摘要
作为一类新型分离介质,无机陶瓷分离膜具有高聚物膜无法比拟的诸多优点,如分离效率高、耐高温、结构稳定性高、低能耗和易于清洗再生等,日益广泛应用于食品工业、医药、冶金、生物技术、环境工程等工业分离过程,是一个方兴未艾的高技术产业领域。随着大批量废液处理、强酸碱介质分离和高温热冲击分离等环境应用对陶瓷膜的强烈需求,商品化的多孔陶瓷分离膜存在诸多问题,如成本高、材质品种少、应用范围窄等,严重影响其大规模工业化应用。本论文从陶瓷分离膜的低成本化、特殊环境应用(高温和强酸碱应用)等角度出发,侧重于研究低成本多孔陶瓷分离膜的制备和性能表征,发展了若干具有实用价值的新型低成本多孔陶瓷分离膜,并依据其性能研究拓展了应用范围,如强酸强碱液体分离、高温气体除尘和收尘等,取得了阶段性成果。主要包括如下几个方面:
1.管状多孔堇青石陶瓷膜支撑体的制备与性能研究
作为经典陶瓷材料的堇青石(2MgO_2·Al_2O_3·5SiO_2)有诸多优点,尤其是低的热膨胀系数,多应用于耐火材料和汽车尾气催化剂载体,据称,日本科技界将其应用于多孔陶瓷的制备,但具体制备过程未见相关文献报道。
本工作研究了堇青石多孔陶瓷膜管的挤出成型制备过程,详尽考察了其耐酸碱腐蚀性能和腐蚀机理。以大颗粒工业堇青石为原料,运用挤出成型-烧结工艺,详细研究了烧结温度对管状支撑体C-1的孔径及分布、孔隙率、机械强度、渗透性能和热膨胀系数等性能的影响,并比较了不同粒径粉体所制备的支撑体的孔隙率、孔径及渗透通量等主要性质,在优化的工艺制度下,分别制得平均孔径为8.66-9.49μm(C-1样品)和17.03-19.24μm(C-2样品)的多孔陶瓷膜管,进而亦可作为制备微滤膜和超滤膜的载体。
为实现特殊环境应用,考察所制备的堇青石多孔陶瓷膜管C-1样品(平均孔径为8.66μm)和商业氧化铝支撑体(平均孔径为2.96μm)的耐酸碱腐蚀性能,对其腐蚀机理进行分析。结果表明,经过10 wt%NaOH溶液4 h的腐蚀,堇青石陶瓷膜管耐酸碱性能好,孔结构变化较小,强度损失率也仅为8.16%,远小于氧化铝膜管的73.6%,这样的结果国际上尚未见报道。相反地,经过强酸的腐蚀(如20wt%H_2SO_4溶液4 h),堇青石陶瓷膜管强度损失率为57.87%,而耐强酸的腐蚀氧化铝陶瓷膜管的仅为3.56%。
因此,商品化氧化铝支撑体宜于处理强酸介质,与之相比,耐强碱腐蚀的低膨胀堇青石陶瓷膜管由于原料廉价易得,烧结温度低,更适合大规模地应用于处理强碱性介质和高温气-固、液-固分离等领域。本研究有望填补多孔陶瓷分离膜在强碱苛性介质分离应用和高温环境应用中的空白。
2.多孔莫来石陶瓷膜支撑体的制备研究
莫来石(3Al_2O_3·2SiO_2)为硅铝酸系中唯一稳定存在的晶相,具有许多独特的优点,是一种优良的结构陶瓷。将其应用于多孔陶瓷膜的制备却少有文献报道。
第一部分,以廉价易得的工业莫来石粉体为主要原料,以碱式碳酸镁和高岭土混合物为添加剂,研究了烧结温度、成孔剂、添加剂对多孔莫来石烧结特性、相组成和孔结构等性能的影响,在1500℃优化烧结温度下,制备了平均孔径为26.21μm、热膨胀系数为6.24×10~(-6)℃~(-1)的低成本莫来石多孔陶瓷。
在国际上,首次以具有“粉煤灰核-氢氧化铝壳”微结构的莫来石前驱体为主要原料,运用反应烧结技术制备出微结构可控的多孔莫来石,详细研究了烧结过程中样品的相转变机理和烧结行为。淀积氢氧化铝涂层,只是适当地提高莫来石多孔陶瓷的烧成温度,却能够获得以下诸多优点:a.拓宽烧结体的烧结温度范围;b.使得烧结体微结构更易控制;c.消除方石英有害相;d.提高烧结体中莫来石相的浓度。本研究解决了粉煤灰多孔陶瓷烧结温度窄、微结构难以控制、易产生有害相和高温烧结时易发泡变形等科学难点,不仅获得了低成本的多孔陶瓷支撑体,也为工业废物的环境治理、高附加值应用提供了一条切实可行的途径。
3.以粉煤灰为原料的管状堇青石微滤膜的制备研究
商品化多孔陶瓷分离膜不能满足大批量地处理废液、高温气-固和液-固分离等环境应用的需求。为此,本工作以上述堇青石陶瓷管(平均孔径:18.00um,开孔隙率:41.40%)为支撑体,在国际上首次利用粉煤灰原位合成结晶相可控的非对称堇青石多元氧化物陶瓷膜。
我们使用球状工业废弃物粉煤灰,辅以少量碱式碳酸镁作为氧化镁源,利用浸涂-喷涂工艺成功地制备非对称堇青石微滤膜。研究了制备过程中烧结膜层的开裂机理及解决措施,膜层结晶相的转变机理和多孔微结构的控制因素,并对微滤膜的气体渗透性能和渗透机理进行了初步分析。研究表明,优化原材料组分是减少膜层开裂的有效措施,在1100℃低温下即可形成堇青石相,在所研究的烧结温度范围内,制备出平均孔径3.6-6.4μm堇青石微滤膜,0.15 MPa平均压力下,氮气渗透性为(7.52-9.82)×10~4 m~3·m~(-2)·h~(-1)·MPa~(-1)。高的氮气渗透通量使得膜内渗透阻力大大降低,加上低的制备成本,有望应用于大批量地预处理含尘热气体和工业废液预处理等分离领域。
