基于臭氧氧化的印染废水生化出水深度处理组合工艺及有机物去除行为研究
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摘要
本课题以某印染废水生化出水为研究对象,依据有机物在不同处理过程中的去除、转化行为,构建了多个基于臭氧氧化(03)的深度处理组合工艺,使处理水水质满足印染行业生产用水要求。
首先,在引入ADMI值(美国染料制造商协会单位)表征水样色度的同时,使用XAD树脂分离、超滤膜(表观)分子量分级和光谱分析技术详细描述了生化出水中有机物(EfOM)的组成和特性。EfOM主要以溶解态的形式(DOM)存在,富含类色氨酸和类腐殖质等化合物。其中,疏水性与亲水性有机物DOC的比值为1.5-2.0：1,水样在254nm处的紫外吸光度(UV254)和ADMI值大部分来自于表观分子量(AMW)在10k Da以上的疏水性物质。
其次,考察了臭氧投加量、水温条件和初始pH等因素对臭氧氧化处理印染废水生化出水的影响,并对EfOM可生化性和可吸附性随比臭氧消耗量发生规律性变化的原因作出了解释。臭氧氧化对各水质指标的去除率遵循：ADMI值>UV254>COD>DOC,根据溶解臭氧暴露量的变化可以确定有机物去除速率的临界时间。由热力学分析可知,03的矿化作用比去除UV254和ADMI值更容易受到水温变化的影响。在水样的原始pH(约8.0)条件下,臭氧氧化的处理效果良好。随着比臭氧消耗量的增大,EfOM的可生化性显著提高,亲水性物质成为溶解性可生物降解有机碳(BDOC)的主要成分。臭氧氧化一方面通过降低有机物的平均分子量,改善了部分DOC的可吸附性,另一方面又会因导致有机物亲水性的增强,使得难吸附DOC的比例不断上升。在理想状态下,预计臭氧氧化-生物活性炭法对生化出水DOC、UV254和ADMI值的去除率可以分别达到83.4%、95.9%和99.6%。
再次,通过分析臭氧预氧化混凝对EfOM的去除效果可知,将臭氧投加量控制在0.6mg O3·mg-1COD,可以在有效降低生化出水色度、UV254和荧光峰强度的同时,限制BDOC的生成,并减小预氧化对后续混凝的不利影响。向臭氧反应器内投加一定量颗粒活性炭(GAC/O3)能显著提高预氧化阶段对中小分子DOM的处理效果,并有利于增强铝盐混凝对疏水性、大分子有机物的去除能力。经过参数优化,梯度混凝-中间GAC/O3氧化新工艺充分利用了不同处理方法的优势和互利关系,实现了对印染废水生化出水的高效净化。生化出水经聚合氯化铝(PACl)预混凝处理(pH8.0)后,pH变化很小,但疏水性有机物的百分比却大幅降低。这有利于GAC/O3体系发挥催化氧化作用,其处理水水质能在较长时间的连续运行中保持稳定。此外,二次混凝(pH5.5)对AMW在1-10k Da的亲水性有机物具有良好的去除效果。当预混凝和二次混凝中PACl投加量均为25mg Al·L-1,GAC/O3氧化中使用3.1mg O3·mg-1COD和10g GAC·L-1时,组合工艺对生化出水浊度、COD、DOC、UV254和ADMI值的去除率分别达到了95.8%、88.1%、68.7%、90.5%和97.5%,每立方米废水的处理成本约为3.20元,中间氧化过程的费用占到了80%。
在去除了水中大部分EfOM的前提下,使用HD-8型强酸阳树脂和D315型弱碱阴树脂串联技术进行脱盐处理。当交换流量为每小时4倍床层数(4BV·h-1)时,单次处理水量可达40-46BV,脱盐水水质(TDS<35mg·L-1,电导率<50μS·cm-1)远优于纺织染整工业回用水水质标准(FZ/T01107-2011)的要求。离子交换树脂经酸碱溶液再生后可以重复使用。
In this study, several hybrid processes based on ozonation (O3) were designed for the reclamation of biotreated textile wastewater, according to removal and transformation behavior of effluent organic matter (EfOM) in the different steps. The quality of treated water was considered to satisfy the requirement of dyeing and printing in textile industry for process use.
