等离子体及联合等离子体光解（CPP）技术降解挥发性有机废气
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摘要
DBD等离子体是一项相对成熟且可行的有机废气治理技术，用DBD降解挥发性有机气体(Volatile Organic Compounds，VOCs)的研究已非常多。然而，已有的研究都集中在静态或低流速动态(反应区流速＜0．1 m／s)条件下的降解，或与其它技术联合降解气态污染物，其研究结果很难直接用于指导工业废气的治理。本文采用DBD等离子体和联合等离子体光解(Combined Plasma Photolysis，CPP)两种技术研究高流速(反应区流速＞1m／s)条件下VOCs的降解，以期为VOCs的治理提供依据。
全文分两部分，第一部分研究了DBD等离子体技术降解“三苯”和乙酸异丁酯废气，考察了DBD降解流动态废气的影响因素，进行了串级和工程应用研究，推测了反应机理并进行了可行性分析，主要结论有：
(1)“三苯”的去除率随输入功率和外施电压的升高而升高，随气体流速和初始浓度的升高而下降。能率随初始浓度和外施电压的升高而升高，流速对能率的影响则比较复杂。对比相同条件下DBD降解“三苯”的效果，发现三者的去除率和能率比较接近。对混合“三苯”废气进行串级实验研究，结果显示：浓度为300～700mg／m~3的“三苯”混合废气，单级DBD降解时去除率达50％以上，三级串联时去除率达89％以上。费用核算表明，单级DBD降解时“三苯”废气处理费用为2～4元／1000m~3。最后指出，要实现DBD降解“三苯”废气工业化，首先要解决管壁结焦和出流气体中的气溶胶粒子问题。
(2)气体流速2．85m~3／h，外施电压9kV，初始浓度为1788mg／m~3的乙酸异丁酯气体，DBD降解时去除率达75．3％。外施电压升高、初始浓度和气体流速下降，乙酸异丁酯的去除率升高。能率随初始浓度升高而升高，最高值达32．9 g／(kW．h)。考察了DBD降解含乙酸异丁酯的工业废气，结果表明：废气流量2000m~3／h，DBD反应管中的气体流速5．4m／s，单个DBD电源输入电压16 kV时，乙酸异丁酯的去除率达80％以上，处理费用为12元／1000m~3。最后，对DBD降解乙酸异丁酯的产物进行了分析并初步探讨了其降解机理。
为进一步优化等离子体对废气的降解，第二部分开发了一项废气治理新技术—联合等离子体光解(CPP)，即用一个高压电源激发气体放电同时产生等离子体和准分子紫外光。研究了CPP降解废气的原理和特点，以VOCs(苯、苯乙烯和乙酸异丁酯)为目标物，考察了CPP对其降解的效果，分析了其影响因素，并对CPP发射的准分子光谱进行了初步分析，主要结论有：
(1)CPP中不宜填充Xe／I_2混合气体降解苯，因为其激发的XeI~*准分子(253nm)波长太长；ICPP(即内置式结构的CPP反应器)降解苯时，苯的去除率低。
采用OCPP(KrI~*／DBD)降解苯时，浓度为800mg／m~3，流量为35L／min的含苯废气9kV条件下降解，去除率比DBD降解时提高了15．9％。同时，OCPP降解苯时，苯的矿化度和CO_2的选择性都高于DBD。OCPP中填充的Kr／I_2压力、配比、石英介质材料对苯的去除率有一定影响。对OCPP产生的KrI~*发射光谱和降解苯的产物进行了分析。
研究还发现，准分子紫外光直接光解苯的效率低，推测准分子紫外光只是作为光电离剂，降低了气体击穿电压。OCPP优于DBD主要体现在六个方面：气体击穿电压降低、微放电数量的增加、·OH浓度增加、能量利用率提高、放电更均匀和降解产物对光的吸收作用。
(2)OCPP(KrI~*／DBD)降解模拟流动态苯乙烯气体，结果表明：Kr26．6 kPa，I_26mg，气体流速3．26 m~3／h，1265 mg／m~3的苯乙烯气体在外施电压9．0kV时去除率达84．4％，与DBD等离子体相比提高了20．6％，能率提高了5．7 g／(kW．h)。同时，研究了OCPP降解苯乙烯的影响因素，包括：填充的Kr和I_2的量、石英材质、气体流速、苯乙烯的初始浓度及反应器的结构形式。最后，采用红外光谱和气质联用分析了结焦产物，探讨了OCPP降解苯乙烯的机理。
(3)初始浓度为2500mg／m~3的乙酸异丁酯气体，气体流速为2．8 m~3／h，在OCPP(内充Kr 35．9 kPa，Br_21．2kPa)中降解，与DBD相比，9kV时，乙酸异丁酯的去除率提高了18．3％。填充的Kr／Br_2混合气体的总压和配比对OCPP降解污染物有一定影响，研究表明，Kr／Br_2配比为30-50之间比较适合污染物降解；在一定范围内总压升高有利于OCPP降解乙酸异丁酯；填充缓冲气体Ar有利于提高OCPP对乙酸异丁酯的去除率。OCPP激发Kr／Br_2主要辐射207nm(KrBr~*)，228nm(KrBr~*)和289nm(Br~*)三个波长的紫外光。207nm KrBr~*准分子光的强度随外施电压升高而升高，随填充气体总压的升高而升高。
