臭氧结合钙基吸收多种污染物及副产物提纯的试验与机理研究
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摘要
随着我国环境保护要求与标准的不断提升,火电行业及其大气污染控制倍受关注。臭氧多脱技术能够有效的进行多种污染物的协同脱除,对缓解日益恶化的环境问题有着重要意义。本文对臭氧实现多种污染物协同脱除的相关问题进行了试验与机理研究。其中主要包括：NO氧化产物与SO2的吸收、副产物处理、等离子体耦合催化剂对NO的氧化以及臭氧氧化多种污染物协同脱除中试试验。
在实现了NO的高效氧化后,主要氧化产物NO2与S02的协同吸收成为整个多脱系统的重要环节。本文从热力学和动力学的角度进行了协同吸收的反应机理与吸收特性的模拟,试验验结果与模拟结果相吻合。当吸收的气体体积与浆液体积的比值M=2870时为临界状态,超过临界后pH值会迅速下降。这表明此时为吸收液完全消耗的临界状态。同时根据传质速率的计算,亚硫酸钠溶液受pH值影响强烈,而亚硫酸钙几乎不受其影响。
分别采用三种吸收剂Na2SO3、Ca(OH)2和CaSO3进行吸收对比,对pH值、烟气组分、液气比等影响因素及液相的吸收产物进行了分析。结果表明,NO2吸收效率随S(IV)离子浓度的增加而提高,同时液相吸收的主要产物为NO2-。当pH<7时,Na2S03对NO2的吸收变差。随着pH值低于5.7,CaSO3表现出比Na2SO3更好的效果。SO2在碱性环境中有利于NO2的吸收,酸性环境中有微弱的抑制作用。氧气量对于NO2的吸收有负面影响,使吸收效率降低10%左右。随着N02-浓度的提高,NO2的吸收也受到限制。液气比的增加能提高NO2的吸收效率。
采用多种添加剂辅助CaS03浆液协同吸收NO2与SO2,同时对吸收产物进行分离提纯亚硝酸钙产品。添加铁、锰、铵等无机盐都能够提高CaSO3浆液对NO2的吸收。FeSO4效果最佳,NO2的吸收效率达到95%,然而由于Fe(Ⅱ)向Fe(Ⅲ)的转化,其损失率也最大。硫酸铵也具有较强的辅助吸收能力同时损失最小。它的吸收效果随着温度的升高而增强,也随pH值的降低而减弱。氧气的存在仍会使NO2的吸收效率下降4%。
采用复盐复分解法进行液相吸收产物Ca(NO2)2的提纯,对影响提纯的因素进行优化。结果表明,加热反应时间30min,反应温度90℃,OR=12(pH5.5)时,提纯达到最优化条件。最后提出了臭氧氧化多种污染物结合钙基吸收以及副产物处理的方案。
应用非热等离子体结合催化剂实现低能耗、低温下NO的氧化。DBD产生的活性分子O、O3、O2*、OH、H2O2、HO2等能够强化NO的氧化。放电电压5kV下,NO的主要氧化产物为NO2。以钻为活性组分,二氧化钛为载体,采用溶胶凝胶法制备钴钛催化剂与非热等离子体结合具有很好的NO氧化性能。分析表明,焙烧温度400℃下,钴负载量达到7.5%时,钴钛催化剂Co(0.75)Ti的催化活性最好。此时钴在催化剂表面分散度高,能够很好地吸附气相活性分子。在4.6kV的放电电压下催化氧化NO,能够在120～210％的反应温度内取得90%以上的氧化效率。放电产生的活性分子吸附于催化剂表面的氧缺位上,NO分子在催化剂表面以弱吸附或碰撞的形式与活性分子发生反应,形成稳定的中间体。随着键长的进一步缩短,生成的NO2分子扩散到气相,实现催化氧化过程。
本文还对臭氧氧化结合钙基吸收多种污染物协同脱除技术进行了中试试验。提出了三种氧气来源的技术方案：空气源、液氧供氧和空分供氧,并进行了对比。中试试验采用操作简单的空气源方案进行。采用Fluent的EDC模型模拟臭氧喷射方式。结果表明三叉式喷嘴的设计能够实现臭氧与烟气的均匀混合。同时大管道内的气相混合反应中,由于气相混合的停留时间大于化学反应时间,因此混合停留时间的长短决定了化学反应是否达到反应平衡,模拟得出O3与NO反应的临界平衡时间为0.45s。
试验工况是采用03结合钙基吸收剂对NOx、SO2、Hg以及VOCs进行协同氧化降解。采用混合吸收浆液协同吸收时脱硝效率超过86%,脱硫为99%。NOx的液相吸收产物为NO2-离子。电厂原烟气经SCR、静电除尘后Hg浓度较低,氧化效率非常明显达到99%以上。二噁英在高浓度的03作用下降解率达到94%左右。PM2.5经过喷淋塔吸收后,尘粒总浓度大量减少。同时,还对臭氧多脱技术成本进行了预估和对比。
With developing requirements and standards of environmental protection, thermal power industry and its atmospheric pollution control has been paid more and more attention. Ozone oxidation technology has effective on the removal of multi-polutions, which is of significance to alleviate the growing environmental problems. Experiment and mechanism of correlative problems based on simultaneous removal of multi-polutions by ozone were studied. It mainly includes the absorption of NO oxidation product and SO2, by-product treatment, catlytic oxidation of NO by NTP-cataltsis and a pilot test for multi-polutions control by ozone.
