超高盐榨菜废水微电解—电解预处理工艺研究
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摘要
超高盐榨菜废水具有高盐度、低pH、高有机物和高氮磷的特点，以及存在氮杂环类等难降解有机污染物。目前，榨菜废水主要采用生物法处理，但废水的高盐度和盐度波动，影响生物处理系统的稳定性。因此，考虑通过物化预处理方法，降低盐度、提高pH、去除难降解有机物，利于后续生物处理。开展超高盐榨菜废水物化预处理工艺研究，考察微电解、二维电解和三维电极法物化预处理单元的可行性，进行工艺优化和机理研究，研究“三级微电解-二维电解”物化预处理组合工艺处理效能，进行“三级微电解-生物”物化-生物组合工艺试验研究。
微电解单因素试验得出，在原水pH、铁水体积比1:1、铁炭体积比1:1和反应时间30min时，去除效果较佳，COD、氨氮、磷酸盐和TN去除率分别为36%-45%、34%-42%、97%-99.9%和34%-53%，盐度去除率为22%-25%，出水pH升高1-2；多级微电解串联试验表明，串联级数为3时去除效果提高显著；正交试验表明，各因子对COD和氨氮去除率影响顺序为：铁水体积比＞初始pH＞反应时间＞铁炭体积比。填料扫描电镜和能谱分析发现，反应后铁炭表面被沉淀物覆盖，自来水冲洗后，沉淀物减少，填料恢复活性；反应后铁炭表面出现Na、P和Cl；沉淀产物XRD结果表明，磷酸盐是以Fe3(PO4)2沉淀形式被去除。
微电解机理研究表明，在原电池反应、氧化还原、电附集、铁离子絮凝沉淀和氢气气浮等共同作用下，有机污染物被降解转化或去除。GC-MS结果表明，原水中有机污染物大部分含有苯环，其中氮杂环化合物5种，氮硫杂环化合物1种，酚类3种，均为难降解污染物，预处理出水有机物种类去除率53.8%，其中氮杂环化合物种类去除率80%。有机物相对分子量结果表明，微电解可使大分子有机物转化为小分子有机物，并去除部分小分子有机物。因此，微电解法对超高盐榨菜废水中的难降解有机物具有良好的去除效果。
二维电解单因素试验表明，在原水pH、电流密度156mA/cm2、极板间距1.5cm、极水比0.8dm2/L、电解时间120min时，去除效果较佳，COD、氨氮和磷酸盐去除率分别为55.74%、99.77%和88.71%，pH由5.07升高为9.54，盐度由7.02%下降为6.39%；通过电流密度对氨氮和COD能耗和阳极效果的影响分析，得出氨氮可以采用前期高电流密度，后期低电流密度的运行模式电解，在电流密度156mA/cm2，电解30min时，氨氮能耗最低96kW·h/Kg，阳极效率最高8.47g/h·m2·A；电流密度为156mA/cm2时，COD能耗最低和阳极效率最高。三维电极单因素试验表明，在原水pH、废水600mL、电流8A、活性炭填充量250g、极板间距6.5cm、电解时间150min时，处理效果较佳，COD、TN和磷酸盐去除率分别为76.47%、89.48%和97.81%；电流为8A时，COD能耗较低和阳极效率较高。
电解机理研究表明有机污染物是在直接氧化和间接氧化共同作用下降解的。通过电解过程中过氧化氢和游离氯检测发现，榨菜废水中过氧化氢和游离氯浓度明显低于氯化钠溶液，表明有机物降解过程中消耗了大量过氧化氢和游离氯，与间接氧化过程有关。GC-MS结果表明，电解出水污染物出峰位置与原水的相比有所变化，多环有机物全部转化为单环或直链结构有机物，说明在电解过程中，难降解有机物被降解转变为易降解中间产物。有机物相对分子量分布表明，二维电解也可使大分子有机物转化为小分子有机物，同时去除部分小分子有机物。三维电极UV-Vis分析认为部分有机物可能被直接氧化为二氧化碳。因此，电解法可转化去除废水中难降解有机污染物。
在微电解、二维电解和三维电极法三种物化预处理小试试验基础上，进一步开展“三级微电解-二维电解”物化预处理组合工艺小试和中试研究，中试出水COD、氨氮、TN和磷酸盐去除率分别为79.41%、86.08%、81.71%和99.65%，pH由4.37升高为6.87，盐度由6.53%下降为2.09%。可知，该组合工艺出水盐度下降，pH升高，COD和氮磷浓度降低，适宜采用生物法处理。
由物化-生物组合工艺试验可知，三级微电解预处理对后续厌氧、好氧和厌氧-好氧生物组合处理有利。“三级微电解-厌氧生物膜-接触氧化”组合工艺出水COD浓度为230-420mg/L，达到《污水综合排放标准》（GB8978-1996）三级排放标准，具有良好的应用前景。
The characteristic of the ultrahigh-salt tuber mustard wastewater were ultra-highsalt, low pH, high organic matter, high nitrogen and phosphorus and the heterocyclerefractory organic pollutants. At present, the tuber mustard wastewater was mainlytreated by biological process, but ultrahigh-salt and salinity fluctuation would affect thebiological treatment systemstability. Therefore, it is considered to meet the subsequentbiological treatment requirements through the the physicochemical pretreatment toreduce salinity, increase the pH, removal of refractory organics. Physicochemicaltreatments of ultrahigh-salt tuber mustard wastewater were researched, includingmicro-electrolysis, two-dimensional electrolysis and three-dimensional electrolysis. Thetreatment efficiency of “three micro-electrolysis-two-dimensional electrolysis” and“three micro-electrolysis-biochemical process’ were studied.
