赤泥质多孔陶瓷滤料表面改性及其在水处理中的应用研究
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摘要
赤泥是我国有色金属行业产量最大的工业有害固体废物,每年产生1000万t以上。赤泥流失和碱渗漏对农田、河流、地下水等造成了严重污染。目前世界上还没有找到大规模利用赤泥的有效途径,赤泥问题已成为制约我国铝工业快速发展的瓶颈。当前油田采出水主要用于回注以提高油层压力,从而为驱油提供动力,而油田采出水中的油分、铁、悬浮物、微生物等污染物质将腐蚀输油管道、堵塞输油管道和地层孔隙,使得开采成本增加,而现有油田采出水处理工艺很难达到SY/T5329-94(《碎屑岩油藏注水水质推荐指标及分析方法》中A1类标准。纺织印染、造纸、塑料及皮革等工业每年都产生大量的染料废水,由于许多染料为含偶氮键、多聚芳香环的复杂有机物,可致畸、致癌、致突变,因此,这类废水中染料的去除非常重要。许多染料抗氧化、难降解,采用吸附剂去除废水中的染料具有较大优势。活性炭是一种有效的吸附剂,但价格昂贵,限制了它的广泛应用,因此制备低成本吸附剂显得尤为必要。然而,以赤泥来处理这两类废水的研究工作尚少,特别是采用便于反洗再生的赤泥质多孔陶瓷滤料来处理的研究更少,关于赤泥质多孔陶瓷滤料处理油田采出水、印染废水的工艺和理论等方面的研究都有待完善。
本文基于将赤泥的安全处置与油田采出水、印染废水的处理结合起来,实现以废治废的目标。首先根据过滤工艺对滤料级配的要求,展开对赤泥质多孔陶瓷滤料的体积密度、气孔率及气孔率与滤料压碎强度平衡的调控研究;首次提出用含氢硅油、无苯生态漆和硝酸铁对赤泥质多孔陶瓷滤料进行表面改性,以分别提高滤料的亲油、疏油和吸附性能,并用FTIR、SEM、XRD等测试手段对相关性能进行了表征;在此基础上提出了用混凝-聚结过滤耦合工艺处理油田采出水和吸附工艺处理亚甲基蓝印染废水,并对影响处理效果的因素、工艺操作参数的优化、污染物去除机理、改性滤料再生展开了一系列研究。主要的研究成果如下:
(1)以添加成孔剂工艺展开了成孔剂种类、加入量、骨料粒径、成孔剂粒径、烧成温度对赤泥质多孔陶瓷滤料的显气孔率、体积密度、压碎强度影响的研究,确定了煤粉为最佳成孔剂,煤粉加入量与赤泥质多孔陶瓷滤料的显气孔率、体积密度成线性关系,因此通过控制煤粉加入量便可实现对多孔陶瓷滤料显气孔率及体积密度的调控。陶瓷滤料显气孔率与压碎强度符合二次曲线关系。因此结合煤粉加入量和陶瓷滤料显气孔率的拟合直线方程便可通过调节煤粉加入量来平衡滤料的显气孔率与抗压强度之间的矛盾,从而获得使显气孔率高且压碎强度也大的多孔陶瓷滤料。
(2)首次对赤泥质多孔陶瓷滤料进行亲油、疏油、涂铁改性。实验结果显示,对赤泥质多孔陶瓷滤料亲油、疏油改性后,其片状测试基体对水的接触角分别为138°、6°,而没有改性的为25°,因而改性滤料的亲油和疏油性得到提高。从而亲油滤料、疏油滤料对油田采出水中油分的湿润聚结和碰撞聚结的能力增强,使得改性滤料的除油率提高。赤泥质多孔陶瓷滤料经涂铁改性后,滤料表面含铁量最高达12.9016mg/g滤料,比表面积为4.987m~2/g,比改性前增加了3.28倍,总孔隙体积由0.005049cm~3/g增至0.01417 cm~3/g,因而改性滤料的吸附性能得到提高。
(3)探讨并确定了新型一体化高效除油装置设计的方案,提出了处理油田采出水的混凝-聚结过滤耦合工艺,利用TS6六联烧杯搅拌机优化了混凝操作参数,通过小试、中试、生产性现场实验优化了新型一体化高效除油装置的设计及操作参数,从而使处理效果明显优于江汉油田采油22队的核桃壳过滤器,出水水质达到A1标准(含油量＜5mg/L、悬浮物＜1.0mg/L、总铁含量＜0.50mg/L),并确定了滤料反洗的操作参数。除油机理主要包括混凝破乳悬浮沉降、亲油滤料表面湿润吸附去除(当亲油滤料表面的油滴长大到一定程度时,它在水力冲击下会从滤料表面脱落而被滤料拦截,而滤料表面得到一定程度更新又会湿润吸附小油滴)、疏油滤料的碰撞聚结去除(小油滴通过碰撞聚结成大油滴上浮或被滤料拦载)和悬浮物协同去除(粘附在SS上的油滴也随SS被滤料拦截去除);悬浮物(SS)去除的机理主要分为阻力截留、重力沉降、接触絮凝三个方面;铁去除的机理主要为沉降、过滤拦截、吸附。
(4)通过静态试验和动态试验考察了涂铁改性滤料吸附去除模拟亚甲基蓝溶液的效果及各种因素对吸附效果的影响。在静态试验中,当pH=11时,涂铁滤料表面带负电荷而有利于带正电荷的MB离子的静电吸附,随着吸附时间增加、MB初始浓度增大,MB去除率增加;等温吸附试验表明,升高温度有利于MB去除,吸附等温线呈“S”型,符合Freundlich等温方程(R~2＞0.89);热力学研究表明涂铁滤料吸附MB是自发的吸热反应,吸附活化能为16.1445kJ/mol,大于8kJ/mol,说明涂铁滤料吸附MB以化学吸附为主;吸附动力学研究表明可用准二级动力学方程和颗粒内扩散方程来描述吸附动力学,吸附速率限制步骤为膜扩散。在动态试验中,利用BDST模型计算和预测了吸附柱的穿透时间,预测值与实验值基本吻合;利用Thomas模型计算得到的平衡吸附量小于在静态下的平衡吸附量,这是由于在动态试验下的平衡时间短于静态试验下的平衡时间;应用pH=3的稀硝酸溶液可对吸附后涂铁滤料实现解吸,但不能全部解吸,静态试验下的解吸效果优于动态试验下的解吸。涂铁滤料吸附去除MB的机理包括物理吸附和化学吸附,以化学吸附为主;物理吸附主要包括静电吸附和范德华力吸附,化学吸附主要包括滤料表面配位络合反应和氢键的形成。