Dielectric barrier discharge (DBD) plasma was a mature and feasible technologyfor organic waste gas treatment.Up to now,there have been many reports on DBDplasma used for treating volatile organic compounds (VOCs) as an alternativeapproach.However,their studies mainly based on pollutants destruction under staticstate or low-flow case (gas flow rate in reaction region＜0.1m/s) and on combinedplasma technology,as a result,their results were hard to be used for practical exhauststreatment directly.In this dissertation,we studied VOCs destruction with DBDplasma and combined plasma photolysis under high gas flow rate (gas flow rate inreaction region＞1m/s) in order to give some valuable proposals to commercialavailability.
This dissertation was mainly composed of two parts.In Part 1,the destruction of“three benzene”(benzene,toluene,xylene) and isobutyl acetate gas with DBDtechnology was studied and the influence factors were investigated.Moreover,weconducted experiment in DBD system in series and actual engineering applicationresearch and inferred reaction mechanisms as well as feasibility.The results mainlyincluded:
(1)The removal efficiency of“three benzene”increased with the increase of inputpower and applied voltage,and decreased with increasing gas flow rate and initialconcentration.The energy yield (Ey) increased with the increase of initialconcentration and applied voltage,while gas flow gas has a relatively complex effecton Ey.Moreover,we found that benzene,toluene and xylene have closed removalefficiency and energy yield with DBD destruction technology under the samecondition.We also carried out“scale-up”experiment on hybrid“three benzene”andthe experimental results showed that“three benzene”removal efficiency was morethan 50% in one DBD and over 89% in three DBD systems in series,when theirconcentrations were in the range of 300-700mg/m~3.Treatment cost assessment of perunit volume“three benzene”hybrid waste gas showed that only 2 to 4 yuan RMB wasneeded per 1000m~3 waste gases with DBD technology.At last,we pointed out that thefirst thing to consider was to remove solid residues in the wall of tube and aerosolparticles in effluent,before“three benzene”destruction with DBD were actuallyapplied.
