CN105944662A - 一种燃煤电厂烟气脱汞脱硝催化吸附剂及其制备方法 - Google Patents
一种燃煤电厂烟气脱汞脱硝催化吸附剂及其制备方法 Download PDFInfo
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000003546 flue gas Substances 0.000 title claims abstract description 23
- 239000003463 adsorbent Substances 0.000 title claims abstract description 16
- 230000003197 catalytic effect Effects 0.000 title abstract description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 56
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002808 molecular sieve Substances 0.000 claims abstract description 20
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 7
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 7
- 238000005342 ion exchange Methods 0.000 claims abstract description 5
- 239000002594 sorbent Substances 0.000 claims description 26
- 239000007787 solid Substances 0.000 claims description 20
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 16
- 239000012298 atmosphere Substances 0.000 claims description 15
- 239000008187 granular material Substances 0.000 claims description 13
- 238000013019 agitation Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- 229910052709 silver Inorganic materials 0.000 claims description 10
- 239000004332 silver Substances 0.000 claims description 10
- 238000005253 cladding Methods 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 3
- -1 ultrasonic after Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 29
- 229910000497 Amalgam Inorganic materials 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000010881 fly ash Substances 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 16
- 238000012360 testing method Methods 0.000 description 13
- 229910052753 mercury Inorganic materials 0.000 description 11