Red mud is the largest number of industrial hazardous waste in nonferrous metals industry of China and its output is more than 10 million ton every year.Red mud loss and lye leakage have brought severe pollution to farmland,river and groundwater.At present,effective ways of extensive utilization to red mud are not found and comprehensive utilization of red mud has become the bottleneck limiting the fast development of aluminum industry in China.Most oilfields adopt water reinjection process from oil field produced water to drive oil from strata in China. Pollutants in oil field produced water,such as oil,iron,suspend substance, microorganism,and so on,will lead to formation plugging,pipeline jam and corrosion and production cost rising.Effluent quality treated by available process can not meet with the Al quality standards of recommended indexes in SY/T5329-94 about the injection water quality for clastic rock oil fields in China.A huge quantity of dye wastewater is discharged by textile,paper,plastic and leather industries every year.As many dyes are complex organic contained azo and poly aromatic ring,which may cause people abnormal,cancerous and mutagenic,the removal of dyes from these wastewaters is a very important subject.Lots of dyes are resistant to oxidation and degradation,so adopting adsorbent to remove the dyes may be superior to other methods.The activated carbon is a very effective adsorbent, but its high price limits its extensive use.So,it is vital that lost-cost adsorbent should be prepared.However,researches on treatment of oil field produced water and dyes wasterwater by red mud are fewer and the studies on process and theory on treatment of oil field produced water and dyes wastewater by porous ceramics filter media based red mud are still expected to be carried out further.
