NO的常温催化氧化及碱液吸收脱除NO_x过程研究
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摘要
氮氧化物(NOx)对生态环境和人类健康造成极大的危害,脱除NOx成为当前环境领域的重要研究课题之一。与燃煤电厂排放的含NOx烟气不同,化工、制药等工厂排放的工业废气中虽然NOx总量较少,但浓度较高,对排放周边局部区域环境污染严重,对这类NOx废气的治理更是刻不容缓。这类废气通常具有如下基本特征：(1)氧气含量高,可达到-20%,几乎与空气相同；(2)水汽含量高,可达到饱和湿含量；(3)NOx氧化度(N02与NOx浓度之比)低,部分企业排放废气中NOx氧化度低于10%；(4)常温常压排放；(5)精细化工厂、制药厂废气呈间歇性排放。由于其与燃煤烟气排放特征巨大的差异,常用的高温条件下以氨(NH3)为还原剂的选择性催化还原NOx脱除技术(NH3-SCR)不适合,而常温常压操作、对NOx浓度波动不敏感并且可回收(亚)硝酸盐的碱液吸收法更适合工业NOx废气的处理。基于此,论文提出采用NO气相催化氧化-碱液吸收法脱除工业废气中NOx的工艺,以此过程为对象进行了以下几方面研究,并获得了相关进展：
1、碱液(包括NaOH溶液、还原性和氧化性NaOH溶液)吸收NOx过程研究
(1)在碱液中添加还原剂(尿素、亚硫酸铵、亚硫酸钠、硫化钠或硫代硫酸钠等)或者氧化剂(双氧水或次氯酸钠等)均能提高吸收液对NOx的脱除率,但NaOH和添加剂(还原剂和氧化剂)浓度对NOx脱除率的影响不显著；随着进口NOx浓度提高,NOx脱除率随之增加；气体停留时间增加,NOx脱除率亦增加,并主要表现为NO2脱除率的增加；
(2)NOx氧化度对NOx脱除率的影响最为显著。在NaOH溶液或添加尿素的NaOH溶液为吸收剂的体系中,进口NOx氧化度为50～70%时NOx脱除率最高,存在最优氧化度；而对于添加氧化剂和还原剂(除尿素外)的NaOH溶液中,进口NOx氧化度越高,NOx脱除率越高。因此,提高工业废气NOx氧化度是保证高效脱除NOx的关键；
(3)碱液吸收NOx系统中,各NOx脱除途径的相对速率如下：通过NO2与亚硫酸铵作用脱除NO2>通过NO+N02→N203与NaOH作用脱除NOx>通过NO2与NaOH或H202作用脱除N02。
2、椰壳基活性炭(AC)及改性活性炭(MAC)、微孔分子筛(高硅H-和Na-ZSM-5分子筛、全硅β分子筛)上NO的常温氧化过程研究
(1)随着反应温度升高,干气条件下NO转化率降低,表现出类似气相均相反应的负活化能效应；在湿气条件下改性活性炭(MAC)和高硅ZSM-5分子筛上NO转化率先增后降,存在最佳反应温度,对于MAC为50～70℃,对高硅ZSM-5分子筛则为20℃,而全硅β分子筛上在10～90℃范围内,NO转化率呈单调下降的趋势；
(2)随着进口NO、02浓度以及空时的增加,NO转化率增加；
(3)水汽的存在对催化剂表面NO的氧化存在抑制作用；由于AC及MAC自身含有宽泛的孔径分布(特别是中孔孔道的存在),导致其对NO氧化的催化活性受水汽影响严重；而对于分子筛而言,提高Si/A1比可减少其对水汽的吸附从而降低水汽的影响,因此,湿气条件下微孔分子筛Si/Al比越高,NO转化率越高；
(4)干、湿气条件下催化剂稳定性实验结果表明,高硅ZSM-5、全硅β分子筛对NO的常温氧化催化活性没有下降,说明高硅ZSM-5、全硅β分子筛具有良好的稳定性,有望在工业上应用；
(5)微孔孔道是保证活性炭、分子筛等材料具有NO氧化催化活性的前提,微孔比表面积和微孔孔容越大,其对NO氧化催化活性越高；
(6)通过TPD/TPSR.原位DRIFTS技术对高硅Na-ZSM-5和全硅β分子筛上NO氧化机理研究表明,分子筛表面的羟基(-OH)和阳离子(如Na+)是NO氧化催化活性位；02在微孔分子筛表面不吸附,而NO在其表面存在强的化学吸附,NO2只存在弱吸附；在NO氧化反应气氛下,NO在Na+上的吸附态以N03(即：OONO)为主,而在羟基(-OH)上的吸附态可能以(NO)2(即：ONNO)为主,由此推测高硅Na-ZSM-5分子筛上存在如下的NO氧化反应机理：NO+σ??NO·σNO·σ+O2N03·6 NO3·σ+NO·σ.?N2O4+2σ?2NO2+2σ
而在全硅β分子筛上NO的氧化反应机理为：NO+σ?NO·σNO·σ+NO·σ?(NO·σ)2 (NO·σ)2+O2?2NO2+2σ?N2O4+2σ
以上研究表明,采用高硅ZSM-5分子筛或全硅β分子筛催化剂可实现在水汽环境中NO的高效气相氧化,提高NOx氧化度；而通过添加氧化剂或还原剂的NaOH溶液可强化碱液对NOx的化学吸收；两项技术的有机组合可有效提高碱液吸收法对NOx的脱除效率,说明本论文提出的气相催化氧化-碱液吸收法工艺和相关技术具有可行性。
The abatement of the nitric oxides (NOx) is becoming one of important challenges since NOx are the source of severe eco-environmental problems and harmful to human health. Differing from the NOx flue gas from the power station by burning fossil fuels such as coal, oil and natural gas, the NOx industrial waste gas exhausts with low quantity but high local NOx concentration leading to severe pollution to local environment, so is urgent to be treated now. Generally, the NOx industrial exhausted gas is discharged under the following conditions of:(1) high oxygen content (-20%(V)); (2) high vapor content which can reach the saturated one in the gas; (3) low NOx oxidation degree (defined as the ratio of the concentration of NO2 and that of NOx in the gas), even lower than 10%; (4) ambient temperature and normal pressure; (5) dramatical fluctuation of NOx concentration due to the batch or non-continuous operation mode of the previous production units. According to these features, the NH3-SCR (Selective Catalytic Reduction) method is not suitable to the