(2)When gas flow rate was 2.58 m~3/h,removal efficiency of isobutyl acetate of 1788 mg/m~3 can reach 75.3% at 9 kV.The removal efficiency of isobutyl acetate increasedwith increasing applied voltage and decreasing initial concentration and gas flow rate.Ey increased with the increase of initial concentration and the highest Ey can reach32.9 g/(kW.h) according to our results.We also investigated the decomposition ofactual industrial waste gas containing isobutyl acetate in terms of three aspectsincluding the removal efficiency,treatment cost and feasibility.The results showedthat removal efficiency of isobutyl acetate was above 80% when applied voltage,gasflow rate,and flow rate in DBD reactor region were set at 16 kV,2000m~3/h,and5.4m/s,respectively.The treatment cost of isobutyl acetate was 12 yuanRMB/1000m~3.At last,the likely reaction mechanisms for the removal of isobutylacetate by DBD were suggested on the basis of byproducts analysis.
In order to optimize DBD plasma for waste gas removal,in part 2,a new-typereactor was designed and constructed,nominated combined plasma photolysis (CPP)that simultaneously produced plasma and excimer UV radiation with onehigh-pressure power supply.Destruction principle and characteristic of CPP for wastegas were discussed.In addition,we investigated degradation performance of CPP withVOCs (benzene,styrene and isobutyl acetate) as targets and analyzed influencefactors.Finally,we measured the excimer spectrum from CPP,and the results were asfollows:
(1)The elementary study showed that it was unsuitable for Xe/I_2 mixture as excimergas filled in CPP reactor,because wavelength of XeI~* excimer (253nm) was too long.When we utilized ICPP (inner combined plasma photolysis) reactor for benzeneremoval,removal efficiency of benzene was lower.
In OCPP (KrI~*/DBD),benzene removal efficiency increased by 15.9% in contrastto DBD,when applied voltage,gas flow rate,and initial concentration of benzenewere set at 9 kV,35 L/min,and 800 mg/m~3,respectively.In addition,themineralization degree and CO_2 selectivity in OCPP was higher than that in DBD.Theeffects of various operational parameters including total pressure,ratio of Kr/I_2,andquartz dielectric characteristics on OCPP performance were investigated.At last,theemission spectra of KrI~* excimer and byproducts analysis were suggested.
The experimental results also showed that benzene has low removal efficiencywhen decomposed only by excimer UV,which by inference only was a lightionization reagent for decreasing breakdown voltage of gas ionization.On the basis of above results,we concluded the reasons for OCPP superior to DBD from six aspects:the decrease of breakdown voltage,the increasing of microdischarge numbers,improvement of OH radical concentration,the enhancement of energy efficiency,more homogeneous discharge and benzene molecule absorption of UV light.
(2)Simulated flowing waste gas containing styrene was decomposed with OCPP(KrI~*/DBD) reactor.The results showed that styrene removal efficiency was up to84.4% in OCPP (Kr 26.6kPa,I_2 6 mg),and removal efficiency was increased by20.6%,Ey increased by 5.7 g/(kW.h) in contrast to DBD plasma,when appliedvoltage,gas flow rate,and initial concentration of styrene were set at 9 kV,3.26 m~3/h,and 1265 mg/m~3,respectively.Moreover,we investigated influence factors of styrenedecomposition including pressure of filled Kr and mass of I_2,quartz material,gas flowrate,initial concentration of styrene,as well as reactor configuration.At last,weanalyzed solid depositions on the internal wall of OCPP reactor by a FourierTransformation Infrared Spectrometer (FTIR) and a Gas Chromatography-MassSpectrometry (GC-MS),on the basis of which,the likely reaction mechanisms for theremoval of styrene by OCPP were discussed.
(3)In OCPP (Kr 35.9 kPa,Br_2 1.2kPa),isobutyl acetate removal efficiency increasedby 18.3% in contrast to DBD,when applied voltage,gas flow rate,and initialconcentration of isobutyl acetate were set at 9 kV,2.8 m~3/h,and 2500mg/m~3,respectively.The results showed that the total pressure and ratio of Kr/Br_2 mixturehave effect on isobutyl acetate destruction.When Kr/Br_2 was in the range of 30-50,good removal efficiency for isobutyl acetate was achieved.The increase of totalpressure and the adding of buffer gas Ar were in favor of isobutyl acetate destructionin OCPP to some extent.Three representative wavelengths at 207 nm (KrBr~*),228nm(KrBr~*) and 289nm (Br~*) were produced from Kr/Br_2 excited by OCPP.The excimerradiation intensity at 207nm was enhanced by the increase of applied voltage and totalpressure of Kr/Br_2 mixture.
