TWI723352B - Method of incineration ash reused for synthesis of porous materials - Google Patents
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本發明提供了一種焚化灰渣合成多孔性材料的方法,尤指一種透過鹼熔水熱法製成多孔性材料的合成方法。The invention provides a method for synthesizing porous materials by incinerating ash and slag, in particular to a method for synthesizing porous materials through alkali fusion hydrothermal method.
一般而言,焚化灰渣(Incineration ash)包含焚化底渣(Bottom ash)與飛灰(Fly ash),其定義為焚化爐燃燒廢棄物所產生之殘餘物。底渣目前大部分採用破碎、分選處理後再利用於各項工程填料或工程材料,或是直接採掩埋處理;而飛灰目前大部分採用固化/穩定化處理後堆置於掩埋場,或經水洗後再利用於水泥添加料。Generally speaking, Incineration ash includes incineration bottom ash (Bottom ash) and fly ash (Fly ash), which is defined as the residue produced by burning waste in an incinerator. At present, most of the bottom slag is crushed and sorted and then reused in various engineering fillers or engineering materials, or directly collected and buried; while most of the fly ash is currently solidified/stabilized and stacked in a landfill, or After washing with water, it can be used as cement additives.
然而底渣與飛灰採掩埋處置時,常常面臨掩埋場容量不足等窘境,致使掩埋無法成為長久可行的處理方式。甚者,灰渣再利用仍有重金屬或戴奧辛等有害物質溶出,造成環境二次污染的疑慮及潛在風險。此外,飛灰採用添加水泥與螯合劑的方式進行固化及穩定化處理,不但會增加體積,進一步加快掩埋空間消耗之外,其中所含氯鹽及氧化鈣等無機成份更容易導致固化所需的反應時間延長,甚至是容易吸濕導以致固化物膨脹崩解等缺點。However, when the bottom slag and fly ash are collected and buryed, they often face the dilemma of insufficient landfill capacity, so that burial cannot be a long-term feasible treatment method. What's more, heavy metals or dioxin and other harmful substances are still eluted in the reuse of ash and slag, causing doubts and potential risks of secondary environmental pollution. In addition, fly ash is cured and stabilized by adding cement and chelating agents, which will not only increase the volume and further accelerate the consumption of landfill space, but the inorganic components such as chloride salts and calcium oxide are more likely to cause the curing required. The reaction time is prolonged, and even it is easy to absorb moisture and cause the cured product to swell and disintegrate.
綜上所述,目前對於焚化底渣急和飛灰的處理方式,有環境污染疑慮及社會觀感不佳等問題,進而影響垃圾焚化處理之穩定發展。也因如此,焚化灰渣的妥善處理與再利用已成為垃圾焚化廠所面臨的迫切問題。In summary, the current treatment methods of incineration bottom slag and fly ash have problems such as environmental pollution concerns and poor social perception, which further affect the stable development of waste incineration. Because of this, the proper treatment and reuse of incineration ash has become an urgent problem faced by waste incineration plants.
近年來,有鑑於焚化飛灰中富含矽、鋁化物等特定成份的物質,具備合成多孔性材料及環保吸濕或吸附材料之潛力。依現有的技術論之,對於合成多孔性材料及環保吸濕或吸附材料,多半利用天然黏土礦料、淨水污泥或廢棄玻璃等其他廢棄物作為原料。In recent years, the incineration fly ash has the potential to synthesize porous materials and environmentally-friendly moisture-absorbing or adsorbent materials due to the fact that the incineration fly ash is rich in specific components such as silicon and aluminum compounds. According to the existing technical theory, for synthetic porous materials and environmentally friendly hygroscopic or absorbent materials, most of them use natural clay minerals, water purification sludge or waste glass and other wastes as raw materials.
有鑑於先前技術中所提及的缺點,本發明提供了一種焚化灰渣合成多孔性材料的方法。本發明所揭露的焚化灰渣合成多孔性材料的方法主要包含七大步驟。In view of the shortcomings mentioned in the prior art, the present invention provides a method for incineration of ash to synthesize porous materials. The method for synthesizing porous materials from incineration ash disclosed in the present invention mainly includes seven major steps.
