CN107010973B - 一种轻质复相多孔隔热耐火材料和莫来石质耐火材料及其制备方法 - Google Patents

一种轻质复相多孔隔热耐火材料和莫来石质耐火材料及其制备方法 Download PDF

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CN107010973B
CN107010973B CN201710325091.XA CN201710325091A CN107010973B CN 107010973 B CN107010973 B CN 107010973B CN 201710325091 A CN201710325091 A CN 201710325091A CN 107010973 B CN107010973 B CN 107010973B
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刘世权
刘志
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Abstract

一种轻质复相多孔隔热耐火材料和莫来石质耐火材料及其制备方法，属于耐火材料领域。耐火材料包括以下重量百分含量的各组份：晶体硅切割废料20~85%；氧化铝粉15~80%。将晶体硅切割废料于250~300oC保温2~4h，再将废料球磨过400目筛，以完成废料的预处理；将预处理后的废料与氧化铝粉均匀混合压制成坯体；脱模后的坯体在110oC干燥2~4h；干燥后的坯体以1~5oC/min的速率升温到1515~1550oC范围内烧结1~4h并随炉冷却。为晶体硅切割废料的回收利用提供新的思路，变废为宝，治理环境污染的同时节约了资源。以晶体硅切割废料中的SiC和Si为硅源，以SiC为成孔剂，无需添加发泡剂或成孔剂，降低生产成本。制备工艺流程简便，产品质量优异，可在建筑领域广泛推广。

