水中油污染物分散与降解机理的研究
摘要
近年来,石油泄漏事故频发,事故发生后残留在水面上的油膜难以有效去除,对海洋、河流等水体的生态环境造成极大危害,针对油泄漏的处理技术是当前的研究热点之一。在水力扰动条件下,油膜被打碎形成小油滴,水体中的悬浮固体微粒将油滴包裹,形成油滴(oil)与悬浮颗粒物(mineral)的聚结物oil-mineral-aggregate。OMA聚结物的形成将有效降低油滴粒径,促进油膜分散,有利于油类污染物的自然降解。本论文系统地研究了影响OMA形成的各种因素,对粘土进行表面改性处理,增强油滴在水中与固体微粒形成OMA的效率,应用于油膜在水中的分散,并对实验数据进行模型拟合,深入探讨了OMA形成的机理,并针对OMA对油被微生物降解过程的促进进行了初步研究。主要研究内容和结果如下：
1.对长江口和杭州湾不同位置的沉积物微粒与柴油、重油OMA的形成机理进行研究,发现颗粒物粒径分布、有机组成、颗粒物浓度是影响OMA形成效率的主要因素,仅粒径小于3μm的微细颗粒能与油滴形成OMA；沉积物的有机质含量高,有利于微粒与油滴的聚结；颗粒物浓度越高,OMA形成效率越高混合液盐度的升高在一定范围内可促进微粒在油滴表面的吸附过程。油膜经表面活性剂分散进入水相后,与固体微粒形成OMA的效率与表面活性剂类型有关,阳离子表面活性剂有利与油滴与固体微粒的聚结。
2.采用不同类型的表面活性剂对粘土进行改性,得出CTAB改性粘土与油滴的聚结效率最高。钠基膨润土Na-B在经过酸预处理后利于CTAB在粘土上的负载,改性时间为6h、改性剂初始浓度为2g/L时,改性反应达到平衡。采用扫描电镜对改性前后的粘土微粒进行观察,发现与Na-B表面特征相比,CTAB-B的表面更粗糙,孔道结构特征更加明显,原本附着在粘土孔道结构中的微细颗粒被释放出来。通过对Na-B和CTAB-B进行红外光谱和元素分析,证实阳离子表面活性剂CTAB的长碳链有机基团被成功负载在粘土颗粒表面,成功制备了改性粘土CTAB-B.热失重试验表明,改性前后的粘土均具有一定的热稳定性,改性前的Na-B吸水性更强,改性后的CTAB-B疏水性好于Na-B。粘土改性前后表面Zeta电位的测定结果表明,改性过程使粘土表面电性发生反转,由原先带负电转为带正电。
3.粘土经改性后,与柴油、重油形成OMA的效率得到大幅提升。通过荧光显微镜观察发现,OMA结构有三种类型,分别为液滴型、片状、固体型。粘土改性前后分别与柴油和重油形成的OMA结构有所不同,CTAB-B在油滴表面的负载量更高,OMA结构更稳定。CTAB-B与柴油形成的OMA粒径分布范围更广,形成OMA聚结体平均粒径小于Na-B与柴油形成的OMA。
4.粘土投加量增加有利于提高OMA形成效率。OMA形成效率在粘土临界浓度、临界盐度值达到最大。表面特性是固体微粒与油滴的结合的关键因素。膨润土经改性后,与油滴间的吸引力增强,结合效率更高。建立了OMA-固体微粒浓度模型,采用线性拟合的方式,计算模型参数,该模型相关系数高于0.9。拟合结果表明,当粘土浓度小于Cs50的50%时,OMA形成效率很低,并不会随粘土浓度上升；当粘土浓度大于等于Cs50时,模型系数n越高,OMA形成效率随粘土浓度升高速率越高。
5.固体微粒FX、Na-B、CTAB-B与柴油、重油形成OMA,有效促进了油滴在水中的分散,同时,微粒的粗糙表面为微生物的附着生长提供有利条件,增大微生物与油滴的接触面积,从而加强了两种油污染物的微生物降解过程。CTAB-B对油污染物降解促进效果最好,柴油、重油在5天内降解基本达到平衡,去除率分别达到73%和79%。水样的盐度对油降解效率产生一定影响。盐度的升高对微生物的活性有一定的抑制,但是当盐度接近CTAB-B与柴油、重油形成OMA效率最大时的临界盐度值时,由于油滴粒径降低,则促进了微生物对油污染物的降解。柴油、重油经微生物降解后生成有机酸类物质,使水样pH降低。Na-B、CTAB-B可以吸附水样中的质子,对水样pH变化起到缓冲作用,Na-B、CTAB-B存在的条件下,油污染物经降解后,水样pH变化不大。柴油、重油经过微生物降解后,短碳链有机物基本被降解,剩余成份主要为长碳链难降解有机物。
以上研究结果有助于了解油污染物在水中的分散状态,对溢油模型的建立和修正提供实验数据和理论基础,为建立以OMA为机理的水体油污染物去除技术提供科学依据。
In recent years, oil slim in water derived from increasing oil spill accidents has been seriously threatened marine ecological environment. The technology of removing oil slim is one of the presently studying hotspots. The oil droplets dispersed from surface slicks caused by local flow and turbulence conditions aggregates with suspended mineral particles naturally and readily forming oil mineral aggregates (OMA), which enhance dispersion of spilled oil and decreases average oil droplet size by preventing the droplets recoalescence. This process is good for oil biodegradation. In this study, the influence of factors on OMA formation was investigated. Clay was modified and then used to form OMA with different oil. Models were developed for experimental data fitting and OMA formation mechanism was further discussed. Besides, the oil biodegradation facilitation by OMA was studied. The main conclusions of this dissertation are as follows:
1. The study on OMA formation with sediment minerals from Yangtze Estuary and Hangzhou Bay found that particulate matter size distribution, organic matter content and concentration were important parameters, and light diesel and heavy oil only formed OMA with minerals with grain diameters less than3μm. High organic matter content of sediment was proved to be good for aggregation between particle and oil droplet. The OMA formation efficiency increased with the particle concentration. Oil droplet separated by different surfactant would have different OMA formation efficiency with mineral and cationic surfactant promote OMA formation.