全文分两部分，第一部分研究了DBD等离子体技术降解“三苯”和乙酸异丁酯废气，考察了DBD降解流动态废气的影响因素，进行了串级和工程应用研究，推测了反应机理并进行了可行性分析，主要结论有：
(1)“三苯”的去除率随输入功率和外施电压的升高而升高，随气体流速和初始浓度的升高而下降。能率随初始浓度和外施电压的升高而升高，流速对能率的影响则比较复杂。对比相同条件下DBD降解“三苯”的效果，发现三者的去除率和能率比较接近。对混合“三苯”废气进行串级实验研究，结果显示：浓度为300～700mg／m~3的“三苯”混合废气，单级DBD降解时去除率达50％以上，三级串联时去除率达89％以上。费用核算表明，单级DBD降解时“三苯”废气处理费用为2～4元／1000m~3。最后指出，要实现DBD降解“三苯”废气工业化，首先要解决管壁结焦和出流气体中的气溶胶粒子问题。
(2)气体流速2．85m~3／h，外施电压9kV，初始浓度为1788mg／m~3的乙酸异丁酯气体，DBD降解时去除率达75．3％。外施电压升高、初始浓度和气体流速下降，乙酸异丁酯的去除率升高。能率随初始浓度升高而升高，最高值达32．9 g／(kW．h)。考察了DBD降解含乙酸异丁酯的工业废气，结果表明：废气流量2000m~3／h，DBD反应管中的气体流速5．4m／s，单个DBD电源输入电压16 kV时，乙酸异丁酯的去除率达80％以上，处理费用为12元／1000m~3。最后，对DBD降解乙酸异丁酯的产物进行了分析并初步探讨了其降解机理。
为进一步优化等离子体对废气的降解，第二部分开发了一项废气治理新技术—联合等离子体光解(CPP)，即用一个高压电源激发气体放电同时产生等离子体和准分子紫外光。研究了CPP降解废气的原理和特点，以VOCs(苯、苯乙烯和乙酸异丁酯)为目标物，考察了CPP对其降解的效果，分析了其影响因素，并对CPP发射的准分子光谱进行了初步分析，主要结论有：
(1)CPP中不宜填充Xe／I_2混合气体降解苯，因为其激发的XeI~*准分子(253nm)波长太长；ICPP(即内置式结构的CPP反应器)降解苯时，苯的去除率低。
采用OCPP(KrI~*／DBD)降解苯时，浓度为800mg／m~3，流量为35L／min的含苯废气9kV条件下降解，去除率比DBD降解时提高了15．9％。同时，OCPP降解苯时，苯的矿化度和CO_2的选择性都高于DBD。OCPP中填充的Kr／I_2压力、配比、石英介质材料对苯的去除率有一定影响。对OCPP产生的KrI~*发射光谱和降解苯的产物进行了分析。
研究还发现，准分子紫外光直接光解苯的效率低，推测准分子紫外光只是作为光电离剂，降低了气体击穿电压。OCPP优于DBD主要体现在六个方面：气体击穿电压降低、微放电数量的增加、·OH浓度增加、能量利用率提高、放电更均匀和降解产物对光的吸收作用。
(2)OCPP(KrI~*／DBD)降解模拟流动态苯乙烯气体，结果表明：Kr26．6 kPa，I_26mg，气体流速3．26 m~3／h，1265 mg／m~3的苯乙烯气体在外施电压9．0kV时去除率达84．4％，与DBD等离子体相比提高了20．6％，能率提高了5．7 g／(kW．h)。同时，研究了OCPP降解苯乙烯的影响因素，包括：填充的Kr和I_2的量、石英材质、气体流速、苯乙烯的初始浓度及反应器的结构形式。最后，采用红外光谱和气质联用分析了结焦产物，探讨了OCPP降解苯乙烯的机理。
(3)初始浓度为2500mg／m~3的乙酸异丁酯气体，气体流速为2．8 m~3／h，在OCPP(内充Kr 35．9 kPa，Br_21．2kPa)中降解，与DBD相比，9kV时，乙酸异丁酯的去除率提高了18．3％。填充的Kr／Br_2混合气体的总压和配比对OCPP降解污染物有一定影响，研究表明，Kr／Br_2配比为30-50之间比较适合污染物降解；在一定范围内总压升高有利于OCPP降解乙酸异丁酯；填充缓冲气体Ar有利于提高OCPP对乙酸异丁酯的去除率。OCPP激发Kr／Br_2主要辐射207nm(KrBr~*)，228nm(KrBr~*)和289nm(Br~*)三个波长的紫外光。207nm KrBr~*准分子光的强度随外施电压升高而升高，随填充气体总压的升高而升高。
Dielectric barrier discharge (DBD) plasma was a mature and feasible technologyfor organic waste gas treatment.Up to now,there have been many reports on DBDplasma used for treating volatile organic compounds (VOCs) as an alternativeapproach.However,their studies mainly based on pollutants destruction under staticstate or low-flow case (gas flow rate in reaction region＜0.1m/s) and on combinedplasma technology,as a result,their results were hard to be used for practical exhauststreatment directly.In this dissertation,we studied VOCs destruction with DBDplasma and combined plasma photolysis under high gas flow rate (gas flow rate inreaction region＞1m/s) in order to give some valuable proposals to commercialavailability.
