WO2021223249A1 - 新型阴阳极电催化协同烟气脱硝的方法 - Google Patents

新型阴阳极电催化协同烟气脱硝的方法 Download PDF

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WO2021223249A1
WO2021223249A1 PCT/CN2020/089711 CN2020089711W WO2021223249A1 WO 2021223249 A1 WO2021223249 A1 WO 2021223249A1 CN 2020089711 W CN2020089711 W CN 2020089711W WO 2021223249 A1 WO2021223249 A1 WO 2021223249A1
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cathode
flue gas
anode
electrocatalysis
gas denitration
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French (fr)
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江波
徐灿程
关雨欣
牛庆赫
刘树梁
孟宪哲
刘奕捷
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青岛理工大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • 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
    • B01D53/32—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 by electrical effects other than those provided for in group B01D61/00
    • B01D53/326—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 by electrical effects other than those provided for in group B01D61/00 in electrochemical cells
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • 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
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B01D53/56—Nitrogen oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases

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  • the invention belongs to the technical field of atmospheric treatment, and in particular relates to a novel method for cooperating with cathode and anode electrocatalysis for flue gas denitration.
  • NOx control technology started relatively late, and currently there are two main types: one is the use of low-NOx combustion technology, such as air staging combustion technology, which can reduce the NOx emission concentration to a certain extent.
  • low-NOx combustion technology such as air staging combustion technology
  • the single use of this technology cannot meet the environmental protection requirements; the other is to remove NOx from the flue gas after combustion, the main methods are dry flue gas denitrification and wet flue gas denitrification.
  • the large-scale commercial application of dry flue gas denitration mainly includes two types: selective catalytic reduction (SCR) and selective non-catalytic reduction (SNCR).
  • SCR selective catalytic reduction
  • SNCR selective non-catalytic reduction
  • reducing agents which can selectively react with NOx in the flue gas to reduce it to pollution-free N 2 and H 2 O.
  • the main advantages are high denitration efficiency, low reaction temperature, and the product will not cause secondary pollution to the environment.
  • the SCR law has shortcomings such as easy catalyst deactivation, narrow operating temperature range, ammonia leakage and high investment cost.
  • urea or ammonia compounds as reducing agents can convert NOx into pollution-free N 2 .
  • the denitration process of the selective non-catalytic reduction method is completed in the combustion chamber of the boiler. Due to the high temperature environment, there is no need for catalysts, no need to modify the flue, and the investment is small, and it does not affect the operation of the unit.
  • wet flue gas denitration technology mainly uses oxidants such as acids or alkalis to oxidize and absorb NO x to remove nitrogen oxides. Commonly used methods are: nitric acid absorption method, complex absorption method, oxidation absorption method, lye absorption method, acid absorption method and so on.
  • the wet flue gas denitrification technology has the advantages of simple equipment and process, easy operation, and labor cost saving. However, the regeneration problem of the absorption liquid of this method and the decrease of denitrification efficiency after regeneration are also a difficult problem of this technology.
  • the strong NOx oxidants represented by ozone, potassium permanganate, hydrogen peroxide, and hypochlorous acid consume large amounts of reagents and increase the subsequent treatment of the waste liquid, so the application of this technology is limited.
  • the purpose of the present invention is to provide a cathode-anode electrocatalytic synergistic flue gas denitration method, which operates at room temperature and pressure, is easy to operate, can be applied to the treatment of room temperature and low concentration NOx, and has high out-of-stock efficiency And the process has no chemical reagents, no secondary pollution, low cost, low consumption, and high safety performance.
  • a new type of cathode and anode electrocatalysis and flue gas denitrification method The anode and cathode electrodes are set in the reactor, and NaCl solution is used as the electrolyte.
  • the flue gas to be denitrated enters the solution from the bottom of the reactor through the microporous aeration device, and is anodized.
