陶瓷膜成套装备与工程应用技术的研究
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摘要
本文以提高膜渗透通量、降低陶瓷膜设备的运行成本为目标，以亚微米、纳米粒子的固液分离以及医药、生化工业的发酵液除菌分离为应用背景，分析了无机陶瓷膜在液相分离领域的应用现状，提出了以强化陶瓷膜过程为手段，解决膜应用过程中的成套装备问题，以实现陶瓷膜在相关领域的工程应用。
在强化陶瓷膜过程的研究中，系统考察了湍流促进器结构、形状对膜的强化过程，认为缠绕式湍流促进器可显著提高膜的渗透通量，降低膜污染，并对其强化机理进行了阐述；研究反冲过程对膜系统的作用机理，并优化了反冲操作条件，为反冲技术的在陶瓷膜工程中的应用奠定了基础。
在膜污染和清洗方法研究中，针对油田采出水这一复杂体系，采用扫描电子显微镜(SEM)和能谱分析(EDX)研究膜表面和断面污染物的形态和成分；采用电渗法和电泳法测定膜材料和废水之间的电位变化关系，认为硫和硅等在膜面发生特征吸附，导致膜污染加重，并随着污染物的累积，导致渗透通量持续下降；采用膜面预处理减弱特征吸附，可有效抑制膜污染的形成；采用酸、表面活性剂、碱并配以合适的脉冲清洗，有效恢复膜的渗透通量。通过对膜污染机理和清洗方法的研究，为陶瓷膜成套装置的长期稳定运行提供了保证。
在亚微米、纳米粒子的固液分离过程中，针对颗粒体系的微滤过程，考察膜孔径、膜厚度等结构参数对膜通量的影响，结合阻力模型分析计算了颗粒体系膜污染的形成过程，认为颗粒体系微滤污染主要由堵塞和滤饼两部分组成；通过对钛白粉水洗液废水处理以及纳米TiO_2粉体的洗涤浓缩过程的研究，建立了粉体洗涤过程的数学模型，优化了洗水过程；设计了年生产500吨的纳米TiO_2生产过程中的陶瓷膜洗涤成套装置，实现了反冲过程的系统控制和洗水方式的自动控制，该装置已稳定运行两年，取得了很好的经济和社会效益，本研究结果已在钛白粉废水处理、纳米粉体的生产中推广应用。
在医药、生化工业的发酵液除菌分离中，对陶瓷膜用于肌苷发酵液的处理进行了深入的研究，开发出絮凝预处理和陶瓷膜分离结合的肌苷除杂新工艺。实验表明，ZrO_2膜处理肌苷发酵液的合适条件为pH=3、操作压力为0.1MPa、膜面流速3m／s、温度大于70度，此时可以获得平均渗透通量150L／m~2h，但由于酸性条件、高温下肌苷降解，导致肌苷收率有所降低，但仍高于传统肌苷提取方法得到的收率；为进一步提高肌苷得率，缩短提取工序，实验研究了絮凝剂预处理发酵液，解决碱性条件下由于蛋白析出导致膜污染加重的问题，研究表明采用CaCl_2絮凝并调节pH=11，可以获得平均渗透通量为180L／m~2h，肌苷得率大于95％；比较了三种肌苷提取工艺得到的产品质量，采用预处理与陶瓷
南京工业大学博士学位论文
膜分离结合的除杂工艺得到的粗昔质量与陶瓷膜分离、离子交换及活性炭吸附
工艺生产的粗普质量相当，均优于传统的提取工艺;设计了每小时处理12一巧
吨肌普发酵液的陶瓷膜成套装置，采用部分内循环的方式降低设备的能耗，简
化了肌昔提取方式，提高了产品的收率和得率，由于减少离子交换和活性炭吸
附，使得工厂废水排放量降低30一40%，降低酸、碱用量，有利于环境保护。
该应用技术和成套装备己在食品、生物化工、医药工业推广应用。
综上所述，通过对陶瓷膜强化过程、膜污染和清洗方法的研究，亚微米、
纳米粒子的固液分离以及医药、生化工业的发酵液除菌分离等行业的成套陶瓷
膜装置的建设和应用技术的开发，极大地推动陶瓷膜技术的发展，夯实了我国
陶瓷膜工程应用的基础，促进了相关行业的技术进步。
The aim of this paper is to enhance the permeate flux of the ceramic membrane and lower the operation cost of the membrane equipment, in the area such as the separation of submicron and nanometer particles, and removal of biomass from fermentation broth in pharmaceutical industry and biochemical engineering. By analyzing the application of ceramic membranes in liquid separation, we proposed a way of membrane separation process intensification to solve some problems in whole set equipment, so that the commercial application of ceramic membrane in these areas on the membrane separation process could be realized. The influences of the configuration and appearance shape of turbulence promoter were systematically investigated. It was founded that the winding turbulence promoter could effectively increase the membrane permeate flux and reduce membrane fouling. The mechanism of intensifying the filtration process was elucidated. On the other hand, the influences of backflushing on flux were examined and the operati
onal conditions were optimized.
