粉和糊精中的一种以上；造孔剂的粒径＜0.005mm。
由于采用上述技术方案，本发明与现有技术相比具有如下积极效果：
本发明以矾土生料和晶体硅切割废液为原料，混合均匀后压制成型，煅烧后即得莫来石碳化硅微孔骨料，生产工艺简单；所用主要原料之一为目前产量很大的晶体硅切割废液，不仅对晶体硅切割废液中的主要成分进行了充分的利用，变废为宝，避免了因排放造成的环境污染，而且大大节约了成本，提高了切割废液的产品附加值。
本发明在烧成过程中：晶体硅切割废液中的聚乙二醇可作为造孔剂，有利于提高微孔在材料内部的形成比例；晶体硅切割废液中的单质硅在氧化过程中形成SiO2，所述SiO2伴随体积膨胀能降低材料的平均孔径；晶体硅切割废液中SiC组分可提高高温下骨料内部液相的粘度，液相流动性变差，大大降低了高温下微孔合并和长大的几率，保证材料在高温下仍有较多的微孔存在。本发明不仅节约了大量晶体硅切割废液的处理费用，而且可以最大程度地变废为宝。另外，碳质造孔剂的引入，亦能提升骨料在高温下的粘度，有助于微孔比例的提高。
本发明所制备的莫来石碳化硅微孔骨料闭气孔率高、孔径小且分布均匀、抗熔渣以及侵蚀性气体侵蚀能力强、强度高、导热系数低和耐磨性好，所制得的莫来石碳化硅微孔骨料经检测：平均孔径为0.8~1.2μm；＜1μm气孔的比例为80%~95%；体积密度为2.3~3.2g/cm3；闭气孔率为10~20%；常温耐压强度为120~150MPa；1000℃时的导热系数为0.7~1.2 W/(m•k)。
因此，本发明具有生产成本低，工艺简单，节约资源和保护环境的特点；所制备的莫来石碳化硅微孔骨料导热系数低、强度高、耐磨性能好和抗侵蚀能力强。
具体实施方式
下面结合具体实施方式对本发明作进一步的描述，并非对其保护范围的限制。
为避免重复，先将本具体实施方式所涉及的原料统一描述如下，在实施例中不再赘述。
所述矾土生料的Al2O3含量≥60wt%；矾土生料粒径＜0.074mm。
所述晶体硅切割废液的化学成分是：SiC含量≥35wt%，Si含量≥15wt%，C含量≥4wt%。
所述无烟煤、竹炭粉和糊精的粒径＜0.005mm。
实施例1
一种莫来石碳化硅微孔骨料及其制备方法。先以45~50wt%的矾土生料和50~55wt%的晶体硅切割废液为原料，外加所述原料0.5~3.0wt%的无烟煤，混合均匀，于20~30MPa条件下压制成型，自然干燥，在60~85℃条件下烘烤12~19h；然后升温至1350~1400℃，保温1~7h，再自然冷却至室温，破碎，制得莫来石碳化硅微孔骨料。
本实施例1所制备的莫来石碳化硅微孔骨料经检测：平均孔径为1.1~1.2μm；<1μm气孔的比例为80~89%；体积密度为2.3~2.6g/cm3；闭气孔率为10~14%；常温耐压强度为120~135MPa；1000℃时的导热系数为1.0~1.2W/(m•k)。
实施例2
一种莫来石碳化硅微孔骨料及其制备方法。先以50~55wt%的矾土生料和45~50wt%的晶体硅切割废液为原料，外加所述原料1.0~3.5wt%的竹炭粉，混合均匀，于25~35MPa条件下压制成型，自然干燥，在65~90℃条件下烘烤13~20h；然后升温至1400~1450℃，保温2~8h，再自然冷却至室温，破碎，制得莫来石碳化硅微孔骨料。
本实施例2所制备的莫来石碳化硅微孔骨料经检测：平均孔径为1.0~1.1μm；＜1μm气孔的比例为82~91%；体积密度为2.5~2.8g/cm3；闭气孔率为12~16%；常温耐压强度为125~140MPa；1000℃时的导热系数为0.9~1.1W/(m•k)。
实施例3
一种莫来石碳化硅微孔骨料及其制备方法。先以55~60wt%的矾土生料和40~45wt%的晶体硅切割废液为原料，外加所述原料1.5~4.0wt%的糊精，混合均匀，于30~40MPa条件下压制成型，自然干燥，在70~95℃条件下烘烤14~21h；然后升温至1450~1500℃，保温3~9h，再自然冷却至室温，破碎，制得莫来石碳化硅微孔骨料。
本实施例3所制备的莫来石碳化硅微孔骨料经检测：平均孔径为0.9~1.0μm；＜1μm气孔的比例为84~93%；体积密度为2.7~3.0g/cm3；闭气孔率为14~18%；常温耐压强度为130~145MPa；1000℃时的导热系数为0.8~1.0W/(m•k)。
实施例4
一种莫来石碳化硅微孔骨料及其制备方法。先以60~65wt%的矾土生料和35~40wt%的晶体硅切割废液为原料，外加所述原料1.0~2.5wt%的无烟煤和1.0~2.0wt%的竹炭粉，混合均匀，于35~45MPa条件下压制成型，自然干燥，在75~100℃条件下烘烤15~22h；然后升温至1500~1550℃，保温4~10h，再自然冷却至室温，破碎，制得莫来石碳化硅微孔骨料。
