CN110252313A - 一种宽温干法烟气脱硝剂及其制备方法 - Google Patents
一种宽温干法烟气脱硝剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种宽温干法烟气脱硝剂及其制备方法,该烟气脱硝剂结构为aAO·bGxOy·mDxOy·nAl2O3,其中A为ⅡA族金属钡、镁、钙中的一种,G为过渡金属铬、铁、钴、锌中的一种,D为铜、锰、和银中的一种。以催化剂的总质量计,AO为28%~42%,GxOy为30%~40%,DxOy为10%~20%,Al2O3为8~12%。该干法烟气脱硝剂可用于工业锅炉、窑炉以及焦化焦炉等烟气的NOx排放控制。具有在较宽的温度范围内实现对NOx的无氨高效转化的优点,适于工业应用。
Description
技术领域
本发明涉及一种宽温干法烟气脱硝剂及其制备方法,特别适用于工业锅炉、窑炉以及焦化焦炉等烟气的NOx排放控制所需干法烟气脱硝剂及其制备方法。
背景技术
氮氧化物(NOx)是主要的大气污染物之一,随着人民生活水平的提高,环保要求越来越苛刻,烟气脱硝势在必行。在众多的烟气脱硝方法中,将NOx催化还原为无害的N2排入大气是很好的选择,目前,世界上广泛使用的成熟的脱硝技术有催化和非催化氨还原技术,选择性催化还原为SCR(selective catalytic reduction),选择性非催化还原为SNCR(selective non-catalytic reduction)。这两种技术均是用氨气或含氨气的物质(氨水、高温分解产生氨气的尿素等)来还原处理烟气中的氮氧化物。其典型的反应如式(1)、(2):
6 N6 NO +4 NH3→5 N2 + 6 H2O (1)
6 NO2 + 8 NH3→7 N2 + 12 H2O (2)
这两种脱硝技术显而易见的短板有两点。其一,脱硝温度高。SNCR工艺,,典型反应温度800-900℃,SCR(选择催化还原)在V-Ti系催化剂上,通常使用温度也是350℃。一般烟气温度都在300℃以下,如若匹配先脱硫后脱硝工艺,温度会更低。其二,带来二次污染。使用大量过量的氨气或氨水,不可避免的氨气逃逸可能导致更严重的环境污染。
专利CN107551782A提供一种干法烟气脱硝方法,先将待脱硝烟气中的一氧化氮氧化为二氧化氮,然后采用以氧化镁为主要成分的脱硝剂在吸收装置中对所述氧化烟气进行干法脱硝,该法存在吸收剂的耗量大和吸收废剂的后处理问题。
上世纪90年代中期丰田公司提出NO的储存-还原法(NSR),催化剂主要包括三种组分:(1)高比表面的载体,通常为γ-Al2O3;(2)NOx储存组分,主要是碱金属或碱土金属。(3)贵金属主要是Pt或Pt/Rh合金,用于NOx的氧化与还原。贵金属将NO氧化成NO2,生成的NO2与碱性组分反应,将NOx以不稳定的硝酸盐储存起来,然后,在还原剂充足的条件下,不稳定的硝酸盐释放出NOx,被还原成N2。该法使用贵金属活性组分,成本高且不耐硫,并且需要补充烃类还原剂。
烟气中一般有含量不稳定的CO,CO具有还原性:
2NO+O2→2NO2 (3)
2NO2+4CO→2N2+4CO2 (4)
综上所述,研发一种宽温干法脱硝剂,在较宽的活性温度范围内,将NO氧化成NO2,生成的NO2与碱性组分反应,将NOx以不稳定的硝酸盐储存起来,然后,在CO充足的条件下,不稳定的硝酸盐释放出NOx,被还原成N2。这是一件有难度但非常有意义的工作。
发明内容
