TWI631986B - Titanium dioxide nanotube adsorbent for water treatment and the preparation method thereof - Google Patents
Titanium dioxide nanotube adsorbent for water treatment and the preparation method thereof Download PDFInfo
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Abstract
本發明提供一種用於水處理之二氧化鈦奈米管吸附劑及其製備方法，其流程係包括：提供二氧化鈦粉末，其次，將二氧化鈦粉末配製為二氧化鈦溶液，並經過水熱法來製成二氧化鈦奈米管吸附劑，藉以形態之改變而增大比表面積，並且二氧化鈦奈米管吸附劑可以在構成溶液的製程中，混合附載石墨烯的磁性顆粒溶液，在經由水熱法而製成附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑， 以提昇吸附能力，在處理水中的重金屬確具有較佳的效能。The invention provides a titanium dioxide nano tube adsorbent for water treatment and a preparation method thereof, the process comprising: providing titanium dioxide powder, and secondly, preparing titanium dioxide powder into a titanium dioxide solution, and hydrothermally preparing titanium dioxide nanometer The tube adsorbent increases the specific surface area by the change of the morphology, and the titanium dioxide nanotube adsorbent can mix the magnetic particle solution carrying the graphene in the process of forming the solution, and the graphene is attached by hydrothermal method. The magnetic particles of the titanium dioxide nanotube adsorbent, in order to enhance the adsorption capacity, the heavy metal in the treated water does have better performance.
Description
本發明係關於一種用於水處理之二氧化鈦奈米管吸附劑及其製備方法，其係涉及於水處理工程的技術領域，尤指製備出二氧化鈦奈米管吸附劑來吸附水中重金屬而降解水污染物的方法。The invention relates to a titanium dioxide nano tube adsorbent for water treatment and a preparation method thereof, relating to the technical field of water treatment engineering, in particular to preparing a titanium dioxide nano tube adsorbent to adsorb heavy metals in water and degrading water pollution. The method of things.
按由重金屬一般係以天然濃度廣泛存在於自然界中，但是由於人類對重金屬的開採、冶煉、加工及商業製造活動日益增多，造成不少如鉛、鎘、鈷、砷等重金屬進入大氣、水、土壤中，引起不可輕忽的環境污染問題。以各種化學形態存在的重金屬，在進入環境或生態系統之後就會留存、累積和遷移以致有危害，重金屬通過大氣、水、食物進入人體，尤其是水，如能將其重金屬有害性有效降低甚至解除、處理、回收，乃是重要課題。Heavy metals generally exist in nature in natural concentrations. However, due to the increasing exploitation, smelting, processing and commercial manufacturing activities of heavy metals, many heavy metals such as lead, cadmium, cobalt and arsenic enter the atmosphere and water. In the soil, it causes environmental pollution problems that cannot be ignored. Heavy metals in various chemical forms will survive, accumulate and migrate after entering the environment or ecosystem. Heavy metals can enter the human body through the atmosphere, water and food, especially water, which can effectively reduce the harmfulness of heavy metals. Disarming, handling, and recycling are important issues.
有鑑於此，本發明人潛心構思並深入研究，終於創作出一種用於水處理之二氧化鈦奈米管吸附劑及其製備方法。In view of this, the inventors have conceived and intensively studied, and finally created a titanium dioxide nanotube adsorbent for water treatment and a preparation method thereof.
本發明提供一種用於水處理之二氧化鈦奈米管吸附劑及其製備方法，其主要目的係製出二氧化鈦奈米管，藉其構成中孔洞材料而顯著增加比表面積大，來提高吸附重金屬的效能。The invention provides a titanium dioxide nano tube adsorbent for water treatment and a preparation method thereof, the main purpose of which is to produce a titanium dioxide nano tube, which can significantly increase the specific surface area by forming a medium pore material, thereby improving the efficiency of adsorbing heavy metals. .
