CN111943716A - 一种新型赤泥-粉煤灰基梯度结构多孔陶瓷的制备方法 - Google Patents
一种新型赤泥-粉煤灰基梯度结构多孔陶瓷的制备方法 Download PDFInfo
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Abstract
本发明公开一种新型赤泥‑粉煤灰基梯度结构多孔陶瓷的制备方法,包括步骤:赤泥和粉煤灰的预处理:将赤泥块状原样进行粉碎处理后干燥、过筛获得赤泥,粉煤灰选用一级灰;粉料混匀:将过完筛的所述赤泥、所述粉煤灰和发泡剂进行混合处理后获得多孔陶瓷粉末原料;压制成坯及发泡:对所述多孔陶瓷粉末原料进行压制成型获得高温预发泡的坯体,将所述坯体在干燥温度下干燥处理后,进行高温发泡并保温,制得平面孔径均匀且竖直截面呈现梯度结构孔洞排布的多孔陶瓷;本发明通过控制工艺过程,无需使用模具及特殊处理手段即可制备出平面孔径分布较为均匀,在竖直截面方向孔洞呈现出较为明显的梯度结构分布的多孔陶瓷。
Description
技术领域
本发明涉及多孔陶瓷制备技术领域,具体涉及一种新型赤泥-粉煤灰基梯度结构多孔陶瓷的制备方法。
背景技术
利用工业固体废弃物来制备多孔陶瓷对于环境保护和资源的再利用具有重大意义。赤泥作为制铝工业中提取氧化铝所产生的一种红色粉状的强碱固体废弃物,每年产生巨大的堆存量,不仅污染环境也造成了资源的浪费;粉煤灰作为火力发电厂所产生的固体废弃物,具有很高的再利用价值。赤泥和粉煤灰中均含有SiO2、Al2O3、Fe2O3和CaO等,根据赤泥和粉煤灰不同的理化性质,协同互补利用制备多孔陶瓷。
目前,制备多孔陶瓷的方法较多。传统方法有颗粒堆积成型法、添加造孔剂法、发泡造孔剂法、有机前驱体浸渍法、固体烧结法、溶胶凝胶法等,其中有些制备方法工作量大,对原料和仪器设备的要求较多,但只有发泡法是目前制备闭孔陶瓷较成熟的一种方法;另外,也有较为新颖的冷冻干燥法、生物模板法、凝胶注模法和自蔓延高温合成法等。冷冻干燥法的原料中需添加分散剂、粘结剂,制备过程中涉及浆料固模成型及真空干燥,工序繁多且复杂;另外几种新兴工艺对于原料及制备过程的要求都较为精细,需要特殊的表面活性剂或化合物模板。在发泡法制备工艺中,刘涛涌等人使用铅锌尾矿、赤泥和硅砂为主要成分,Na2B4O7为助熔剂,在900℃~1000℃制备一种高孔隙率泡沫陶瓷,微观观察到大量封闭气孔,但是在发泡中不同的发泡机理导致大量不同孔径的闭孔随机分布,这也是目前所见的多孔陶瓷的主要孔型结构。随机的泡孔分布使得多孔陶瓷作为保温材料时出现热导率单一的问题,若泡孔按一定规律排布,则多孔陶瓷在与环境接触的不同面会出现不同的热导率,从而满足于对隔热、保温有特殊要求的领域。
鉴于上述缺陷,本发明创作者经过长时间的研究和实践终于获得了本发明。
发明内容
为解决上述技术缺陷,本发明采用的技术方案在于,提供一种利用赤泥-粉煤灰制备新型梯度结构多孔陶瓷的方法,包括步骤:
S1,赤泥和粉煤灰的预处理:将赤泥块状原样进行粉碎处理后干燥、过筛获得赤泥,粉煤灰选用一级灰;
S2,粉料混匀:将过完筛的所述赤泥、所述粉煤灰和发泡剂进行混合处理后获得多孔陶瓷粉末原料;
S3,压制成坯及发泡:对所述多孔陶瓷粉末原料进行压制成型获得高温预发泡的坯体,将所述坯体在干燥温度下干燥处理后,进行高温发泡并保温,制得平面孔径均匀且竖直截面呈现梯度结构孔洞排布的多孔陶瓷。