本发明的目的是提供一种新的宽温干法烟气脱硝剂。该催化剂具有在较宽的温度范围内实现对NOx的无氨高效转化的优点。本发明的另一个目的是提供一种上述宽温干法烟气脱硝剂的制备方法。
本发明解决其技术问题所采用的技术方案为:一种宽温干法烟气脱硝剂,结构为aAO·bGxOy·mDxOy·nAl2O3的复合氧化物,其中A为ⅡA族金属钡、镁、钙中的一种,充当NOx储存组分;G为过渡金属铬、铁、钴、锌中的一种,有较好将NO氧化成NO2的SCO催化活性;D为铜、锰、和银中的一种,在CO充足的条件下,不稳定的硝酸盐释放出NOx,被D组分催化还原成N2。aAO·bGxOy·mDxOy·nAl2O3复合氧化物能够在较宽的温度范围内实现对NOx的无氨高效转化。
本发明宽温干法烟气脱硝剂的制备方法,可通过包括下述主要步骤方法制备:
(1)以Al2O3为担体共沉淀aAO·bGxOy。(a)称取一定量的钡、镁、钙 以及铬、铁、钴、锌的各一种金属的硝酸盐共两种盐溶于水中,形成溶液。(b)将一定量的拟薄水铝石加入步骤(a)配制的溶液,搅拌成浆状液。(c)将计算量的沉淀剂配成溶液,加入步骤(b)配制的溶液,搅拌反应后,老化2~5h。然后,将步骤(c)混合物过滤,洗涤后,在80~120℃烘干1~4h;
(2)采用混捏法制得脱硝剂产品。(a)将计算量的铜、锰、和银中的一种的硝酸盐和一定量的水配成溶液。(b)将步骤(1)得到的混合物加入一定量的田菁粉,研磨均匀再添加(a)溶液,搅拌碾压均匀后挤压成型,放置5h后,经110~150℃干燥3~4h,再在400~600℃焙烧6~8h后制得宽温干法烟气脱硝剂。
与现有技术比较,本发明的有益效果是:(1)具备宽温脱硝活性。aAO·bGxOy·mDxOy·nAl2O3复合氧化物在温度120~300℃,对NOx有良好的催化氧化及催化还原活性。(2)能够将NOx无氨转化为N2排入大气,不会带来二次污染。aAO·bGxOy·mDxOy·nAl2O3复合氧化物将NO氧化成NO2,生成的NO2与碱性组分反应,将NOx以不稳定的硝酸盐储存起来,然后,在烟气中CO充足的条件下,不稳定的硝酸盐释放出NOx,被还原成N2。(3)干法脱硝活性好。aAxOy·bGO·mDxOy·nMO3的复合氧化物在温度120~300℃,空速1000~5000 h-1,烟气中NOx的脱除率≥95%。
具体实施方案
下面结合具体实验方案对本发明做进一步的详细描述。但发明的权利不受下述实施例的限制。以下各实施例中,涉及百分含量时均为质量百分比。
实施例1
将47.8g硝酸钡和202g九水硝酸铁溶于200ml去离子水,加热至50℃。再加入17.2g拟薄水铝石,搅拌成浆状液;称取118g碳酸钠溶于350 ml去离子水,加入到浆状液中,保持温度为50℃,并用氨水将PH值调为10,反应完毕,老化2h,然后过滤,洗涤,120℃烘1h。称取CuSO4·5H2O62.5g溶于100ml去离子水,加入到烘干滤渣和3g田菁粉的混合物中并研磨均匀,再挤压成型,放置5h后,经110℃干燥4h,再在500℃焙烧7h后即制得所述的宽温干法烟气脱硝剂产品,其中BaO为28% ,Fe2O3为40% ,CuO为20% ,Al2O3为12%。堆密度为0.90g/cm3,比表面积95g/m2,孔容0.25ml/g。该催化剂在300℃,空速5000h-1的条件下,可将7.2%CO2+5.8%O2+0.12%NOx+0.3%CO+78.58%N2+8%H2O中的NOx脱除至60ppm,烟气中NOx的脱除率为95%。
实施例2