為達前述目的，本發明用於水處理之二氧化鈦奈米管吸附劑及其方法，係如下所列：To achieve the foregoing objects, the titanium dioxide nanotube adsorbent and method for water treatment of the present invention are as follows:
提供二氧化鈦粉末；Providing titanium dioxide powder;
製備二氧化鈦溶液：將二氧化鈦粉末溶解於一溶劑中以形成一具有設定濃度之二氧化鈦溶液；Preparing a titanium dioxide solution: dissolving the titanium dioxide powder in a solvent to form a titanium dioxide solution having a set concentration;
水熱法處理：將二氧化鈦溶液經由過濾、蒸餾水洗、酸洗、乾燥及鍛燒以製出二氧化鈦奈米管吸附劑。Hydrothermal treatment: The titanium dioxide solution is filtered, washed with water, pickled, dried and calcined to produce a titanium dioxide nanotube adsorbent.
所述之用於水處理之二氧化鈦奈米管吸附劑之方法，其中，該二氧化鈦溶液為載體，而與一包含石墨烯的磁性顆粒混合溶液，經混合均勻，經由水熱法而反應製備出一附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑。The method for treating a titanium dioxide nanotube adsorbent for water treatment, wherein the titanium dioxide solution is a carrier, and a solution mixed with a magnetic particle containing graphene is uniformly mixed and reacted by a hydrothermal method to prepare a solution. A titanium dioxide nanotube adsorbent carrying magnetic particles of graphene.
由前述可知，本發明用於水處理之二氧化鈦奈米管吸附劑及其製備方法可達到下列之功效：It can be seen from the foregoing that the titanium dioxide nanotube adsorbent for water treatment of the present invention and the preparation method thereof can achieve the following effects:
本發明以二氧化鈦粉末，配合將二氧化鈦配製為二氧化鈦溶液，並經由水熱法來製成二氧化鈦奈米管吸附劑以二氧化鈦奈米管吸附劑的粒徑在於200~400nm之間，粒徑更小，而使二氧化鈦奈米管吸附劑的比表面積加大，較一般傳的二氧化鈦粉末增加至少3倍；而且本發明還可在二氧化鈦溶液的製程中，混合附載石墨烯的磁性顆粒溶液，在經由水熱反應，即能製成附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑，使二氧化鈦奈米管複合石墨烯，引入的石墨烯，其具有優異的電子傳輸特性，以及具有高比表面積而有較佳的吸附特性，將可提高二氧化鈦的光催活性以增強吸附力，讓水處理在解除重金屬上，具有更優異的處理效率。The invention combines titanium dioxide powder into titanium dioxide solution, and prepares titanium dioxide nano tube adsorbent by hydrothermal method. The particle size of the titanium dioxide nano tube adsorbent is between 200 and 400 nm, and the particle size is smaller. The specific surface area of the titanium dioxide nanotube adsorbent is increased by at least 3 times compared with the generally transmitted titanium dioxide powder; and the present invention can also mix the graphene-loaded magnetic particle solution in the process of the titanium dioxide solution, in the case of passing through the water heat. The reaction can be made into a titanium dioxide nanotube adsorbent carrying magnetic particles of graphene, the titanium dioxide nanotube composite graphene, the introduced graphene, which has excellent electron transport characteristics and has a high specific surface area. The excellent adsorption characteristics will increase the photocatalytic activity of titanium dioxide to enhance the adsorption force, and allow the water treatment to remove heavy metals and have superior processing efficiency.
附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑，利用石墨烯具有活性強官能團，可成為對金屬處理效能良好之吸附劑，而氧化石墨對金屬陽離子具有高的吸附能力，石墨烯奈米片對金屬陽離子和陰離子都有很強的吸附，是以，氧化石墨和有機物或者金屬離子結合改質之後，此官能團複合材料用來處理重金屬，本發明吸附劑的比表面積為131.8 m 2g -1m 2g -1，與以往二氧化鈦粉末相比，其比表面積增加至少3倍，使本發明處理水中重金屬的吸附效果上更為優異。 A titanium dioxide nanotube adsorbent carrying magnetic particles of graphene, which has a strong reactive functional group, can be an adsorbent with good metal treatment efficiency, and graphite oxide has high adsorption capacity for metal cations, graphene nanosheet It has strong adsorption to metal cations and anions. After the graphite oxide is combined with organic or metal ions, the functional group composite is used to treat heavy metals. The specific surface area of the adsorbent of the present invention is 131.8 m 2 g -1 . m 2 g -1 has a specific surface area increase of at least 3 times as compared with the conventional titanium dioxide powder, and the adsorption effect of heavy metals in the treated water of the present invention is more excellent.