The micro-electrolysis experiments found that under the condition of raw water pH,Fe/C volume ratio of1:1, Fe/H2O volume ratio of1:1and reaction time of30min,removals of COD, ammonia, phosphate, TN and salinity were36%-45%,34%-42%,97%-99.9%,34%-53%and22%-25%, meanwhile, the effluent pH increased1-2. Theseries of multi-level micro-electrolysis experiments showed that the removal efficiencyincreased significantly at the level of three. The orthogonal tests showed that each factoron the order of COD and ammonia removal rates were as follow: Fe/H2O volume ratio＞initial pH＞reaction time＞Fe/C volume ratio. The SEM analysis showed that thesurface of iron and carbon after reaction were covered by lots of sediment, after waterbackwash, the sediment decreased, the activity of iron and carbon recovered. The SEManalysis showed that the surface of iron and carbon after reaction increased Na, P and Cl.The XRD result of precipitation product indicated that phosphate was removed byFe3(PO4)2.
The mechanism of micro-electrolysis had shown that organic pollutants weredegraded by the combined effects of chemical battery reaction, oxidation-reduction,filtration-adsorption, flocculation-precipitation and air floatation. The GC-MS resultsshowed that the organic pollutants of raw wastewater containing benzene ring werebiodegradable pollutants, including five kinds of heterocyclic compounds, one kind ofnitrogen and sulfur heterocyclic compounds, three kinds of phenols. The removal rate oforganic matter was53.8%by micro-electrolysis pretreatment, with heterocyclic compounds removal efficiency of80%. The organic molecular weight distributionexplained that the micro-electrolysis could convert macromolecular organics into smallorganic molecules, with the removal of some small organic molecules. Refractoryorganics in ultrahigh-salt tuber mustard wastewater were effectively removed bymicro-electrolysis.
The two-dimensional electrolysis experiments found that under the optimalconditions of raw water pH, current density of156mA/cm2, electrode distance of1.5cm and electrode plate area/water volume ratio of0.8dm2/L, removals of COD,ammonia and phosphate were55.74%,99.77%and88.71%within120min. In addition,pH increased from5.07to9.54, the salinity decreased from7.02%to6.39%. Theanalysis of the current density on energy consumption and anode efficiency indicatedthat ammonia can use the electrolysis mode of pre-high and late-low current density.Under current density of156mA/cm2and electrolysis of30min, the ammonia energyconsumption was lowest96kW·h/Kg, the ammonia anode efficiency was highest8.47g/h·m2·A. Under current density156mA/cm2, the COD energy consumption was thelowest and the COD anode efficiency was the highest. The three-dimensionalelectrolysis tests found that under the condition of wastewater volume of600mL, rawwater pH, electrolysis current of8A, amount of activated carbon filling quantity of250g, distance between main electrode plates of6.5cm, electrolysis time of150min,removals of COD,TN and phosphate were76.47%,89.48%and97.81%. Under current8A, the COD energy consumption was lower and the COD anode efficiency was higher.