较佳的,所述步骤S1中,所述赤泥块状原样在粉碎机中的粉碎处理时间在1min~5min,粉碎后在100℃干燥12h再进行过筛处理,完全过筛后获得所述赤泥粒度为100目~400目。
较佳的,所述步骤S2中,将质量分数为50%~90%的所述赤泥和质量分数为10%~50%的所述粉煤灰进行混合,所述发泡剂的添加量在0.5wt%~1.5wt%。
较佳的,所述发泡剂为碳化硅、碳酸钙、萤石、硫酸钙和二氧化锰中的一种或几种组成的混合物。
较佳的,所述步骤S2中,将所述赤泥、所述粉煤灰和所述发泡剂在混料机中的混匀时间为1h~3h。
较佳的,所述步骤S3中,对所述多孔陶瓷粉末原料进行压制时压力为50MPa~300MPa,所述坯体的干燥处理温度为100℃~140℃,干燥处理时间为6h~12h。
较佳的,所述步骤S3中的高温发泡过程中温度控制为:当前温度小于300℃时,升温速率为4℃/min~8℃/min;当前温度为300℃时,保温20min~60min;当前温度大于300℃时升温速率为3℃/min~5℃/min直至到达发泡温度并保温,所述发泡温度为1220℃~1280℃,保温30min~90min。
与现有技术比较本发明的有益效果在于:1,本发明中除了发泡剂以外,使用的原料完全是工业固废,极大的降低了生产成本,减少了污染,对环保具有重要意义;2,本发明操作简单、成本较低,制备过程中减少了其他辅助性材料的添加及其处理,降低了生产工艺过程的复杂程度;3,本发明通过控制工艺过程,无需使用模具及特殊处理手段即可制备出平面孔径分布较为均匀,在竖直截面方向孔洞呈现出较为明显的梯度结构分布的多孔陶瓷;4,本发明发泡升温程序较为简单,安全可靠,制备出的多孔陶瓷梯度结构孔洞分布与一般的多孔陶瓷具有较为明显的差别。
附图说明
图1为原料赤泥的XRD图;
图2为原料粉煤灰的XRD图;
图3为实施例中制备出的多孔陶瓷竖直方向截面实物图;
图4为制备出的多孔陶瓷平面方向孔洞分布情况。
具体实施方式
以下结合附图,对本发明上述的和另外的技术特征和优点作更详细的说明。
本发明所述利用赤泥-粉煤灰制备新型梯度结构多孔陶瓷的方法,包括步骤:
S1,赤泥和粉煤灰的预处理:将赤泥块状原样在固体试样粉碎机中进行一定时间粉碎处理后,干燥、过筛获得赤泥,粉煤灰选用一级灰;
S2,粉料混匀:将过完筛的所述赤泥、所述粉煤灰和发泡剂按照一定配比进行混合处理,在混料机中混合一段时间后得到制备多孔陶瓷粉末原料;
S3,压制成坯及发泡:对所述多孔陶瓷粉末原料进行压制成型获得高温预发泡的坯体,将所述坯体在一定温度下干燥处理一段时间后,放入高温炉中通过控制升温程序进行高温发泡,保温一段时间后,即可制得平面孔径均匀且竖直截面呈现梯度结构孔洞排布的多孔陶瓷。
所述步骤S1中,所述赤泥块状原样在固体粉碎机中的粉碎处理时间为1min~5min,粉碎后在100℃干燥12h再进行过筛处理,完全过筛后获得所述赤泥粒度为100目~400目。
所述步骤S2中,所述赤泥和所述粉煤灰需按照质量分数分别为50%~90%、10%~50%的量进行混合,发泡剂的添加量为0.5wt%~1.5wt%,发泡剂为碳化硅、碳酸钙、萤石、硫酸钙或二氧化锰等当中的一种或几种组成的混合物。
所述步骤S2中,将配比好的原料在混料机中充分混匀1h~3h。
所述步骤S3中,对所述多孔陶瓷粉末原料进行压制时压力为50MPa~300MPa,且坯体的干燥处理温度为100℃~140℃,时间控制为6h~12h,旨在除去样品中的水分,减少对发泡的影响。