Description

一种轻质复相多孔隔热耐火材料和莫来石质耐火材料及其制 备方法
技术领域
本发明涉及一种轻质复相多孔隔热耐火材料和莫来石质耐火材料及其制备方法，属于耐火材料技术领域。
背景技术
轻质多孔隔热耐火材料具有隔热、防火、耐高温等功能，是一种新型工业窑炉用耐火材料。徐明扬等以晶体硅切割废料和Al2O3为主要原料，添加石墨粉作成孔剂，烧结制备出多孔SiC陶瓷。Al2O3和石墨粉掺量分别为30%和10%、烧结温度为1450oC、烧结时间为4h时制备的多孔陶瓷气孔率达42.21%、热膨胀系数为6.64×10-6K-1。杨道媛等则以高铝矾土和冶金硅灰为主要原料，添加聚苯乙烯球作成孔剂，制备出轻质高强的莫来石-刚玉耐火材料。王华等以安徽合肥粉煤灰和当地的黏土为主要原料，添加0.3%的十二烷基苯磺酸钠作发泡剂，采用发泡注浆法在1200oC制备了轻质莫来石耐火制品。这些利用固体废弃物制备轻质多孔隔热耐火材料均需添加发泡剂或成孔剂，工序过程较复杂，成本较高。
莫来石具有耐高温、导热系数小、荷重软化温度高等优良性能，近年来研究人员已成功利用煤矸石、用后Al2O3-C滑板砖、稻壳灰、铝渣等固体废弃物制备出莫来石质耐火材料。晶体硅切割废料是晶体硅片切割过程中排放的固体废弃物，主要由磨料SiC、晶体Si和Fe组成，还含有一定量的聚乙二醇等。晶体硅切割废料堆放占用大量土地，并造成环境污染，还会造成资源的浪费。但并未出现利用晶体硅切割废料为主要原料来制备莫来石质耐火材料的报道。
发明内容
本发明提供一种经由晶体硅切割废料，仅添加不同含量氧化铝制得的坯体，直接加热制备轻质复相多孔隔热耐火材料和莫来石质耐火材料及其制备方法。该方法的思想是通过控制烧结温度和升温速率来控制晶体硅切割废料的氧化过程、SiC氧化比例和晶体硅切割废料与Al2O3粉的比例，使坯体中的SiO2适合与Al2O3生成粘度适中的液相，同时在此液相形成温度范围内另一部分SiC的氧化产生CO2气体，气体封闭于液相中，最终冷却形成多孔结构。另一方面，使SiO2与Al2O3仅生成少量液相，仅起促进坯体烧结致密的作用；减少晶体硅切割废料含量，使SiC较快氧化完全，且生成莫来石相。
本发明通过以下技术方案予以实现：
提供一种轻质复相多孔隔热耐火材料，包括以下重量百分含量的各组份：
晶体硅切割废料 50~85重量份；
氧化铝粉 15~50重量份。
提供一种莫来石质耐火材料，包括以下重量百分含量的各组份：
晶体硅切割废料 20~33重量份；
氧化铝粉 67~80重量份。
所述的晶体硅切割废料主要成分为SiC和Si，SiC所占重量百分含量为55~65%，Si所占重量百分含量为25~30%；作为优选，晶体硅切割废料包括以下重量百分含量的各组份：SiC62.63%，Si27.49%，Fe8.58%，Al2O30.38%，CuO0.31%，CaO0.25%，ZnO0.13%，SO30.13%，Na2O0.10%。
本发明所述轻质复相多孔隔热耐火材料的烧结温度为1515~1535oC，主晶相为莫来石和方石英，且气孔率可由晶体硅切割废料在坯体中所占的重量百分含量和烧结温度制度控制，所述晶体硅切割废料在原料中所占的重量百分含量优选为70~80%。
本发明所述轻质复相多孔隔热耐火材料随晶体硅切割废料在坯体中所占的重量百分含量的增加，莫来石相含量一直增加，方石英相含量一直减少，而气孔率先增加后减小，导热系数先减小后增加，耐火度一直增加。
本发明所述轻质复相多孔隔热耐火材料随烧结温度的增加，莫来石相含量增加，方石英相含量减少，气孔率增加，导热系数减小，耐火度略有增加。
本发明所述莫来石质耐火材料的莫来石相含量可由晶体硅切割废料在坯体中所占的重量百分含量控制，优选为25~30%。
本发明所述莫来石质耐火材料随晶体硅切割废料在坯体中所占的重量百分含量的增加，方石英相含量一直减少，刚玉相含量一直增加，而莫来石相含量先增加后减少，气孔率先减少后增加，耐火度均大于1800oC。
本发明提供了所述轻质复相多孔隔热耐火材料的制备方法，包括以下步骤：
(1)将晶体硅切割废料置于高温电阻炉中于250~300oC保温2~4h，以除掉废料中的大部分聚乙二醇；
(2)将经步骤(1)处理的晶体硅切割废料球磨至全部过400目筛，得到预处理后的晶体硅切割废料；
(3)将预处理后的晶体硅切割废料与氧化铝粉按比例混合均匀得混合料；
(4)将混合料置于模具中以50MPa的压力挤压成型，脱模后得到一定形状的坯体；
(5)将坯体置于恒温干燥箱中经110oC干燥2~4h即得耐火材料干坯；
(6)将耐火材料干坯置于高温电阻炉内以5oC/min的速率升温到900oC，再以3oC/min的速率升温到1400oC，最后以1oC/min的速率升温到1515~1535oC范围内并烧结1~4h，随炉冷却后即可得到多孔轻质隔热耐火材料产品。
本发明同时提供了所述莫来石质耐火材料的制备方法，包括以下步骤：
(1)将晶体硅切割废料置于高温电阻炉中于250~300oC保温2~4h，以除掉废料中的大部分聚乙二醇；
(2)将经步骤(1)处理的晶体硅切割废料球磨至全部过400目筛，得到预处理后的晶体硅切割废料；
(3)将预处理后的晶体硅切割废料与氧化铝粉按比例混合均匀得混合料；
(4)将混合料置于模具中以50MPa的压力挤压成型，脱模后得到一定形状的坯体；
(5)将坯体置于恒温干燥箱中经110oC干燥2~4h即得耐火材料干坯；
(6)将耐火材料干坯置于高温电阻炉内以5oC/min的速率升温到900oC，再以3oC/min的速率升温到1400oC，最后以1oC/min的速率升温到1530~1550oC范围内并烧结1~4h，随炉冷却后即可得到莫来石质耐火材料产品。
本发明的有益效果：
本发明的制备方法工艺简单，可以制备轻质复相多孔隔热耐火材料和莫来石质耐火材料，较大限度地利用了晶体硅切割废料中的各组份，产品附加值高。
本发明所述的轻质复相多孔隔热耐火材料，以晶体硅切割废料中的SiC为成孔材料，无需发泡剂或成孔剂等添加剂，降低生产成本。
本发明所述的莫来石质耐火材料，以晶体硅切割废料中的SiC和Si为硅源，实现了废物利用。