removal of NOx from the industrial process since SCR process needs high temperature and excellent control of the addition of NH3 content, while alkaline solution absorption process operating at normal temperature and normal pressure may be more suitable because the absorption process is insensitive to the fluctuation of NOx content and even can recover nitrite and nitrate salts. However, the low NO solubility in aqueous solution could lead to low NOx removal efficiency for this wet scrubbing process. So the process of NO gas phase catalytic oxidation and alkaline solution absorption was proposed, and then investigated in detail in this paper. Some conclusions have been drawn as following:
1. Study on the absorption process of NOx by the alkaline solution including NaOH solution without and with the addition of the reductants or the oxidants
(1) The addition of the reductants (including urea, ammonium sulfite, sodium sulfite, sodium sulfide or sodium hyposulfite, etc.) or the oxidants (including hydrogen peroxide or sodium hypochlorite, etc.) promote the absorption of NOx, but the NOx removal efficiency is insensitive to the concentration of NaOH and the additives (including the reductants and the oxidants). With the increase of the inlet NOx concentration, the removal efficiency of NOx will increase. The increase of the gas phase resident time will make for the removal efficiency of NOx especially that of NO2.
(2) Among the operation conditions, the inlet NOx oxidation degree is the most significant one which effects the NOx removal, and exists the optimal value of 50～70%when using the NaOH solution or the urea-NaOH solution as the absorption solvents, but the higher inlet NOx oxidation degree will lead to the higher NOx removal efficiency when using the oxidant-NaOH solutions or the reductant-NaOH solutions (except urea additive). So, the key of the high NOx removal efficiency will result from the increase of the inlet NOx oxidation degree.
(3) The relative rate of NOx removal by the alkaline solution absorption process can be sorted as followed:the rate of NO2 removal through the reaction of NO2 and (NH4)2SO3> the rate of NOx removal through the reaction of NaOH and N2O3 equilibrated with NO and NO2> the rate of NO2 removal through the reaction of NO2 and NaOH or H2O2.
2. The study on the NO oxidation at ambient temperature by oxygen in the NOx waste gas on the catalysts including the coconut-based activated carbon (AC) and the modified activated carbon (MAC), the micro porous-based molecular sieve (high silica H-and Na-ZSM-5, pure silicaβ-ype molecular sieve)
(1) With the increase of the reaction temperature, the NO conversion in the NO catalytic oxidation decreases under the dry NOx waste gas, but exists maximum value under the humid NOx waste gas at the temperature of 50～70℃over MAC and 20°C over ZSM-5 molecular sieve, while decreases monotonously over pure silicaβ-type molecular sieve during the range of the reaction temperature from 10°C to 90°C.
(2) The increase of the inlet concentrations of NO and O2 and the space time benefits the NO conversion.