所述步骤S3中的升温程序控制如下:当前温度小于300℃时升温速率为4℃/min~8℃/min,300℃保温20min~60min;当前温度大于300℃时升温速率为3℃/min~5℃/min,发泡温度1220℃~1280℃,保温30min~90min。
如图1和图2所示,图1为原料赤泥的XRD图;图2为原料粉煤灰的XRD图;由XRD图可看出原料赤泥和原料粉煤灰所含的主要成分为制备多孔陶瓷提供了可行性。
本发明中除了发泡剂以外,使用的原料完全是工业固废,极大的降低了生产成本,减少了污染,对环保具有重要意义;本发明操作简单、成本较低,制备过程中减少了其他辅助性材料的添加及其处理,降低了生产工艺过程的复杂程度;本发明通过控制工艺过程、合理优化配料及工艺参数,无需使用模具及特殊处理手段即可制备出平面孔径分布较为均匀,在竖直截面方向孔洞呈现出较为明显的梯度结构分布的多孔陶瓷;本发明发泡升温程序较为简单,安全可靠,制备出的多孔陶瓷梯度结构孔洞分布与一般的多孔陶瓷具有较为明显的差别。
实施例一
原料的预处理与配料:将赤泥粉碎处理使其粒径达到100目,赤泥和粉煤灰在100℃下干燥处理12h,以赤泥加入量为88.65wt%,粉煤灰加入量为9.85wt%,发泡剂的加入量为1.5wt%,在混料机中混料1h;
压制成坯与处理:将混匀的预发泡粉末原料,在压力50MPa下保压60s压制成Φ20×5mm的圆柱形坯体,脱模后的坯体放入干燥箱中140℃处理6h;
发泡程序与降温:将干燥后的坯体放入莫来石匣体中,在高温炉中升温至1220℃,保温30min后,即可得一种新型赤泥-粉煤灰多孔陶瓷,并且孔洞竖直截面方向分布呈现梯度结构。
实施例二
原料的预处理与配料:将赤泥粉碎处理使其粒径达到150目,赤泥与粉煤灰在100℃下干燥12h,以赤泥加入量为78.8wt%,粉煤灰加入量为19.7wt%,发泡剂加入量为1.5wt%,在混料机中混匀1.5h;
压制成坯与处理:将混匀的预发泡粉末原料,在压力125MPa下保压60s压制成Φ20×5mm的圆柱形坯体,脱模后的坯体放入干燥箱中130℃干燥处理8h;
发泡程序与降温:干燥后的样品放入莫来石匣体中,在高温炉中升温至1240℃,保温时间为40min,即可得一种新型赤泥-粉煤灰多孔陶瓷,并且孔洞竖直截面方向分布呈现梯度结构,实物如图3(a)所示。
实施例三
原料的预处理与配料:将赤泥粉碎处理使其粒径达到200目,赤泥与粉煤灰在100℃下干燥12h,以赤泥加入量为69.3wt%,粉煤灰加入量为29.7wt%,发泡剂加入量为1.0wt%,在混料机中混匀2h;
压制成坯与处理:将混匀的预发泡粉末原料,在压力175MPa下保压90s压制成Φ20×5mm的圆柱形坯体,脱模后的坯体放入干燥箱中120℃干燥处理10h;
发泡程序与降温:干燥后的样品放入莫来石匣体中,在高温炉中升温至1260℃,保温时间为50min,即可得一种新型赤泥-粉煤灰多孔陶瓷,并且孔洞竖直截面方向分布呈现梯度结构。
实施例四
原料的预处理与配料:将赤泥粉碎处理使其粒径达到300目,赤泥与粉煤灰在100℃下干燥12h,以赤泥加入量为59.4wt%,粉煤灰加入量为39.6wt%,发泡剂加入量为1.0wt%,在混料机中混匀2.5h;
压制成坯与处理:将混匀的预发泡粉末原料,在压力225MPa下保压120s压制成Φ20×5mm的圆柱形坯体,脱模后的坯体放入干燥箱中110℃干燥处理10h;