To investigate the mechanism of membrane fouling and cleaning method, oilfield produced water, a complex system, was selected as a research object. Contaminant on membrane surface and cross section were analyzed by the scanning electron microscopy and EDX. The electric potential of membrane material and waster water was measured with electroosmosis and electrophoresis. It confirmed that sulfur and silicon were selectively adsorbed on the membrane surface, which result in more membrane fouling. With the accumulation of the contaminants, the permeation flux decreased continuously. The adsorption could be receded and the fouling could be controlled through pretreatment to membrane. The permeation flux can be recovered by washing with acid, surfactant and base as well as appropriate pulse washing. The determination of the method to investigate the membrane fouling mechanism and to clean the membrane gave the long-term stable operation of the membrane equipment. The effects of the structure parameters of the memb
rane, such as the pore size and the thickness on the permeation flux were examined in the MF process of submicron and nanometer suspensions. The process of membrane fouling in this kind of separation process was simulated based on the resistance model. It was thought that the membrane fouling in a particle system was composed of the blockage of the process the filtration cake. Wastewater containing titanium pigment was treated by microfiltration membrane, Nanometer titanium can be purified and concentrated by use of microfiltration. Operational conditions were optimized and the model was built. Finally, the amount of wash water was reduced. Based on the above research, the whole set equipment was designed, which can meet the needs in a titanium industry with a capability of 500 ton per year. Backflush and automatic control were used in the equipment, which has been steadily run two years, has been widely adopted in titanium industry. The technology has been widely adopted in titanium industry.
In the recent years, whole set equipment of ceramic membrane was increasingly used in the recovery of desired production from fermentation broth in China. A new membrane process integrated with pretreatment of flocculation or coagulation was exploited to recover Inosine. ZrO2 ceramic membrane was used in the work, and the average permeation flux could reach 150L/m2.h under pH value of 3, transmembrane pressure 0.1MPa, CFV 3m/s, and temperature higher than 70C. The recovery ratio of inosine is higher than traditional recovery method, although inosine degraded under acidic and high temperature condition. To improve the recovery ratio of inosine and shorten the process, microfiltation under basic condition was investigated. Generally, proteins prefer to precipitate under basic condition, which would result in membrane fouling. Membrane fouling could be decreased and permeation flux could be effectively improved by adding coagulant. When CaCl2 was added in the fermentation broth
在强化陶瓷膜过程的研究中，系统考察了湍流促进器结构、形状对膜的强化过程，认为缠绕式湍流促进器可显著提高膜的渗透通量，降低膜污染，并对其强化机理进行了阐述；研究反冲过程对膜系统的作用机理，并优化了反冲操作条件，为反冲技术的在陶瓷膜工程中的应用奠定了基础。
在膜污染和清洗方法研究中，针对油田采出水这一复杂体系，采用扫描电子显微镜(SEM)和能谱分析(EDX)研究膜表面和断面污染物的形态和成分；采用电渗法和电泳法测定膜材料和废水之间的电位变化关系，认为硫和硅等在膜面发生特征吸附，导致膜污染加重，并随着污染物的累积，导致渗透通量持续下降；采用膜面预处理减弱特征吸附，可有效抑制膜污染的形成；采用酸、表面活性剂、碱并配以合适的脉冲清洗，有效恢复膜的渗透通量。通过对膜污染机理和清洗方法的研究，为陶瓷膜成套装置的长期稳定运行提供了保证。
在亚微米、纳米粒子的固液分离过程中，针对颗粒体系的微滤过程，考察膜孔径、膜厚度等结构参数对膜通量的影响，结合阻力模型分析计算了颗粒体系膜污染的形成过程，认为颗粒体系微滤污染主要由堵塞和滤饼两部分组成；通过对钛白粉水洗液废水处理以及纳米TiO_2粉体的洗涤浓缩过程的研究，建立了粉体洗涤过程的数学模型，优化了洗水过程；设计了年生产500吨的纳米TiO_2生产过程中的陶瓷膜洗涤成套装置，实现了反冲过程的系统控制和洗水方式的自动控制，该装置已稳定运行两年，取得了很好的经济和社会效益，本研究结果已在钛白粉废水处理、纳米粉体的生产中推广应用。
在医药、生化工业的发酵液除菌分离中，对陶瓷膜用于肌苷发酵液的处理进行了深入的研究，开发出絮凝预处理和陶瓷膜分离结合的肌苷除杂新工艺。实验表明，ZrO_2膜处理肌苷发酵液的合适条件为pH=3、操作压力为0.1MPa、膜面流速3m／s、温度大于70度，此时可以获得平均渗透通量150L／m~2h，但由于酸性条件、高温下肌苷降解，导致肌苷收率有所降低，但仍高于传统肌苷提取方法得到的收率；为进一步提高肌苷得率，缩短提取工序，实验研究了絮凝剂预处理发酵液，解决碱性条件下由于蛋白析出导致膜污染加重的问题，研究表明采用CaCl_2絮凝并调节pH=11，可以获得平均渗透通量为180L／m~2h，肌苷得率大于95％；比较了三种肌苷提取工艺得到的产品质量，采用预处理与陶瓷
南京工业大学博士学位论文
膜分离结合的除杂工艺得到的粗昔质量与陶瓷膜分离、离子交换及活性炭吸附
工艺生产的粗普质量相当，均优于传统的提取工艺;设计了每小时处理12一巧
吨肌普发酵液的陶瓷膜成套装置，采用部分内循环的方式降低设备的能耗，简
化了肌昔提取方式，提高了产品的收率和得率，由于减少离子交换和活性炭吸
附，使得工厂废水排放量降低30一40%，降低酸、碱用量，有利于环境保护。
该应用技术和成套装备己在食品、生物化工、医药工业推广应用。
综上所述，通过对陶瓷膜强化过程、膜污染和清洗方法的研究，亚微米、