本实施例4所制备的莫来石碳化硅微孔骨料经检测：平均孔径为0.8~0.9μm；＜1μm气孔的比例为86~95%；体积密度为2.9~3.2g/cm3；闭气孔率为16~20%；常温耐压强度为135~150MPa；1000℃时的导热系数为0.7~0.9W/(m•k)。
实施例5
一种莫来石碳化硅微孔骨料及其制备方法。先以65~70wt%的矾土生料和30~55wt%的晶体硅切割废液为原料，外加所述原料1.5~2.5wt%的无烟煤和1.0~2.5wt%的糊精，混合均匀，于40~50MPa条件下压制成型，自然干燥，在80~105℃条件下烘烤16~23h；然后升温至1350~1400℃，保温5~11h，再自然冷却至室温，破碎，制得莫来石碳化硅微孔骨料。
本实施例5所制备的莫来石碳化硅微孔骨料经检测：平均孔径为1.0~1.1μm；＜1μm气孔的比例为84~93%；体积密度为2.9~3.2g/cm3；闭气孔率为16~20%；常温耐压强度为130~145MPa；1000℃时的导热系数为0.7~0.9W/(m•k)。
实施例6
一种莫来石碳化硅微孔骨料及其制备方法。先以60~65wt%的矾土生料和35~40wt%的晶体硅切割废液为原料，外加所述原料0.5~1.5wt%的无烟煤、1.0~1.5wt%竹炭粉和1.0~2,0wt%的糊精，混合均匀，于35~45MPa条件下压制成型，自然干燥，在85~110℃条件下烘烤17~24h；然后升温至1500~1550℃，保温6~12h，再自然冷却至室温，破碎，制得莫来石碳化硅微孔骨料。
本实施例6所制备的莫来石碳化硅微孔骨料经检测：平均孔径为1.1~1.2μm；＜1μm气孔的比例为82~91%；体积密度为2.7~3.0g/cm3；闭气孔率为14~18%；常温耐压强度为125~140MPa；1000℃时的导热系数为0.8~1.0W/(m•k)。
本具体实施方式与现有技术相比具有如下积极效果：
本具体实施方式以矾土生料和晶体硅切割废液为原料，混合均匀后压制成型，煅烧后即得莫来石碳化硅微孔骨料，生产工艺简单；所用主要原料之一为目前产量很大的晶体硅切割废液，不仅对晶体硅切割废液中的主要成分进行了充分的利用，变废为宝，避免了因排放造成的环境污染，而且大大节约了成本，提高了切割废液的产品附加值。
本具体实施方式在烧成过程中：晶体硅切割废液中的聚乙二醇可作为造孔剂，有利于提高微孔在材料内部的形成比例；晶体硅切割废液中的单质硅在氧化过程中形成SiO2，所述SiO2伴随体积膨胀能降低材料的平均孔径；晶体硅切割废液中SiC组分可提高高温下骨料内部液相的粘度，液相流动性变差，大大降低了高温下微孔合并和长大的几率，保证材料在高温下仍有较多的微孔存在。本具体实施方式不仅节约了大量晶体硅切割废液的处理费用，而且可以最大程度地变废为宝。另外，碳质造孔剂的引入，亦能提升骨料在高温下的粘度，有助于微孔比例的提高。
本具体实施方式所制备的莫来石碳化硅微孔骨料闭气孔率高、孔径小且分布均匀、抗熔渣以及侵蚀性气体侵蚀能力强、强度高、导热系数低和耐磨性好，所制得的莫来石碳化硅微孔骨料经检测：平均孔径为0.8~1.2μm；＜1μm气孔的比例为80%~95%；体积密度为2.3~3.2g/cm3；闭气孔率为10~20%；常温耐压强度为120~150MPa；1000℃时的导热系数为0.7~1.2 W/(m•k)。
因此，本具体实施方式具有生产成本低，工艺简单，节约资源和保护环境的特点；所制备的莫来石碳化硅微孔骨料导热系数低、强度高、耐磨性能好和抗侵蚀能力强。

Claims (5)

1.一种莫来石碳化硅微孔骨料的制备方法，其特征在于先以45~70wt%的矾土生料和30~55wt%的晶体硅切割废液为原料，外加所述原料0.5~5.0wt%的造孔剂，混合均匀，于20~50MPa条件下压制成型，自然干燥，在60~110℃条件下烘烤12~24h；然后升温至1350~1550℃，保温1~12h，再自然冷却至室温，破碎，制得莫来石碳化硅微孔骨料。
2.根据权利要求1所述的莫来石碳化硅微孔骨料的制备方法，其特征在于所述矾土生料的Al2O3含量≥60wt%；矾土生料粒径＜0.074mm。
3.根据权利要求1所述的莫来石碳化硅微孔骨料的制备方法，其特征在于所述晶体硅切割废液的化学成分是：SiC含量≥35wt%，Si含量≥15wt%，C含量≥4wt%。
4.根据权利要求1所述的莫来石碳化硅微孔骨料的制备方法，其特征在于所述的造孔剂为无烟煤、竹炭粉和糊精中的一种以上；造孔剂的粒径＜0.005mm。
5.一种莫来石碳化硅微孔骨料，其特征在于所述莫来石碳化硅微孔骨料是按照权利要求1~4项中任一项所述的莫来石碳化硅微孔骨料的制备方法所制备的莫来石碳化硅微孔骨料。
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