发泡程序与降温:干燥后的样品放入莫来石匣体中,在高温炉中升温至1270℃,保温时间为60min,即可得一种新型赤泥-粉煤灰多孔陶瓷,并且孔洞竖直截面方向分布呈现梯度结构,实物如图3(b)所示。
实施例五
原料的预处理与配料:将赤泥粉碎处理使其粒径达到400目,赤泥与粉煤灰在100℃下干燥12h,以赤泥加入量为49.75wt%,粉煤灰加入量为49.75wt%,发泡剂加入量为0.5wt%,在混料机中混匀3h;
压制成坯与处理:将混匀的预发泡粉末原料,在压力300MPa下保压120s压制成Φ20×5mm的圆柱形坯体,脱模后的坯体放入干燥箱中100℃干燥处理12h;
发泡程序与降温:干燥后的样品放入莫来石匣体中,在高温炉中升温至1280℃,保温时间为90min,即可得一种新型赤泥-粉煤灰多孔陶瓷,并且孔洞竖直截面方向分布呈现梯度结构。
以上所述仅为本发明的较佳实施例,对本发明而言仅仅是说明性的,而非限制性的。本专业技术人员理解,在本发明权利要求所限定的精神和范围内可对其进行许多改变,修改,甚至等效,但都将落入本发明的保护范围内。
Claims (7)
1.一种利用赤泥-粉煤灰制备新型梯度结构多孔陶瓷的方法,其特征在于,包括步骤:
S1,赤泥和粉煤灰的预处理:将赤泥块状原样进行粉碎处理后干燥、过筛获得赤泥,粉煤灰选用一级灰;
S2,粉料混匀:将过完筛的所述赤泥、所述粉煤灰和发泡剂进行混合处理后获得多孔陶瓷粉末原料;
S3,压制成坯及发泡:对所述多孔陶瓷粉末原料进行压制成型获得高温预发泡的坯体,将所述坯体在干燥温度下干燥处理后,进行高温发泡并保温,制得平面孔径均匀且竖直截面呈现梯度结构孔洞排布的多孔陶瓷。
2.如权利要求1所述的利用赤泥-粉煤灰制备新型梯度结构多孔陶瓷的方法,其特征在于,所述步骤S1中,所述赤泥块状原样在粉碎机中的粉碎处理时间在1min~5min,粉碎后在100℃干燥12h再进行过筛处理,完全过筛后获得所述赤泥粒度为100目~400目。
3.如权利要求1所述的利用赤泥-粉煤灰制备新型梯度结构多孔陶瓷的方法,其特征在于,所述步骤S2中,将质量分数为50%~90%的所述赤泥和质量分数为10%~50%的所述粉煤灰进行混合,所述发泡剂的添加量在0.5wt%~1.5wt%。
4.如权利要求3所述的利用赤泥-粉煤灰制备新型梯度结构多孔陶瓷的方法,其特征在于,所述发泡剂为碳化硅、碳酸钙、萤石、硫酸钙和二氧化锰中的一种或几种组成的混合物。
5.如权利要求1所述的利用赤泥-粉煤灰制备新型梯度结构多孔陶瓷的方法,其特征在于,所述步骤S2中,将所述赤泥、所述粉煤灰和所述发泡剂在混料机中的混匀时间为1h~3h。
6.如权利要求1所述的利用赤泥-粉煤灰制备新型梯度结构多孔陶瓷的方法,其特征在于,所述步骤S3中,对所述多孔陶瓷粉末原料进行压制时压力为50MPa~300MPa,所述坯体的干燥处理温度为100℃~140℃,干燥处理时间为6h~12h。
7.如权利要求6所述的利用赤泥-粉煤灰制备新型梯度结构多孔陶瓷的方法,其特征在于,所述步骤S3中的高温发泡过程中温度控制为:当前温度小于300℃时,升温速率为4℃/min~8℃/min;当前温度为300℃时,保温20min~60min;当前温度大于300℃时升温速率为3℃/min~5℃/min直至到达发泡温度并保温,所述发泡温度为1220℃~1280℃,保温30min~90min。
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