CN114195482A - 一种贝壳粉基多孔耐高温材料及其制备方法、应用 - Google Patents

一种贝壳粉基多孔耐高温材料及其制备方法、应用 Download PDF

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CN114195482A
CN114195482A CN202111666252.4A CN202111666252A CN114195482A CN 114195482 A CN114195482 A CN 114195482A CN 202111666252 A CN202111666252 A CN 202111666252A CN 114195482 A CN114195482 A CN 114195482A
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胡先海
房利生
梁运动
钱丰
吴秀秀
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Anhui Shiqing Environmental Protection Technology Co ltd
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Abstract

本发明公开一种贝壳粉基多孔耐高温材料及其制备方法、应用,由以下质量份原料制成:贝壳粉80~90份、活性炭5~15份、磷酸铝3~5份、活性前驱体溶液3~7份、聚乙烯醇水溶液2~5份、液态石蜡1~10份;该活性前驱体溶液制备方法为:将可溶性铁盐、可溶性铋盐、氯铂酸溶于去离子水中,加入结构导向剂,60℃反应3~6h;其制备方法为:(1)混合贝壳粉、活性炭、磷酸铝并机械球磨;(2)继续加入活性前驱体溶液、聚乙烯醇水溶液、液态石蜡,搅拌均匀并制成素坯,烘干;(3)烧结所得烘干胚体b,即得。本发明制备的多孔高温材料具高强度、高催化活性、高孔隙率、高比表面积、抗热震性能好、烧结温度低等优点,可作为高温烟气过滤材料和车辆尾气净化材料。