It is an important part of the system to absorb the main oxidation product of NO2and SO2simultaneously after NO being oxidized high effectively. The reaction mechanism and the absorption properties of synergistic absorption were simulated from the point of view of thermodynamic and kinetic. The experimental results validate the simulation very well. The critical state is M=2870, which is the ratio of the gas volume absorbed and liquid volume. The value of pH decreases rapidly exceeding this point. It also shows that absorbent is comsumed completely. According to the calculation of mass transfer rate, the sodium sulfite solution is badly influenced by pH value, but not calcium sulfite.
Three kinds of absorbents Na2SO3, Ca(OH)2and CaSO3were compared. Effects of different pH, flue gas components, liquid-gas ratio et al. and liquid absorbent product were investigated. Results indicate that NO2absorption efficiency was increasing with S(IV), and NO2-is the main component of liquid. NO2absorption is adverse in Na2SO3solution below pH7. When pH is less than5.7, CaSO3is more efficiency than Na2SO3. The initial concentration of SO2has weak inhibition effects on NO2absorption in acidic environment, whereas NO2absorption efficiency can be enhanced by adding SO2in alkali condition. O2is so unfavorable as to drop about10%NO2absorption efficiency. It is adverse for NO2absorption with increasing the concentration of NO2as well. NO2absorption efficiency is increasing with liquid-gas ratio.
NO2and SO2were simultaneously absorbed by CaSO3with several additives, and calcium nitrite was purified by separation of absorption products. The additives can enhance the absorption of NO2in CaSO3slurry, including Fe, Mn, ammonium salts et al.. FeSO4is the most effective additive with absorption efficiency reaching95%, but the loss of additive is the highest due to the oxidation of Fe(Ⅱ) into Fe(Ⅲ).(NH4)2SO4also has better absorption capacity and the loss is lowest. Its absorption efficiency improves with increasing temperature and decreases with decreasing pH. The presence of O2causes a4%decrease in NO2absorption.
Calcium nitrite was purified by double decomposition of double salt. At the same time, the influencing factors were optimized on purify process. Experimental results indicate that reaction time30min, temperature90℃and OR=12(pH5.5) are the optimal parameters for the recovery of nitrite. Finaly, a scheme of simultaneous removal of NOx and SO2by ozone with help of calcium-absorption and by-product recovery system was proposed.