4.以天然沸石为原料的管状陶瓷微滤膜的制备与表征
天然沸石矿物由于具有丰富的内部活性微孔,以颗粒形式广泛用于吸附和离子交换领域。本实验室前期工作将其用于多孔分离膜的制备,将活性微孔和粒间堆积孔结合起来,成功发展了具有离子交换和分离耦合功能的天然沸石基矿物多孔支撑体。
为发展更具实用价值的低成本矿物膜,我们以廉价、矿藏丰富的片沸石(Ca[Al_2Si_7O_(18)]·6H_2O)矿物为原料,在管状多孔矿物支撑体上利用悬浮粒子浸涂工艺制备了三层结构的矿物微滤膜。系统研究了制备过程各工艺参数的影响,如粉体的分级,膜层的形成和烧结。XRD结果表明,膜层结晶相组成与烧结温度密切相关,最终膜层主晶相为石英和钠长石;从SEM结果可看出,膜层内矿物粒子在碱、碱土金属氧化物助熔剂作用下,850℃开始烧结。优化的烧结温度范围内(850-950℃),中间层的平均孔径为0.69-1.10μm,以此为支撑体制备出平均孔径为0.54μm的顶层膜。0.1 MPa膜端压和室温条件下,非对称三层膜的氮气通量和纯水通量分别为1.96×10~5 1·m~(-2)·h~(-1)·bar~(-1)和3.20×10~3 1·m~(-2)·h~(-1)·bar~(-1)。所制备的矿物基陶瓷分离膜制备成本低,适合应用于大规模分离中性介质,为液体分离陶瓷膜增加了新品种,也将引起开发矿物材料的技术革新。
5.低成本陶瓷膜材料莫来石的合成及性能表征
从某种意义上说,陶瓷支撑体材料的选择和合成是无机陶瓷膜研究的基础。本工作首次以廉价、矿藏丰富的富铝矿物-天然铝矾土作为氧化铝源,来代替工业氧化铝,进行陶瓷膜材料莫来石的合成研究。详尽研究了铝矾土、粉煤灰和基于3:2莫来石的混合物的相变机理和烧结特性。结果表明,≤1300℃,方石英和刚玉通过固态反应二次莫来石化,在更高的温度,刚玉熔于短暂玻璃相中进一步发展了二次莫来石化;二次莫来石化导致样品的体积膨胀,而非烧结收缩。此外,对不同温度烧结样品的性质,如相对致密度、孔隙率、微结构、热及机械性能进行了表征。在1600℃优化的烧结温度下,样品的相对致密度和抗弯强度分别为93.94%和186.19 MPa,烧结体中仅有少量的闭气孔存在。1600℃莫来石烧结样品在强酸强碱热溶液中表现出较好的耐腐蚀性能,其腐蚀过程可分为两个阶段:快速阶段(0-5 h)和低速阶段(5-20 h),这分别对应于表面腐蚀和体腐蚀过程。
合成低成本、高性能的莫来石陶瓷体材料,然后经过粉碎分级,以作为制备多孔陶瓷膜,尤其是多孔陶瓷支撑体的原材料,这样的研究对于陶瓷膜制备领域,也有重大的意义和价值。
As a type of novel separation media,inorganic ceramic separation membranes exhibit more merits than their high polymer counterparts,such as high separation efficiency,good high temperature resistance,good structural stability,low energy consumption and easy clean-regeneration.As a result,they are increasingly applied in many industrial separation fields,including food industry,medical industry, metallurgy,bio-technology.With the strong environmental demands for ceramic membranes nowadays,such as massive liquid waste treatment,strong acidic or alkali media separation and high temperature thermal shock applications,commercialized porous ceramic separation membranes could not be used on a large scale in industry due to their several drawbacks,such as high cost,rare membrane materials and narrow application range.Accordingly,in my Ph.D dissertation work,the efforts were focused on the investigation of preparation and performance