陶瓷膜处理含油乳化废水的技术开发及传递模型研究
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摘要
含油乳化废水是一种处理难度较大的废水，在大型钢铁企业、机械加工业中大量存在。虽然在近十几年里，处理技术得到了相应的提高，但随着各行各业对轧制板材的要求越来越高，各大型钢铁企业都在钢材表面涂层技术和钢材表面洁净技术上做了大量的技术改进，尤其是为了保证高附加值产品在轧制过程的质量稳定，所采用乳化液中的乳化油分子量越来越小，乳化剂组成越来越复杂，随之而来的轧钢废水的污染成分产生了质与量的变化，对现有的处理技术带来极大的困难和挑战。为此，本论文选择长期以来一直困扰着冶金系统的含油乳化废水的治理作为论文的选题和工业应用背景。
论文在比较各种处理技术的优缺点基础上，选择了近年来发展迅速的膜法分离技术作为处理手段。针对国内引进的有机超滤膜装置，在处理含油乳化液废水中存在的问题，采用了能耐酸、碱和高温、化学稳定性好的管式陶瓷微滤膜装置，对含油废水的膜分离技术进行了深入的开发研究。论文从基础实验和理论上系统研究了关键参数对膜分离过程的影响，膜污染控制，探索了提高膜渗透通量和截留率的途径，提出强化传递和优化过程的手段，建立了通用的数学模型。本文主要进行了以下几方面的研究工作。
在基础实验研究中，探讨了各参数对分离过程的影响，着重考察了膜孔径、膜材质、操作压差、膜面流速、料液温度、料液浓度及pH值等对膜通量和截留率的影响规律，由此确定合适的操作条件。实验结果表明：采用孔径为0.2μm氧化锆膜能获得较高的渗透通量(260Lh~(-1)m~(-2))和较高的截留率，渗透侧中油含量小于10mg／L。体系的压力控制区在0～0.15 MPa，过滤压力可在0.1～0.2 MPa范围选择。过高和过低的膜面流速都不利通量提高，但对截留率影响不大，适宜的膜面流速为5m／s左右。料液温度提高有利于通量的提高，但渗透液中油含量有增大趋势。料液浓度大于2～3％后，料液浓度对通量影响不大，但当料液浓度大于5％后，若不采取措施，渗透液中油含量将可能大于10mg／L。测定了膜的主要结构参数(孔径分布、孔隙率、表层厚度)和料液的基本性质。
针对有机物对微量油含量的干扰特别提出了CPA—紫外分光光度法，较好地解决了含油量测不准的问题。测定了料液性质(粒径分布、粘度、膜面浓度等)和膜的结构参数(孔径分布、孔隙率、表层厚度)。
对陶瓷膜处理含油乳化废水过程中膜污染阻力机理、膜污染控制、强化传质和膜的清洗方法进行了研究和分析。在本实验体系下，微滤过程的污染阻力主要
摘 要
是出浓差极化、凝胶层、膜孔污染和膜管本身四部分阻力组成，各阻力的分布分
别为：凝胶层阻力占总阻力的58－65％、浓差极化占6－10％、膜孔污染占13－18
％、膜本身阻力占13～17％，凝胶层为主要污染阻力。在膜管中置入缠绕式扰动
元件能强化传质过程，在较低的流速下（膜面流速山 4～6m八降至 2～3m／s）可
获得较高的膜通量（比空管提高 45％），定性地分析了扰动元件的强化机理。采
用气顶液反冲技术能有效地控制膜污染，使过程维持在较高通量（比不采用反冲
提高30％）下进行。为获得较好的反冲效果，反冲压力应大于0．3MPa，反冲周期
应小于10分钟，反冲持续时间在l～2秒内。采用酸、碱、洗涤液交替清洗方法
能有效地恢复膜通量，膜的纯水通量可恢复到80％，料液通量可基本恢复。
在传递理论基础上，结合膜过程的传质方程和湍流的k一。模型，建立了适
用于微滤和超滤过程的“沿膜管二维湍流膜分离数学模型”。类似的通用数学模
型尚未见诸文献报道。用相关的文献数据和本文实测数据对模型进行了检验，模
型的可靠性和准确性得到很好的验证。所建立的模型可方便地应用于过程的模拟
计算和相关的模过程设计。在有渗透流的情况下，对速度、压力、浓度二维分布
进行了模拟计算，讨论了这些参变量在膜入日段的沿截面和沿管程的变化规律。
在此基础上考察了 Reynolds数、Schmidt数、Peclet数对传质系数和 Sherwood
数的影响规律。利用通量衡算方程和本模型计算的膜面浓度建立了预测膜通量的
方法，预测了在不同流量、温度。压力和料液浓度下的膜通量值及其变化规律，
通量预测值与本文实验值吻合较好，通量预测方法的可行性和准确性得到较好的
验证。过程的模拟计算和通量的预测为深入分析膜过程的传质机理和膜分离过程
的优化提供了重要的手段。
建立了一套每小时能处理12．5 立方米冷轧乳化废水的陶瓷膜工业试验装
置，在武汉钢铁股份有限公司进行了冷轧含油废水的现场试验。经过2年多的连
续运转，陶瓷膜装置经受了轧钢工艺条件和乳化液成分变化波动，长期运行稳定
平均膜通量为80～100Lin－V，处理后的排放液中油含量小于10mg／L，清洗周期
为3天左右。陶瓷膜装置处理每吨冷轧乳化废水的费用不超过5元人民币，约为
进口设备处理费用的六分之一，具有与国外技术竞争的优势地位。
本文的结论是，陶瓷膜处理含油乳化废水技术是一种先进的、高效的、经济
的新技术，论文所提出的传递膜模型可川于膜过程设计，过程优化和膜
The oily emulsion wastewater by produced in large steel factories and machine works is the most difficult in the wastewater treatment. Although in recent decades the technologies have been improved much, all large-scale steel factories have been improved their technologies about coating and cleaning the surface of products in order to get stable quality in the rolling process and to gain high profits because of the higher demand to rolled plate from all