2. Different types of surfactant were used to modify the clay. CTAB modified clay has the higest aggregation efficiency with oil droplet. Acid pretreatment clay had better CTAB modifiy efficiency. The reaction equilibrium reached at6h with initial CTAB concentration of2g/L. The surface structure of clay before and after modified was studied with SEM. Modified clay (CTAB-B) has a more rough surface and more apparent structural channels features compared to original clay (Na-B). IR results showed that long carbon chain of CTAB was introduced to the surface of clay which confirmed the successful modification. TG curves of clays indicated that both CTAB-B and Na-B had preferable thermostability. CTAB-B had better hydrophobicity than Na-B. Zeta potential test result demonstrated that Na-B was negative charged and CTAB-B was positive charged.
3. Light diesel and heavy oil OMA formation efficiency has increased sharply with modified clay. Under UV epi-fluorescence observation, it was found that there are three different structure types of OMA:droplet, solid and flake. OMA formed with CTAB-B and Na-B had different structure. Much more CTAB-B particles adhered to the surface of oil droplet, by which OMA formed with CTAB-B was more stable. The size of OMA formed with CTAB-B was wider ranged and the average of it was smaller.
4. OMA formation efficiency increased with clay dosage. Maximum efficiency reaches at critical clay concentration and salinity. Surface property is the key factor for the aggregation. Surface modification increased the affinity between oil droplet and particle. OMA-particle concentration model was set up and the experimental data was linear fitted. Correlation coefficients of the model were more than0.9. The fitting results indicated that OMA formation efficiency was very low as the particle concentration was lower than50%of CS50, and OMA formation efficiency increased with particle concentration as which was more than50%of CS50. The increasing rate of efficiency with particle concentration went up with the model parameter n.
5. The diameter of oil droplet decreased because of OMA formation with particle FX、 Na-B and CTAB-B. Meanwhile, larger rough surface provided by particles was beneficial for bacteria culture. Oil biodegradation was consequently enhanced by this process. Furthermore, oil biodegraded at the highest rate with addition of CTAB-B, and light diesel and heavy oil removal efficiency reached73%and79%in five days respectively. Yet increasing salinity restrained the microorganisms' growth, the size of oil droplet decreased with increasing salinity by which oil biodegradation was facilitated. pH of the water was reduced due to organic acids produced by oil degradation. Na-B、CTAB-B played a important role on pH balance by adsorption of hydrogen ion. Most of the organics with short carbon chain in light diesel and heavy oil was removed and only a small fraction of residual oil with long carbon chain was left.
