CN110681345A - 一种载硒和硫脱汞材料的制备方法 - Google Patents
一种载硒和硫脱汞材料的制备方法 Download PDFInfo
- Publication number
- CN110681345A CN110681345A CN201910851297.5A CN201910851297A CN110681345A CN 110681345 A CN110681345 A CN 110681345A CN 201910851297 A CN201910851297 A CN 201910851297A CN 110681345 A CN110681345 A CN 110681345A
- Authority
- CN
- China
- Prior art keywords
- selenium
- sulfur
- water
- demercuration
- loaded
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000463 material Substances 0.000 title claims abstract description 67
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000011669 selenium Substances 0.000 title claims abstract description 40
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 38
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 23
- 239000011593 sulfur Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 13
- 229940065287 selenium compound Drugs 0.000 claims abstract description 12
- 150000003343 selenium compounds Chemical class 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012876 carrier material Substances 0.000 claims abstract description 10
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 8
- 238000011068 loading method Methods 0.000 claims abstract description 8
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005260 corrosion Methods 0.000 claims abstract description 7
- 230000007797 corrosion Effects 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 55
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 claims description 8
- ZQRRBZZVXPVWRB-UHFFFAOYSA-N [S].[Se] Chemical compound [S].[Se] ZQRRBZZVXPVWRB-UHFFFAOYSA-N 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229940082569 selenite Drugs 0.000 claims description 4
- MCAHWIHFGHIESP-UHFFFAOYSA-L selenite(2-) Chemical compound [O-][Se]([O-])=O MCAHWIHFGHIESP-UHFFFAOYSA-L 0.000 claims description 4
- 150000003342 selenium Chemical class 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 28
- 229910052753 mercury Inorganic materials 0.000 abstract description 26
- 238000001179 sorption measurement Methods 0.000 abstract description 14
- 238000000746 purification Methods 0.000 abstract description 3
- 238000011069 regeneration method Methods 0.000 abstract description 3
- 230000008929 regeneration Effects 0.000 abstract description 2
- 229940091258 selenium supplement Drugs 0.000 description 31
- 239000000243 solution Substances 0.000 description 13
- 239000007788 liquid Substances 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000011781 sodium selenite Substances 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 229910021536 Zeolite Inorganic materials 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 239000003546 flue gas Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- 229910003424 Na2SeO3 Inorganic materials 0.000 description 3
- 229910018143 SeO3 Inorganic materials 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 229960001471 sodium selenite Drugs 0.000 description 2
- 235000015921 sodium selenite Nutrition 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910018162 SeO2 Inorganic materials 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0262—Compounds of O, S, Se, Te
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0262—Compounds of O, S, Se, Te
- B01J20/0266—Compounds of S
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
- B01J20/3204—Inorganic carriers, supports or substrates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3234—Inorganic material layers
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treating Waste Gases (AREA)