fields. Thus, the molecular weight of emulsified oils is smaller and smaller, and the composition of emulsifiers is more and more complex, which results in dramatically change of the contaminative components in such wastewater. This brings forward us great difficulty and meanwhile gives us enormous challenges. So, it was chosen that the treatment of oily wastewater puzzled the metallurgical industry for long-term as the research subject of this thesis.
Through comparison to many other methods, the membrane separation which developed fast in recent years was selected. According to the existing problems of organic ultrafiltration(UF) apparatus from USA, the ceramic microfiltration(MF) equipment was chosen, by means of which acid, alkali, high temperature and chemical property changes could be resisted. Systemic researches for ceramic technology to treat oily wastewater had been done in this thesis and the main conclusions are shown as follows.
In the fundamental experiment part, the effects of parameters (including distribution of pore sizes, character of membrane materials, operational pressure, cross-flow velocity, feed temperature and concentration, pH value) on the membrane process, especially membrane permeability flux and retention rate were discussed in order to fix on a appropriate separation conditions. Experimental results show that zirconia membrane with pore size around 0.2 m owed high permeation flux(260Lh-1m-2) and high retention rate(99.9%), the oil content is less than 10mg/L in the permeated side. Operational pressure should be controlled in the range of 0.1-0.2 MPa. Too high or too low cross-flow velocity is no good to increase of the flux, but doesn't affect the retention rate and the proper velocity is about 5m/s. Higher temperature is good to increases of flux, but the retention rate decrease. The increase of the feed-in oil concentration has little effect to the flux when oil concentration is greater than 2-3%, but once oil
concentration is above 5%, the permeated fluid's oil content may be higher than 10mg/L. pH value affects greatly flux, the proper pH
should be selected by solution property.
A new measuring method, CPA-ultraviolet spectrophotometry, was proposed for the determination of tiny oil concentration accurately, which could eliminate availably the disturbance of other organic matters. Main structure parameters of membrane (distribution of pore size, porosity, thickness of surface layer) and the basic characters of feed (distribution of oil size, temperature-viscosity curve, membrane surface's oil concentration) were determined.