Description

一种贝壳粉基多孔耐高温材料及其制备方法、应用
技术领域
本发明属于多孔高温材料技术领域,具体涉及一种贝壳粉基多孔耐高温材料及其制备方法、应用。
背景技术
烟气是气体和烟尘的混合物,是污染居民区大气的主要原因,其主要污染物包括二氧化硫、一氧化碳、碳氢化合物以及氮氧化合物等,烟尘包括燃料的灰分、煤粒、油滴以及高温裂解产物等。汽车尾气是汽车运行时产生的废气,其主要污染物有固体悬浮微粒、一氧化碳、碳氢化合物、氮氧化合物、铅及硫氧化合物等。一氧化碳:一氧化碳和人体红血球中的血红蛋白有很强的亲合力,它的亲合力比氧强250倍,亲合后生成碳氧血红蛋白,从而消弱血液向各组织输送氧的功能,造成感觉、反应、理解、记忆力等机能障碍,重者危害血液循环系统,导致生命危险。氮氧化物:氮氧化物主要是指NO、NO2,危害人体呼吸系统。碳氢化合物在太阳光紫外线照射后,产生一种复杂的光化学反应,形成光化学烟雾。二氧化硫及其他硫氧化合物是导致酸雨形成的最主要原因。因此,如何高效率净化及降解烟气和汽车尾气是亟待解决的技术问题。
贝壳粉以天然贝壳为原料,通过多重清洗,高温煅烧,精细研磨等多重加工工序制成具有天然多孔结构材料,具有吸附有害气体及调节空气湿度等功能,不仅保护了资源,净化了环境,而且整个生产过程不释放有害物质,绿色环保。但是现有贝壳粉材料比表面积不高、孔隙率低,吸附性能有待提高,且当贝壳粉材料达到吸附饱和时,就无法继续脱除有害气体,无法达到持续性净化、吸附的效果。因此,如何制备出具有催化降解能力、可持续净化有毒有害排放物的贝壳粉基材料具有重要意义。
发明内容
针对现有技术的不足之处,本发明的目的在于提供一种贝壳粉基多孔耐高温材料及其制备方法、应用。
本发明的技术方案概述如下:
一种贝壳粉基多孔耐高温材料,由以下质量份原料制成:
Figure BDA0003451208960000021
所述活性前驱体溶液的制备方法为:将可溶性铁盐、可溶性铋盐、氯铂酸加入去离子水中,搅拌溶解后,加入结构导向剂,60℃水浴搅拌反应3~6h,得活性前驱体溶液;所述可溶性铁盐、可溶性铋盐、氯铂酸、去离子水、结构导向剂的用量比例为0.1mol:0.1mol:(0.01~0.03)mol:200mL:(3~5)g。
优选的是,所述磷酸铝为磷酸二氢铝、三聚磷酸铝、偏磷酸铝的一种或多种。
优选的是,所述聚乙烯醇水溶液的质量分数为1~10%。
优选的是,所述可溶性铁盐为硝酸铁、氯化铁、硫酸铁中的一种或多种;所述可溶性铋盐为硝酸铋、氯化铋、醋酸铋中的一种或多种。
优选的是,所述结构导向剂包括十六烷基三甲基溴化铵、聚乙烯吡咯烷酮中的一种或两种。
优选的是,所述液态石蜡为轻蜡油或重蜡油一种或两种。
本发明还提供上述贝壳粉基多孔耐高温材料的制备方法,包括以下步骤:
(1)将贝壳粉、活性炭、磷酸铝混合均匀后,机械球磨至平均粒径≥600目,得到混合粉体a;
(2)在混合粉体a中加入活性前驱体溶液、聚乙烯醇水溶液、液态石蜡,并搅拌均匀,用干压法或挤出法制成素坯,60~90℃烘干2~6h,得烘干胚体b;
(3)将烘干胚体b置于高温炉中,并以1.5~2℃/min的升温速率升温到200℃,然后以3~4℃/min的升温速率升温至500~700℃,再保温烧结1~1.5h以氧化除去活性炭,并生成铂掺杂铁酸铋纳米组分,最后以4~4.5℃/min的升温速率升温至1250~1350℃,保温烧结2~6h,自然冷却后,即得所述贝壳粉基多孔耐高温材料。
优选的是,所述素坯形状包括平板、管式、蜂窝状。
本发明还提供上述贝壳粉基多孔耐高温材料在高温烟气过滤中的应用。
本发明还提供上述贝壳粉基多孔耐高温材料在车辆尾气净化中的应用。
本发明的有益效果:
1、本发明贝壳粉基多2孔耐高温材料含活性前驱体溶液,在高温烧结过程中,形成纳米氧化铂及纳米铂掺杂铁酸铋,协同催化氧化有毒有害排放气体,对所吸附的CO、碳氢化合物、氟氯烃、甲醛、挥发苯等有害气体进行实时分解,进而使贝壳粉基多孔耐高温材料处于动态吸附不饱和状态,进而达到持续性净化、吸附的效果。
2、本发明以铂掺杂铁酸铋为催化剂,具有高催化活性,与有机污染物接触后,能快速氧化降解,将其转化为CO2和H2O,并吸附NOx、SOx等排放气体,净化空气,绿色环保。
3、本发明以活性炭为造孔剂,在高温氧化热解作用下,形成多孔腔结构材料,提高贝壳粉基材料的孔隙率和比表面积。
4、本发明制备的多孔高温材料具高强度、高孔隙率、高比表面积、抗热震性能好、烧结温度低等优点,可以作为高温烟气过滤材料和车辆尾气净化的载体材料。
附图说明
图1为本发明贝壳粉基多孔耐高温材料的制备方法流程图;
图2为实施例1制出的贝壳粉基多孔耐高温材料SEM正面图;
图3为实施例2制出的贝壳粉基多孔耐高温材料SEM侧面图。
具体实施方式
下面结合实施例对本发明做进一步的详细说明,以令本领域技术人员参照说明书文字能够据以实施。
实施例1
一种贝壳粉基多孔耐高温材料的制备方法,包括以下步骤:
(1)将硝酸铁、硝酸铋、氯铂酸加入去离子水中,搅拌溶解后,加入十六烷基三甲基溴化铵,60℃水浴搅拌反应3h,得活性前驱体溶液;所述可溶性铁盐、可溶性铋盐、氯铂酸、去离子水、十六烷基三甲基溴化铵的用量比例为0.1mol:0.1mol:0.01mol:200mL:3g;