- 239000007789 gas Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- KEZYHIPQRGTUDU-UHFFFAOYSA-N 2-[dithiocarboxy(methyl)amino]acetic acid Chemical compound SC(=S)N(C)CC(O)=O KEZYHIPQRGTUDU-UHFFFAOYSA-N 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000269350 Anura Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052908 analcime Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000001925 catabolic effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012717 electrostatic precipitator Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052677 heulandite Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052679 scolecite Inorganic materials 0.000 description 1
- ORVGYTXFUWTWDM-UHFFFAOYSA-N silicic acid;sodium Chemical compound [Na].O[Si](O)(O)O ORVGYTXFUWTWDM-UHFFFAOYSA-N 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 229910052665 sodalite Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052815 sulfur oxide Inorganic materials 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
- B01J29/48—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing arsenic, antimony, bismuth, vanadium, niobium tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
本发明公开了一种燃煤电厂烟气脱汞脱硝催化吸附剂及其制备方法,该催化吸附剂由磁性的Fe3O4,分子筛,银纳米颗粒和活性组分V2O5组成。磁性Fe3O4可使催化吸附剂与飞灰有效分离,便于回收、再生和循环。分子筛由于具有良好的热稳定性,高比表面积,出色的离子交换能力,是一种优良的载体。银纳米颗粒可基于汞齐机制吸附单质汞。V2O5不仅能催化氧化NO,也可氧化单质汞。该催化吸附剂的制备步骤如下:首先在Fe3O4表面包覆一层SiO2,在甲苯溶剂中与分子筛混合,通过煅烧得到磁性分子筛,然后通过浸渍和煅烧负载上V2O5,最后通过离子交换和热还原负载纳米银,得到多功能磁性催化吸附剂。该催化吸附剂制备简单,易于回收再生,成本低廉,具有工业应用前景。
Description
技术领域
本发明属于环境保护及大气污染控制技术领域,涉及一种燃煤电厂烟气脱汞脱硝催化吸附剂设计及其制备方法。
背景技术
燃煤汞污染是继燃煤硫和氮氧化物污染之后的又一大气污染问题,引起人们广泛关注。燃煤电厂被认为是最重要的人为汞排放源之一。利用电厂现有的大气污染物控制设备实现汞的脱除在很大程度上取决于烟气中汞的形态分布。燃烧中汞的排放有三种形态:气相单质汞(Hg0)、气相氧化态汞(Hg2+)和颗粒态汞(HgP)。氧化态汞由于具有水溶性可被湿法脱硫装置脱除,大部分颗粒态汞则可被静电除尘器或布袋除尘器脱除(取决于除尘效益),而气相单质汞绝大部分会以气态的形式进入到大气中。传统的汞排放控制技术是采用活性炭及改性活性炭喷射,主要依靠物理或者物理化学吸附,但是存在难以分离和再生,成本高昂,造成飞灰的二次污染等问题,因此难以大规模的应用。
利用贵金属如Pd,Pt,Au,Ag能与汞形成稳定的汞齐是有效捕集汞的另一途径,但需要合适的载体。分子筛是一种优良的载体,廉价易得,水热稳定性好,机械强度高,比表面积大,能够通过离子交换负载贵金属纳米颗粒,增加吸附汞的能力,提升利用效率。研究表明,负载纳米银颗粒的磁性菱沸石在150℃下其脱汞效率几乎达到100%,而汞齐银在227℃以上可分解释放汞实现再生。鉴于易分离,再生和循环使用的特征,磁性载银菱沸石已经用于实际电厂测试。但是,这种材料只用于单污染物汞的控制。