(3) The vapor inhibits the oxidation of NO on all the investigated catalysts, but the extent of inhibitory effect depends on the nature of the catalysts. The effect of vapor on the NO oxidation on the AC (MAC) may be the most serious one due to its wide pore size distribution, especially the exist of the mesopore. Nevertheless, there is another situation to the molecular sieve, that is, the high hydrophobic surface can be obtained on the molecular sieve with high Si/Al ratio, which leads to less adsorption to vapor. So, the higher NO conversion under the wet NOx gas will be obtained on the molecular sieve with the higher Si/Al ratio.
(4) The catalytic activity of the high silica ZSM-5 molecular sieve and the pure silicaβ-type molecular sieve demonstrates high stability both in the dry NOx gas and in the saturated wet NOx gas during the long periodic stability test, which means their potential industrial application in the NOx removal process.
(5) The micro porous channels guarantee the catalytic activity of ACs and the molecular sieves to NO oxidation at ambient temperature, and the high catalytic activity can be obtained over the catalysts with high micro porous specific superficial area and volume.
(6) The characterizations of TPD/TPSR and in-situ DRIFTS of the adsorbed NOx species on the high silica Na-ZSM-5 and the pure silicaβ-type molecular sieve reveal the reaction mechanisms of NO catalytic oxidation at ambient temperature. The molecular sieves exhibit the high catalytic activity through the active adsorption sites of the hydroxyl group (-OH) and cation (such as Na+). There is no adsorbing oxygen and only weakly-adsorbing NO2 can be detected on the surface of the molecular sieve, while NO can adsorb strongly on it. The adsorbing species of NO depends on the types of the active sites, e.g., the adsorbing NO3 (i.e., OONO) specie mainly exists in cation such as Na+, while the adsorbing (NO)2 (i.e., ONNO) specie may be in the hydroxyl group (-OH). Based on these, the catalytic reaction mechanism of NO oxidation at ambient temperature on the high silica Na-ZSM-5 molecular sieve can be speculated as following:
NO+σ?NO·σ
NO·σ+O2?NO3·σ
NO3·σ+NO·σ?N2O4+2σ?2NO2+2σWhile the reaction mechanism on the pure silicaβ-type molecular sieve may be shown as:
NO+σ?NO·σ
NO·σ?(NO·σ)2
(NO·σ)2+O2?2NO2+2σ?N2O4+2σ
All above investigations show that the NOx oxidation degree can efficiently be increased through the NO oxidation by O2 at the ambient temperature under the wet NOx waste gas using the high silica ZSM-5 or the pure silicaβ-type molecular sieve as the catalysts, and the chemical absorption of NOx can be enhanced by the addition of the reductant or the oxidant into the alkaline solution as the absorption solvent. Furthermore, the combination of the above two technologies synergically will lead to high NOx removal efficiency of the wet scrubbing process for NOx abatement, and the feasibility of the process of NO gas phase catalytic oxidation and alkaline solution absorption for the NOx removal from the industrial exhausted gas is then proved.
1、碱液(包括NaOH溶液、还原性和氧化性NaOH溶液)吸收NOx过程研究
(1)在碱液中添加还原剂(尿素、亚硫酸铵、亚硫酸钠、硫化钠或硫代硫酸钠等)或者氧化剂(双氧水或次氯酸钠等)均能提高吸收液对NOx的脱除率,但NaOH和添加剂(还原剂和氧化剂)浓度对NOx脱除率的影响不显著；随着进口NOx浓度提高,NOx脱除率随之增加；气体停留时间增加,NOx脱除率亦增加,并主要表现为NO2脱除率的增加；
(2)NOx氧化度对NOx脱除率的影响最为显著。在NaOH溶液或添加尿素的NaOH溶液为吸收剂的体系中,进口NOx氧化度为50～70%时NOx脱除率最高,存在最优氧化度；而对于添加氧化剂和还原剂(除尿素外)的NaOH溶液中,进口NOx氧化度越高,NOx脱除率越高。因此,提高工业废气NOx氧化度是保证高效脱除NOx的关键；
(3)碱液吸收NOx系统中,各NOx脱除途径的相对速率如下：通过NO2与亚硫酸铵作用脱除NO2>通过NO+N02→N203与NaOH作用脱除NOx>通过NO2与NaOH或H202作用脱除N02。
