CN110681345A - 一种载硒和硫脱汞材料的制备方法 - Google Patents
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- B01J20/0262—Compounds of O, S, Se, Te
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本发明提供了一种载硒和硫脱汞材料的制备方法，所要解决的技术问题是：针对现有改性材料脱汞净化深度不足、吸附容量小、难以再生等问题，以便于再生的骨架材料为载体，利用硒、硫协同脱汞，提高材料脱汞效率和容量，实现汞污染治理。本发明的要点是：选择大比表面积耐腐蚀材料浸渍水溶性正价态硒化合物，干燥后用水溶性硫化物或硫化氢气体还原硒，反应产物硒和硫直接负载到载体材料表面，水洗去除水溶物后干燥既得产品。
Description
技术领域
本发明属于环保吸附材料技术领域，具体涉及一种在骨架材料上同时负载活性硒和硫的方法，用于气态单质汞的净化。
背景技术
汞在常温下呈液体存在，蒸汽分压较高，主要以气态单质汞形态释放进入环境，造成严重的汞污染。常规治理技术，一般能达到0.1-0.5mg/m3，随着各行业烟气排放标准的提高，很难实现达标排放，末端仍需进一步处理。目前最常用的是活性炭吸附，但活性炭吸附效率及容量普遍较低，需要进行改性处理。
公布号CN106582517A公开了一种负载纳米硒的活性炭及其化学制备与应用，将亚硒酸钠溶于0.01-0.5%的聚乙烯醇水溶液中，加入粉体活性炭，室温下以抗坏血酸还原，得到负载纳米硒的活性炭，用于去除大气中的汞蒸气。该方法除汞效率虽然可达94-99%，因亚硒酸钠价格较高，为提高材料吸附容量而提高硒含量时造成产品成本过高，限制了产品的工业应用。
公告号 CN 101474551 B提供了一种用于烟气脱汞的载硫活性炭及其制备方法，通过加热使硫磺在氮气中升华并在活性炭上沉积，冷却后得到含硫18-30%的载硫活性炭，能够有效脱除烟气中的汞。脱汞载硫活性炭并非硫含量越高越好，含硫过高易堵塞活性炭孔径而降低材料比表面积，从而降低硫的活性及利用率，影响脱汞效果。
公布号CN 108579711 A提出一种活性炭脱汞吸附剂的载硫热再生方法，将失活的活性炭脱汞吸附剂与硫磺单质以质量比(0.5-2 ):1混合均匀；置于惰性气体气氛下，于反应温度400-700℃下恒温保持0.5-3h；在惰性气体气氛保护下停止加热，冷却至室温，实现活性炭脱汞吸附剂的载硫热再生。其本质也是活性炭热载硫，已吸附的汞没有出口。
在烟气脱汞应用中，载硒或载硫活性炭均有应用，载硒活性炭脱汞效果较好，但因其高成本而使用受限，载硫活性炭脱汞效果较差但具有成本优势，利用载硒和载硫活性炭的优势，在深度脱汞、吸附容量及材料成本等综合性能方面进行优化，以提高材料在不同行业中的适用性和各项综合指标。
发明内容
本发明的目的是：提供一种载硒和硫脱汞材料的制备方法，针对现有改性材料脱汞净化深度不足、吸附容量小、材料成本高等问题，以高比表面积的骨架材料为载体，利用硒、硫协同脱汞，提高材料脱汞效率和容量，降低材料成本，实现汞污染治理。
本发明通过如下方法实现：一种载硒和硫脱汞材料的制备方法，其特征是：选择大比表面积耐腐蚀骨架材料浸渍水溶性正价态硒化合物，干燥后用水溶性硫化物或硫化氢气体还原硒，反应产物硒和硫直接负载到载体材料表面，水洗去除水溶物后干燥既得产品。
进一步的：所述骨架材料为粉状或颗粒状活性炭、活性氧化铝、土质材料。
进一步的：水溶性正价态硒化合物为二氧化硒或亚硒酸盐或硒酸盐或硒盐。
进一步的：浸硒、还原、水洗过程在温度为0-100℃，时间为0.5-24小时，搅动或溶液循环条件下进行。
进一步的：骨架材料负载硒量为2-10%，还原剂用量为理论量的100-150%。
进一步的：浸硒和产品干燥温度为50-120℃。
本发明的优点是：按骨架材料的吸水量和负载硒量配制含硒溶液，骨架材料吸附含硒溶液饱和后干燥，硒化合物附着于骨架材料内表面，再进行还原。本发明的还原剂采用水溶性硫化物或硫化氢气体，利用氧化还原反应将反应产物硒和硫直接负载到骨架材料上，可保证硒和硫的均匀分布并保持高活性，提高材料的脱汞效率和容量并实现深度脱汞。
具体实施方式
本发明提供了一种载硒和硫脱汞材料的制备方法，选择大比表面积耐腐蚀骨架材料浸渍水溶性正价态硒化合物溶液，干燥后用水溶性硫化物或硫化氢气体还原硒，反应产物硒和硫直接负载到载体材料表面，水洗去除水溶物后干燥既得产品。
优选的：所述大比表面积耐腐蚀骨架材料为活性炭或活性氧化铝或土质材料；形态为粉状或颗粒状；比表面积在500㎡/g以上。
优选的：所述水溶性正价态硒化合物为二氧化硒或亚硒酸盐或硒酸盐或硒盐。
优选的：浸渍、还原、水洗过程中，温度为0-100℃，时间为0.5-24小时，在搅动或溶液循环条件下进行。
优选的：骨架材料负载硒量为骨架材料总质量的2-10%，还原剂用量为理论量的100-150%，理论量可根据材料增重和溶液组成来计算。