氮氧化物(NOX)也是一种来自煤燃烧的大气污染物。目前比较成熟的技术是采用氨气选择性催化还原(SCR)来控制氮氧化物的污染。商用的SCR脱硝催化剂主要组成是V2O5–WO3(MoO3)/TiO2,其中V2O5是主要的活性组分。有研究发现,V2O5基催化剂不仅能还原NOX,而且能把Hg0氧化成Hg2+。目前为止,尚未有人在分子筛上同时负载银和氧化钒,并做成磁性材料而实现协同脱除燃煤烟气中的汞和氮氧化物。
发明内容
本发明的目的在于提供一种能同时实现脱汞脱硝功能的催化吸附剂及其制备方法。本发明制备的多功能材料既可吸附和催化氧化Hg0,也可催化还原NOx,在不增加燃煤电厂烟气污染物控制设备的前提下,实现了Hg0和NOx的协同脱除。而且合成方法简单可靠,易于回收和再生,具有良好的工业化应用前景。
为实现本发明的目的,采用以下技术方案:
一种燃煤电厂烟气脱汞脱硝催化吸附剂,主要由磁性中心Fe3O4,载体分子筛,银纳米颗粒和活性组分V2O5组成。磁性中心通过包覆的一层SiO2与分子筛连接,银纳米颗粒和活性组分V2O5负载于载体上。
所述分子筛是可进行离子交换的一系列分子筛,包括天然沸石如方沸石,菱沸石,钙沸石,片沸石,钠沸石,丝光沸石,辉沸石和人造沸石,如A型分子筛(3A,4A,5A),X型分子筛(10X,13X),Y型分子筛,ZSM系列分子筛(ZSM-5,ZSM-11,ZSM-22),氢型的ZSM系列分子筛(HZSM-5,HZSM-11,HZSM-22),SAPO系列分子筛(SAPO-11,SAPO-34)。
所述包覆一层SiO2后的Fe3O4占催化吸附剂的质量分数为10%~40%,分子筛占催化吸附剂的质量分数为30%~88.5%,活性组分V2O5占催化吸附剂的质量分数为0.5%~10%,银纳米颗粒占据催化吸附剂的质量分数为1%~20%。
一种上述燃煤电厂烟气脱汞脱硝催化吸附剂的制备方法,包括以下步骤:
(1)将Fe3O4和去离子水的悬浊液超声后于80℃下机械搅拌,向上述悬浊液中加入1mol/L的硅酸钠溶液,然后滴加0.1~0.5mol/L的盐酸或者硫酸维持溶液的pH在9.3~9.7之间,保温1小时后冷却至室温,包覆了一层SiO2的Fe3O4颗粒通过磁铁分离,并用去离子水洗涤两次,超声将分子筛和甲苯混合,加入包覆后的Fe3O4颗粒,超声后,悬浮液分层,倒出上层甲苯液体,剩余的甲苯在真空下除去;将沉淀的固体300℃惰性气体氛围下煅烧1小时,然后将煅烧后的固体研磨筛分至100目以下,得到磁性分子筛;
(2)偏钒酸铵和草酸按照1:2的摩尔比溶于去离子水得到溶液,将步骤(1)得到的磁性分子筛加入到上述溶液中,超声1~3小时后浸渍15~72小时,于80~110℃蒸干,得到的固体在450~550℃下煅烧3~6小时,冷却至室温,筛分至100目以下,得到负载活性组分V2O5的磁性分子筛;
(3)将步骤(2)得到的负载活性组分V2O5的磁性分子筛加入硝酸银溶液中,80℃下机械搅拌6~12小时,让其充分的进行离子交换,将离子交换后的固体过滤,多次洗涤,在80~110℃下干燥,然后放于管式炉中400℃惰性气体氛围下煅烧1小时,得到同时负载银纳米颗粒和活性组分V2O5的磁性分子筛催化吸附剂。筛分至100目以下,其中,步骤(1)中的硅酸钠溶液为硅酸钠和硅溶胶配置而成;
步骤(1)和步骤(3)的惰性气体气氛是氮气或者氩气;
步骤(2)中的煅烧气氛是空气或者惰性气体气氛;
步骤(3)中的硝酸银溶液浓度0.01~2mol/L,用量根据催化吸附剂需要负载的银含量确定。
本发明提供了一种燃煤电厂烟气脱硝脱汞的催化吸附剂,与传统技术相比,本发明具有以下优点和效果:
(1)具备良好脱汞和脱硝能力,可协同脱除燃煤烟气中的单质汞和氮氧化物,降低了设备安装和使用费用;
(2)该催化吸附剂由于具有磁性,易于与飞灰分离,避免了飞灰的二次污染;同时该催化吸附剂易于回收,再生简单,可循环使用,大大降低了成本,因此适合工业化大规模生产。
附图说明
图1为本发明的合成流程。
具体实施方式
以下结合具体实施例来对本发明作进一步的说明,但本发明所要求保护的范围并不局限于实施例所描述之范围。
各实施例中所使用的化学品均可通过公开商业途径获得。
实施例1