将155.4g硝酸镁和125.3g硝酸铬溶于300ml去离子水,加热至75℃。再加入11.5g拟薄水铝石,搅拌成浆状液;称取234g碳酸钠溶于650 ml去离子水,加入到浆状液中,保持温度为75℃,并用氨水将PH值调为10,反应完毕,老化5h,然后过滤,洗涤,80℃烘4h。称取AgNO314.7g溶于60ml去离子水,加入到烘干滤渣和3g田菁粉的混合物中并研磨均匀,再挤压成型,放置5h后,经150℃干燥3h,再在400℃焙烧8h后即制得所述的宽温干法烟气脱硝剂产品,其中MgO为42% ,Cr2O3为40% ,Ag2O为10% ,Al2O3为8%。堆密度为1.25g/cm3,比表面积65g/m2,孔容0.16ml/g。该催化剂在120℃,空速1000h-1的条件下,可将7.2%CO2+5.8%O2+0.05%NOx+0.12%CO+78.83%N2+8%H2O中的NOx脱除至20ppm,烟气中NOx的脱除率为96%。
实施例3
将102.5g硝酸钙和135.8g六水硝酸钴溶于500ml去离子水,加热至60℃。再加入14.3g拟薄水铝石,搅拌成浆状液;称取207g碳酸氢铵溶于600 ml去离子水,加入到浆状液中,保持温度为60℃,并用氨水将PH值调为10,反应完毕,老化4h,然后过滤,洗涤,100℃烘3h。称取硝酸锰41.2g溶于120ml去离子水,加入到烘干滤渣和3g田菁粉的混合物中并研磨均匀,再挤压成型,放置5h后,经120℃干燥4h,再在600℃焙烧6h后即制得所述的宽温干法烟气脱硝剂产品,其中CaO为35% ,CoO为35% ,MnO2为20% ,Al2O3为10%。堆密度为1.05g/cm3,比表面积80g/m2,孔容0.20ml/g。该催化剂在200℃,空速3000h-1的条件下,可将7.2%CO2+5.8%O2+0.06%NOx+0.14%CO+78.8%N2+8%H2O中的NOx脱除至25ppm,烟气中NOx的脱除率为95.8%。
实施例4
将117.2g硝酸钙和146.7g六水硝酸锌溶于600ml去离子水,加热至65℃。再加入14.3g拟薄水铝石,搅拌成浆状液;称取229g碳酸氢铵溶于650 ml去离子水,加入到浆状液中,保持温度为65℃,并用氨水将PH值调为10,反应完毕,老化3h,然后过滤,洗涤,110℃烘3h。称取CuSO4·5H2O31.3g溶于65ml去离子水,加入到烘干滤渣和3g田菁粉的混合物中并研磨均匀,再挤压成型,放置5h后,经130℃干燥3h,再在450℃焙烧7h后即制得所述的宽温干法烟气脱硝剂产品,其中CaO为40% ,ZnO为40% ,CuO为10% ,Al2O3为10%。堆密度为0.95g/cm3,比表面积90g/m2,孔容0.22ml/g。该催化剂在150℃,空速2000h-1的条件下,可将7.2%CO2+5.8%O2+0.04%NOx+0.1%CO+78.86%N2+8%H2O中的NOx脱除至12ppm,烟气中NOx的脱除率为97%。
实施例5
将155.4g硝酸镁和 116.4g六水硝酸钴溶于550ml去离子水,加热至55℃。再加入14.3g拟薄水铝石,搅拌成浆状液;称取183g碳酸钠溶于650 ml去离子水,加入到浆状液中,保持温度为55℃,并用氨水将PH值调为10,反应完毕,老化4h,然后过滤,洗涤,130℃烘2h。称取硝酸锰37.1g溶于80ml去离子水,加入到烘干滤渣和3g田菁粉的混合物中并研磨均匀,再挤压成型,放置5h后,经140℃干燥3h,再在480℃焙烧6.5h后即制得所述的宽温干法烟气脱硝剂产品,其中MgO为42% ,CoO为30% ,MnO2为18% ,Al2O3为10%。堆密度为0.88g/cm3,比表面积92g/m2,孔容0.24ml/g。该催化剂在180℃,空速1000h-1的条件下,可将7.2%CO2+5.8%O2+0.045%NOx+0.1%CO+78.855%N2+8%H2O中的NOx脱除至22ppm,烟气中NOx的脱除率为95.1%。