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℃。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910851297.5A CN110681345A (zh) | 2019-09-10 | 2019-09-10 | 一种载硒和硫脱汞材料的制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910851297.5A CN110681345A (zh) | 2019-09-10 | 2019-09-10 | 一种载硒和硫脱汞材料的制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110681345A true CN110681345A (zh) | 2020-01-14 |
Family
ID=69108044
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910851297.5A Pending CN110681345A (zh) | 2019-09-10 | 2019-09-10 | 一种载硒和硫脱汞材料的制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110681345A (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112159049A (zh) * | 2020-10-28 | 2021-01-01 | 浙江大学 | 一种同步去除硒污染和硫化物污染的处理方法与装置 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58114728A (ja) * | 1981-12-28 | 1983-07-08 | Mitsubishi Metal Corp | 水銀除去剤およびその製造方法 |
| SE463653B (sv) * | 1988-06-06 | 1991-01-07 | Abb Stal Ab | Saett att avlaegsna kvicksilver ur roekgaser |
| CN101657382A (zh) * | 2007-02-28 | 2010-02-24 | 康宁股份有限公司 | 包含活性碳的吸附剂、其制备方法和应用 |
| US20100078390A1 (en) * | 2008-09-26 | 2010-04-01 | Cross Joseph B | Mercury removal process |
| CN110170302A (zh) * | 2019-05-31 | 2019-08-27 | 贵州重力科技环保有限公司 | 原位级纳米硒炭基脱汞吸附材料的制备方法及材料和应用 |
-
2019
- 2019-09-10 CN CN201910851297.5A patent/CN110681345A/zh active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58114728A (ja) * | 1981-12-28 | 1983-07-08 | Mitsubishi Metal Corp | 水銀除去剤およびその製造方法 |
| SE463653B (sv) * | 1988-06-06 | 1991-01-07 | Abb Stal Ab | Saett att avlaegsna kvicksilver ur roekgaser |
| CN101657382A (zh) * | 2007-02-28 | 2010-02-24 | 康宁股份有限公司 | 包含活性碳的吸附剂、其制备方法和应用 |
| US20100078390A1 (en) * | 2008-09-26 | 2010-04-01 | Cross Joseph B | Mercury removal process |
| CN110170302A (zh) * | 2019-05-31 | 2019-08-27 | 贵州重力科技环保有限公司 | 原位级纳米硒炭基脱汞吸附材料的制备方法及材料和应用 |
Non-Patent Citations (1)
| Title |
|---|
| 刘宗寅: "《中学生实用化学方程式手册》", 31 January 1989 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112159049A (zh) * | 2020-10-28 | 2021-01-01 | 浙江大学 | 一种同步去除硒污染和硫化物污染的处理方法与装置 |
| CN112159049B (zh) * | 2020-10-28 | 2022-04-22 | 浙江大学 | 一种同步去除硒污染和硫化物污染的处理方法与装置 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4210628A (en) | Removal of nitrogen oxides | |
| CN112852430B (zh) | 一种修复汞污染土壤钝化剂及其制备方法和应用 | |
| CN107486133B (zh) | 一种天然气脱汞吸附剂及制备方法 | |
| CN111718719B (zh) | 一种硫化纳米零价铁-酸活化蒙脱石复合材料及其制备方法与应用 | |
| CN110841606A (zh) | 一种捕集二氧化碳的复合材料及其制备方法与应用 | |
| CA3113375A1 (en) | Nitrogen oxide absorption slurry and its preparation and use method thereof | |
| JPS6040893B2 (ja) | エチレン吸収剤およびその製造法 | |
| CN114100590A (zh) | 一种用于深度净化含铅废水的二硫化钼活性炭纤维复合吸附剂及其制备方法 | |
| CN111921363B (zh) | 一种煤气干法净化用高效脱硫剂及其制备方法和应用 | |
| CN114870808B (zh) | 一种高效稀土改性除氟材料及其制备方法 | |
| CN110681345A (zh) | 一种载硒和硫脱汞材料的制备方法 | |
| CN114100576B (zh) | 一种二硫化钴/炭复合材料及其制备方法和应用 | |
| CN115178239A (zh) | 同步吸附水中氮磷的金属改性多孔炭材料及制备方法 | |
| CN110255594B (zh) | 一种活性氧化铝的制备方法 | |
| CN113713757A (zh) | 一种用于废气液高效汞吸附剂的制备方法及产品 | |
| CN110743617A (zh) | 一种石墨炔基复合材料催化剂及其制备方法与应用 | |
| CN113398890A (zh) | 一种煤基腐植酸钠/沸石制备重金属复合吸附剂的方法 | |
| CN112221488A (zh) | 一种协同脱硝脱汞的新型核壳结构催化剂及制备方法 | |
| CN102179234B (zh) | 一种脱除氯化汞的专用活性炭的生产方法 | |
| CN113041992B (zh) | 一种去除放射性i-的埃洛石基高效吸附剂及其制备方法 | |
| CN112191227B (zh) | 一种用于天然气的脱汞剂及其制备方法 | |
| CN101343571A (zh) | 纳米复合锆锰基氧化物介孔脱硫剂的制备方法 | |
| CN114505047A (zh) | 一种巯基改性的sba-15及其制备方法、铋基吸附剂及其制备方法和应用 | |
| CN111675215A (zh) | 载硫活性炭材料及其制备方法和应用 | |
| CN113952924A (zh) | 一种用于含氰废气净化的吸附剂及其制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200114 |
|
| RJ01 | Rejection of invention patent application after publication |