In this paper,safe disposal of red mud will be combined with treatment of oil field produced water and dyes waster water in order to implement the target based on waste control by waste.According to filter material gradation demand in the filtration process,regulation study on volume density,apparent porosity and the balance of apparent porosity with crushing strength is going to be evolved. Superficial modification to porous ceramics filter materials based on red mud was first put forward with hydrogen-containing silicone oil,benzeneless ecological paint and ferric nitrate and related properties were characterized by test measures such as FTIR,SEM and XRD.Based on these,coagulation-coalescence filtration coupling process for oil field produced water and adsorption process for methylene blue were brought forward.At the same time,a series of researches on influencing factors about treatment effect,optimization of process operation parameters,pollutant removal mechanism and regeneration of modified filter material were made.The main achievements are as follows:
(1)Effect of pore-forming agent kinds,pore-forming agent addition,graded aggregate,graded pore-forming agent,firing temperature on apparent porosity, volume density and crush strength of filter material was studied.Coal was chosen as optimal pore-forming agent and the relation between coal addition with apparent porosity and volume density of filter material was linear.So,regulation to apparent porosity and volume density of filter media could be come true by coal addition.The relation between apparent porosity and crush strength of filter material accorded with quadratic curve.Thus,contradiction between apparent porosity and crush strength of filter material was conciliated by control to coal addition combining imitative straight line equation about coal addition and apparent porosity,which could make apparent porosity and crush strength a higher value.
(2)Superficial modification to porous ceramics filter materials based on red mud was first put forward with hydrogen-containing silicone oil,benzeneless ecological paint and ferric nitrate.After oleophylic and oleophobic modification, contact angles for water of patch test matrixes were from 25°to 138°and 6°, suggesting that oleophylic and oleophobic performance of filter material increased, which lead to the capacity increase of wet and collision coalescence of filter material. At last,oil removal rate in the oil field produced water rose by use of modified filter material.After modification with iron oxide compound,special surface area and iron overlay quantity of filter material were 4.987m~2/g,12.9016mg/g,respectively and its total pore volume increased from 0.005049cm~3/g to 0.01417cm~3/g.So,the adsorption capability of filter material was improved.
(3)The design was discussed on newly integrated and high efficiency oil removal equipment and coagulation-coalescence filtration coupling processes for oil field produced water were brought forward.Coagulation process parameters were optimized by parallel 6 beakers mixer.Design and operation parameters of newly integrated equipment were also optimized by small experiment,pilot test and productive field experiment.The results were that treatment efficiency was better integrated equipment than walnut shell filter of oil production team 22 of Jianhan Oilfield in China and effluent quality met with the Al quality standards(Oil content, SS,total iron content were less than 5mg/L,1mg/L,and 0.5mg/L,respectively). Mechanisms of oil removal included coagulation(which lead to demulsification of emulsified oil,and demulsifying oil was suspension or settlement),wetting adsorption coalescence of oleophylic filter material(when coalescing oil on filtration media arrived at some size and thickness,it would fall off from filtration media surface at water flow impact,at the same time,desquamated oil was intercepted between filtration media),collision coalescence of oleophobic filter material(Small size oil drop assembled to big size oil drop,which lead to oil floating upward or intercepted between filtration media)and synergistic effect of SS(Oil drop adhering to SS were intercepted between filtration media).SS removal mechanisms consisted of resistance interception,gravity sedimentation and contact flocculation.Major removal mechanisms of iron included settlement,interception based on filtration and adsorption.