2、椰壳基活性炭(AC)及改性活性炭(MAC)、微孔分子筛(高硅H-和Na-ZSM-5分子筛、全硅β分子筛)上NO的常温氧化过程研究
(1)随着反应温度升高,干气条件下NO转化率降低,表现出类似气相均相反应的负活化能效应；在湿气条件下改性活性炭(MAC)和高硅ZSM-5分子筛上NO转化率先增后降,存在最佳反应温度,对于MAC为50～70℃,对高硅ZSM-5分子筛则为20℃,而全硅β分子筛上在10～90℃范围内,NO转化率呈单调下降的趋势；
(2)随着进口NO、02浓度以及空时的增加,NO转化率增加；
(3)水汽的存在对催化剂表面NO的氧化存在抑制作用；由于AC及MAC自身含有宽泛的孔径分布(特别是中孔孔道的存在),导致其对NO氧化的催化活性受水汽影响严重；而对于分子筛而言,提高Si/A1比可减少其对水汽的吸附从而降低水汽的影响,因此,湿气条件下微孔分子筛Si/Al比越高,NO转化率越高；
(4)干、湿气条件下催化剂稳定性实验结果表明,高硅ZSM-5、全硅β分子筛对NO的常温氧化催化活性没有下降,说明高硅ZSM-5、全硅β分子筛具有良好的稳定性,有望在工业上应用；
(5)微孔孔道是保证活性炭、分子筛等材料具有NO氧化催化活性的前提,微孔比表面积和微孔孔容越大,其对NO氧化催化活性越高；
(6)通过TPD/TPSR.原位DRIFTS技术对高硅Na-ZSM-5和全硅β分子筛上NO氧化机理研究表明,分子筛表面的羟基(-OH)和阳离子(如Na+)是NO氧化催化活性位；02在微孔分子筛表面不吸附,而NO在其表面存在强的化学吸附,NO2只存在弱吸附；在NO氧化反应气氛下,NO在Na+上的吸附态以N03(即：OONO)为主,而在羟基(-OH)上的吸附态可能以(NO)2(即：ONNO)为主,由此推测高硅Na-ZSM-5分子筛上存在如下的NO氧化反应机理：NO+σ??NO·σNO·σ+O2N03·6 NO3·σ+NO·σ.?N2O4+2σ?2NO2+2σ
而在全硅β分子筛上NO的氧化反应机理为：NO+σ?NO·σNO·σ+NO·σ?(NO·σ)2 (NO·σ)2+O2?2NO2+2σ?N2O4+2σ
以上研究表明,采用高硅ZSM-5分子筛或全硅β分子筛催化剂可实现在水汽环境中NO的高效气相氧化,提高NOx氧化度；而通过添加氧化剂或还原剂的NaOH溶液可强化碱液对NOx的化学吸收；两项技术的有机组合可有效提高碱液吸收法对NOx的脱除效率,说明本论文提出的气相催化氧化-碱液吸收法工艺和相关技术具有可行性。
The abatement of the nitric oxides (NOx) is becoming one of important challenges since NOx are the source of severe eco-environmental problems and harmful to human health. Differing from the NOx flue gas from the power station by burning fossil fuels such as coal, oil and natural gas, the NOx industrial waste gas exhausts with low quantity but high local NOx concentration leading to severe pollution to local environment, so is urgent to be treated now. Generally, the NOx industrial exhausted gas is discharged under the following conditions of:(1) high oxygen content (-20%(V)); (2) high vapor content which can reach the saturated one in the gas; (3) low NOx oxidation degree (defined as the ratio of the concentration of NO2 and that of NOx in the gas), even lower than 10%; (4) ambient temperature and normal pressure; (5) dramatical fluctuation of NOx concentration due to the batch or non-continuous operation mode of the previous production units. According to these features, the NH3-SCR (Selective Catalytic Reduction) method is not suitable to the removal of NOx from the industrial process since SCR process needs high temperature and excellent control of the addition of NH3 content, while alkaline solution absorption process operating at normal temperature and normal pressure may be more suitable because the absorption process is insensitive to the fluctuation of NOx content and even can recover nitrite and nitrate salts. However, the low NO solubility in aqueous solution could lead to low NOx removal efficiency for this wet scrubbing process. So the process of NO gas phase catalytic oxidation and alkaline solution absorption was proposed, and then investigated in detail in this paper. Some conclusions have been drawn as following:
1. Study on the absorption process of NOx by the alkaline solution including NaOH solution without and with the addition of the reductants or the oxidants
(1) The addition of the reductants (including urea, ammonium sulfite, sodium sulfite, sodium sulfide or sodium hyposulfite, etc.) or the oxidants (including hydrogen peroxide or sodium hypochlorite, etc.) promote the absorption of NOx, but the NOx removal efficiency is insensitive to the concentration of NaOH and the additives (including the reductants and the oxidants). With the increase of the inlet NOx concentration, the removal efficiency of NOx will increase. The increase of the gas phase resident time will make for the removal efficiency of NOx especially that of NO2.