為使貴審查委員對本發明之目的、特徵及功效能夠有更進一步之瞭解與認識，以下茲請配合圖式簡單說明詳述如後：In order to enable your review committee to have a better understanding and understanding of the purpose, features and effects of the present invention, please refer to the following for a brief description of the following:
本發明之二氧化鈦奈米管吸附劑之製備方法，流程係如圖1所示：The preparation method of the titanium dioxide nano tube adsorbent of the present invention is shown in Figure 1:
提供二氧化鈦粉末；Providing titanium dioxide powder;
製備二氧化鈦溶液：將二氧化鈦粉末溶解於一溶劑中以形成一具有設定濃度之二氧化鈦溶液；更具體之實施方法，如秤取5g二氧化鈦粉末加入10N氫氧化鈉中，定義為二氧化鈦溶液， 將前述二氧化鈦溶液置放於鐵氟龍容器，並於室温下攪拌30分鐘，使其均勻；Preparing a titanium dioxide solution: dissolving the titanium dioxide powder in a solvent to form a titanium dioxide solution having a set concentration; more specifically, for example, weighing 5 g of titanium dioxide powder into 10N sodium hydroxide, defined as a titanium dioxide solution, the foregoing titanium dioxide solution Place in a Teflon container and stir at room temperature for 30 minutes to make it uniform;
水熱法處理：將二氧化鈦溶液放置於高壓釜反應器中封閉，以於130℃下進行24小時水熱反應，之後取出，放置於室温冷卻，再將第一混合溶液上層液倒掉以取下層白色粉末，將其利用0.1鹽酸酸洗及去離子水洗淨至PH＜1.6，最後以離心法將白色粉末放置100℃烘乾4小時、400℃鍛燒一小時；Hydrothermal treatment: The titanium dioxide solution is placed in an autoclave reactor for blocking, and subjected to hydrothermal reaction at 130 ° C for 24 hours, then taken out, left at room temperature for cooling, and the first mixed solution upper layer liquid is poured off to remove the lower layer. White powder, which was washed with 0.1 hydrochloric acid pickling and deionized water to pH<1.6. Finally, the white powder was dried by centrifugation at 100 ° C for 4 hours and 400 ° C for one hour;
製出二氧化鈦奈米管吸附劑：最終形成二氧化鈦奈米管吸附劑， 其粒徑係介於200~400nm之間。The titanium dioxide nano tube adsorbent is prepared: finally, a titanium dioxide nano tube adsorbent is formed, and the particle size is between 200 and 400 nm.