Oxidation of NO in the condition of low energy consumption and low temperature was achieved by non-thermal plasma combined with catalyst. It can be enhanced by active molecule from DBD reactor, including O, O3, O2*, OH, H2O2, HO2et al.. NO2is the main oxidation product of NO below5kV discharge voltage. The catalyst was prepared by sol-gel method, using cobalt as the active component and titanium dioxide as the carrier. Combined NTP with catalyst has well on the oxidation performance of NO. The results show that Co(0.75)Ti catalyst has the best catalytic activity, which was prepared at the calcination temperature400℃and7.5%cobalt loading. Since the cobalt has high dispersion in the catalyst surface, the gas active molecules can be adsorbed. Catalytic oxidation efficiency of NO is more than90%at the temperature range of120～210℃and4.6kV discharge voltage. Active molecules by DBD adsorb on the oxygen vacancies of catalyst surface. NO molecule reacts with active molecules to product a stable intermediate through weak adsorption on the catalyst surface or collision with active molecules. With further shortening the bond length, NO2diffuses to gas and the catalytic oxidation process is achieved.
Simultaneously removal of multi-polutions by ozone with calcium based absorbent has been studied in the pilot test. Three technical programs of oxygen source including air source, liquid oxygen and air separation were proposed and compared. The air source program was used for easily operation in the pilot. Ozone injection was simulated using EDC model based on Fluent. The results show that the trigeminal nozzle was designed to achieve uniform mixing of ozone and flue gas. Since residence time of mixed gas is greater than the chemical reaction time, it is determined by residence time whether the chemical reaction reaches the reaction equilibrium or not when mixed gas reacts in the large pipe. The critical time is0.45s by simulation of O3and NO reaction.
Synergistic removal of NOx, SO2, Hg, and VOCs by O3with calcium-based sorbent was discussed in the test conditions. Using the mixing slurry as the absorbent, the removal efficiency of NOx and SO2is86%and99%respectively. NO2-is the main component of liquid for NOx absorption. Hg concentration is lower after the flue gas through the SCR and electric dust precipitation, and the oxidation efficiency is greatly more than99%. Removal of dioxin is about94%due to the high ozone concentration. For PM2.5, dust concentration is significantly reduced at the outlet of washing tower. Moreover, investment and operation cost of ozone oxidation technology were estimated and compared with others.
在实现了NO的高效氧化后,主要氧化产物NO2与S02的协同吸收成为整个多脱系统的重要环节。本文从热力学和动力学的角度进行了协同吸收的反应机理与吸收特性的模拟,试验验结果与模拟结果相吻合。当吸收的气体体积与浆液体积的比值M=2870时为临界状态,超过临界后pH值会迅速下降。这表明此时为吸收液完全消耗的临界状态。同时根据传质速率的计算,亚硫酸钠溶液受pH值影响强烈,而亚硫酸钙几乎不受其影响。