  • the generated strong oxidizing hydroxyl radicals and active chlorine oxidize NO in the flue gas to high-valence NOx that is easily soluble in water, and the NOx absorbed by the water phase is converted into nitrite and nitrate.
  • the dissolved nitrate nitrogen can be The cathode is converted into nitrogen or ammonium by catalytic reduction, and the generated ammonium can be finally oxidized to nitrogen by hypochlorous acid generated by anode electrolysis, thereby completing the electrocatalytic denitrification reaction.
  • the working current density in the electrocatalytic denitration reaction is 1-50 mA/cm 2 ; the input voltage waveform is direct current or pulse.
  • the anode is one of ruthenium iridium electrode, lead oxide, and Sb-SnO 2 .
  • the cathode is a nitrate reduction catalyst.
  • the cathode is one of precious metals or inexpensive metals and their oxides; more preferably, the cathode is Pd, P, copper, One of indium, cobalt or their oxides.
  • the electrode spacing between the anode and the cathode is 1-10 cm.
  • the concentration of the NaCl solution is 0.001-1.0M.
  • the microporous aeration device is one of a membrane type microporous aerator, a tube type aerator, a disc type aerator, and a microporous ceramic aerator.
  • a spray device is also provided on the top of the reactor, and part of the electrolyte is lifted to the spray device by a lift pump to form a spray, which absorbs and degrades part of the overflowing NO.
  • the principle of the technical scheme of the present invention is: NO passes through the microporous aeration tray 12 and enters the solution from the inlet hose 9 at the bottom of the reactor. Using NaCl solution as electrolyte, Cl - will oxidize at anode 10 to generate Cl free radicals and ClO - . The anodic oxidation will oxidize NO in the flue gas into high-valence NOx that is easily soluble in water, and the NOx absorbed by the water phase will be converted into sub Nitrate and nitrate, and the dissolved nitrate nitrogen can be converted into nitrogen or ammonium by catalytic reduction on the cathode 7.
  • the generated ammonium can be finally oxidized to nitrogen by the hypochlorous acid generated by the anode electrolysis.
  • the gas outlet 2 overflow.
  • the system uses a lift pump to lift the solution to the top of the reaction device, and the spray nozzle 3 of the spray device forms a spray, which further increases the contact time and contact area of NO with the solution and improves the treatment efficiency.
  • the chemical (ionic) equation of the reaction is:
  • the technology operates at room temperature and pressure, and can be applied to the treatment of room temperature and low concentration NOx, and the process has no chemical reagents added, no secondary pollution, low cost, low consumption, and high safety performance.
  • Figure 1 Schematic diagram of the denitration reaction device of the present invention, in which, in the figure: 1-outlet hose, 2-gas outlet, 3-spray nozzle, 4-flange, 5-circulation hose, 6-cathode connection port, 7-cylinder cathode, 8-circulating water opening, 9-inlet hose, 10-anode, 11-anode connection port, 12-microporous aeration tray.
  • Use Ti/IrO 2 -RuO 2 as the anode, metal copper as the cathode, and the electrode spacing is 5 cm.
  • the NO concentration is 500ppm, and the flow rate is 1L/min into the solution through the membrane microporous aerator.
  • the electrolyte is sprayed from the spray device on the top through the lift pump, and part of the gas overflowing from the solution is brought back to the solution.
  • the treated gas is introduced into a gas cylinder after overflowing from the top of the reactor, and its concentration is measured with a flue gas analyzer to monitor the degree of treatment of NOx in real time.
  • the lead oxide electrode is used as the anode, the metal Pd coating is used as the cathode, and the electrode spacing is 5 cm.
  • the NO concentration is 500ppm, and the flow rate is 1.2L/min into the solution through the membrane microporous aerator.
  • the electrolyte is sprayed from the spray device on the top through the lift pump, and part of the gas overflowing from the solution is brought back to the solution.
  • the treated gas is introduced into a gas cylinder after overflowing from the top of the reactor, and its concentration is measured with a flue gas analyzer to monitor the degree of treatment of NOx in real time.
  • the Sb-SnO 2 electrode is used as the anode, and the metal cobalt is used as the cathode, and the distance between the electrodes is 6 cm.
  • 0.08M NaCl as the electrolyte, the initial pH value was adjusted to 7.
  • the NO concentration is 500ppm, and the flow rate is 1.3L/min into the solution through the membrane microporous aerator. No spraying device is used. After the treated gas overflows from the top of the reactor, it is introduced into a gas cylinder, and its concentration is measured by a flue gas analyzer to monitor the degree of treatment of NOx in real time.