优选的：浸渍时温度为50-100℃，干燥时温度为50-120℃。
本方法具体的步骤如下：
1、载体材料选择：选择大比表面积的耐腐蚀材料，如活性炭、活性氧化铝、土质材料等，可以是粉状或颗粒状；
2、硒液配制：按材料载硒量计算投料量，以二氧化硒或亚硒酸盐或硒酸盐或硒盐溶于水制得；
3、还原剂准备：选取硫化物配制成水溶液或以硫化氢替代，投料量为使用的硒化合物质量的100-150%，硒化合物质量按式（1）或（2）计算；
SeO3 2-+2S2-+ 6H+=Se+2S+3H2O (1)
SeO4 2-+3S2-+8H+ =Se+3S+4H2O (2)
4、浸硒：在温度5-60℃下，将载体材料浸泡于硒液中，通过搅动或硒液循环保持硒液成分均匀，在0.5-6小时后固液分离并于60-110℃干燥；
5、还原：在温度5-60℃下，将浸硒载体材料投入还原剂溶液中，通过搅动或还原剂溶液循环流动保持溶液成分均匀，0.5-6小时后固液分离；或者通入硫化氢气体穿过浸硒载体材料层进行还原；
6、洗涤干燥：还原后的材料在温度5-60℃下水洗0.5-6小时除去其中残留的水溶物并于60-110℃干燥。
下面结合实施例对本发明做出进一步说明。
实施例1
选取柱状煤质活性炭，比表面积800m2/g，干燥后称取100g；称取5.5g SeO2溶于100ml水中；将活性炭加入SeO2水溶液中并在常温下震荡4h；取出活性炭沥干后干燥得浸硒活性炭101.5g；称取6.5g Na2S·9H2O溶于100ml水中；将浸硒活性炭加入Na2S水溶液中并在常温下震荡4h；取出活性炭加水100ml常温震荡水洗2h，沥水并于80℃干燥得产品102g。将此改性活性炭进行吸汞性能评价，在常温下吸附停留时间2s，大气汞浓度由1800μg/m3降为12μg/m3，吸附效率达99.33%，饱和吸附容量达到31.5mg/g。
实施例2
选取φ3球状活性氧化铝，干燥后称取100g；配制60g/l Na2SeO3水溶液100ml；将氧化铝球加入Na2SeO3水溶液中并在常温下震荡6h；取出氧化铝球沥干后干燥得浸硒氧化铝100.5g；将浸硒氧化铝球放入φ50玻璃管内，材料两端压实；称取5g Na2S·9H2O置于三口烧瓶中，滴加过量稀硫酸制取硫化氢，将其引入装填浸硒氧化铝球的玻璃管内，气体常温循环2h；取出氧化铝球加水100ml常温震荡水洗3h，沥水并于100℃干燥得产品101g。将此改性氧化铝进行吸汞性能评价，在常温下吸附停留时间2s，大气汞浓度由1800μg/m3降为46μg/m3，吸附效率达97.44%，饱和吸附容量达到17.2mg/g。
实施例3
选取60目沸石粉，干燥后称取50g；称取2.4g Na2SeO3溶于50ml水中；将沸石粉加入Na2SeO3水溶液中并在常温下震荡8h；称取2.2g (NH4)2S溶于50ml水中, 在常温下滴加到沸石粉的Na2SeO3混浊液中并震荡2h；固液分离后沸石粉加水100ml常温震荡水洗2h；再次固液分离后于80℃干燥得产品52g。将此改性活性炭进行吸汞性能评价，在常温下吸附停留时间2s，大气汞浓度由1970μg/m3降为9μg/m3，吸附效率达99.54%，饱和吸附容量达到56.8mg/g。
通过本发明方法制备的载硒和硫脱汞材料，按骨架材料的吸水量和负载硒量配制含硒溶液，骨架材料吸附含硒溶液饱和后干燥，硒化合物附着于骨架材料内表面，再进行还原。本发明的还原剂采用水溶性硫化物或硫化氢气体，利用氧化还原反应将反应产物硒和硫直接负载到骨架材料上，可保证硒和硫的均匀分布并保持高活性，提高材料的脱汞效率和容量并实现深度脱汞。本方法所制备的载硒和硫脱汞材料，有效解决了现有改性材料脱汞净化深度不足、吸附容量小、材料成本高等问题，以高比表面积的骨架材料为载体，利用硒、硫协同脱汞，提高材料脱汞效率和容量，降低材料成本，实现汞污染治理。
Claims (6)
1.一种载硒和硫脱汞材料的制备方法，其特征是：选择大比表面积耐腐蚀骨架材料浸渍水溶性正价态硒化合物溶液，干燥后用水溶性硫化物或硫化氢气体还原硒，反应产物硒和硫直接负载到载体材料表面，水洗去除水溶物后干燥既得产品。
2.根据权利要求1所述的载硒和硫脱汞材料的制备方法，其特征是：所述大比表面积耐腐蚀骨架材料为粉状或颗粒状的活性炭或活性氧化铝。
3.根据权利要求1所述的载硒和硫脱汞材料的制备方法，其特征是：所述水溶性正价态硒化合物为二氧化硒或亚硒酸盐或硒酸盐或硒盐。
4.根据权利要求1所述的载硒和硫脱汞材料的制备方法，其特征是：浸渍、还原、水洗过程中，温度为0-100℃，时间为0.5-24小时，在搅动或溶液循环条件下进行。
5.根据权利要求1所述的载硒和硫脱汞材料的制备方法，其特征是：骨架材料负载硒量为2-10%，还原剂用量为理论量的100-150%。
6.根据权利要求1所述的载硒和硫脱汞材料的制备方法，其特征是：浸渍时温度为50-100℃，干燥时温度为50-120℃。
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