本文選題：冷凍塑形 + 水泥膜��； 參考：《中國(guó)海洋大學(xué)》2015年碩士論文

【摘要】：水泥是一種粉狀水硬性無(wú)機(jī)膠凝材料,其與水充分?jǐn)嚢韬笮纬烧吵淼臐{料,在空氣中或水中能夠發(fā)生水化反應(yīng)并且可以將砂石等粗細(xì)骨料粘結(jié)在一起,形成一種強(qiáng)度較高且能抵抗鹽水腐蝕的常用無(wú)機(jī)材料一混凝土。水泥是通過(guò)加熱煅燒粘土、石灰石或者其他類(lèi)似生料混合物,并輔以適量外加劑制備而成的。由于制備水泥所需的原材料成本低廉,購(gòu)置渠道廣泛,這使得水泥成為了世界上成本最低的無(wú)機(jī)材料之一。與此同時(shí),水泥基復(fù)合材料也是工業(yè)領(lǐng)域最重要和最多樣的建筑材料。水泥漿料不僅具有良好的流變性能,且能夠在一定的養(yǎng)護(hù)條件下發(fā)生水化反應(yīng),該反應(yīng)產(chǎn)生眾多的水化產(chǎn)物并成為水泥基復(fù)合材料的強(qiáng)度來(lái)源。與其他無(wú)機(jī)材料制備所需的工藝相比(燒結(jié)、煅燒),水泥的養(yǎng)護(hù)方法幾乎沒(méi)有成本與能耗,且工藝極為簡(jiǎn)便,是一種環(huán)保無(wú)污染的制備手段。多孔水泥基復(fù)合材料已被廣泛的應(yīng)用到各個(gè)領(lǐng)域之中,如人工骨骼替代,原油吸附,電磁干擾屏蔽,然而極少有報(bào)道涉及到關(guān)于制備定向多孔水泥基材料在分離領(lǐng)域中的應(yīng)用。無(wú)機(jī)多孔材料的制備方法有許多,如發(fā)泡法、等靜壓法、造孔劑溶出法、固態(tài)粒子高溫氣化法等。其中造孔劑溶出法也被稱作粒子溶出法,是通過(guò)造孔劑在溶液中的溶出的形式成孔,是一種制備三維多孔結(jié)構(gòu)的有效方法,常用于骨組織工程的搭建；固態(tài)粒子燒結(jié)法即高溫氣化法,它是通過(guò)在高溫下將造孔劑氣化的方式造孔,是制備多孔陶瓷的一種常見(jiàn)方法；冷凍塑形作為一種新興的制孔工藝,于近年來(lái)受到諸多科研人員的廣泛關(guān)注。通過(guò)改變幾個(gè)關(guān)鍵的制備要素,冷凍塑形法能夠制得不同孔徑大小及不同孔隙率范圍的多孔材料,更因所制備的孔道具有定向均勻排列的特性,最終使多孔材料具有良好的力學(xué)性能以及可觀的通量。本研究通過(guò)上述三種不同的制備方法研制了三種具有不同結(jié)構(gòu)的多孔材料,通過(guò)對(duì)他們的結(jié)構(gòu)與性能進(jìn)行表征分析后發(fā)現(xiàn),粒子溶出法所制備的多孔水泥基材料雖然具有可調(diào)控的孔隙率,但其所形成的孔道不連續(xù),通孔比例較小,孔徑尺寸較大(50μm～100μm),純水滲透性實(shí)驗(yàn)也說(shuō)明了其滲透性能較差。高溫氣化法制備的多孔水泥基材料雖然具有一定的孔隙率,但由于高溫處理時(shí)水泥基材料極易受到破壞,且致孔劑(淀粉)在氣化后所形成的孔道分布不均勻,孔道連續(xù)性較差,純水滲透性實(shí)驗(yàn)也證明其滲透性能極差。冷凍塑形工藝是一種制備具有定向孔道的水泥基復(fù)合多孔材料(水泥膜)的有效方法。該實(shí)驗(yàn)通過(guò)球磨將水或叔丁醇,有機(jī)粘結(jié)劑分散劑,硅酸鹽水泥充分混合攪拌均勻制得穩(wěn)定的水泥基混合漿料,通過(guò)冷凍塑形的方法將該漿料定向冷凍為凍坯,隨后將其置于冷凍干燥機(jī)內(nèi)使造孔劑揮發(fā)完全以得到素坯,最終使多孔水泥基素坯在一定養(yǎng)護(hù)條件下充分反應(yīng)得到定向多孔水泥基材料。本實(shí)驗(yàn)研究了水泥膜的各項(xiàng)性能與制備條件之間的關(guān)系,同時(shí)利用光學(xué)顯微鏡、掃描電子顯微鏡、壓汞儀、X射線衍射儀、抗壓強(qiáng)度測(cè)試儀、氮?dú)馕絻x、紫外吸收光譜儀等儀器設(shè)備對(duì)制備的水泥膜結(jié)構(gòu)性能進(jìn)行表征,最后利用自制膜評(píng)價(jià)儀對(duì)水泥膜的滲透性能及分離性能做了詳細(xì)研究。實(shí)驗(yàn)結(jié)果表明：冷凍塑形法成功的將水泥基復(fù)合材料制備成新型的定向多孔水泥膜：冷凍溫度、漿料固含量、養(yǎng)護(hù)周期都對(duì)水泥膜的結(jié)構(gòu)性能造成了不同的影響；孔道尺寸隨著冷凍溫度的下降、固含量的增加而減小,反之亦然;孔隙率隨著冷凍溫度的上升、固含量的減少而增加,反之亦然：由叔丁醇作為造孔劑制備所得的水泥膜在操作壓力為0.2MPa時(shí),對(duì)牛血清蛋白(BSA)的截留率達(dá)到74.8%,通量能保持在400 L·m-2·h-1到500 L·m-2·h-1。
[Abstract]:Cement is a hard powdery inorganic cementitious material, which is stirred with water to form a viscous slurry, which can be hydrated in the air or in water and can bind the coarse and fine aggregate, such as sand and stone, to form a concrete material with high strength and resistance to brine corrosion. The cement is calcined by heating. A mixture of clay, limestone, or other similar raw material, which is made up with an appropriate amount of admixture, is made up of an appropriate amount of admixture. Due to the low cost of the raw materials needed to prepare the cement and the wide channel of purchase, the cement has become one of the lowest cost inorganic materials in the world. At the same time, water mud matrix composites are also the most important and most important in the industrial field. The cement paste not only has good rheological properties, but also can produce hydration reaction under certain curing conditions. This reaction produces many hydrated products and becomes the strength source of cement based composites. Compared with other inorganic materials, the curing method of cement is almost no better than the other processes needed for the preparation of inorganic materials. The cost and energy consumption, and the process is very simple, is a kind of environmentally friendly and non pollution preparation means. Porous cement based composites have been widely used in various fields, such as artificial bone replacement, crude oil adsorption, electromagnetic interference shielding, but few reports involve the application of the preparation of directional porous cement-based materials in the field of separation. There are many methods for preparing inorganic porous materials, such as foaming, isostatic pressure, pore solution dissolution, solid particle