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Abstract

一种阴阳极电催化协同烟气脱硝的方法，在反应器中设置阴阳电极，以NaCl溶液做电解质，待脱硝的烟气经微孔曝气装置，从反应器底部进入溶液，阳极氧化产生的强氧化性羟基自由基和活性氯将烟气中NO氧化为易溶于水体的高价态的NOx，被水相吸收的NOx转化为亚硝酸盐和硝酸盐，同时溶解的硝氮可在阴极上通过催化还原作用转化为氮气或者铵根，产生的铵根最终可被阳极电解生成的次氯酸氧化为氮气，以此完成电催化脱硝反应。

Description

新型阴阳极电催化协同烟气脱硝的方法 技术领域
本发明属于大气处理技术领域，具体涉及一种新型阴阳极电催化协同烟气脱硝的方法。
背景技术
我国能源结构以煤炭为主，其燃烧过程产生的烟气中含有大量的NOx，其中90-95％为难溶性的NO，会引发臭氧层空洞、光化学烟雾、酸雨、雾霾等一系列环境问题。因此，近些年烟气脱硫脱硝是我国能源与环境领域的战略要点，特别是对于治理当前备受关注的雾霾污染具有重要的环境与社会意义。
NOx的控制技术起步比较晚，目前主要有两种：一种是采用低NOx燃烧技术，如空气分级燃烧技术等，可在一定程度上降低NOx排放浓度。但随着环保要求日趋严格，单一采用该技术并不能达到环保要求；另一种是从燃烧后的烟气中脱除NOx，主要方法有干法烟气脱硝和湿法烟气脱硝。目前，大规模商业应用的干法烟气脱硝主要有：选择性催化还原法(SCR)和选择性非催化还原法(SNCR)两种。SCR脱硝原理：在一定温度和催化剂的作用下，以NH 3、CO、H 2等作为还原剂，可选择性的与烟气中的NOx反应，将其还原成无污染的N 2和H 2O。主要优点是脱硝效率高，反应温度低，并且产物不会造成环境的二次污染。另一方面，SCR法则存在催化剂易失活，操作温度范围窄，氨泄漏以及投资成本高等缺点。SNCR中，作为还原剂的尿素或氨类化合物可将NOx转化为无污染的N 2。选择性非催化还原法的脱硝过程是在锅炉燃烧室内完成，由于高温环境，无需催化剂，无需改造烟道，投资小，并且不影响机组运行。但其脱硝效率比较低下，操作温度高、氨易泄漏。湿法烟气脱硝技术主要利用酸或碱等氧化剂将NO x进行氧化吸收等过程而除去氮氧化物。常用的方法有：硝酸吸收法、络合吸收法、氧化吸收法、碱液吸收法、酸吸收法等。湿法烟气脱硝技术具有设备及流程简单、易操作、节约人工成本等优点，但是该法的吸收液再生问题及再生后的脱硝效率下降也是该技术的一项难题。以臭氧、高锰酸钾、双氧水、次氯酸为代表的NOx强氧化剂由于试剂消耗大、增加了对废液的后续处理，因此该技术应用受到限制。
发明内容
根据以上现有技术的不足，本发明的目的在于提供一种阴阳极电催化协同烟气脱硝方法，该技术常温常压运行，易操作，可应用于常温、低浓度NOx的治理，脱销效率高，且该过程无化学试剂添加，无二次污染，低成本低消耗安全性能高。
为了达到上述目的，本发明采用如下技术方案：
一种新型阴阳极电催化协同烟气脱硝的方法，在反应器中设置阴阳电极，以NaCl溶液做电解质，待脱硝的烟气经微孔曝气装置，从反应器底部的进入溶液，阳极氧化产生的强氧化性羟基自由基和活性氯将烟气中NO氧化为易溶于水体的高价态的NOx，被水相吸收的NOx转化为亚硝酸盐和硝酸盐，同时溶解的硝氮可在阴极上通过催化还原作用转化为氮气或者铵根，产生的铵根最终可被阳极电解生成的次氯酸氧化为氮气，以此完成电催化脱硝反应。
在上述方案的基础上，所述电催化脱硝反应中工作电流密度为1-50mA/cm 2；输入电压波形为直流或者脉冲。
在上述方案的基础上，所述阳极为钌铱电极、氧化铅、Sb-SnO 2中的一种。
在上述方案的基础上，所述阴极为硝氮还原催化剂，优选地，所述阴极为贵金属或者廉价金属及其氧化物中的一种；更加优选地，所述阴极为Pd、P、铜、铟、钴或其氧化物中的一种。
在上述方案的基础上，所述的阳极、阴极之间电极间距为1-10cm。
在上述方案的基础上，所述的NaCl溶液的浓度为0.001-1.0M。