(2) Among the operation conditions, the inlet NOx oxidation degree is the most significant one which effects the NOx removal, and exists the optimal value of 50～70%when using the NaOH solution or the urea-NaOH solution as the absorption solvents, but the higher inlet NOx oxidation degree will lead to the higher NOx removal efficiency when using the oxidant-NaOH solutions or the reductant-NaOH solutions (except urea additive). So, the key of the high NOx removal efficiency will result from the increase of the inlet NOx oxidation degree.
(3) The relative rate of NOx removal by the alkaline solution absorption process can be sorted as followed:the rate of NO2 removal through the reaction of NO2 and (NH4)2SO3> the rate of NOx removal through the reaction of NaOH and N2O3 equilibrated with NO and NO2> the rate of NO2 removal through the reaction of NO2 and NaOH or H2O2.
2. The study on the NO oxidation at ambient temperature by oxygen in the NOx waste gas on the catalysts including the coconut-based activated carbon (AC) and the modified activated carbon (MAC), the micro porous-based molecular sieve (high silica H-and Na-ZSM-5, pure silicaβ-ype molecular sieve)
(1) With the increase of the reaction temperature, the NO conversion in the NO catalytic oxidation decreases under the dry NOx waste gas, but exists maximum value under the humid NOx waste gas at the temperature of 50～70℃over MAC and 20°C over ZSM-5 molecular sieve, while decreases monotonously over pure silicaβ-type molecular sieve during the range of the reaction temperature from 10°C to 90°C.
(2) The increase of the inlet concentrations of NO and O2 and the space time benefits the NO conversion.
(3) The vapor inhibits the oxidation of NO on all the investigated catalysts, but the extent of inhibitory effect depends on the nature of the catalysts. The effect of vapor on the NO oxidation on the AC (MAC) may be the most serious one due to its wide pore size distribution, especially the exist of the mesopore. Nevertheless, there is another situation to the molecular sieve, that is, the high hydrophobic surface can be obtained on the molecular sieve with high Si/Al ratio, which leads to less adsorption to vapor. So, the higher NO conversion under the wet NOx gas will be obtained on the molecular sieve with the higher Si/Al ratio.
(4) The catalytic activity of the high silica ZSM-5 molecular sieve and the pure silicaβ-type molecular sieve demonstrates high stability both in the dry NOx gas and in the saturated wet NOx gas during the long periodic stability test, which means their potential industrial application in the NOx removal process.
(5) The micro porous channels guarantee the catalytic activity of ACs and the molecular sieves to NO oxidation at ambient temperature, and the high catalytic activity can be obtained over the catalysts with high micro porous specific superficial area and volume.
(6) The characterizations of TPD/TPSR and in-situ DRIFTS of the adsorbed NOx species on the high silica Na-ZSM-5 and the pure silicaβ-type molecular sieve reveal the reaction mechanisms of NO catalytic oxidation at ambient temperature. The molecular sieves exhibit the high catalytic activity through the active adsorption sites of the hydroxyl group (-OH) and cation (such as Na+). There is no adsorbing oxygen and only weakly-adsorbing NO2 can be detected on the surface of the molecular sieve, while NO can adsorb strongly on it. The adsorbing species of NO depends on the types of the active sites, e.g., the adsorbing NO3 (i.e., OONO) specie mainly exists in cation such as Na+, while the adsorbing (NO)2 (i.e., ONNO) specie may be in the hydroxyl group (-OH). Based on these, the catalytic reaction mechanism of NO oxidation at ambient temperature on the high silica Na-ZSM-5 molecular sieve can be speculated as following:
NO+σ?NO·σ
NO·σ+O2?NO3·σ
NO3·σ+NO·σ?N2O4+2σ?2NO2+2σWhile the reaction mechanism on the pure silicaβ-type molecular sieve may be shown as:
NO+σ?NO·σ
NO·σ?(NO·σ)2
(NO·σ)2+O2?2NO2+2σ?N2O4+2σ
All above investigations show that the NOx oxidation degree can efficiently be increased through the NO oxidation by O2 at the ambient temperature under the wet NOx waste gas using the high silica ZSM-5 or the pure silicaβ-type molecular sieve as the catalysts, and the chemical absorption of NOx can be enhanced by the addition of the reductant or the oxidant into the alkaline solution as the absorption solvent. Furthermore, the combination of the above two technologies synergically will lead to high NOx removal efficiency of the wet scrubbing process for NOx abatement, and the feasibility of the process of NO gas phase catalytic oxidation and alkaline solution absorption for the NOx removal from the industrial exhausted gas is then proved.
引文
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