The resistance distribution of membrane, membrane fouling control, enhanced mass transfer and methods of membrane cleaning were studied and analyzed. In this experimental system, fouling resistance of ceramic MF mainly consists of four aspects: concentration polarization, gel layer, membrane pore adsorbed stain and membrane itself. Resistance distribution is respectively as follows: gel layer is 58-65% of total resistance, concentration polarization resistance is 6-10%, pore stain resistance is 13-18%, membrane resistance is 13-17%. So, gel layer resistance is the main resistance. Set some twist components to disturb flow in the membrane tube may strengthen the process of mass transfer, thus higher membrane flux (45% higher than hollow tube) could be got under lower flow rate (flow rate get down from 4~6m/s to 2-3m/s), qualitative analysis had been done to the strengthen mechanism of the disturbance components. The gas-liquid back-flush technology can control membrane fouling efficiently,
论文在比较各种处理技术的优缺点基础上，选择了近年来发展迅速的膜法分离技术作为处理手段。针对国内引进的有机超滤膜装置，在处理含油乳化液废水中存在的问题，采用了能耐酸、碱和高温、化学稳定性好的管式陶瓷微滤膜装置，对含油废水的膜分离技术进行了深入的开发研究。论文从基础实验和理论上系统研究了关键参数对膜分离过程的影响，膜污染控制，探索了提高膜渗透通量和截留率的途径，提出强化传递和优化过程的手段，建立了通用的数学模型。本文主要进行了以下几方面的研究工作。
在基础实验研究中，探讨了各参数对分离过程的影响，着重考察了膜孔径、膜材质、操作压差、膜面流速、料液温度、料液浓度及pH值等对膜通量和截留率的影响规律，由此确定合适的操作条件。实验结果表明：采用孔径为0.2μm氧化锆膜能获得较高的渗透通量(260Lh~(-1)m~(-2))和较高的截留率，渗透侧中油含量小于10mg／L。体系的压力控制区在0～0.15 MPa，过滤压力可在0.1～0.2 MPa范围选择。过高和过低的膜面流速都不利通量提高，但对截留率影响不大，适宜的膜面流速为5m／s左右。料液温度提高有利于通量的提高，但渗透液中油含量有增大趋势。料液浓度大于2～3％后，料液浓度对通量影响不大，但当料液浓度大于5％后，若不采取措施，渗透液中油含量将可能大于10mg／L。测定了膜的主要结构参数(孔径分布、孔隙率、表层厚度)和料液的基本性质。
针对有机物对微量油含量的干扰特别提出了CPA—紫外分光光度法，较好地解决了含油量测不准的问题。测定了料液性质(粒径分布、粘度、膜面浓度等)和膜的结构参数(孔径分布、孔隙率、表层厚度)。
对陶瓷膜处理含油乳化废水过程中膜污染阻力机理、膜污染控制、强化传质和膜的清洗方法进行了研究和分析。在本实验体系下，微滤过程的污染阻力主要
摘 要
是出浓差极化、凝胶层、膜孔污染和膜管本身四部分阻力组成，各阻力的分布分
别为：凝胶层阻力占总阻力的58－65％、浓差极化占6－10％、膜孔污染占13－18
％、膜本身阻力占13～17％，凝胶层为主要污染阻力。在膜管中置入缠绕式扰动
元件能强化传质过程，在较低的流速下（膜面流速山 4～6m八降至 2～3m／s）可
获得较高的膜通量（比空管提高 45％），定性地分析了扰动元件的强化机理。采
用气顶液反冲技术能有效地控制膜污染，使过程维持在较高通量（比不采用反冲
提高30％）下进行。为获得较好的反冲效果，反冲压力应大于0．3MPa，反冲周期
应小于10分钟，反冲持续时间在l～2秒内。采用酸、碱、洗涤液交替清洗方法
能有效地恢复膜通量，膜的纯水通量可恢复到80％，料液通量可基本恢复。
在传递理论基础上，结合膜过程的传质方程和湍流的k一。模型，建立了适
用于微滤和超滤过程的“沿膜管二维湍流膜分离数学模型”。类似的通用数学模
型尚未见诸文献报道。用相关的文献数据和本文实测数据对模型进行了检验，模
型的可靠性和准确性得到很好的验证。所建立的模型可方便地应用于过程的模拟
计算和相关的模过程设计。在有渗透流的情况下，对速度、压力、浓度二维分布
进行了模拟计算，讨论了这些参变量在膜入日段的沿截面和沿管程的变化规律。
在此基础上考察了 Reynolds数、Schmidt数、Peclet数对传质系数和 Sherwood
数的影响规律。利用通量衡算方程和本模型计算的膜面浓度建立了预测膜通量的
方法，预测了在不同流量、温度。压力和料液浓度下的膜通量值及其变化规律，
通量预测值与本文实验值吻合较好，通量预测方法的可行性和准确性得到较好的
验证。过程的模拟计算和通量的预测为深入分析膜过程的传质机理和膜分离过程
的优化提供了重要的手段。
建立了一套每小时能处理12．5 立方米冷轧乳化废水的陶瓷膜工业试验装
置，在武汉钢铁股份有限公司进行了冷轧含油废水的现场试验。经过2年多的连
续运转，陶瓷膜装置经受了轧钢工艺条件和乳化液成分变化波动，长期运行稳定
平均膜通量为80～100Lin－V，处理后的排放液中油含量小于10mg／L，清洗周期
为3天左右。陶瓷膜装置处理每吨冷轧乳化废水的费用不超过5元人民币，约为
进口设备处理费用的六分之一，具有与国外技术竞争的优势地位。
本文的结论是，陶瓷膜处理含油乳化废水技术是一种先进的、高效的、经济
的新技术，论文所提出的传递膜模型可川于膜过程设计，过程优化和膜
The oily emulsion wastewater by produced in large steel factories and machine works is the most difficult in the wastewater treatment. Although in recent decades the technologies have been improved much, all large-scale steel factories have been improved their technologies about coating and cleaning the surface of products in order to get stable quality in the rolling process and to gain high profits because of the higher demand to rolled plate from all fields. Thus, the molecular weight of emulsified oils is smaller and smaller, and the composition of emulsifiers is more and more complex, which results in dramatically change of the contaminative components in such wastewater. This brings forward us great difficulty and meanwhile gives us enormous challenges. So, it was chosen that the treatment of oily wastewater puzzled the metallurgical industry for long-term as the research subject of this thesis.