characterization of low cost porous ceramic membranes based on the needs of lowering cost and meeting the specific environmental applications(high temperature,strong acidic or alkali applications).Several cost-effective novel porous separation membranes with applied value have been developed.And the application performances were also studied from the viewpoint of extending application fields,for example,separation of strong acidic or alkali liquids and the removal or recovery of solids from powder-containing hot gas. Some phasic achievements have been obtained.The work in this dissertation can be described briefly as follows.
1.Preparation and performance investigation of tubular porous cordierite ceramic membrane supports
As a classic ceramic material,cordierite(2MgO_2·Al_2O_3·5SiO_2)is usually applied in the fields of refractory products and automobile exhaust catalyst carriers due to its many advantages,especially low thermal expansion co-efficient.It is said that in Janpan' scientific and technical community cordierite has been used in the preparation of porous ceramics.However,specific preparation process has not been reported in the relevant literatures.
In this work,the preparation process of cordierite ceramic membrane tubes was studied.The corrosion performances and the corresponding mechanism were also studied in detail.Low cost commercial grade coarse cordierite powders were used as the starting materials,while the "extrusion-sintering" process was adopted.The effects of sintering temperature on pore size and its distribution,porosity,mechanical strength,permeation flux and thermal expansion coefficient were studied in detail. The main properties(porosity,pore size and permeation flux)of these two supports prepared from different powders were compared.Under the optimized process system, two tubular ceramic membrane tubes with average pore sizes of 8.66-9.49μm and 17.03-19.24μm were prepared respectively.Furthermore,these porous tubes could be used as the supports for the preparation of micro-filtration or ultra-filtration membranes.
