CN110156075B - 一种用烧结烟气脱硫灰低温制备CaZrO3粉体的方法 - Google Patents
一种用烧结烟气脱硫灰低温制备CaZrO3粉体的方法 Download PDFInfo
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Abstract
本发明提供一种用烧结烟气脱硫灰低温制备CaZrO3粉体的方法，属于工业固废综合利用与无机非金属材料制备技术领域。本发明具体包括如下步骤：将烧结烟气脱硫灰、ZrO2和含有碳酸盐在内的碱金属盐粉体混合加热至850℃以上煅烧，所得产物用水浸泡，经过滤、清洗、干燥后即得到CaZrO3粉体。本发明以廉价的烧结烟气脱硫灰为Ca源，合成温度较传统固相法有显著降低，且所得产品粒径较小。该发明方法工艺简单、成本低，可实现烧结烟气脱硫灰的高附加值利用，具有显著的社会经济效益。
Description
技术领域
本发明属于工业固废综合利用与无机非金属材料制备技术领域，具体涉及一种用烧结烟气脱硫灰低温制备CaZrO3粉体的方法，
背景技术
烧结烟气脱硫技术的成熟与发展，有效解决了烟气污染问题，但随之产生了大量的脱硫灰，造成了新的固废污染。目前，脱硫灰处理技术还不够成熟，大多只能堆存处理，不仅占用了大量宝贵的土地资源，还可能会对环境造成二次污染。现有脱硫灰的开发利用主要集中在水泥、墙体填充材料、土壤改性等方面，产品附加值相对较低。
钙钛矿型CaZrO3的熔点高达2345℃，其热膨胀系数小、机械强度高、化学性能稳定好，并且具有良好的高温质子导电性、抗水化性能、优良的抗热震性、较高的荷重软化温度、优异的抗硅酸盐水泥熟料的侵蚀等性能，是一种应用前景广泛的高温结构材料和高温功能材料。目前，CaZrO3粉体的制备方法主要有以下三种：(1)高温固相法：以含Ca物质(CaCO3、Ca(OH)2、CaC2O4等)与 ZrO2的混合粉体为原料进行高温煅烧；该法工艺简单，原料来源广泛，生产量大，后续处理问题小，但存在烧结温度高(≥1500℃)、产物均匀性差和活性度低等缺点。(2)机械力化学法：以CaO与ZrO2的混合粉体为原料，经高能球磨过程中产生的机械力给予反应物能量，促使化学反应发生；该法工艺简单，但存在反应产物纯度过低、反应不完全、反应时间长、产率低等缺点。(3)液相法：包括共沉淀法、水热法、溶胶凝胶法等；所制备的CaZrO3粉体纯度高、粒径小，但原料成本高且工艺复杂，最终还需要高温煅烧处理。从以上分析可知，寻求一种工艺、成本、性能兼顾的制备方法对于拓展CaZrO3材料的应用范围具有非常重要的意义。
发明内容
为克服现有技术的不足，本发明要解决的技术问题是提供一种用烧结烟气脱硫灰低温制备CaZrO3粉体的方法，以期原料成本低廉、制备工艺简单且制备温度较现有技术显著降低。
为解决上述技术问题，本发明是通过以下技术方案予以实现的。
本发明一种用烧结烟气脱硫灰低温制备CaZrO3粉体的方法，具体包括如下步骤：
(1)将烧结烟气脱硫灰、ZrO2和碱金属盐粉体混合；
所述烧结烟气脱硫灰中Ca元素和ZrO2的摩尔比为1：1；所述碱金属盐为 Na2CO3、K2CO3、Li2 CO3、NaCl、KCl、LiCl、Na2SO4、K2SO4、Li2SO4中的一种或多种，且至少含有一种碳酸盐，碱金属盐中CO3 2-离子和烧结烟气脱硫灰中S 元素的摩尔比为1～3：1。
(2)将步骤(1)得到的混合粉体放入刚玉坩埚中，加热煅烧后自然冷却；
所述煅烧温度为850℃以上，保温时间为1～5h。
(4)将步骤(2)得到的混合物放入水中浸泡1～3h，经过滤、清洗、干燥后即得到CaZrO3粉体。
作为一种优化，所述碱金属盐为Na2CO3。
本发明所用主要原料为半干法烧结烟气脱硫灰，主要结晶性物质为 CaSO3.0.5H2O和CaCO3，其典型成分见表1。该脱硫灰中的Ca元素的含量高达 42.36wt.％，可为CaZrO3的合成提供Ca源。此外，该脱硫灰中还含有丰富的SO3 2-或SO4 2-、Cl-、K+和Na+等。