(1)将2g Fe3O4和140mL去离子水的悬浊液超声5分钟后于80℃下机械搅拌,取4.466g五水硅酸钠溶于20mL硅溶胶,加入到上述悬浊液中,然后滴加0.1mol/L的盐酸维持溶液的pH在9.3~9.7之间,保温1小时后冷却至室温,包覆了一层SiO2的Fe3O4颗粒通过磁铁分离,并用去离子水冲洗两次,超声将6g硅铝比(摩尔比,以下实施例同)25的HZSM-5分子筛和60mL甲苯混合,加入包覆后的Fe3O4颗粒,用细胞粉碎机超声20分钟,待悬浮液分层后,倒出上层甲苯液体,剩余的甲苯在真空下除去。将沉淀的固体300℃氮气氛围下煅烧1小时,然后将煅烧后的固体研磨筛分至100目以下,得到磁性分子筛;
(2)将0.105g偏钒酸铵和0.226g草酸溶于5mL去离子水,取8g步骤(1)得到的磁性分子筛加入到上述溶液中,超声3小时后浸渍15小时,将混合物中的液体于110℃蒸干,得到的固体在550℃空气氛围下煅烧4小时,冷却至室温,筛分至100目以下,得到V2O5含量质量分数为1%的磁性分子筛;
(3)取7.5g步骤(2)得到的负载V2O5的磁性分子筛按照固液比1:10(质量比,以下实施例同)的比例加入到0.05mol/L的硝酸银溶液中,80℃下机械搅拌12小时,过滤,洗涤,110℃下干燥12小时,放于管式炉中400℃氮气氛围下煅烧1小时,得到同时负载银纳米颗粒和活性组分V2O5的磁性分子筛催化吸附剂。
首先测试了催化吸附剂吸附汞的容量,测试条件为载气N2流量为40ml/min,Hg0浓度为520μg/m3,测试汞20%穿透时其脱汞容量约为18μg/g。将合成的催化吸附剂置于模拟烟气的实验系统上进行脱汞脱硝性能测试。模拟烟气条件如下:5%O2,12%CO2,400ppm NO,400ppm NH3,600ppm SO2,30ppm HCl,Hg0浓度为79μg/m3,平衡气体为N2,流量为400ml/min,其协同脱汞脱硝结果为,Hg0最大脱除效率98%,NOx脱除效率为56%。
实施例2
(1)将2g Fe3O4和140mL去离子水的悬浊液超声5分钟后于80℃下机械搅拌,取4.466g五水硅酸钠溶于20mL硅溶胶,加入到上述悬浊液中,然后滴加0.1mol/L的硫酸维持溶液的pH在9.3~9.7之间,保温1小时后冷却至室温,包覆了一层SiO2的Fe3O4颗粒通过磁铁分离,并用去离子水冲洗两次,超声将6g硅铝比25的HZSM-5分子筛和60mL甲苯混合,加入包覆后的Fe3O4颗粒,用细胞粉碎机超声20分钟,待悬浮液分层后,倒出上层甲苯液体,剩余的甲苯在真空下除去。将沉淀的固体300℃氩气氛围下煅烧1小时,然后将煅烧后的固体研磨筛分至100目以下,得到磁性分子筛;
(2)将0.547g偏钒酸铵和1.172g草酸溶于6mL去离子水,取8g步骤(1)得到的磁性分子筛加入到上述溶液中,超声2小时后浸渍24小时,将混合物中的液体于80℃蒸干,得到的固体在500℃氮气氛围下煅烧4小时,冷却至室温,筛分至100目以下,得到V2O5含量质量分数为5%的磁性分子筛;
(3)取7.5g步骤(2)得到的负载V2O5的磁性分子筛按照固液比1:5的比例加入到0.2mol/L的硝酸银溶液中,80℃下机械搅拌12小时,过滤,洗涤,80℃下干燥12小时,放于管式炉中400℃氩气氛围下煅烧1小时,得到同时负载银纳米颗粒和活性组分V2O5的磁性分子筛催化吸附剂。
首先测试了催化吸附剂吸附汞的容量,测试条件为载气N2流量为40ml/min,Hg0浓度为520μg/m3,测试汞20%穿透时其脱汞容量约为20μg/g。将合成的催化吸附剂置于模拟烟气的实验系统上进行脱汞脱硝性能测试。模拟烟气条件如下:5%O2,12%CO2,400ppm NO,400ppm NH3,600ppm SO2,30ppm HCl,Hg0浓度为79μg/m3,平衡气体为N2,流量为400ml/min,其协同脱汞脱硝结果为,Hg0最大脱除效率98%,NOx脱除效率为70%。
实施例3
(1)将2g Fe3O4和140mL去离子水的悬浊液超声5分钟后于80℃下机械搅拌,取3.349g五水硅酸钠溶于15mL硅溶胶,加入到上述悬浊液中,然后滴加0.1mol/L的硫酸维持溶液的pH在9.3~9.7之间,保温1小时后冷却至室温,包覆了一层SiO2的Fe3O4颗粒通过磁铁分离,并用去离子水冲洗两次,超声将4g硅铝比25的HZSM-5分子筛和40mL甲苯混合,加入包覆后的Fe3O4颗粒,用细胞粉碎机超声20分钟,待悬浮液分层后,倒出上层甲苯液体,剩余的甲苯在真空下除去。将沉淀的固体300℃氩气氛围下煅烧1小时,然后将煅烧后的固体研磨筛分至100目以下,得到磁性分子筛;