Through comparison to many other methods, the membrane separation which developed fast in recent years was selected. According to the existing problems of organic ultrafiltration(UF) apparatus from USA, the ceramic microfiltration(MF) equipment was chosen, by means of which acid, alkali, high temperature and chemical property changes could be resisted. Systemic researches for ceramic technology to treat oily wastewater had been done in this thesis and the main conclusions are shown as follows.
In the fundamental experiment part, the effects of parameters (including distribution of pore sizes, character of membrane materials, operational pressure, cross-flow velocity, feed temperature and concentration, pH value) on the membrane process, especially membrane permeability flux and retention rate were discussed in order to fix on a appropriate separation conditions. Experimental results show that zirconia membrane with pore size around 0.2 m owed high permeation flux(260Lh-1m-2) and high retention rate(99.9%), the oil content is less than 10mg/L in the permeated side. Operational pressure should be controlled in the range of 0.1-0.2 MPa. Too high or too low cross-flow velocity is no good to increase of the flux, but doesn't affect the retention rate and the proper velocity is about 5m/s. Higher temperature is good to increases of flux, but the retention rate decrease. The increase of the feed-in oil concentration has little effect to the flux when oil concentration is greater than 2-3%, but once oil
concentration is above 5%, the permeated fluid's oil content may be higher than 10mg/L. pH value affects greatly flux, the proper pH
should be selected by solution property.
A new measuring method, CPA-ultraviolet spectrophotometry, was proposed for the determination of tiny oil concentration accurately, which could eliminate availably the disturbance of other organic matters. Main structure parameters of membrane (distribution of pore size, porosity, thickness of surface layer) and the basic characters of feed (distribution of oil size, temperature-viscosity curve, membrane surface's oil concentration) were determined.
The resistance distribution of membrane, membrane fouling control, enhanced mass transfer and methods of membrane cleaning were studied and analyzed. In this experimental system, fouling resistance of ceramic MF mainly consists of four aspects: concentration polarization, gel layer, membrane pore adsorbed stain and membrane itself. Resistance distribution is respectively as follows: gel layer is 58-65% of total resistance, concentration polarization resistance is 6-10%, pore stain resistance is 13-18%, membrane resistance is 13-17%. So, gel layer resistance is the main resistance. Set some twist components to disturb flow in the membrane tube may strengthen the process of mass transfer, thus higher membrane flux (45% higher than hollow tube) could be got under lower flow rate (flow rate get down from 4~6m/s to 2-3m/s), qualitative analysis had been done to the strengthen mechanism of the disturbance components. The gas-liquid back-flush technology can control membrane fouling efficiently,
引文
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