分别采用三种吸收剂Na2SO3、Ca(OH)2和CaSO3进行吸收对比,对pH值、烟气组分、液气比等影响因素及液相的吸收产物进行了分析。结果表明,NO2吸收效率随S(IV)离子浓度的增加而提高,同时液相吸收的主要产物为NO2-。当pH<7时,Na2S03对NO2的吸收变差。随着pH值低于5.7,CaSO3表现出比Na2SO3更好的效果。SO2在碱性环境中有利于NO2的吸收,酸性环境中有微弱的抑制作用。氧气量对于NO2的吸收有负面影响,使吸收效率降低10%左右。随着N02-浓度的提高,NO2的吸收也受到限制。液气比的增加能提高NO2的吸收效率。
采用多种添加剂辅助CaS03浆液协同吸收NO2与SO2,同时对吸收产物进行分离提纯亚硝酸钙产品。添加铁、锰、铵等无机盐都能够提高CaSO3浆液对NO2的吸收。FeSO4效果最佳,NO2的吸收效率达到95%,然而由于Fe(Ⅱ)向Fe(Ⅲ)的转化,其损失率也最大。硫酸铵也具有较强的辅助吸收能力同时损失最小。它的吸收效果随着温度的升高而增强,也随pH值的降低而减弱。氧气的存在仍会使NO2的吸收效率下降4%。
采用复盐复分解法进行液相吸收产物Ca(NO2)2的提纯,对影响提纯的因素进行优化。结果表明,加热反应时间30min,反应温度90℃,OR=12(pH5.5)时,提纯达到最优化条件。最后提出了臭氧氧化多种污染物结合钙基吸收以及副产物处理的方案。
应用非热等离子体结合催化剂实现低能耗、低温下NO的氧化。DBD产生的活性分子O、O3、O2*、OH、H2O2、HO2等能够强化NO的氧化。放电电压5kV下,NO的主要氧化产物为NO2。以钻为活性组分,二氧化钛为载体,采用溶胶凝胶法制备钴钛催化剂与非热等离子体结合具有很好的NO氧化性能。分析表明,焙烧温度400℃下,钴负载量达到7.5%时,钴钛催化剂Co(0.75)Ti的催化活性最好。此时钴在催化剂表面分散度高,能够很好地吸附气相活性分子。在4.6kV的放电电压下催化氧化NO,能够在120～210％的反应温度内取得90%以上的氧化效率。放电产生的活性分子吸附于催化剂表面的氧缺位上,NO分子在催化剂表面以弱吸附或碰撞的形式与活性分子发生反应,形成稳定的中间体。随着键长的进一步缩短,生成的NO2分子扩散到气相,实现催化氧化过程。
本文还对臭氧氧化结合钙基吸收多种污染物协同脱除技术进行了中试试验。提出了三种氧气来源的技术方案：空气源、液氧供氧和空分供氧,并进行了对比。中试试验采用操作简单的空气源方案进行。采用Fluent的EDC模型模拟臭氧喷射方式。结果表明三叉式喷嘴的设计能够实现臭氧与烟气的均匀混合。同时大管道内的气相混合反应中,由于气相混合的停留时间大于化学反应时间,因此混合停留时间的长短决定了化学反应是否达到反应平衡,模拟得出O3与NO反应的临界平衡时间为0.45s。
试验工况是采用03结合钙基吸收剂对NOx、SO2、Hg以及VOCs进行协同氧化降解。采用混合吸收浆液协同吸收时脱硝效率超过86%,脱硫为99%。NOx的液相吸收产物为NO2-离子。电厂原烟气经SCR、静电除尘后Hg浓度较低,氧化效率非常明显达到99%以上。二噁英在高浓度的03作用下降解率达到94%左右。PM2.5经过喷淋塔吸收后,尘粒总浓度大量减少。同时,还对臭氧多脱技术成本进行了预估和对比。
With developing requirements and standards of environmental protection, thermal power industry and its atmospheric pollution control has been paid more and more attention. Ozone oxidation technology has effective on the removal of multi-polutions, which is of significance to alleviate the growing environmental problems. Experiment and mechanism of correlative problems based on simultaneous removal of multi-polutions by ozone were studied. It mainly includes the absorption of NO oxidation product and SO2, by-product treatment, catlytic oxidation of NO by NTP-cataltsis and a pilot test for multi-polutions control by ozone.
It is an important part of the system to absorb the main oxidation product of NO2and SO2simultaneously after NO being oxidized high effectively. The reaction mechanism and the absorption properties of synergistic absorption were simulated from the point of view of thermodynamic and kinetic. The experimental results validate the simulation very well. The critical state is M=2870, which is the ratio of the gas volume absorbed and liquid volume. The value of pH decreases rapidly exceeding this point. It also shows that absorbent is comsumed completely. According to the calculation of mass transfer rate, the sodium sulfite solution is badly influenced by pH value, but not calcium sulfite.