(4)Effect of factors on adsorption removal of MB from aqueous solution using iron-oxide coated porous ceramics filter media(IOCPCFM)was investigated in batch mode and column mode.In batch mode,at pH=11,negative charge in IOCPCFM surface was favor of adsorption of MB which was positive ion;MB removal rate increased when adsorption time or initial concentration of MB increasing;isothermal adsorption experiment disclosed that temperature rise made for MB removal and adsorption isotherm presented S type fitted with Freundlich equation(R~2＞0.89);Thermodynamic research suggested that the adsorption of MB onto IOCPCFM was spontaneous,endothermic and chemical reaction which was further proved by the adsorption activation energy value;the pseudo-second-order rate model and the intraparticle diffusion model well described adsorption kinetics of MB onto IOCPCFM and adsorption rate limiting step was film diffusion.In column mode,breakthrough time of adsorption column was calculated and forecasted by BDST mode,and a good agreement was found between model predictions and experimental data;because equilibrium time of column mode was shorter, equilibrium adsorption capacity from Thomas was lower than that of batch mode; some desorption of IOCPCFM after adsorption was achieved by dilute nitric acid(pH=3)and desorption effect was better in batch mode;adsorption removal mechanisms of MB included physics adsorption and chemical adsorption and chemical adsorption was major,while physics adsorption consisted of static adsorption and van der waals force adsorption,at the same time,chemical adsorption was composed of surface coordination-complex reaction and hydrogen bond formation.
本文基于将赤泥的安全处置与油田采出水、印染废水的处理结合起来,实现以废治废的目标。首先根据过滤工艺对滤料级配的要求,展开对赤泥质多孔陶瓷滤料的体积密度、气孔率及气孔率与滤料压碎强度平衡的调控研究;首次提出用含氢硅油、无苯生态漆和硝酸铁对赤泥质多孔陶瓷滤料进行表面改性,以分别提高滤料的亲油、疏油和吸附性能,并用FTIR、SEM、XRD等测试手段对相关性能进行了表征;在此基础上提出了用混凝-聚结过滤耦合工艺处理油田采出水和吸附工艺处理亚甲基蓝印染废水,并对影响处理效果的因素、工艺操作参数的优化、污染物去除机理、改性滤料再生展开了一系列研究。主要的研究成果如下:
(1)以添加成孔剂工艺展开了成孔剂种类、加入量、骨料粒径、成孔剂粒径、烧成温度对赤泥质多孔陶瓷滤料的显气孔率、体积密度、压碎强度影响的研究,确定了煤粉为最佳成孔剂,煤粉加入量与赤泥质多孔陶瓷滤料的显气孔率、体积密度成线性关系,因此通过控制煤粉加入量便可实现对多孔陶瓷滤料显气孔率及体积密度的调控。陶瓷滤料显气孔率与压碎强度符合二次曲线关系。因此结合煤粉加入量和陶瓷滤料显气孔率的拟合直线方程便可通过调节煤粉加入量来平衡滤料的显气孔率与抗压强度之间的矛盾,从而获得使显气孔率高且压碎强度也大的多孔陶瓷滤料。
(2)首次对赤泥质多孔陶瓷滤料进行亲油、疏油、涂铁改性。实验结果显示,对赤泥质多孔陶瓷滤料亲油、疏油改性后,其片状测试基体对水的接触角分别为138°、6°,而没有改性的为25°,因而改性滤料的亲油和疏油性得到提高。从而亲油滤料、疏油滤料对油田采出水中油分的湿润聚结和碰撞聚结的能力增强,使得改性滤料的除油率提高。赤泥质多孔陶瓷滤料经涂铁改性后,滤料表面含铁量最高达12.9016mg/g滤料,比表面积为4.987m~2/g,比改性前增加了3.28倍,总孔隙体积由0.005049cm~3/g增至0.01417 cm~3/g,因而改性滤料的吸附性能得到提高。
(3)探讨并确定了新型一体化高效除油装置设计的方案,提出了处理油田采出水的混凝-聚结过滤耦合工艺,利用TS6六联烧杯搅拌机优化了混凝操作参数,通过小试、中试、生产性现场实验优化了新型一体化高效除油装置的设计及操作参数,从而使处理效果明显优于江汉油田采油22队的核桃壳过滤器,出水水质达到A1标准(含油量＜5mg/L、悬浮物＜1.0mg/L、总铁含量＜0.50mg/L),并确定了滤料反洗的操作参数。除油机理主要包括混凝破乳悬浮沉降、亲油滤料表面湿润吸附去除(当亲油滤料表面的油滴长大到一定程度时,它在水力冲击下会从滤料表面脱落而被滤料拦截,而滤料表面得到一定程度更新又会湿润吸附小油滴)、疏油滤料的碰撞聚结去除(小油滴通过碰撞聚结成大油滴上浮或被滤料拦载)和悬浮物协同去除(粘附在SS上的油滴也随SS被滤料拦截去除);悬浮物(SS)去除的机理主要分为阻力截留、重力沉降、接触絮凝三个方面;铁去除的机理主要为沉降、过滤拦截、吸附。
(4)通过静态试验和动态试验考察了涂铁改性滤料吸附去除模拟亚甲基蓝溶液的效果及各种因素对吸附效果的影响。在静态试验中,当pH=11时,涂铁滤料表面带负电荷而有利于带正电荷的MB离子的静电吸附,随着吸附时间增加、MB初始浓度增大,MB去除率增加;等温吸附试验表明,升高温度有利于MB去除,吸附等温线呈“S”型,符合Freundlich等温方程(R~2＞0.89);热力学研究表明涂铁滤料吸附MB是自发的吸热反应,吸附活化能为16.1445kJ/mol,大于8kJ/mol,说明涂铁滤料吸附MB以化学吸附为主;吸附动力学研究表明可用准二级动力学方程和颗粒内扩散方程来描述吸附动力学,吸附速率限制步骤为膜扩散。在动态试验中,利用BDST模型计算和预测了吸附柱的穿透时间,预测值与实验值基本吻合;利用Thomas模型计算得到的平衡吸附量小于在静态下的平衡吸附量,这是由于在动态试验下的平衡时间短于静态试验下的平衡时间;应用pH=3的稀硝酸溶液可对吸附后涂铁滤料实现解吸,但不能全部解吸,静态试验下的解吸效果优于动态试验下的解吸。涂铁滤料吸附去除MB的机理包括物理吸附和化学吸附,以化学吸附为主;物理吸附主要包括静电吸附和范德华力吸附,化学吸附主要包括滤料表面配位络合反应和氢键的形成。