纳米粒子的固液分离以及医药、生化工业的发酵液除菌分离等行业的成套陶瓷
膜装置的建设和应用技术的开发，极大地推动陶瓷膜技术的发展，夯实了我国
陶瓷膜工程应用的基础，促进了相关行业的技术进步。
The aim of this paper is to enhance the permeate flux of the ceramic membrane and lower the operation cost of the membrane equipment, in the area such as the separation of submicron and nanometer particles, and removal of biomass from fermentation broth in pharmaceutical industry and biochemical engineering. By analyzing the application of ceramic membranes in liquid separation, we proposed a way of membrane separation process intensification to solve some problems in whole set equipment, so that the commercial application of ceramic membrane in these areas on the membrane separation process could be realized. The influences of the configuration and appearance shape of turbulence promoter were systematically investigated. It was founded that the winding turbulence promoter could effectively increase the membrane permeate flux and reduce membrane fouling. The mechanism of intensifying the filtration process was elucidated. On the other hand, the influences of backflushing on flux were examined and the operati
onal conditions were optimized.
To investigate the mechanism of membrane fouling and cleaning method, oilfield produced water, a complex system, was selected as a research object. Contaminant on membrane surface and cross section were analyzed by the scanning electron microscopy and EDX. The electric potential of membrane material and waster water was measured with electroosmosis and electrophoresis. It confirmed that sulfur and silicon were selectively adsorbed on the membrane surface, which result in more membrane fouling. With the accumulation of the contaminants, the permeation flux decreased continuously. The adsorption could be receded and the fouling could be controlled through pretreatment to membrane. The permeation flux can be recovered by washing with acid, surfactant and base as well as appropriate pulse washing. The determination of the method to investigate the membrane fouling mechanism and to clean the membrane gave the long-term stable operation of the membrane equipment. The effects of the structure parameters of the memb
rane, such as the pore size and the thickness on the permeation flux were examined in the MF process of submicron and nanometer suspensions. The process of membrane fouling in this kind of separation process was simulated based on the resistance model. It was thought that the membrane fouling in a particle system was composed of the blockage of the process the filtration cake. Wastewater containing titanium pigment was treated by microfiltration membrane, Nanometer titanium can be purified and concentrated by use of microfiltration. Operational conditions were optimized and the model was built. Finally, the amount of wash water was reduced. Based on the above research, the whole set equipment was designed, which can meet the needs in a titanium industry with a capability of 500 ton per year. Backflush and automatic control were used in the equipment, which has been steadily run two years, has been widely adopted in titanium industry. The technology has been widely adopted in titanium industry.
In the recent years, whole set equipment of ceramic membrane was increasingly used in the recovery of desired production from fermentation broth in China. A new membrane process integrated with pretreatment of flocculation or coagulation was exploited to recover Inosine. ZrO2 ceramic membrane was used in the work, and the average permeation flux could reach 150L/m2.h under pH value of 3, transmembrane pressure 0.1MPa, CFV 3m/s, and temperature higher than 70C. The recovery ratio of inosine is higher than traditional recovery method, although inosine degraded under acidic and high temperature condition. To improve the recovery ratio of inosine and shorten the process, microfiltation under basic condition was investigated. Generally, proteins prefer to precipitate under basic condition, which would result in membrane fouling. Membrane fouling could be decreased and permeation flux could be effectively improved by adding coagulant. When CaCl2 was added in the fermentation broth
引文
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