Three kinds of absorbents Na2SO3, Ca(OH)2and CaSO3were compared. Effects of different pH, flue gas components, liquid-gas ratio et al. and liquid absorbent product were investigated. Results indicate that NO2absorption efficiency was increasing with S(IV), and NO2-is the main component of liquid. NO2absorption is adverse in Na2SO3solution below pH7. When pH is less than5.7, CaSO3is more efficiency than Na2SO3. The initial concentration of SO2has weak inhibition effects on NO2absorption in acidic environment, whereas NO2absorption efficiency can be enhanced by adding SO2in alkali condition. O2is so unfavorable as to drop about10%NO2absorption efficiency. It is adverse for NO2absorption with increasing the concentration of NO2as well. NO2absorption efficiency is increasing with liquid-gas ratio.
NO2and SO2were simultaneously absorbed by CaSO3with several additives, and calcium nitrite was purified by separation of absorption products. The additives can enhance the absorption of NO2in CaSO3slurry, including Fe, Mn, ammonium salts et al.. FeSO4is the most effective additive with absorption efficiency reaching95%, but the loss of additive is the highest due to the oxidation of Fe(Ⅱ) into Fe(Ⅲ).(NH4)2SO4also has better absorption capacity and the loss is lowest. Its absorption efficiency improves with increasing temperature and decreases with decreasing pH. The presence of O2causes a4%decrease in NO2absorption.
Calcium nitrite was purified by double decomposition of double salt. At the same time, the influencing factors were optimized on purify process. Experimental results indicate that reaction time30min, temperature90℃and OR=12(pH5.5) are the optimal parameters for the recovery of nitrite. Finaly, a scheme of simultaneous removal of NOx and SO2by ozone with help of calcium-absorption and by-product recovery system was proposed.
Oxidation of NO in the condition of low energy consumption and low temperature was achieved by non-thermal plasma combined with catalyst. It can be enhanced by active molecule from DBD reactor, including O, O3, O2*, OH, H2O2, HO2et al.. NO2is the main oxidation product of NO below5kV discharge voltage. The catalyst was prepared by sol-gel method, using cobalt as the active component and titanium dioxide as the carrier. Combined NTP with catalyst has well on the oxidation performance of NO. The results show that Co(0.75)Ti catalyst has the best catalytic activity, which was prepared at the calcination temperature400℃and7.5%cobalt loading. Since the cobalt has high dispersion in the catalyst surface, the gas active molecules can be adsorbed. Catalytic oxidation efficiency of NO is more than90%at the temperature range of120～210℃and4.6kV discharge voltage. Active molecules by DBD adsorb on the oxygen vacancies of catalyst surface. NO molecule reacts with active molecules to product a stable intermediate through weak adsorption on the catalyst surface or collision with active molecules. With further shortening the bond length, NO2diffuses to gas and the catalytic oxidation process is achieved.
Simultaneously removal of multi-polutions by ozone with calcium based absorbent has been studied in the pilot test. Three technical programs of oxygen source including air source, liquid oxygen and air separation were proposed and compared. The air source program was used for easily operation in the pilot. Ozone injection was simulated using EDC model based on Fluent. The results show that the trigeminal nozzle was designed to achieve uniform mixing of ozone and flue gas. Since residence time of mixed gas is greater than the chemical reaction time, it is determined by residence time whether the chemical reaction reaches the reaction equilibrium or not when mixed gas reacts in the large pipe. The critical time is0.45s by simulation of O3and NO reaction.
Synergistic removal of NOx, SO2, Hg, and VOCs by O3with calcium-based sorbent was discussed in the test conditions. Using the mixing slurry as the absorbent, the removal efficiency of NOx and SO2is86%and99%respectively. NO2-is the main component of liquid for NOx absorption. Hg concentration is lower after the flue gas through the SCR and electric dust precipitation, and the oxidation efficiency is greatly more than99%. Removal of dioxin is about94%due to the high ozone concentration. For PM2.5, dust concentration is significantly reduced at the outlet of washing tower. Moreover, investment and operation cost of ozone oxidation technology were estimated and compared with others.
引文
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