(2)按质量份依次称取贝壳粉80份、活性炭5份、磷酸二氢铝3份、活性前驱体溶液3份、质量分数为1%的聚乙烯醇水溶液2份、轻蜡油1份;
(3)将贝壳粉、活性炭、磷酸二氢铝混合均匀后,机械球磨至平均粒径≥600目,得到混合粉体a;
(4)在混合粉体a中加入活性前驱体溶液、质量分数为1%的聚乙烯醇水溶液、轻蜡油,并搅拌均匀,用干压法或挤出法制成平板状素坯,60℃烘干2h,得烘干胚体b;
(5)将烘干胚体b置于高温炉中,并以1.5℃/min的升温速率升温到200℃,然后以3℃/min的升温速率升温至500℃,再保温烧结1h以氧化除去活性炭,并生成铂掺杂铁酸铋纳米组分,最后以4℃/min的升温速率升温至1250℃,保温烧结2h,自然冷却后,即得所述贝壳粉基多孔耐高温材料。
实施例2
一种贝壳粉基多孔耐高温材料的制备方法,包括以下步骤:
(1)将氯化铁、氯化铋、氯铂酸加入去离子水中,搅拌溶解后,加入聚乙烯吡咯烷酮,60℃水浴搅拌反应5h,得活性前驱体溶液;所述可溶性铁盐、可溶性铋盐、氯铂酸、去离子水、结构导向剂的用量比例为0.1mol:0.1mol:0.02mol:200mL:4g;
(2)按质量份依次称取贝壳粉85份、活性炭10份、三聚磷酸铝4份、活性前驱体溶液5份、质量分数为6%的聚乙烯醇水溶液3.5份、重蜡油5.5份;
(3)将贝壳粉、活性炭、三聚磷酸铝混合均匀后,机械球磨至平均粒径≥600目,得到混合粉体a;
(4)在混合粉体a中加入活性前驱体溶液、质量分数为6%的聚乙烯醇水溶液、重蜡油,并搅拌均匀,用干压法或挤出法制成管式素坯,75℃烘干4h,得烘干胚体b;
(5)将烘干胚体b置于高温炉中,并以2℃/min的升温速率升温到200℃,然后以3.5℃/min的升温速率升温至600℃,再保温烧结1.5h以氧化除去活性炭,并生成铂掺杂铁酸铋纳米组分,最后以4.5℃/min的升温速率升温至1300℃,保温烧结4h,自然冷却后,即得所述贝壳粉基多孔耐高温材料。
实施例3
一种贝壳粉基多孔耐高温材料的制备方法,包括以下步骤:
(1)将硝酸铁、醋酸铋、氯铂酸加入去离子水中,搅拌溶解后,加入结构导向剂,60℃水浴搅拌反应6h,得活性前驱体溶液;所述可溶性铁盐、可溶性铋盐、氯铂酸、去离子水、十六烷基三甲基溴化铵的用量比例为0.1mol:0.1mol:0.03mol:200mL:5g;
(2)按质量份依次称取贝壳粉90份、活性炭15份、偏磷酸铝5份、活性前驱体溶液7份、质量分数为10%的聚乙烯醇水溶液5份、轻蜡油10份;
(3)将贝壳粉、活性炭、偏磷酸铝混合均匀后,机械球磨至平均粒径≥600目,得到混合粉体a;
(4)在混合粉体a中加入活性前驱体溶液、质量分数为10%的聚乙烯醇水溶液、轻蜡油,并搅拌均匀,用干压法或挤出法制成蜂窝状素坯,90℃烘干6h,得烘干胚体b;
(5)将烘干胚体b置于高温炉中,并以2℃/min的升温速率升温到200℃,然后以4℃/min的升温速率升温至700℃,再保温烧结1.5h以氧化除去活性炭,并生成铂掺杂铁酸铋纳米组分,最后以4.5℃/min的升温速率升温至1350℃,保温烧结6h,自然冷却后,即得所述贝壳粉基多孔耐高温材料。
实施例1~3制出的贝壳粉基多孔耐高温材料可应用于高温烟气过滤及车辆尾气净化。
对比例与实施例1相同,区别在于:在制备过程中,不添加活性前驱体溶液。
在本发明中,各参数的测定采用如下方法:
1.孔隙率的测试方法采用GB5935-1986轻工产品金属镀层的孔隙率测试方法。
2.孔径测试方法采用GB/T 19587-2004《气体吸附BET法测定固态物质比表面积》。
3.气体渗透性能测试方法采用GB/T 40260-2021高分子膜材料气体渗透性能测试方法。
4.将10mg贝壳粉基多孔耐高温材料样品置于装满1000mg/m3 CO的1L密闭装置中,25℃处理3h,再按GBT 18204.23-2000测定方法测定CO处理后浓度c,根据100%×(1-c/1000)计算CO去除率。
表1贝壳粉基多孔耐高温材料性能试验结果及达标情况
表1
检验项目 实施例1 实施例2 实施例3 对比例
孔隙率(%) 71 67 66 70.5
平均孔径(μm) 13 12 11 13.5
气体渗透率m<sup>3</sup>/m<sup>2</sup>hbar 24000 23000 22500 23800
CO降解率(%) 95.8 96.2 98.4 67.5
实施例1~3贝壳粉基多孔耐高温材料含活性前驱体溶液,在高温烧结过程中,形成纳米氧化铂及纳米铂掺杂铁酸铋,协同催化氧化有毒有害排放气体,对所吸附的CO、碳氢化合物、氟氯烃、甲醛、挥发苯等有害气体进行实时分解,进而使贝壳粉基多孔耐高温材料处于动态吸附不饱和状态,进而达到持续性净化、吸附的效果。
实施例1~3以铂掺杂铁酸铋为催化剂,具有高催化活性,与有机污染物接触后,能快速氧化降解,将其转化为CO2和H2O,并吸附NOx、SOx等排放气体,净化空气,绿色环保。
实施例1~3以活性炭为造孔剂,在高温氧化热解作用下,形成多孔腔结构材料,提高贝壳粉基材料的孔隙率和比表面积。
实施例1~3制备的多孔高温材料具高强度、高孔隙率、高比表面积、抗热震性能好、烧结温度低等优点,可以作为高温烟气过滤材料和车辆尾气净化的载体材料。
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节。