Firstly, with the color being represented by ADMI value (American Dye Manufactures Institute), EfOM characterization was conducted by XAD resin absorbents and Ultra filtration cut-off fractionation, and spectroscopy technologies. Results showed that dissolved organic matter (DOM) predominated in EfOM, being rich in tryptophan-like and humic-like compounds. The percent ratio between hydrophobic and hydrophilic fractions was around1.5～2.0:1in terms of DOC, while both UV254and ADMI value of raw sample were mostly contributed by hydrophobic one of apparent molecular weight (AMW) higher than10k Da.
Secondly, effects of ozone dose, reaction temperature and intial pH on the ozonation efficacy of biotreated textile wastewater were evaluated, and the regular changes of EfOM biodegradability and adsorbability on activated carbon with the specific ozone consumption were also elucidated. The removal efficiencies of water quality parameters in ozonation were in the following order:ADMI value>UV254> COD> DOC. The critical time of EfOM removal rate could be indentified, based on ozone exposure in the aqueous phase. It was known from thermodynamics analysis that, the minerlization efficiency in ozonation was more sensitive to the change of reaction temperature than the removal of UV254and ADMI value. At original pH (around8.0), the ozonation efficacy was proved to be acceptable. In addition, the increase of specific ozone consumption improved EfOM biodegradability significantly, with hydrophilic organic matter as the predominate fraction of biodegradable DOC (BDOC) produced by O3. On the one hand, ozonation improved the adsorbability of some compounds by causing the decrease of average apparent molecular weight of EfOM, and on the other, resulted in the acculumation of non-adsorbable fraction by increasing its hydrophilicity. Idealy, the estimated removal efficiencies of DOC, UV254and ADMI value in biotreated textile wastewater by using ozonation followed by biological activated carbon could reach83.4%,95.9%and99.6%, respectively.
The performance of coagulation with pre-ozonation made it obvious that, the ozone dose of0.6mg03·mg-1COD employed in pre-oxidation step, not only helped reducing samples UV254, ADMI value and fluorescence intensity, but also limited the formation of BDOC and the adverse effect on subsequent coagulation. Ozonatin in the presence of granular activated carbon (GAC/O3) presented a higher pre-oxidation efficacy, and improved the treatability of hydrophobic and high molecular weight fractions by aluminium coagulation. After the optimization design, a novel hybrid process including stepwise coagulation and intermediate GAC/O3oxidation was employed in the reclamation of biotreated textile wastewater. It made full use of each technology advantages and their beneficial interactions. Pre-coagulation using polyalumium chloride (PACl) at pH8.0did not result in an obvious decrease of samples pH, but the effective removal of hydrophobic compounds, which was in favor of maintaining a strong catalytic ozonation in GAC/O3, even under continuous operation lasting several hours, and enhanced the removal of hydrophilic fractions of AMW in1～10k Da via post-coagulation at pH5.5. When the PAC1dose of25mg·L-1as A1was used in both pre-and post-coagulation, and3.1mg03·mg-1COD and10g GAC·L-1were applied in GAC/O3, the highest removal efficiencies of water quality parameters like turbidity, colour, COD, DOC and UV254were95.8%,97.5%,88.1%,68.7%and90.5%, respectively. Under this condition, its operating cost was3.20yuan per ton wastewater, in which the percent of intermediate oxidation step was around80%.
Following the effective removal of EfOM, the desalination of reclaimed water was conducted by the ion exchange resin train, including strong acid type HD-8cation one and weak base type D315anion one. With the exchange flow rate of4times resin bed volume (BV) per hour, the water yield in one turn was around40to46BV. Its quality, such as total dissolved solid (TDS) less than35mg·L-1and conductivity less than50μS·cm-1etc, was far superior to the requirements of reuse water quality standard in textile industry (FZ/T01107-2011). Additionally, ion exchange resin could be reused, after being regenerated sufficiently by HCl or NaOH solution.