This dissertation was mainly composed of two parts.In Part 1,the destruction of“three benzene”(benzene,toluene,xylene) and isobutyl acetate gas with DBDtechnology was studied and the influence factors were investigated.Moreover,weconducted experiment in DBD system in series and actual engineering applicationresearch and inferred reaction mechanisms as well as feasibility.The results mainlyincluded:
(1)The removal efficiency of“three benzene”increased with the increase of inputpower and applied voltage,and decreased with increasing gas flow rate and initialconcentration.The energy yield (Ey) increased with the increase of initialconcentration and applied voltage,while gas flow gas has a relatively complex effecton Ey.Moreover,we found that benzene,toluene and xylene have closed removalefficiency and energy yield with DBD destruction technology under the samecondition.We also carried out“scale-up”experiment on hybrid“three benzene”andthe experimental results showed that“three benzene”removal efficiency was morethan 50% in one DBD and over 89% in three DBD systems in series,when theirconcentrations were in the range of 300-700mg/m~3.Treatment cost assessment of perunit volume“three benzene”hybrid waste gas showed that only 2 to 4 yuan RMB wasneeded per 1000m~3 waste gases with DBD technology.At last,we pointed out that thefirst thing to consider was to remove solid residues in the wall of tube and aerosolparticles in effluent,before“three benzene”destruction with DBD were actuallyapplied.
(2)When gas flow rate was 2.58 m~3/h,removal efficiency of isobutyl acetate of 1788 mg/m~3 can reach 75.3% at 9 kV.The removal efficiency of isobutyl acetate increasedwith increasing applied voltage and decreasing initial concentration and gas flow rate.Ey increased with the increase of initial concentration and the highest Ey can reach32.9 g/(kW.h) according to our results.We also investigated the decomposition ofactual industrial waste gas containing isobutyl acetate in terms of three aspectsincluding the removal efficiency,treatment cost and feasibility.The results showedthat removal efficiency of isobutyl acetate was above 80% when applied voltage,gasflow rate,and flow rate in DBD reactor region were set at 16 kV,2000m~3/h,and5.4m/s,respectively.The treatment cost of isobutyl acetate was 12 yuanRMB/1000m~3.At last,the likely reaction mechanisms for the removal of isobutylacetate by DBD were suggested on the basis of byproducts analysis.