在上述方案的基础上，所述的微孔曝气装置为膜片式微孔曝气器、管式曝气器、盘式曝气器、微孔陶瓷曝气器中的一种。
在上述方案的基础上，所述反应器的顶部还设置有喷淋装置，通过提升泵将部分电解液提升至喷淋装置，形成喷雾，吸收和降解部分溢出的NO。
本发明的技术方案的原理是：NO经过微孔曝气盘12微孔曝气，从反应器底部进口软管9进入溶液。以NaCl溶液做电解质，Cl -会在阳极10氧化生成Cl自由基和ClO -，利用阳极氧化将烟气中NO氧化为易溶于水体的高价态的NOx，被水相吸收的NOx转化为亚硝酸盐和硝酸盐，同时溶解的硝氮可在阴极7上通过催化还原作用转化为氮气或者铵根，产生的铵根最终可被阳极电解生成的次氯酸氧化为氮气从装置顶部气体出口2溢出。该体系利用提升泵将溶液提升至反应装置顶部，经喷淋装置的喷淋喷头3形成喷雾，进一步增加了NO与溶液的接触时间和接触面积，提升了处理效率。反应的化学(离子)方程式为：
NO+HClO→NO 2+HCl    3NO 2+H 2O→2HNO 3+NO
NO 2+H 2O→HNO 3+HNO 2    HNO 2+HClO→HNO 3+HCl
NO 3 -+2e -+2H +→NO 2 -+3H 2O    NO 2 -+6e -+8H +→NH 4 ++2H 2O
2NO 2 -+10e -+12H +→N 2+6H 2O    2NH 4 ++3HOCl→N 2+3H 2O+3Cl -+5H +
本发明的优点在于：
(1)利用阳极氧化、阴极还原协同处理NOx，将NOx(主要是NO)转化为无毒无害的N 2，简单方便，脱销效率高。
(2)该技术常温常压运行，可应用于常温、低浓度NOx的治理，且该过程无化学试剂添加，无二次污染，低成本低消耗安全性能高。
附图说明
图1本发明脱硝反应装置示意图，其中，图中：1-出口软管，2-气体出口，3-喷淋喷头，4-法兰盘，5-循环软管，6-阴极接电口，7-圆筒阴极，8-循环水开口，9-进口软管，10-阳极，11-阳极接电口，12-微孔曝气盘。
具体实施方式
在本发明中所使用的术语，除非有另外说明，一般具有本领域普通技术人员通常理解的含义。
下面接合具体实施例，并参照数据进一步详细的描述本发明。以下实施例只是为了举例说明本发明，而非以任何方式限制本发明的范围。
实施例1
采用Ti/IrO 2-RuO 2为阳极，金属铜为阴极，电极间距为5cm。采用0.05M NaCl为电解液，初始pH值调节为7。NO浓度为500ppm，以流量为1L/min通过膜片式微孔曝气器进入溶液中。电解液通过提升泵从顶部的喷淋装置形成喷雾，将部分溢出溶液的气体重新带回溶液。经过处理后的气体，从反应器的顶部溢出后引入一个气瓶，使用烟气分析仪测其浓度，实时监测NOx的处理程度。
工作电流密度为20mA/cm 2时，NO转化率为90％。
实施例2
采用氧化铅电极为阳极，金属Pd涂层为阴极，电极间距为5cm。采用0.07M NaCl为电解液，初始pH值调节为7。NO浓度为500ppm，以流量为1.2L/min通过膜片式微孔曝气器进入溶液中。电解液通过提升泵从顶部的喷淋装置形成喷雾，将部分溢出溶液的气体重新带回溶液。经过处理后的气体，从反应器的顶部溢出后引入一个气瓶，使用烟气分析仪测其浓度，实时监测NOx的处理程度。
工作电流密度为25mA/cm 2时，NO转化率为92％。
实施例3
采用Sb-SnO 2电极为阳极，金属钴为阴极，电极间距为6cm。采用0.08M NaCl为电解 液，初始pH值调节为7。NO浓度为500ppm，以流量为1.3L/min通过膜片式微孔曝气器进入溶液中。不采用喷淋装置，经过处理后的气体，从反应器的顶部溢出后引入一个气瓶，使用烟气分析仪测其浓度，实时监测NOx的处理程度。
工作电流密度为30mA/cm 2时，NO转化率为80％。
以上所述，仅是本发明的较佳实施例而已，并非是对本发明作其它形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。