具体实施方式：
下面结合具体实施例来进一步详细说明本发明。
实施例1
一种轻质复相多孔隔热耐火材料，包括以下重量百分含量的各组份：
晶体硅切割废料 85%；
氧化铝粉 15%。
所述的晶体硅切割废料主要成分为SiC和Si，包括以下重量百分含量的各组份：SiC62.63%，Si27.49%，Fe8.58%，Al2O30.38%，CuO0.31%，CaO0.25%，ZnO0.13%，SO30.13%，Na2O0.10%。
制备过程如下：
(1)将晶体硅切割废料置于高温电阻炉中于250~300oC保温2~4h，以除掉废料中的大部分聚乙二醇；
(2)将经步骤(1)处理的晶体硅切割废料球磨至全部过400目筛，得到预处理后的晶体硅切割废料；
(3)将预处理后的晶体硅切割废料与氧化铝粉按比例混合均匀得混合料；
(4)将混合料置于模具中以50MPa的压力挤压成型，脱模后得到一定形状的坯体；
(5)将坯体置于恒温干燥箱中经110oC干燥2~4h即得耐火材料干坯；
(6)将耐火材料干坯置于高温电阻炉内以5oC/min的速率升温到900oC，再以3oC/min的速率升温到1400oC，最后以1oC/min的速率升温到1515oC并烧结1~4h，随炉冷却后即可得到多孔复相轻质隔热耐火材料产品。
测定产品的性能如下：
莫来石相含量/% 22.90
方石英相含量/% 77.10
体积密度/(g﹒cm-3) 0.87
气孔率/% 52.37
导热系数/[W﹒(m﹒K)-1] 0.544
耐火度/oC 1550
上述轻质多孔隔热耐火材料以方石英和莫来石相为主，密度小、气孔率高、导热系数低、耐火度高，可用作高温隔热保温耐火材料广泛使用。
实施例2
一种轻质复相多孔隔热耐火材料，各组份的重量百分含量同实施例1。
所述的晶体硅切割废料中各组份的重量百分含量同实施例1。
除烧结温度改为1535oC外，制备方法同实施例1。
测定产品的性能如下：
莫来石相含量/% 30.25
方石英相含量/% 69.75
体积密度/(g﹒cm-3) 0.68
气孔率/% 66.15
导热系数/[W﹒(m﹒K)-1] 0.345
耐火度/oC 1560
上述轻质多孔隔热耐火材料以方石英和莫来石相为主，密度小、气孔率高、导热系数低、耐火度高，可用作高温隔热保温耐火材料广泛使用。
实施例3
一种轻质多孔隔热耐火材料，包括以下重量百分含量的各组份：
晶体硅切割废料 67%；
氧化铝粉 33%。
所述的晶体硅切割废料中各组份的重量百分含量同实施例1。
制备方法同实施例1。
测定产品的性能如下：
莫来石相含量/% 42.81
方石英相含量/% 55.75
刚玉相含量/% 1.44
体积密度/(g﹒cm-3) 0.85
气孔率/% 64.19
导热系数/[W﹒(m﹒K)-1] 0.442
耐火度/oC 1560
上述轻质多孔隔热耐火材料以方石英和莫来石相为主，密度小、气孔率高、导热系数低、耐火度高，可用作高温隔热保温耐火材料广泛使用。
实施例4
一种轻质多孔隔热耐火材料，包括以下重量百分含量的各组份：
晶体硅切割废料 50%；
氧化铝粉 50%。
所述的晶体硅切割废料中各组份的重量百分含量同实施例1。
制备方法同实施例1。
测定产品的性能如下：
莫来石相含量/% 54.71
方石英相含量/% 42.07
刚玉相含量/% 3.22
体积密度/(g﹒cm-3) 1.24
气孔率/% 52.44
导热系数/[W﹒(m﹒K)-1] 0.718
耐火度/oC 1600
上述轻质多孔隔热耐火材料以方石英和莫来石相为主，密度小、气孔率高、导热系数低、耐火度高，可用作高温隔热保温耐火材料广泛使用。
实施例5
一种莫来石质耐火材料，包括以下重量百分含量的各组份：
晶体硅切割废料 33%；
氧化铝粉 67%。
所述的晶体硅切割废料中各组份的重量百分含量同实施例1。
制备过程如下：
(1)将晶体硅切割废料置于高温电阻炉中于250~300oC保温2~4h，以除掉废料中的大部分聚乙二醇；
(2)将经步骤(1)处理的晶体硅切割废料球磨至全部过400目筛，得到预处理后的晶体硅切割废料；
(3)将预处理后的晶体硅切割废料与氧化铝粉按比例混合均匀得混合料；
(4)将混合料置于模具中以50MPa的压力挤压成型，脱模后得到一定形状的坯体；
(5)将坯体置于恒温干燥箱中经110oC干燥2~4h即得耐火材料干坯；
(6)将耐火材料干坯置于高温电阻炉内以5oC/min的速率升温到900oC，再以3oC/min的速率升温到1400oC，最后以1oC/min的速率升温到1550oC并烧结1~4h，随炉冷却后即可得到莫来石质耐火材料产品。
测定产品的性能如下：
莫来石相含量/% 86.03
方石英相含量/% 9.64
刚玉相含量/% 4.33
体积密度/(g﹒cm-3) 1.48
气孔率/% 27.41
耐火度/oC >1800
上述莫来石质耐火材料以莫来石相为主，耐火度高，可作为高温窑炉用耐火材料广泛使用。
实施例6
一种莫来石质耐火材料，包括以下重量百分含量的各组份：
晶体硅切割废料 25%；
氧化铝粉 75%。
所述的晶体硅切割废料中各组份的重量百分含量同实施例1。
制备方法同实施例5。
测定产品的性能如下：
莫来石相含量/% 92.99
方石英相含量/% 0.59
刚玉相含量/% 6.42
体积密度/(g﹒cm-3) 1.63
气孔率/% 25.17
耐火度/oC >1800
上述莫来石质耐火材料以莫来石相为主，耐火度高，可作为高温窑炉用耐火材料广泛使用。
实施例7
一种莫来石质耐火材料，包括以下重量百分含量的各组份：
晶体硅切割废料 20%；
氧化铝粉 80%。
所述的晶体硅切割废料中各组份的重量百分含量同实施例1。
制备方法同实施例5。
测定产品的性能如下：
莫来石相含量/% 89.80
方石英相含量/% ---
刚玉相含量/% 10.20
体积密度/(g﹒cm-3) 1.55
气孔率/% 26.22
耐火度/oC >1800
上述莫来石质耐火材料以莫来石相为主，耐火度高，可作为高温窑炉用耐火材料广泛使用。