首先,在引入ADMI值(美国染料制造商协会单位)表征水样色度的同时,使用XAD树脂分离、超滤膜(表观)分子量分级和光谱分析技术详细描述了生化出水中有机物(EfOM)的组成和特性。EfOM主要以溶解态的形式(DOM)存在,富含类色氨酸和类腐殖质等化合物。其中,疏水性与亲水性有机物DOC的比值为1.5-2.0：1,水样在254nm处的紫外吸光度(UV254)和ADMI值大部分来自于表观分子量(AMW)在10k Da以上的疏水性物质。
其次,考察了臭氧投加量、水温条件和初始pH等因素对臭氧氧化处理印染废水生化出水的影响,并对EfOM可生化性和可吸附性随比臭氧消耗量发生规律性变化的原因作出了解释。臭氧氧化对各水质指标的去除率遵循：ADMI值>UV254>COD>DOC,根据溶解臭氧暴露量的变化可以确定有机物去除速率的临界时间。由热力学分析可知,03的矿化作用比去除UV254和ADMI值更容易受到水温变化的影响。在水样的原始pH(约8.0)条件下,臭氧氧化的处理效果良好。随着比臭氧消耗量的增大,EfOM的可生化性显著提高,亲水性物质成为溶解性可生物降解有机碳(BDOC)的主要成分。臭氧氧化一方面通过降低有机物的平均分子量,改善了部分DOC的可吸附性,另一方面又会因导致有机物亲水性的增强,使得难吸附DOC的比例不断上升。在理想状态下,预计臭氧氧化-生物活性炭法对生化出水DOC、UV254和ADMI值的去除率可以分别达到83.4%、95.9%和99.6%。
再次,通过分析臭氧预氧化混凝对EfOM的去除效果可知,将臭氧投加量控制在0.6mg O3·mg-1COD,可以在有效降低生化出水色度、UV254和荧光峰强度的同时,限制BDOC的生成,并减小预氧化对后续混凝的不利影响。向臭氧反应器内投加一定量颗粒活性炭(GAC/O3)能显著提高预氧化阶段对中小分子DOM的处理效果,并有利于增强铝盐混凝对疏水性、大分子有机物的去除能力。经过参数优化,梯度混凝-中间GAC/O3氧化新工艺充分利用了不同处理方法的优势和互利关系,实现了对印染废水生化出水的高效净化。生化出水经聚合氯化铝(PACl)预混凝处理(pH8.0)后,pH变化很小,但疏水性有机物的百分比却大幅降低。这有利于GAC/O3体系发挥催化氧化作用,其处理水水质能在较长时间的连续运行中保持稳定。此外,二次混凝(pH5.5)对AMW在1-10k Da的亲水性有机物具有良好的去除效果。当预混凝和二次混凝中PACl投加量均为25mg Al·L-1,GAC/O3氧化中使用3.1mg O3·mg-1COD和10g GAC·L-1时,组合工艺对生化出水浊度、COD、DOC、UV254和ADMI值的去除率分别达到了95.8%、88.1%、68.7%、90.5%和97.5%,每立方米废水的处理成本约为3.20元,中间氧化过程的费用占到了80%。
在去除了水中大部分EfOM的前提下,使用HD-8型强酸阳树脂和D315型弱碱阴树脂串联技术进行脱盐处理。当交换流量为每小时4倍床层数(4BV·h-1)时,单次处理水量可达40-46BV,脱盐水水质(TDS<35mg·L-1,电导率<50μS·cm-1)远优于纺织染整工业回用水水质标准(FZ/T01107-2011)的要求。离子交换树脂经酸碱溶液再生后可以重复使用。
In this study, several hybrid processes based on ozonation (O3) were designed for the reclamation of biotreated textile wastewater, according to removal and transformation behavior of effluent organic matter (EfOM) in the different steps. The quality of treated water was considered to satisfy the requirement of dyeing and printing in textile industry for process use.