Red mud is the largest number of industrial hazardous waste in nonferrous metals industry of China and its output is more than 10 million ton every year.Red mud loss and lye leakage have brought severe pollution to farmland,river and groundwater.At present,effective ways of extensive utilization to red mud are not found and comprehensive utilization of red mud has become the bottleneck limiting the fast development of aluminum industry in China.Most oilfields adopt water reinjection process from oil field produced water to drive oil from strata in China. Pollutants in oil field produced water,such as oil,iron,suspend substance, microorganism,and so on,will lead to formation plugging,pipeline jam and corrosion and production cost rising.Effluent quality treated by available process can not meet with the Al quality standards of recommended indexes in SY/T5329-94 about the injection water quality for clastic rock oil fields in China.A huge quantity of dye wastewater is discharged by textile,paper,plastic and leather industries every year.As many dyes are complex organic contained azo and poly aromatic ring,which may cause people abnormal,cancerous and mutagenic,the removal of dyes from these wastewaters is a very important subject.Lots of dyes are resistant to oxidation and degradation,so adopting adsorbent to remove the dyes may be superior to other methods.The activated carbon is a very effective adsorbent, but its high price limits its extensive use.So,it is vital that lost-cost adsorbent should be prepared.However,researches on treatment of oil field produced water and dyes wasterwater by red mud are fewer and the studies on process and theory on treatment of oil field produced water and dyes wastewater by porous ceramics filter media based red mud are still expected to be carried out further.
In this paper,safe disposal of red mud will be combined with treatment of oil field produced water and dyes waster water in order to implement the target based on waste control by waste.According to filter material gradation demand in the filtration process,regulation study on volume density,apparent porosity and the balance of apparent porosity with crushing strength is going to be evolved. Superficial modification to porous ceramics filter materials based on red mud was first put forward with hydrogen-containing silicone oil,benzeneless ecological paint and ferric nitrate and related properties were characterized by test measures such as FTIR,SEM and XRD.Based on these,coagulation-coalescence filtration coupling process for oil field produced water and adsorption process for methylene blue were brought forward.At the same time,a series of researches on influencing factors about treatment effect,optimization of process operation parameters,pollutant removal mechanism and regeneration of modified filter material were made.The main achievements are as follows:
(1)Effect of pore-forming agent kinds,pore-forming agent addition,graded aggregate,graded pore-forming agent,firing temperature on apparent porosity, volume density and crush strength of filter material was studied.Coal was chosen as optimal pore-forming agent and the relation between coal addition with apparent porosity and volume density of filter material was linear.So,regulation to apparent porosity and volume density of filter media could be come true by coal addition.The relation between apparent porosity and crush strength of filter material accorded with quadratic curve.Thus,contradiction between apparent porosity and crush strength of filter material was conciliated by control to coal addition combining imitative straight line equation about coal addition and apparent porosity,which could make apparent porosity and crush strength a higher value.