The mechanism of electrolysis had shown that organic pollutants were degradedtogether in the direct oxidation and indirect oxidation. Through hydrogen peroxide andfree chlorine tests in the electrolysis process, found that hydrogen peroxide and freechlorine concentrations in ultrahigh-salt tuber mustard wastewater were significantlylower than in the sodium chloride solution, during the organic degradation processconsumed a lot of hydrogen peroxide and free chlorine, relating to the indirect oxidationprocess. The GC-MS results showed that the pollutants peak position of electrolyticeffluent were different of the raw water’s. The polycyclic organic matters werecompletely converted to organic compounds of a single ring or straight-chain structure.In the electrolysis process, biodegradable organic matters were changed into easilydegradable middleproduct. The organic molecular weight distribution showed that thetwo-dimensional electrolysis could convert macromolecular organics into small organicmolecules, with the removal of some small organic molecules. The wavelength scan of three-dimensional electrode indicated that a part of the organic matters were directlyoxidized to carbon dioxide. Refractory organics in ultrahigh-salt tuber mustardwastewater were also effectively removed by electrolysis.
On the basis of micro-electrolysis, two-dimensional electrolysis andthree-dimensional electrode tests, the physicochemical combined process "threemicro-electrolysis-two-dimensional electrolysis" were further studied. The pilot testsof combined process showed that the removals of COD, ammonia, TN and phosphatewere79.41%,86.08%,81.71%and99.65%, pH increased from4.37to6.87, salinitydecreased from6.53%to2.09%. The effluent of physicochemical combined processwas suitable for biological treatment.
The combination of physicochemical and biological tests showed that the threemicro-electrolytic pretreatment of water was conducive to the following anaerobic,aerobic and anaerobic-aerobic biological combination treatment.The effluent COD of“three micro-electrolysis-anaerobic biofilm-contact oxidation” combined process was230-420mg/L, achieved the three emission standard of “integrated WastewaterDischarge Standard”(GB8978-1996). The “micro-electrolysis-anaerobic biofilm-contact oxidation” combined process had a good prospect.
微电解单因素试验得出，在原水pH、铁水体积比1:1、铁炭体积比1:1和反应时间30min时，去除效果较佳，COD、氨氮、磷酸盐和TN去除率分别为36%-45%、34%-42%、97%-99.9%和34%-53%，盐度去除率为22%-25%，出水pH升高1-2；多级微电解串联试验表明，串联级数为3时去除效果提高显著；正交试验表明，各因子对COD和氨氮去除率影响顺序为：铁水体积比＞初始pH＞反应时间＞铁炭体积比。填料扫描电镜和能谱分析发现，反应后铁炭表面被沉淀物覆盖，自来水冲洗后，沉淀物减少，填料恢复活性；反应后铁炭表面出现Na、P和Cl；沉淀产物XRD结果表明，磷酸盐是以Fe3(PO4)2沉淀形式被去除。
微电解机理研究表明，在原电池反应、氧化还原、电附集、铁离子絮凝沉淀和氢气气浮等共同作用下，有机污染物被降解转化或去除。GC-MS结果表明，原水中有机污染物大部分含有苯环，其中氮杂环化合物5种，氮硫杂环化合物1种，酚类3种，均为难降解污染物，预处理出水有机物种类去除率53.8%，其中氮杂环化合物种类去除率80%。有机物相对分子量结果表明，微电解可使大分子有机物转化为小分子有机物，并去除部分小分子有机物。因此，微电解法对超高盐榨菜废水中的难降解有机物具有良好的去除效果。