表1烧结烟气脱硫灰的主要化学成分(wt.％)
本发明的主要反应过程及原理如下：
(1)加入的碱金属盐中的CO3 2-离子在加热过程中将烧结烟气脱硫灰中的 CaSO3转换成CaCO3，并将SO3 2-氧化成SO4 2-；
(2)上述反应生成的CaCO3，以及烧结烟气脱硫灰中原来含有的CaCO3、 CaO、Ca(OH)2等与ZrO2反应生成CaZrO3；
(3)原料中或反应产生的SO4 2-、Cl-、K+、Na+、Ca2+等离子在煅烧过程中促进低熔点物质的形成，为反应提供了一个液相环境，促进反应物质的扩散与反应，有效降低合成温度并抑制产物颗粒的晶粒长大。
与现有技术相比，本发明具有以下技术效果：
(1)以烧结烟气脱硫灰为Ca源，原料成本低廉。
(2)充分利用了烧结烟气脱硫灰中大量的SO3 2-、SO4 2-、Cl-、K+、Na+、Ca2+等离子在煅烧过程中能促进生成液相物质的特性，可使CaZrO3的合成温度从传统固相法的1500℃降至850-1050℃，并且产物颗粒尺寸细小，而这些离子最后可通过简单的水洗方式去除。
(3)该法工艺简单、成本低，可实现烧结烟气脱硫灰的高附加值利用，具有显著的社会经济效益。
附图说明
图1为实施例1制得的CaZrO3粉体的X射线衍射(XRD)图谱。
图2为实施例1制得的CaZrO3粉体的扫描电子显微镜(SEM)照片。
具体实施方式
为了进一步了解本发明的技术内容，以下结合附图和实施例详述本发明，但本发明不局限于下述实施例。
实施例1
将1.000g烧结烟气脱硫灰，1.302g ZrO2及1.119g Na2CO3粉体混合均匀后放入刚玉坩埚中，加热至850℃，保温5h后自然冷却，然后将产物放入中浸泡2h，过滤，分别用水和乙醇清洗多次，干燥即得到CaZrO3粉体。
图1为本实施例所制备CaZrO3粉体的XRD图谱，可以看出，本实施例所制备的粉体为结晶CaZrO3，基本无其它杂质相。图2为本实施例所制备CaZrO3粉体的SEM照片，可以看出，该粉体的粒径为100～200nm。
实施例2
将1.000g烧结烟气脱硫灰，1.302g ZrO2及1.459g K2CO3粉体混合均匀后放入刚玉坩埚中，加热至900℃，保温3h后自然冷却，然后将产物放入中浸泡2h，过滤，分别用水和乙醇清洗多次，干燥即得到CaZrO3粉体。
实施例3
将1.000g烧结烟气脱硫灰，1.302g ZrO2及2.506g Na2CO3粉体混合均匀后放入刚玉坩埚中，加热至950℃，保温2h后自然冷却，然后将产物放入中浸泡2h，过滤，分别用水和乙醇清洗多次，干燥即得到CaZrO3粉体。
实施例4
将1.000g烧结烟气脱硫灰、1.302g ZrO2、0.425g Na2CO3及0.466g KCl粉体混合均匀后放入刚玉坩埚中，加热至1050℃，保温1h后自然冷却，然后将产物放入中浸泡3h，过滤，分别用水和乙醇清洗多次，干燥即得到CaZrO3粉体。
Claims (2)
1.一种用烧结烟气脱硫灰低温制备CaZrO3粉体的方法，其特征在于包括如下步骤：
(1)将烧结烟气脱硫灰、ZrO2和碱金属盐粉体混合；
所述烧结烟气脱硫灰中Ca元素和ZrO2的摩尔比为1：1；所述碱金属盐为Na2CO3、K2CO3、Li2 CO3、NaCl、KCl、LiCl、Na2SO4、K2SO4、Li2SO4中的一种或多种，且至少含有一种碳酸盐，碱金属盐中CO3 2-离子和烧结烟气脱硫灰中S元素的摩尔比为1～3：1；
(2)将步骤(1)得到的混合粉体放入刚玉坩埚中，加热煅烧后自然冷却；
所述煅烧温度为850℃以上，保温时间为1～5h；
(3)将步骤(2)得到的混合物放入水中浸泡1～3h，经过滤、清洗、干燥后即得到CaZrO3粉体。
2.如权利要求1所述的一种用烧结烟气脱硫灰低温制备CaZrO3粉体的方法，其特征在于，所述碱金属盐为Na2CO3。
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