另如圖2之流程示意圖，其係另一較佳實施例，其係以二氧化鈦奈米管吸附劑為載體，來製備出具有附載石墨烯磁性顆粒，其方法步驟如下：Another schematic diagram of FIG. 2 is another preferred embodiment, which uses a titanium dioxide nanotube adsorbent as a carrier to prepare magnetic particles with graphene attached, and the method steps are as follows:
備料：提供二氧化鈦粉末，以及含石墨烯分散液，以及磁性顆料溶液；Preparation: providing titanium dioxide powder, and graphene-containing dispersion, and magnetic particle solution;
製備二氧化鈦溶液：將二氧化鈦粉末溶解於一溶劑中以形成一具有設定濃度之二氧化鈦溶液；更具體之實施方法，如秤取5g二氧化鈦粉末加入10N氫氧化鈉中，定義為二氧化鈦溶液， 將前述二氧化鈦溶液置放於鐵氟龍容器，並於室温下攪拌30分鐘，使其均勻；Preparing a titanium dioxide solution: dissolving the titanium dioxide powder in a solvent to form a titanium dioxide solution having a set concentration; more specifically, for example, weighing 5 g of titanium dioxide powder into 10N sodium hydroxide, defined as a titanium dioxide solution, the foregoing titanium dioxide solution Place in a Teflon container and stir at room temperature for 30 minutes to make it uniform;
混合：秤取0.25g磁性顆粒(含50%量之石墨烯)於100毫升之去離子水中，再加0.25g石墨烯分散液，即為附載石墨烯的磁性顆粒之混合溶液，並將此溶液與二氧化鈦溶液進行混合，置放於鐵氟龍容器，並於室温下攪拌30分鐘，使其均勻；Mixing: 0.25 g of magnetic particles (containing 50% of graphene) in 100 ml of deionized water, plus 0.25 g of graphene dispersion, which is a mixed solution of graphene-loaded magnetic particles, and this solution Mix with titanium dioxide solution, place in Teflon container, and stir at room temperature for 30 minutes to make it uniform;
水熱法處理：將附載石墨烯的磁性顆粒之混合溶液，以及二氧化鈦溶液兩者的兩者混合溶液，透過水熱法來反應，水熱法的流程，係將混合均勻之附載石墨烯的磁性顆粒之混合溶液、二氧化鈦溶液， 放置於高壓釜反應器中封閉，以進行2小時水熱反應，再經過濾、蒸餾水洗、酸洗、400℃鍛燒1小時，即形成附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑。Hydrothermal treatment: a mixed solution of magnetic particles carrying graphene and a mixed solution of both of the titanium dioxide solution are reacted by hydrothermal method, and the hydrothermal process is to mix the magnetic properties of the graphene loaded uniformly The mixed solution of the particles and the titanium dioxide solution are placed in an autoclave reactor for blocking for 2 hours of hydrothermal reaction, followed by filtration, distillation with water washing, pickling, and calcination at 400 ° C for 1 hour to form magnetic particles carrying graphene. Titanium dioxide nanotube adsorbent.
如此一來，本發明使二氧化鈦奈米管吸附劑複合了石墨烯，利用石墨烯，具有優異的電子傳輸特性，以及具有高比表面積而有良好吸附能力，將可提高二氧化鈦的光催活性，並且增強吸附力，快速有效地吸附水中的重金屬污染。In this way, the present invention combines the titanium dioxide nanotube adsorbent with graphene, utilizes graphene, has excellent electron transport properties, and has a high specific surface area and good adsorption capacity, which can enhance the photocatalytic activity of titanium dioxide, and Enhance the adsorption force and quickly and effectively adsorb heavy metal pollution in water.
本發明製出之附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑，如圖4經由穿透式電子顯微圖像來顯示，經改變形態之吸附劑，管壁由多層組成，具有約0.78奈米片間距(幾乎是銳鈦礦晶格參數的2倍)，鈦管的兩側和總層數不相同，表示奈米管結構係從片狀結構蜷曲，但在比表面積(體積與表面積的比例)的部份卻比原本一般傳統二氧化鈦還要大上8倍，約為400㎡/g，一般傳統二氧化鈦約僅為50㎡/g，使得本發明附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑，其提供的吸附能力可顯著提昇，因此能夠處理較一般二氧化鈦吸附劑更高濃度的污染物。The titanium dioxide nano tube adsorbent of the graphene-loaded magnetic particles prepared by the invention is shown in Fig. 4 via a transmission electron microscopic image, and the modified adsorbent has a tube wall composed of a plurality of layers, having about 0.78 The spacing of the nanosheets (almost twice the lattice parameter of anatase), the sides of the titanium tube and the total number of layers are different, indicating that the nanotube structure is distorted from the sheet structure, but in the specific surface area (volume and surface area) The proportion of the ratio is 8 times larger than the conventional conventional titanium dioxide, about 400 m2 / g, and the conventional titanium dioxide is only about 50 m 2 / g, so that the titanium dioxide of the magnetic particles of the present invention is attached with graphene. The tube adsorbent, which provides a significant increase in adsorption capacity, is capable of handling higher concentrations of contaminants than typical titanium dioxide adsorbents.