二维电解单因素试验表明，在原水pH、电流密度156mA/cm2、极板间距1.5cm、极水比0.8dm2/L、电解时间120min时，去除效果较佳，COD、氨氮和磷酸盐去除率分别为55.74%、99.77%和88.71%，pH由5.07升高为9.54，盐度由7.02%下降为6.39%；通过电流密度对氨氮和COD能耗和阳极效果的影响分析，得出氨氮可以采用前期高电流密度，后期低电流密度的运行模式电解，在电流密度156mA/cm2，电解30min时，氨氮能耗最低96kW·h/Kg，阳极效率最高8.47g/h·m2·A；电流密度为156mA/cm2时，COD能耗最低和阳极效率最高。三维电极单因素试验表明，在原水pH、废水600mL、电流8A、活性炭填充量250g、极板间距6.5cm、电解时间150min时，处理效果较佳，COD、TN和磷酸盐去除率分别为76.47%、89.48%和97.81%；电流为8A时，COD能耗较低和阳极效率较高。
电解机理研究表明有机污染物是在直接氧化和间接氧化共同作用下降解的。通过电解过程中过氧化氢和游离氯检测发现，榨菜废水中过氧化氢和游离氯浓度明显低于氯化钠溶液，表明有机物降解过程中消耗了大量过氧化氢和游离氯，与间接氧化过程有关。GC-MS结果表明，电解出水污染物出峰位置与原水的相比有所变化，多环有机物全部转化为单环或直链结构有机物，说明在电解过程中，难降解有机物被降解转变为易降解中间产物。有机物相对分子量分布表明，二维电解也可使大分子有机物转化为小分子有机物，同时去除部分小分子有机物。三维电极UV-Vis分析认为部分有机物可能被直接氧化为二氧化碳。因此，电解法可转化去除废水中难降解有机污染物。
在微电解、二维电解和三维电极法三种物化预处理小试试验基础上，进一步开展“三级微电解-二维电解”物化预处理组合工艺小试和中试研究，中试出水COD、氨氮、TN和磷酸盐去除率分别为79.41%、86.08%、81.71%和99.65%，pH由4.37升高为6.87，盐度由6.53%下降为2.09%。可知，该组合工艺出水盐度下降，pH升高，COD和氮磷浓度降低，适宜采用生物法处理。
由物化-生物组合工艺试验可知，三级微电解预处理对后续厌氧、好氧和厌氧-好氧生物组合处理有利。“三级微电解-厌氧生物膜-接触氧化”组合工艺出水COD浓度为230-420mg/L，达到《污水综合排放标准》（GB8978-1996）三级排放标准，具有良好的应用前景。
The characteristic of the ultrahigh-salt tuber mustard wastewater were ultra-highsalt, low pH, high organic matter, high nitrogen and phosphorus and the heterocyclerefractory organic pollutants. At present, the tuber mustard wastewater was mainlytreated by biological process, but ultrahigh-salt and salinity fluctuation would affect thebiological treatment systemstability. Therefore, it is considered to meet the subsequentbiological treatment requirements through the the physicochemical pretreatment toreduce salinity, increase the pH, removal of refractory organics. Physicochemicaltreatments of ultrahigh-salt tuber mustard wastewater were researched, includingmicro-electrolysis, two-dimensional electrolysis and three-dimensional electrolysis. Thetreatment efficiency of “three micro-electrolysis-two-dimensional electrolysis” and“three micro-electrolysis-biochemical process’ were studied.
The micro-electrolysis experiments found that under the condition of raw water pH,Fe/C volume ratio of1:1, Fe/H2O volume ratio of1:1and reaction time of30min,removals of COD, ammonia, phosphate, TN and salinity were36%-45%,34%-42%,97%-99.9%,34%-53%and22%-25%, meanwhile, the effluent pH increased1-2. Theseries of multi-level micro-electrolysis experiments showed that the removal efficiencyincreased significantly at the level of three. The orthogonal tests showed that each factoron the order of COD and ammonia removal rates were as follow: Fe/H2O volume ratio＞initial pH＞reaction time＞Fe/C volume ratio. The SEM analysis showed that thesurface of iron and carbon after reaction were covered by lots of sediment, after waterbackwash, the sediment decreased, the activity of iron and carbon recovered. The SEManalysis showed that the surface of iron and carbon after reaction increased Na, P and Cl.The XRD result of precipitation product indicated that phosphate was removed byFe3(PO4)2.