Claims (6)

1.一种轻质复相多孔隔热耐火材料的制备方法，其特征在于包括以下步骤：
(1)按以下重量百分比分别称取原料：
晶体硅切割废料 50～85％；
氧化铝粉 15～50％；
其中，晶体硅切割废料含SiC，Si，Fe主要成分；SiC所占重量百分含量为55～65％，Si所占重量百分含量为25～30％；
(2)将晶体硅切割废料置于高温电阻炉中于250～300℃保温2～4h，以除掉废料中的大部分聚乙二醇；
(3)将经步骤(2)处理的晶体硅切割废料球磨至全部过400目筛，得到预处理后的晶体硅切割废料；
(4)将预处理后的晶体硅切割废料与氧化铝粉按比例混合均匀得混合料；
(5)将混合料置于模具中以50MPa的压力挤压成型，脱模后得到一定形状的坯体；
(6)将坯体置于恒温干燥箱中经110℃干燥2～4h即得耐火材料干坯；
(7)将耐火材料干坯置于高温电阻炉内以5℃/min的速率升温到900℃，再以3℃/min的速率升温到1400℃，最后以1℃/min的速率升温到1515～1535℃范围内并烧结1～4h，随炉冷却后即可得到轻质复相多孔隔热耐火材料产品。
2.一种根据权利要求1所述方法制备的轻质复相多孔隔热耐火材料，其特征在于晶相为莫来石、方石英和刚玉，莫来石相含量为22～55％，方石英相含量42～78％，刚玉相含量为0～4％。
3.根据权利要求2所述轻质复相多孔隔热耐火材料，其特征在于体积密度为0.75～1.25g/cm3，气孔率为50～68％，导热系数为0.350～0.720W/(m·K)，耐火度为1550～1600℃。
4.一种莫来石质耐火材料的制备方法，其特征在于包括以下步骤：
(1)按以下重量百分比分别称取原料：
晶体硅切割废料 20～33％；
氧化铝粉 67～80％；
其中，晶体硅切割废料晶体硅切割废料含SiC，Si，Fe主要成分；SiC所占重量百分含量为55～65％，Si所占重量百分含量为25～30％；
(2)将晶体硅切割废料置于高温电阻炉中于250～300℃保温2～4h，以除掉废料中的大部分聚乙二醇；
(3)将经步骤(2)处理的晶体硅切割废料球磨至全部过400目筛，得到预处理后的晶体硅切割废料；
(4)将预处理后的晶体硅切割废料与氧化铝粉按比例混合均匀得混合料；
(5)将混合料置于模具中以50MPa的压力挤压成型，脱模后得到一定形状的坯体；
(6)将坯体置于恒温干燥箱中经110℃干燥2～4h即得耐火材料干坯；
(7)将耐火材料干坯置于高温电阻炉内以5℃/min的速率升温到900℃，再以3℃/min的速率升温到1400℃，最后以1℃/min的速率升温到1530～1550℃范围内并烧结1～4h，随炉冷却后即可得到莫来石质耐火材料产品。
5.一种根据权利要求4所述方法制备的莫来石质耐火材料，其特征在于晶相为莫来石、方石英和刚玉，莫来石相含量为86～93％，方石英相含量0～10％，刚玉相含量为4～10％。
6.根据权利要求5所述的莫来石质耐火材料，其特征在于体积密度为1.45～1.65g/cm3，气孔率为25～28％，耐火度为大于1800℃。
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