本發明選用砷溶液污染物來做為水處理應用的例子，依本發明製出之吸附劑，可配合耦合電漿光譜儀來分析，並配合一儲存瓶裝置，而如圖3所示，其係包括一儲存瓶1、數用以固定儲存瓶1的固定夾2、一温度控制器3、一供儲存瓶1、固定夾2安置之恆温水槽4；本實施例中：該儲存瓶1是供砷溶液裝入的容器；各該固定夾2是當儲存瓶1在搖晃的時候，能夠使用固定夾2將該儲存瓶1的瓶身固定住，不讓儲存瓶1任意倒塌；該温度控制器3是為了測定15℃,25℃,35℃,45℃對砷移除效率的影響，所以該温度控制器3可以調整溫度；該恆温水槽4是一種水浴，它能夠在25分鐘的實驗過程中保持在15℃,25℃,35℃,45℃。要實施分析之時，將附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑，以及選用重金屬砷溶液，緩慢倒入儲存瓶1內，並以130rpm/分的轉速來搖晃，藉以吸附砷溶液的砷無機物，透過耦合電漿光譜儀來分析，本發明提昇砷溶液之重金屬砷的降解效率。The invention selects the arsenic solution contaminant as an example of the water treatment application, and the adsorbent prepared according to the invention can be analyzed by the coupled plasma spectrometer and matched with a storage bottle device, and as shown in FIG. 3, the system is The utility model comprises a storage bottle, a fixed clamp 2 for fixing the storage bottle 1, a temperature controller 3, a constant temperature water tank 4 for storing the storage bottle 1, and the fixed clamp 2. In the embodiment: the storage bottle 1 is for a container filled with the arsenic solution; each of the fixing clips 2 is capable of fixing the bottle body of the storage bottle 1 using the fixing clip 2 when the storage bottle 1 is shaking, so that the storage bottle 1 is not collapsed arbitrarily; the temperature controller 3 is to determine the effect of 15 ° C, 25 ° C, 35 ° C, 45 ° C on the efficiency of arsenic removal, so the temperature controller 3 can adjust the temperature; the constant temperature water tank 4 is a water bath, which can be in the course of 25 minutes of the experiment Maintain at 15 ° C, 25 ° C, 35 ° C, 45 ° C. To carry out the analysis, the titanium dioxide nanotube adsorbent carrying the magnetic particles of graphene and the heavy metal arsenic solution are slowly poured into the storage bottle 1 and shaken at a speed of 130 rpm, thereby adsorbing the arsenic solution. The arsenic inorganic substance is analyzed by a coupled plasma spectrometer, and the present invention improves the degradation efficiency of heavy metal arsenic in the arsenic solution.
因此如圖5、6、7、8所示，其分別顯示本發明附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑之在氮氣等温吸附/脫附儀圖譜、傅立葉紅外線光譜儀、x光繞射光譜儀、於不同濃度下之吸附效率。如圖5所示之圖表，說明了在相對壓力下，吸附和解吸的數量約呈正比態度，證明本發明所製出之吸附劑具有極佳之吸附效果，依據該些實驗圖表，可以得知本發明吸附效率提高，此乃本發明之二氧化鈦奈米管呈管狀中孔材料，因此具有較大的比表面積，配合磁性顆粒附載了石墨烯，利用石墨烯熱穩定性佳，以及石墨烯係具有活性強官能團，氧化石墨對金屬陽離子具有高的吸附能力，石墨烯奈米片對金屬陽離子和陰離子都有很強的吸附，故而氧化石墨和有機物或者金屬離子結合改質之後，此官能團複合材料可以用來處理重金屬，因此大幅增強吸附能力。Therefore, as shown in FIGS. 5, 6, 7, and 8, respectively, the titanium dioxide nanotube adsorbent of the graphene-loaded magnetic particles of the present invention is analyzed by a nitrogen isotherm adsorption/desorption instrument, a Fourier infrared spectrometer, and an x-ray diffraction. Spectrometer, adsorption efficiency at different concentrations. The graph shown in Fig. 5 shows that the amount of adsorption and desorption is approximately proportional to the relative pressure under the relative pressure, which proves that the adsorbent prepared by the invention has an excellent adsorption effect, and according to the experimental charts, it can be known The adsorption efficiency of the invention is improved, and the titanium dioxide nanotube of the invention has a tubular mesoporous material, so has a large specific surface area, the magnetic particles are loaded with graphene, the thermal stability of the graphene is good, and the graphene has Reactive strong functional group, graphite oxide has high adsorption capacity for metal cations, graphene nanosheets have strong adsorption to metal cations and anions, so after the combination of graphite oxide and organic or metal ions, the functional group composite can Used to treat heavy metals, thus greatly enhancing the adsorption capacity.