The mechanism of micro-electrolysis had shown that organic pollutants weredegraded by the combined effects of chemical battery reaction, oxidation-reduction,filtration-adsorption, flocculation-precipitation and air floatation. The GC-MS resultsshowed that the organic pollutants of raw wastewater containing benzene ring werebiodegradable pollutants, including five kinds of heterocyclic compounds, one kind ofnitrogen and sulfur heterocyclic compounds, three kinds of phenols. The removal rate oforganic matter was53.8%by micro-electrolysis pretreatment, with heterocyclic compounds removal efficiency of80%. The organic molecular weight distributionexplained that the micro-electrolysis could convert macromolecular organics into smallorganic molecules, with the removal of some small organic molecules. Refractoryorganics in ultrahigh-salt tuber mustard wastewater were effectively removed bymicro-electrolysis.
The two-dimensional electrolysis experiments found that under the optimalconditions of raw water pH, current density of156mA/cm2, electrode distance of1.5cm and electrode plate area/water volume ratio of0.8dm2/L, removals of COD,ammonia and phosphate were55.74%,99.77%and88.71%within120min. In addition,pH increased from5.07to9.54, the salinity decreased from7.02%to6.39%. Theanalysis of the current density on energy consumption and anode efficiency indicatedthat ammonia can use the electrolysis mode of pre-high and late-low current density.Under current density of156mA/cm2and electrolysis of30min, the ammonia energyconsumption was lowest96kW·h/Kg, the ammonia anode efficiency was highest8.47g/h·m2·A. Under current density156mA/cm2, the COD energy consumption was thelowest and the COD anode efficiency was the highest. The three-dimensionalelectrolysis tests found that under the condition of wastewater volume of600mL, rawwater pH, electrolysis current of8A, amount of activated carbon filling quantity of250g, distance between main electrode plates of6.5cm, electrolysis time of150min,removals of COD,TN and phosphate were76.47%,89.48%and97.81%. Under current8A, the COD energy consumption was lower and the COD anode efficiency was higher.
The mechanism of electrolysis had shown that organic pollutants were degradedtogether in the direct oxidation and indirect oxidation. Through hydrogen peroxide andfree chlorine tests in the electrolysis process, found that hydrogen peroxide and freechlorine concentrations in ultrahigh-salt tuber mustard wastewater were significantlylower than in the sodium chloride solution, during the organic degradation processconsumed a lot of hydrogen peroxide and free chlorine, relating to the indirect oxidationprocess. The GC-MS results showed that the pollutants peak position of electrolyticeffluent were different of the raw water’s. The polycyclic organic matters werecompletely converted to organic compounds of a single ring or straight-chain structure.In the electrolysis process, biodegradable organic matters were changed into easilydegradable middleproduct. The organic molecular weight distribution showed that thetwo-dimensional electrolysis could convert macromolecular organics into small organicmolecules, with the removal of some small organic molecules. The wavelength scan of three-dimensional electrode indicated that a part of the organic matters were directlyoxidized to carbon dioxide. Refractory organics in ultrahigh-salt tuber mustardwastewater were also effectively removed by electrolysis.
On the basis of micro-electrolysis, two-dimensional electrolysis andthree-dimensional electrode tests, the physicochemical combined process "threemicro-electrolysis-two-dimensional electrolysis" were further studied. The pilot testsof combined process showed that the removals of COD, ammonia, TN and phosphatewere79.41%,86.08%,81.71%and99.65%, pH increased from4.37to6.87, salinitydecreased from6.53%to2.09%. The effluent of physicochemical combined processwas suitable for biological treatment.
The combination of physicochemical and biological tests showed that the threemicro-electrolytic pretreatment of water was conducive to the following anaerobic,aerobic and anaerobic-aerobic biological combination treatment.The effluent COD of“three micro-electrolysis-anaerobic biofilm-contact oxidation” combined process was230-420mg/L, achieved the three emission standard of “integrated WastewaterDischarge Standard”(GB8978-1996). The “micro-electrolysis-anaerobic biofilm-contact oxidation” combined process had a good prospect.
引文
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