(2)将0.866g偏钒酸铵和1.857g草酸溶于4mL去离子水,取6g步骤(1)得到的磁性分子筛加入到上述溶液中,超声2小时后浸渍24小时,将混合物中的液体于80℃蒸干,得到的固体在500℃空气氛围下煅烧4小时,冷却至室温,筛分至100目以下,得到V2O5含量质量分数为10%的磁性分子筛;
(3)取5.5g步骤(2)得到的负载V2O5的磁性分子筛按照固液比1:10的比例加入到0.2mol/L的硝酸银溶液中,80℃下机械搅拌12小时,过滤,洗涤,80℃下干燥12小时,放于管式炉中400℃氩气氛围下煅烧1小时,得到同时负载银纳米颗粒和活性组分V2O5的磁性分子筛催化吸附剂。
首先测试了催化吸附剂吸附汞的容量,测试条件为载气N2流量为40ml/min,Hg0浓度为520μg/m3,测试汞20%穿透时其脱汞容量约为25μg/g。将合成的催化吸附剂置于模拟烟气的实验系统上进行脱汞脱硝性能测试。模拟烟气条件如下:5%O2,12%CO2,400ppm NO,400ppm NH3,600ppm SO2,30ppm HCl,Hg0浓度为79μg/m3,平衡气体为N2,流量为400ml/min,其协同脱汞脱硝结果为,Hg0最大脱除效率100%,NOx脱除效率为73%。
实施例4
(1)将2g Fe3O4和140mL去离子水的悬浊液超声5分钟后于80℃下机械搅拌,取4.466g五水硅酸钠溶于20mL硅溶胶,加入到上述悬浊液中,然后滴加0.1mol/L的硫酸维持溶液的pH在9.3~9.7之间,保温1小时后冷却至室温,包覆了一层SiO2的Fe3O4颗粒通过磁铁分离,并用去离子水冲洗两次,超声将6g 4A分子筛和60mL甲苯混合,加入包覆后的Fe3O4颗粒,用细胞粉碎机超声20分钟,待悬浮液分层后,倒出上层甲苯液体,剩余的甲苯在真空下除去。将沉淀的固体300℃氩气氛围下煅烧1小时,然后将煅烧后的固体研磨筛分至100目以下,得到磁性分子筛;
(2)将0.547g偏钒酸铵和1.172g草酸溶于6mL去离子水,取8g步骤(1)得到的磁性分子筛加入到上述溶液中,超声2小时后浸渍24小时,将混合物中的液体于80℃蒸干,得到的固体在500℃氮气氛围下煅烧4小时,冷却至室温,筛分至100目以下,得到V2O5含量质量分数为5%的磁性分子筛;
(3)取7.5g步骤(2)得到的负载V2O5的磁性分子筛按照固液比1:5的比例加入到0.2mol/L的硝酸银溶液中,80℃下机械搅拌12小时,过滤,洗涤,80℃下干燥12小时,放于管式炉中400℃氩气氛围下煅烧1小时,得到同时负载银纳米颗粒和活性组分V2O5的磁性分子筛催化吸附剂。
首先测试了催化吸附剂吸附汞的容量,测试条件为载气N2流量为40ml/min,Hg0浓度为520μg/m3,测试汞20%穿透时其脱汞容量约为50μg/g。将合成的催化吸附剂置于模拟烟气的实验系统上进行脱汞脱硝性能测试。模拟烟气条件如下:5%O2,12%CO2,400ppm NO,400ppm NH3,600ppm SO2,30ppm HCl,Hg0浓度为79μg/m3,平衡气体为N2,流量为400ml/min,其协同脱汞脱硝结果为,Hg0最大脱除效率100%,NOx脱除效率为71%。
上述各实施例对本发明进行了更详细的描述,不应将此理解为本发明的主题范围仅限于上述实施例。只要在本发明的精神和原则之内,所作的任何修改、等同替换、改进等均属于本发明的保护范围之内。
Claims (8)
1.一种燃煤电厂烟气脱汞脱硝催化吸附剂,其特征在于:包括磁性中心Fe3O4,载体分子筛,银纳米颗粒和活性组分V2O5组成。磁性中心通过包覆的一层SiO2与载体分子筛连接,银纳米颗粒和活性组分V2O5负载于载体分子筛上。
2.根据权利要求1所述的一种燃煤电厂烟气脱汞脱硝催化吸附剂,其特征在于:所述分子筛是能进行离子交换的分子筛。
3.根据权利要求1或2所述的一种燃煤电厂烟气脱汞脱硝催化吸附剂,其特征在于包覆一层SiO2后的Fe3O4占催化吸附剂的质量分数为10%~40%,分子筛占催化吸附剂的质量分数为30%~88.5%,活性组分V2O5占催化吸附剂的质量分数为0.5%~10%,银纳米颗粒占据催化吸附剂的质量分数为1%~20%。