Claims (10)

  1. 一种新型阴阳极电催化协同烟气脱硝的方法，其特征在于，在反应器中设置阴阳电极，以NaCl溶液做电解质，待脱硝的烟气经微孔曝气装置，从反应器底部的进入溶液，阳极氧化产生的强氧化性羟基自由基和活性氯将烟气中NO氧化为易溶于水体的高价态的NOx，被水相吸收的NOx转化为亚硝酸盐和硝酸盐，同时溶解的硝氮可在阴极上通过催化还原作用转化为氮气或者铵根，产生的铵根最终可被阳极电解生成的次氯酸氧化为氮气，以此完成电催化脱硝反应。
  2. 根据权利要求1所述新型阴阳极电催化协同烟气脱硝的方法，其特征在于，所述电催化脱硝反应中工作电流密度为1-50mA/cm 2；输入电压波形为直流或者脉冲。
  3. 根据权利要求1所述新型阴阳极电催化协同烟气脱硝的方法，其特征在于，所述阳极为钌铱电极、氧化铅、Sb-SnO 2中的一种。
  4. 根据权利要求1所述新型阴阳极电催化协同烟气脱硝的方法，其特征在于，所述阴极为硝氮还原催化剂。
  5. 根据权利要求4所述新型阴阳极电催化协同烟气脱硝的方法，其特征在于，所述阴极为贵金属或者廉价金属及其氧化物中的一种。
  6. 根据权利要求5所述新型阴阳极电催化协同烟气脱硝的方法，其特征在于，所述阴极为Pd、P、铜、铟、钴或其氧化物中的一种。
  7. 根据权利要求1所述新型阴阳极电催化协同烟气脱硝的方法，其特征在于，所述的阳极、阴极之间电极间距为1-10cm。
  8. 根据权利要求1所述新型阴阳极电催化协同烟气脱硝的方法，其特征在于，所述的NaCl溶液的浓度为0.001-1.0M。
  9. 根据权利要求1所述新型阴阳极电催化协同烟气脱硝的方法，其特征在于，所述的微孔曝气装置为膜片式微孔曝气器、管式曝气器、盘式曝气器、微孔陶瓷曝气器中的一种。
  10. 根据权利要求1～9任一项所述新型阴阳极电催化协同烟气脱硝的方法，其特征在于，所述反应器的顶部还设置有喷淋装置，通过提升泵将部分电解液提升至喷淋装置，形成喷雾，吸收和降解部分溢出的NO。
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