实施例6
将68.3g硝酸钡和110g六水硝酸锌溶于600ml去离子水,加热至60℃。再加入17.2g拟薄水铝石,搅拌成浆状液;称取104.4g碳酸钠溶于400 ml去离子水,加入到浆状液中,保持温度为60℃,并用氨水将PH值调为10,反应完毕,老化2h,然后过滤,洗涤,120℃烘2.5h。称取CuSO4·5H2O56.3g溶于80ml去离子水,加入到烘干滤渣和3g田菁粉的混合物中并研磨均匀,再挤压成型,放置5h后,经120℃干燥4h,再在500℃焙烧7h后即制得所述的宽温干法烟气脱硝剂产品,其中BaO为40% ,ZnO为30% ,CuO为18% ,Al2O3为12%。堆密度为1.20g/cm3,比表面积75g/m2,孔容0.21ml/g。该催化剂在280℃,空速5000h-1的条件下,可将7.2%CO2+5.8%O2+0.10%NOx+0.23%CO+78.67%N2+8%H2O中的NOx脱除至40ppm,烟气中NOx的脱除率为96%。
Claims (8)
1.一种宽温干法烟气脱硝剂,其特征在于:所述的烟气脱硝剂结构为aAO·bGxOy·mDxOy·nAl2O3,其中A为ⅡA金属钡、镁、钙中的一种,G为过渡金属铬、铁、钴、锌中的一种,D为铜、锰、和银中的一种。
2.根据权利要求1所述的宽温干法烟气脱硝剂,其特征在于:以重量百分比计各组分含量:AO为28%~42%, GxOy为30%~40%,DxOy为10%~20%,Al2O3为8~12%。
3.权利要求1或2所述的宽温干法烟气脱硝剂,其特征在于:所述的烟气脱硝剂堆密度为0.90~1.25g/cm3,比表面积65~95g/m2,孔容0.16~0.25ml/g。
4.如权利要求1所述的宽温干法烟气脱硝剂的制备方法,其特征在于:该方法包括以下步骤:
(1)称取一定量的钡、镁、钙 以及铬、铁、钴、锌的各一种金属的硝酸盐共两种盐溶于水中,形成溶液;
(2)将一定量的拟薄水铝石加入步骤(1)配制的溶液,搅拌成浆状液;
(3)将计算量的沉淀剂配成溶液,在一定温度下,加入步骤(2)配制的溶液,调节pH值,搅拌反应,然后老化2~5h;
(4)将步骤(3)混合物过滤,洗涤后,在80~120℃烘干1~4h;
(5)将计算量的铜、锰、和银中的一种的硝酸盐和一定量的水配成溶液;
(6)将步骤(4)得到的混合物加入一定量的田菁粉,研磨均匀再添加(5)溶液,搅拌碾压均匀后挤压成型,放置5h后,经110~150℃干燥3~4h,再在400~600℃焙烧6~8h后制得宽温干法烟气脱硝剂。
5.根据权利要求4所述的方法,其特征在于:步骤(3)所用的沉淀剂为碳酸钠或碳酸氢铵。
6.根据权利要求4所述的方法,其特征在于:步骤(3)共沉淀的温度为50~75℃。
7.根据权利要求4所述的方法,其特征在于:步骤(3)用氨水调至pH为10。
8.权利要求1所述的宽温干法烟气脱硝剂,其应用条件为:温度120~300℃,空速1000~5000 h-1,烟气中NOx的脱除率≥95%。
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