(2)Superficial modification to porous ceramics filter materials based on red mud was first put forward with hydrogen-containing silicone oil,benzeneless ecological paint and ferric nitrate.After oleophylic and oleophobic modification, contact angles for water of patch test matrixes were from 25°to 138°and 6°, suggesting that oleophylic and oleophobic performance of filter material increased, which lead to the capacity increase of wet and collision coalescence of filter material. At last,oil removal rate in the oil field produced water rose by use of modified filter material.After modification with iron oxide compound,special surface area and iron overlay quantity of filter material were 4.987m~2/g,12.9016mg/g,respectively and its total pore volume increased from 0.005049cm~3/g to 0.01417cm~3/g.So,the adsorption capability of filter material was improved.
(3)The design was discussed on newly integrated and high efficiency oil removal equipment and coagulation-coalescence filtration coupling processes for oil field produced water were brought forward.Coagulation process parameters were optimized by parallel 6 beakers mixer.Design and operation parameters of newly integrated equipment were also optimized by small experiment,pilot test and productive field experiment.The results were that treatment efficiency was better integrated equipment than walnut shell filter of oil production team 22 of Jianhan Oilfield in China and effluent quality met with the Al quality standards(Oil content, SS,total iron content were less than 5mg/L,1mg/L,and 0.5mg/L,respectively). Mechanisms of oil removal included coagulation(which lead to demulsification of emulsified oil,and demulsifying oil was suspension or settlement),wetting adsorption coalescence of oleophylic filter material(when coalescing oil on filtration media arrived at some size and thickness,it would fall off from filtration media surface at water flow impact,at the same time,desquamated oil was intercepted between filtration media),collision coalescence of oleophobic filter material(Small size oil drop assembled to big size oil drop,which lead to oil floating upward or intercepted between filtration media)and synergistic effect of SS(Oil drop adhering to SS were intercepted between filtration media).SS removal mechanisms consisted of resistance interception,gravity sedimentation and contact flocculation.Major removal mechanisms of iron included settlement,interception based on filtration and adsorption.
(4)Effect of factors on adsorption removal of MB from aqueous solution using iron-oxide coated porous ceramics filter media(IOCPCFM)was investigated in batch mode and column mode.In batch mode,at pH=11,negative charge in IOCPCFM surface was favor of adsorption of MB which was positive ion;MB removal rate increased when adsorption time or initial concentration of MB increasing;isothermal adsorption experiment disclosed that temperature rise made for MB removal and adsorption isotherm presented S type fitted with Freundlich equation(R~2＞0.89);Thermodynamic research suggested that the adsorption of MB onto IOCPCFM was spontaneous,endothermic and chemical reaction which was further proved by the adsorption activation energy value;the pseudo-second-order rate model and the intraparticle diffusion model well described adsorption kinetics of MB onto IOCPCFM and adsorption rate limiting step was film diffusion.In column mode,breakthrough time of adsorption column was calculated and forecasted by BDST mode,and a good agreement was found between model predictions and experimental data;because equilibrium time of column mode was shorter, equilibrium adsorption capacity from Thomas was lower than that of batch mode; some desorption of IOCPCFM after adsorption was achieved by dilute nitric acid(pH=3)and desorption effect was better in batch mode;adsorption removal mechanisms of MB included physics adsorption and chemical adsorption and chemical adsorption was major,while physics adsorption consisted of static adsorption and van der waals force adsorption,at the same time,chemical adsorption was composed of surface coordination-complex reaction and hydrogen bond formation.
引文
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