The above results are helpful to understand oil dispersity in water, provide experimental data and theoretical basis to predict and model the transportation of spilled oil, and offer quantitative evidence that supports further development of practical operational oil removal techniques based on OMA formation.
1.对长江口和杭州湾不同位置的沉积物微粒与柴油、重油OMA的形成机理进行研究,发现颗粒物粒径分布、有机组成、颗粒物浓度是影响OMA形成效率的主要因素,仅粒径小于3μm的微细颗粒能与油滴形成OMA；沉积物的有机质含量高,有利于微粒与油滴的聚结；颗粒物浓度越高,OMA形成效率越高混合液盐度的升高在一定范围内可促进微粒在油滴表面的吸附过程。油膜经表面活性剂分散进入水相后,与固体微粒形成OMA的效率与表面活性剂类型有关,阳离子表面活性剂有利与油滴与固体微粒的聚结。
2.采用不同类型的表面活性剂对粘土进行改性,得出CTAB改性粘土与油滴的聚结效率最高。钠基膨润土Na-B在经过酸预处理后利于CTAB在粘土上的负载,改性时间为6h、改性剂初始浓度为2g/L时,改性反应达到平衡。采用扫描电镜对改性前后的粘土微粒进行观察,发现与Na-B表面特征相比,CTAB-B的表面更粗糙,孔道结构特征更加明显,原本附着在粘土孔道结构中的微细颗粒被释放出来。通过对Na-B和CTAB-B进行红外光谱和元素分析,证实阳离子表面活性剂CTAB的长碳链有机基团被成功负载在粘土颗粒表面,成功制备了改性粘土CTAB-B.热失重试验表明,改性前后的粘土均具有一定的热稳定性,改性前的Na-B吸水性更强,改性后的CTAB-B疏水性好于Na-B。粘土改性前后表面Zeta电位的测定结果表明,改性过程使粘土表面电性发生反转,由原先带负电转为带正电。
3.粘土经改性后,与柴油、重油形成OMA的效率得到大幅提升。通过荧光显微镜观察发现,OMA结构有三种类型,分别为液滴型、片状、固体型。粘土改性前后分别与柴油和重油形成的OMA结构有所不同,CTAB-B在油滴表面的负载量更高,OMA结构更稳定。CTAB-B与柴油形成的OMA粒径分布范围更广,形成OMA聚结体平均粒径小于Na-B与柴油形成的OMA。
4.粘土投加量增加有利于提高OMA形成效率。OMA形成效率在粘土临界浓度、临界盐度值达到最大。表面特性是固体微粒与油滴的结合的关键因素。膨润土经改性后,与油滴间的吸引力增强,结合效率更高。建立了OMA-固体微粒浓度模型,采用线性拟合的方式,计算模型参数,该模型相关系数高于0.9。拟合结果表明,当粘土浓度小于Cs50的50%时,OMA形成效率很低,并不会随粘土浓度上升；当粘土浓度大于等于Cs50时,模型系数n越高,OMA形成效率随粘土浓度升高速率越高。
5.固体微粒FX、Na-B、CTAB-B与柴油、重油形成OMA,有效促进了油滴在水中的分散,同时,微粒的粗糙表面为微生物的附着生长提供有利条件,增大微生物与油滴的接触面积,从而加强了两种油污染物的微生物降解过程。CTAB-B对油污染物降解促进效果最好,柴油、重油在5天内降解基本达到平衡,去除率分别达到73%和79%。水样的盐度对油降解效率产生一定影响。盐度的升高对微生物的活性有一定的抑制,但是当盐度接近CTAB-B与柴油、重油形成OMA效率最大时的临界盐度值时,由于油滴粒径降低,则促进了微生物对油污染物的降解。柴油、重油经微生物降解后生成有机酸类物质,使水样pH降低。Na-B、CTAB-B可以吸附水样中的质子,对水样pH变化起到缓冲作用,Na-B、CTAB-B存在的条件下,油污染物经降解后,水样pH变化不大。柴油、重油经过微生物降解后,短碳链有机物基本被降解,剩余成份主要为长碳链难降解有机物。
以上研究结果有助于了解油污染物在水中的分散状态,对溢油模型的建立和修正提供实验数据和理论基础,为建立以OMA为机理的水体油污染物去除技术提供科学依据。
In recent years, oil slim in water derived from increasing oil spill accidents has been seriously threatened marine ecological environment. The technology of removing oil slim is one of the presently studying hotspots. The oil droplets dispersed from surface slicks caused by local flow and turbulence conditions aggregates with suspended mineral particles naturally and readily forming oil mineral aggregates (OMA), which enhance dispersion of spilled oil and decreases average oil droplet size by preventing the droplets recoalescence. This process is good for oil biodegradation. In this study, the influence of factors on OMA formation was investigated. Clay was modified and then used to form OMA with different oil. Models were developed for experimental data fitting and OMA formation mechanism was further discussed. Besides, the oil biodegradation facilitation by OMA was studied. The main conclusions of this dissertation are as follows:
1. The study on OMA formation with sediment minerals from Yangtze Estuary and Hangzhou Bay found that particulate matter size distribution, organic matter content and concentration were important parameters, and light diesel and heavy oil only formed OMA with minerals with grain diameters less than3μm. High organic matter content of sediment was proved to be good for aggregation between particle and oil droplet. The OMA formation efficiency increased with the particle concentration. Oil droplet separated by different surfactant would have different OMA formation efficiency with mineral and cationic surfactant promote OMA formation.