high temperature gasification, etc., in which the dissolution method of pore making agent is also called particle dissolution method. It is an effective method to prepare three-dimensional porous structure by the form of pore forming agent in solution. It is often used in bone tissue engineering. The solid particle sintering method, the high temperature gasification process, is a common method for preparing porous ceramics by gasification of pore forming agents at high temperature. As a new hole making process, freezing molding has been widely used by many researchers in recent years. By changing several key preparation factors, freezing is frozen. The molding method can produce porous materials with different pore size and different porosity range, and the porous material has the characteristic of directional and uniform arrangement, and finally makes the porous material have good mechanical properties and good flux. In this study, three kinds of porous materials with different structures were developed by the three different preparation methods mentioned above. Material, after characterization and analysis of their structure and properties, it is found that the porous cement based material prepared by the particle dissolution method has a controllable porosity, but its pore channel is discontinuous, the pore size is small and the pore size is larger (50 to 100 m to 100 mu). The permeability test of pure water also shows that its permeability is poor. Although the porous cement based material prepared by gasification has a certain porosity, the cementitious material is easily damaged due to high temperature treatment, and the pore distribution of the pore agent (starch) is not uniform after gasification, and the continuity of the pore is poor. The permeability experiment of pure water shows that the permeability is very poor. The cryopreservation process is a kind of system. An effective method for preparing cement based composite porous material (cement film) with a directional channel. The experiment is made by ball milling to produce a stable cement based mixture of water or TERT butanol, organic binder dispersant and Portland cement. The slurry is frozen into a freeze-blank by the method of freezing and shaping, and then it is placed. In the freeze dryer, the pore forming agent is volatilized completely to get the plain billet, and the porous cement base billet is finally reacted to the porous cement-based material under certain curing conditions. The relationship between the properties of the cement film and the preparation conditions is studied in this experiment. At the same time, the optical microscope, scanning electron microscope, mercury injection instrument and X ray are used. Diffractometer, compressive strength tester, nitrogen adsorption apparatus, ultraviolet absorption spectrometer and other instruments and equipment to characterize the structure and properties of the prepared cement film. Finally, the permeability and separation properties of the cement film were studied in detail by the self-made membrane evaluator. The experimental results showed that the cold plastic method successfully prepared the cement matrix composite. The new directional porous cement film: freezing temperature, slurry solid content and curing period have different effects on the structure and properties of the cement film. The pore size decreases with the decrease of freezing temperature, the increase of solid content, and vice versa; the porosity increases with the rise of freezing temperature and the decrease of solid content, and vice versa: vice versa. The retention of bovine serum protein (BSA) is 74.8% when the operation pressure is 0.2MPa, and the flux can be maintained at 400 L. M-2. H-1 to 500 L. M-2. H-1.
【學(xué)位授予單位】：中國(guó)海洋大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類(lèi)號(hào)】：TU528

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