Claims (10)

1.一种贝壳粉基多孔耐高温材料,其特征在于,由以下质量份原料制成:
Figure FDA0003451208950000011
所述活性前驱体溶液的制备方法为:将可溶性铁盐、可溶性铋盐、氯铂酸加入去离子水中,搅拌溶解后,加入结构导向剂,60℃水浴搅拌反应3~6h,得活性前驱体溶液;所述可溶性铁盐、可溶性铋盐、氯铂酸、去离子水、结构导向剂的用量比例为0.1mol:0.1mol:(0.01~0.03)mol:200mL:(3~5)g。
2.根据权利要求1所述一种贝壳粉基多孔耐高温材料,其特征在于,所述磷酸铝为磷酸二氢铝、三聚磷酸铝、偏磷酸铝的一种或多种。
3.根据权利要求1所述一种贝壳粉基多孔耐高温材料,其特征在于,所述聚乙烯醇水溶液的质量分数为1~10%。
4.根据权利要求1所述一种贝壳粉基多孔耐高温材料,其特征在于,所述可溶性铁盐为硝酸铁、氯化铁、硫酸铁中的一种或多种;所述可溶性铋盐为硝酸铋、氯化铋、醋酸铋中的一种或多种。
5.根据权利要求1所述一种贝壳粉基多孔耐高温材料,其特征在于,所述结构导向剂包括十六烷基三甲基溴化铵、聚乙烯吡咯烷酮中的一种或两种。
6.根据权利要求1所述一种贝壳粉基多孔耐高温材料,其特征在于,所述液态石蜡为轻蜡油或重蜡油一种或两种。
7.根据权利要求1~6任一项所述的一种贝壳粉基多孔耐高温材料的制备方法,其特征在于,包括以下步骤:
(1)将贝壳粉、活性炭、磷酸铝混合均匀后,机械球磨至平均粒径≥600目,得到混合粉体a;
(2)在混合粉体a中加入活性前驱体溶液、聚乙烯醇水溶液、液态石蜡,并搅拌均匀,用干压法或挤出法制成素坯,60~90℃烘干2~6h,得烘干胚体b;
(3)将烘干胚体b置于高温炉中,并以1.5~2℃/min的升温速率升温到200℃,然后以3~4℃/min的升温速率升温至500~700℃,再保温烧结1~1.5h以氧化除去活性炭,并生成铂掺杂铁酸铋纳米组分,最后以4~4.5℃/min的升温速率升温至1250~1350℃,保温烧结2~6h,自然冷却后,即得所述贝壳粉基多孔耐高温材料。
8.根据权利要求7所述的一种贝壳粉基多孔耐高温材料的制备方法,其特征在于,所述素坯形状包括平板、管式、蜂窝状。
9.根据权利要求1~6任一项所述的一种贝壳粉基多孔耐高温材料在高温烟气过滤中的应用。
10.根据权利要求1~6任一项所述的一种贝壳粉基多孔耐高温材料在车辆尾气净化中的应用。
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