2. Different types of surfactant were used to modify the clay. CTAB modified clay has the higest aggregation efficiency with oil droplet. Acid pretreatment clay had better CTAB modifiy efficiency. The reaction equilibrium reached at6h with initial CTAB concentration of2g/L. The surface structure of clay before and after modified was studied with SEM. Modified clay (CTAB-B) has a more rough surface and more apparent structural channels features compared to original clay (Na-B). IR results showed that long carbon chain of CTAB was introduced to the surface of clay which confirmed the successful modification. TG curves of clays indicated that both CTAB-B and Na-B had preferable thermostability. CTAB-B had better hydrophobicity than Na-B. Zeta potential test result demonstrated that Na-B was negative charged and CTAB-B was positive charged.
3. Light diesel and heavy oil OMA formation efficiency has increased sharply with modified clay. Under UV epi-fluorescence observation, it was found that there are three different structure types of OMA:droplet, solid and flake. OMA formed with CTAB-B and Na-B had different structure. Much more CTAB-B particles adhered to the surface of oil droplet, by which OMA formed with CTAB-B was more stable. The size of OMA formed with CTAB-B was wider ranged and the average of it was smaller.
4. OMA formation efficiency increased with clay dosage. Maximum efficiency reaches at critical clay concentration and salinity. Surface property is the key factor for the aggregation. Surface modification increased the affinity between oil droplet and particle. OMA-particle concentration model was set up and the experimental data was linear fitted. Correlation coefficients of the model were more than0.9. The fitting results indicated that OMA formation efficiency was very low as the particle concentration was lower than50%of CS50, and OMA formation efficiency increased with particle concentration as which was more than50%of CS50. The increasing rate of efficiency with particle concentration went up with the model parameter n.
5. The diameter of oil droplet decreased because of OMA formation with particle FX、 Na-B and CTAB-B. Meanwhile, larger rough surface provided by particles was beneficial for bacteria culture. Oil biodegradation was consequently enhanced by this process. Furthermore, oil biodegraded at the highest rate with addition of CTAB-B, and light diesel and heavy oil removal efficiency reached73%and79%in five days respectively. Yet increasing salinity restrained the microorganisms' growth, the size of oil droplet decreased with increasing salinity by which oil biodegradation was facilitated. pH of the water was reduced due to organic acids produced by oil degradation. Na-B、CTAB-B played a important role on pH balance by adsorption of hydrogen ion. Most of the organics with short carbon chain in light diesel and heavy oil was removed and only a small fraction of residual oil with long carbon chain was left.
The above results are helpful to understand oil dispersity in water, provide experimental data and theoretical basis to predict and model the transportation of spilled oil, and offer quantitative evidence that supports further development of practical operational oil removal techniques based on OMA formation.
引文
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