In order to optimize DBD plasma for waste gas removal,in part 2,a new-typereactor was designed and constructed,nominated combined plasma photolysis (CPP)that simultaneously produced plasma and excimer UV radiation with onehigh-pressure power supply.Destruction principle and characteristic of CPP for wastegas were discussed.In addition,we investigated degradation performance of CPP withVOCs (benzene,styrene and isobutyl acetate) as targets and analyzed influencefactors.Finally,we measured the excimer spectrum from CPP,and the results were asfollows:
(1)The elementary study showed that it was unsuitable for Xe/I_2 mixture as excimergas filled in CPP reactor,because wavelength of XeI~* excimer (253nm) was too long.When we utilized ICPP (inner combined plasma photolysis) reactor for benzeneremoval,removal efficiency of benzene was lower.
In OCPP (KrI~*/DBD),benzene removal efficiency increased by 15.9% in contrastto DBD,when applied voltage,gas flow rate,and initial concentration of benzenewere set at 9 kV,35 L/min,and 800 mg/m~3,respectively.In addition,themineralization degree and CO_2 selectivity in OCPP was higher than that in DBD.Theeffects of various operational parameters including total pressure,ratio of Kr/I_2,andquartz dielectric characteristics on OCPP performance were investigated.At last,theemission spectra of KrI~* excimer and byproducts analysis were suggested.
The experimental results also showed that benzene has low removal efficiencywhen decomposed only by excimer UV,which by inference only was a lightionization reagent for decreasing breakdown voltage of gas ionization.On the basis of above results,we concluded the reasons for OCPP superior to DBD from six aspects:the decrease of breakdown voltage,the increasing of microdischarge numbers,improvement of OH radical concentration,the enhancement of energy efficiency,more homogeneous discharge and benzene molecule absorption of UV light.
(2)Simulated flowing waste gas containing styrene was decomposed with OCPP(KrI~*/DBD) reactor.The results showed that styrene removal efficiency was up to84.4% in OCPP (Kr 26.6kPa,I_2 6 mg),and removal efficiency was increased by20.6%,Ey increased by 5.7 g/(kW.h) in contrast to DBD plasma,when appliedvoltage,gas flow rate,and initial concentration of styrene were set at 9 kV,3.26 m~3/h,and 1265 mg/m~3,respectively.Moreover,we investigated influence factors of styrenedecomposition including pressure of filled Kr and mass of I_2,quartz material,gas flowrate,initial concentration of styrene,as well as reactor configuration.At last,weanalyzed solid depositions on the internal wall of OCPP reactor by a FourierTransformation Infrared Spectrometer (FTIR) and a Gas Chromatography-MassSpectrometry (GC-MS),on the basis of which,the likely reaction mechanisms for theremoval of styrene by OCPP were discussed.
(3)In OCPP (Kr 35.9 kPa,Br_2 1.2kPa),isobutyl acetate removal efficiency increasedby 18.3% in contrast to DBD,when applied voltage,gas flow rate,and initialconcentration of isobutyl acetate were set at 9 kV,2.8 m~3/h,and 2500mg/m~3,respectively.The results showed that the total pressure and ratio of Kr/Br_2 mixturehave effect on isobutyl acetate destruction.When Kr/Br_2 was in the range of 30-50,good removal efficiency for isobutyl acetate was achieved.The increase of totalpressure and the adding of buffer gas Ar were in favor of isobutyl acetate destructionin OCPP to some extent.Three representative wavelengths at 207 nm (KrBr~*),228nm(KrBr~*) and 289nm (Br~*) were produced from Kr/Br_2 excited by OCPP.The excimerradiation intensity at 207nm was enhanced by the increase of applied voltage and totalpressure of Kr/Br_2 mixture.
引文
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