4.制备如权利要求1-3任意一项所述一种燃煤电厂烟气脱汞脱硝催化吸附剂的方法,其特征在于,包括以下步骤:
(1)将Fe3O4和去离子水的悬浊液超声后于80℃下机械搅拌,向上述悬浊液中加入1mol/L的硅酸钠溶液,然后滴加0.1~0.5mol/L的盐酸或者硫酸维持溶液的pH在9.3~9.7之间,保温1小时后冷却至室温,包覆了一层SiO2的Fe3O4颗粒通过磁铁分离,并用去离子水洗涤两次,超声将分子筛和甲苯混合,加入包覆后的Fe3O4颗粒,超声后,悬浮液分层,倒出上层甲苯液体,剩余的甲苯在真空下除去;将沉淀的固体300℃惰性气体氛围下煅烧1小时,然后将煅烧后的固体研磨筛分至100目以下,得到磁性分子筛;
(2)偏钒酸铵和草酸按照1:2的摩尔比溶于去离子水得到溶液,将步骤(1)得到的磁性分子筛加入到上述溶液中,超声1~3小时后浸渍15~72小时,于80~110℃蒸干,得到的固体在450~550℃下煅烧3~6小时,冷却至室温,筛分至100目以下,得到负载活性组分V2O5的磁性分子筛;
(3)将步骤(2)得到的负载活性组分V2O5的磁性分子筛加入硝酸银溶液中,80℃下机械搅拌6~12小时,让其充分的进行离子交换,将离子交换后的固体过滤,多次洗涤,在80~110℃下干燥,然后放于管式炉中400℃惰性气体氛围下煅烧1小时,得到同时负载银纳米颗粒和活性组分V2O5的磁性分子筛催化吸附剂。
5.根据权利要求4所述的方法,其特征在于,步骤(1)中的硅酸钠溶液为硅酸钠和硅溶胶配置而成。
6.根据权利要求4所述的方法,其特征在于,步骤(1)和步骤(3)的惰性气体气氛是氮气或者氩气。
7.根据权利要求4所述的方法,其特征在于,步骤(2)煅烧气氛是空气或者惰性气体气氛。
8.根据权利要求4所述的方法,其特征在于,步骤(3)中的硝酸银溶液浓度0.01~2mol/L。
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CN106693882A (zh) * | 2016-12-09 | 2017-05-24 | 清华大学 | 一种燃煤电厂烟气脱汞吸附剂及其制备方法 |
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WO2020133574A1 (zh) * | 2018-12-27 | 2020-07-02 | 天津大学 | 一种消除并回收利用燃烧尾气中的氮氧化物的方法 |
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CN106422666B (zh) * | 2016-12-07 | 2023-10-03 | 西安热工研究院有限公司 | 一种燃煤电厂烟气循环吸附剂脱汞装置及脱汞方法 |
CN106693882A (zh) * | 2016-12-09 | 2017-05-24 | 清华大学 | 一种燃煤电厂烟气脱汞吸附剂及其制备方法 |
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CN106732347B (zh) * | 2016-12-09 | 2019-08-13 | 清华大学 | 一种用于燃煤电厂烟气脱汞sba-15基载银吸附剂的制备方法 |
CN107029667A (zh) * | 2017-05-18 | 2017-08-11 | 郑州轻工业学院 | 一种Fe3O4‑rGO‑Ag复合材料及其制备方法与应用 |
CN107335468A (zh) * | 2017-07-07 | 2017-11-10 | 国电环境保护研究院 | 一种V‑Cu‑4A沸石‑KX‑凹土复合烟气脱硝脱汞板式催化剂及其制备方法 |
CN107754799A (zh) * | 2017-11-23 | 2018-03-06 | 北京工业大学 | 一种硅铁渣制备中温脱汞催化材料的方法 |
WO2020133574A1 (zh) * | 2018-12-27 | 2020-07-02 | 天津大学 | 一种消除并回收利用燃烧尾气中的氮氧化物的方法 |
CN113731356A (zh) * | 2021-07-07 | 2021-12-03 | 生态环境部华南环境科学研究所 | 一种改性活性炭吸附剂及其制备方法和应用 |
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