To verify the practicability in the specific environmental applications,the acidic and alkali corrosion resistance tests were carried out for the fabricated cordierite tubes C-1(average pore size:8.66μm)and the commercial alumina supports(average pore size:2.96μm).In particular,their corrosion mechanisms were analyzed.The results indicated that,after 10 wt%NaOH solution corrosion for 4 h,the alkali-resistant cordierite ceramic membrane tubes exhibited a slight change in pore-structure,and lower strength loss ration(8.16%)than the alumina supports(73.6%).This has not been reported in international research community.On the contrary,after the acid corrosion(for example,20 wt.%H_2SO_4 solution for 4 h),the strength loss ratio of the cordierite ceramic membrane tubes was 54.87%,while that of acid-resistant alumina ceramic tubes is only 3.56%.
Therefore,the commercial alumina supports are suitable for the treatment of strong acidic liquids.By comparison,due to cheap and abundant raw materials and low sintering temperature,the fabricated alkali-resistant cordierite supports with low expansion co-efficient are expected to have potential large-scale applications in the pre-treatment of strong alkali media and high temperature solid-gas or liquid-solid separation.This study is expected to fill the research blank of the environmental application of porous ceramic membrane in the separation of alkali caustic media and high temperature hot gas.
2.Preparation investigation of porous mullite ceramic membrane supports
Mullite(3Al_2O_3·2SiO_2)is the only stable existing phase for the Si-Al system.As an excellent structural ceramic,it shows many unique advantages.However,the use of mullite for the porous ceramic membrane preparation is rarely reported in the literatures.
In the first part,industrial coarse mullite was used as the aggregate materials while the mixture of kaolin and basic carbonate magnesium as additive.The influences of sintering temperature,pore-forming agent,additives on the properties of the porous mullite were studied,such as sintering characteristics,phase composition and pore structure.At the optimized sintering temperature of 1500℃,low-cost porous mullite ceramics with average pore size of 26.21μm and thermal expansion co-efficient of 6.24×10~(-6)℃~(-1)were prepared.
In the second part,for the first time,the porous mullite ceramic membrane supports with controllable micro-structure were prepared from the mullite precursors(fly ash core and aluminum hydroxide shell)by the reaction sintering technique.The phase transition mechanism and sintering behavior were studied in detail during the course of heat treatment.Although there is a slight increase in sintering temperature for porous mullite,some advantages could be still achieved as follows:a.extension of sintering temperature range;b.easier control of micro-structure of the sintered bodies; c.consumption of harmful phase cristobalite;d.increase in the phase concentration of mullite.This study solved the scientific difficulties for the sintering of fly ash porous ceramic,such as narrow sintering temperature range,difficult control of micro-structure,production of harmful phase and foam/deformation during high-temperature sintering.This not only has access to obtain the low-cost porous ceramic supports,but also provides a feasible practical way for high value-added utilization and environmental governance of industrial waste.
3.Preparation investigation of tubular cordierite micro-filtration membranes with fly ash as the main starting materials
Commercialized porous ceramic membrane can not meet the demands for environmental applications,such as the large-scale waste liquid treatment, high-temperature gas-solid or liquid-solid separation.In the work,for the first time, low-cost asymmetric cordierite multiple-oxide porous membranes with controllable crystalline phases were in situ synthesized using fly ash as the main starting materials on the above-mentioned tubular supports(average pore size:18 um,open porosity: 41.40%).