Firstly, with the color being represented by ADMI value (American Dye Manufactures Institute), EfOM characterization was conducted by XAD resin absorbents and Ultra filtration cut-off fractionation, and spectroscopy technologies. Results showed that dissolved organic matter (DOM) predominated in EfOM, being rich in tryptophan-like and humic-like compounds. The percent ratio between hydrophobic and hydrophilic fractions was around1.5～2.0:1in terms of DOC, while both UV254and ADMI value of raw sample were mostly contributed by hydrophobic one of apparent molecular weight (AMW) higher than10k Da.
Secondly, effects of ozone dose, reaction temperature and intial pH on the ozonation efficacy of biotreated textile wastewater were evaluated, and the regular changes of EfOM biodegradability and adsorbability on activated carbon with the specific ozone consumption were also elucidated. The removal efficiencies of water quality parameters in ozonation were in the following order:ADMI value>UV254> COD> DOC. The critical time of EfOM removal rate could be indentified, based on ozone exposure in the aqueous phase. It was known from thermodynamics analysis that, the minerlization efficiency in ozonation was more sensitive to the change of reaction temperature than the removal of UV254and ADMI value. At original pH (around8.0), the ozonation efficacy was proved to be acceptable. In addition, the increase of specific ozone consumption improved EfOM biodegradability significantly, with hydrophilic organic matter as the predominate fraction of biodegradable DOC (BDOC) produced by O3. On the one hand, ozonation improved the adsorbability of some compounds by causing the decrease of average apparent molecular weight of EfOM, and on the other, resulted in the acculumation of non-adsorbable fraction by increasing its hydrophilicity. Idealy, the estimated removal efficiencies of DOC, UV254and ADMI value in biotreated textile wastewater by using ozonation followed by biological activated carbon could reach83.4%,95.9%and99.6%, respectively.
The performance of coagulation with pre-ozonation made it obvious that, the ozone dose of0.6mg03·mg-1COD employed in pre-oxidation step, not only helped reducing samples UV254, ADMI value and fluorescence intensity, but also limited the formation of BDOC and the adverse effect on subsequent coagulation. Ozonatin in the presence of granular activated carbon (GAC/O3) presented a higher pre-oxidation efficacy, and improved the treatability of hydrophobic and high molecular weight fractions by aluminium coagulation. After the optimization design, a novel hybrid process including stepwise coagulation and intermediate GAC/O3oxidation was employed in the reclamation of biotreated textile wastewater. It made full use of each technology advantages and their beneficial interactions. Pre-coagulation using polyalumium chloride (PACl) at pH8.0did not result in an obvious decrease of samples pH, but the effective removal of hydrophobic compounds, which was in favor of maintaining a strong catalytic ozonation in GAC/O3, even under continuous operation lasting several hours, and enhanced the removal of hydrophilic fractions of AMW in1～10k Da via post-coagulation at pH5.5. When the PAC1dose of25mg·L-1as A1was used in both pre-and post-coagulation, and3.1mg03·mg-1COD and10g GAC·L-1were applied in GAC/O3, the highest removal efficiencies of water quality parameters like turbidity, colour, COD, DOC and UV254were95.8%,97.5%,88.1%,68.7%and90.5%, respectively. Under this condition, its operating cost was3.20yuan per ton wastewater, in which the percent of intermediate oxidation step was around80%.
Following the effective removal of EfOM, the desalination of reclaimed water was conducted by the ion exchange resin train, including strong acid type HD-8cation one and weak base type D315anion one. With the exchange flow rate of4times resin bed volume (BV) per hour, the water yield in one turn was around40to46BV. Its quality, such as total dissolved solid (TDS) less than35mg·L-1and conductivity less than50μS·cm-1etc, was far superior to the requirements of reuse water quality standard in textile industry (FZ/T01107-2011). Additionally, ion exchange resin could be reused, after being regenerated sufficiently by HCl or NaOH solution.
引文
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