上述實施例僅為例示性說明本發明之技術及其功效，而非用於限制本發明。任何熟於此項技術人士均可在不違背本發明之技術原理及精神的情況下，對上述實施例進行修改及變化，因此本發明之權利保護範圍應如後所述之申請專利範圍所列。The above embodiments are merely illustrative of the technology of the present invention and its effects, and are not intended to limit the present invention. Any person skilled in the art can modify and change the above embodiments without departing from the technical spirit and spirit of the present invention. Therefore, the scope of protection of the present invention should be as listed in the patent application scope mentioned later. .
儲存瓶1 固定夾2 温度控制器3 恆温水槽4Storage bottle 1 retaining clip 2 temperature controller 3 thermostatic sink 4
圖1 為本發明製備二氧化鈦奈米管吸附劑的流程方塊示意圖。 圖2 為本發明製備附載石墨烯的磁性顆粒之二氧化鈦奈米管吸附劑的流程方塊示意圖。 圖3 為本發明恆温水槽之裝置示意立體圖。 圖4 為本發明穿透式電子顯微鏡圖像。 圖5 為本發明氮氣等温吸附/脫附儀圖譜。 圖6 為本發明傅立葉紅外線光譜儀。 圖7 為本發明X光繞射光譜儀。 圖8 為本發明於不同含量下的砷吸附效率圖。1 is a schematic block diagram showing the preparation of a titanium dioxide nanotube adsorbent according to the present invention. 2 is a schematic block diagram of a titanium dioxide nanotube adsorbent for preparing magnetic particles carrying graphene according to the present invention. Figure 3 is a schematic perspective view of the apparatus for the constant temperature water tank of the present invention. Figure 4 is a transmission electron microscope image of the present invention. Figure 5 is a map of a nitrogen isothermal adsorption/desorption apparatus of the present invention. Figure 6 is a Fourier infrared spectrometer of the present invention. Figure 7 is an X-ray diffraction spectrometer of the present invention. Figure 8 is a graph showing the adsorption efficiency of arsenic at different contents according to the present invention.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1915835A (en) * | 2006-07-27 | 2007-02-21 | 北京先讯东泰科技有限公司 | Method for preparing Nano line of titania, and application of the prepared Nano line of titania |
| CN102826600A (en) * | 2012-09-20 | 2012-12-19 | 电子科技大学 | Method for preparing titanium dioxide nanowire |
| CN104332611A (en) * | 2014-08-27 | 2015-02-04 | 中国工程物理研究院化工材料研究所 | Graphene/titanium dioxide nano fiber composite material, preparation method and applications thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1915835A (en) * | 2006-07-27 | 2007-02-21 | 北京先讯东泰科技有限公司 | Method for preparing Nano line of titania, and application of the prepared Nano line of titania |
| CN102826600A (en) * | 2012-09-20 | 2012-12-19 | 电子科技大学 | Method for preparing titanium dioxide nanowire |
| CN104332611A (en) * | 2014-08-27 | 2015-02-04 | 中国工程物理研究院化工材料研究所 | Graphene/titanium dioxide nano fiber composite material, preparation method and applications thereof |
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