Asymmetric cordierite-based porous ceramic micro-filtration membranes were prepared using spherical industrial waste fly ash as the starting materials with basic magnesium carbonate as source of magnesium by the spray-coating/dip-coating process.Crack-forming mechanism of membrane layer and the corresponding dissolution method,phase transition mechanism and the control factors of micro-structure were studied during the preparation process.Also,the gas permeation performances and permeation mechanism were preliminarily studied.Optimization of the raw materials ratio was found to be necessary to avoid crack formation during sintering.The results also confirm thatα-cordierite was formed above 1100℃,and that the optimized sintering temperature range(1150-1200℃),cordierite-based porous membranes showed average pore size in the range of 3.6-6.4μm and nitrogen permeance of 7.52-9.82×10~4 m~3·m~(-2)·h~(-1)·MPa~(-1)under the average pressure of 0.15 MPa. Because the high nitrogen flux makes penetration resistance greatly reduced,also for low preparation cost,the fabricated membranes are expected to be applied in the massive pretreatment of dust-containing hot gas and waste liquids.
4.Fabrication and characterization of tubular micro-filtration mineral membranes from natural zeolite
The natural zeolite granulars are widely used in the fields of adsorption and ion-exchange because of its abundant active micro-pores.However,natural zeolite was applied to membrane preparation in our previous work.The narural zeolite-based porous mineral supports with coupling function of separation an ion-exchange have been successfully developed based on the combination of active micro-pores and the gaps between the accumulated particles.
In order to develop low-cost mineral membranes with applied value,tri-layer mineral micro-filtration membranes have been fabricated on tubular porous mineral supports by dip-coating using cheap and abundant natural Heulandite (Ca[Al_2Si_7O_(18)]·6H_2O)mineral as the starting materials.The influence of the parameters during the preparation process,including the powder classification,the forming and sintering of membranes,was systematically studied.The XRD results reveals that the phase compositions of the membranes were related to the sintering temperature and the final major phases were almost quartz and albite.SEM studies subsequently indicate that solids in the membrane begun to sinter at about 850℃with alkali metal oxides as the aid fluxes.The inter-layers with average pore size in the range of 0.69-1.10μm were obtained at the optimum firing temperature(850- 950℃).Then,the top-layer membrane with average pore size of 0.54μm could be prepared on the above support.Nitrogen gas permeation flux and pure water permeation flux of the resulting tri-layer membranes are 1.96×10~5l·m~(-2)·h~(-1)·bar~(-1)and 3.20×10~3l·m~(-2)·h~(-1)·bar~(-1),respectively,with the trans-membrane pressure of 0.1 MPa at room temperature.The prepared mineral ceramic membranes with low preparation cost are suitable for the large-scale separation of neutral medium.This not only added a new species for liquid separation ceramic membranes,but will lead to the technological innovations for the development of mineral materials.
5.Synthesis and property characterization of low-cost ceramic membrane materials-mullite
In a sense,the choice and synthesis of the ceramic support material are the basis for the inorganic ceramic membrane study.In the work,low cost mullite ceramics were for the first time prepared with natural bauxite as resource of alumina,which is a cheap and abundant substitute material for industrial grade alumina.The fired samples, including fly ash,bauxite and their mixture based on the composition of 3:2 mullite, were studied in terms of phase development mechanism and sintering characteristics. The results indicate that the secondary mullitization occurred by the solid state reaction of cristobalite and corundum below 1300℃,followed by the dissolution of corundum into transitory glassy phase at higher temperatures.The dilatometric results reveal that the formation of secondary mullite resulted in slight expansion despite of the shrinkage induced by sintering.In addition,the samples were fired at elevated temperatures and then characterized in terms of relative density,porosity, micro-structure and thermal and mechanical performances.At the optimized sintering temperature of 1600℃,the relative density and bending strength are 93.94%and 186.14 MPa,respectively.Only a small amount of nearly spherical closed pores were observed in the sintered body.The 1600℃sintered mullite samples exhibited better corrosion resistant performance in the strong acid or alkali solutions.The corrosion process can be divided into two stages:high-speed stage(0-5h)and low-speed stage (5-20 h),which was respectively corresponded with the surface corrosion and bulk corrosion process.
The synthesized low-cost,high-performance mullite ceramic materials is suitable for the preparation of porous ceramic membranes,in particular the porous ceramic membrane supports after size reduction for classification.The study is of great significance and value for ceramic membrane preparation field.
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