首先,執行步驟(a),提供一焚化灰渣(Incineration ash),接著執行步驟(b),調整該焚化灰渣中矽化合物及鋁化合物的一矽鋁比值後,進行步驟(c),加入一鹼活化劑混合攪拌,並進行一鹼熔反應。First, perform step (a) to provide an incineration ash, and then perform step (b) to adjust the silicon-to-aluminum ratio of the silicon compound and aluminum compound in the incineration ash, then proceed to step (c), add An alkali activator is mixed and stirred, and an alkali fusion reaction is carried out.
執行步驟(d),進行一水解反應後分離為一固體及一水解溶液,再執行步驟(e),將該水解溶液加入一調整液後攪拌形成一前驅液。接著將獲得的前驅液進行步驟(f),將該前驅液進行一水熱合成反應並獲得一沉澱物,最後透過步驟(g),將該沉澱物取出清洗後烘乾並煅燒,形成一多孔性材料。其中,步驟(e)之該調整液包含一硫酸,並將該前驅液之pH值調整至8-12。Step (d) is performed to separate a solid and a hydrolyzed solution after a hydrolysis reaction is performed, and then step (e) is performed to add the hydrolyzed solution to a conditioning solution and stir to form a precursor solution. Then the obtained precursor liquid is subjected to step (f), the precursor liquid is subjected to a hydrothermal synthesis reaction to obtain a precipitate, and finally through step (g), the precipitate is taken out, washed, dried and calcined to form a poly Porous materials. Wherein, the adjustment solution of step (e) contains a sulfuric acid, and the pH value of the precursor solution is adjusted to 8-12.
藉此,本發明可成功將焚化灰渣回收再利用,並於適當地調整控制條件,合成出多孔性材料。除了讓焚化灰渣可自行回收再利用之外,更可以應用於焚化廠之空氣污染與水污染控制,開創焚化灰渣之另一種處理方法及再利用管道,減少焚化灰渣處理量與降低可能產生的環境污染,提高焚化灰渣回收與資源化產品的價值與應用效益。Thereby, the present invention can successfully recover and reuse the incineration ash, and appropriately adjust the control conditions to synthesize porous materials. In addition to allowing the incineration ash to be recycled and reused by itself, it can also be used for air pollution and water pollution control in incineration plants, creating another treatment method and reuse pipeline for incineration ash, reducing the amount of incineration ash treatment and reducing the possibility The resulting environmental pollution improves the value and application benefits of incineration ash recovery and resource recycling products.
以上對本發明的簡述,目的在於對本發明之數種面向和技術特徵作一基本說明。發明簡述並非對本發明的詳細表述,因此其目的不在特別列舉本發明的關鍵性或重要元件,也不是用來界定本發明的範圍,僅為以簡明的方式呈現本發明的數種概念而已。The above brief description of the present invention aims to provide a basic description of several aspects and technical features of the present invention. The brief description of the invention is not a detailed description of the invention. Therefore, its purpose is not to specifically enumerate the key or important elements of the invention, nor to define the scope of the invention. It merely presents several concepts of the invention in a concise manner.
為能瞭解本發明的技術特徵及實用功效,並可依照說明書的內容來實施,茲進一步以如圖式所示的較佳實施例,詳細說明如後:In order to understand the technical features and practical effects of the present invention, and implement it in accordance with the content of the specification, the preferred embodiment shown in the figure is further described in detail as follows:
請參照圖1,圖1為本發明實施例焚化灰渣合成多孔性材料的方法之步驟流程圖。如圖1所示,本發明實施例所稱之焚化灰渣合成多孔性材料的方法主要包含七大步驟。Please refer to FIG. 1, which is a flow chart of a method for incineration of ash and slag to synthesize a porous material according to an embodiment of the present invention. As shown in Fig. 1, the method for synthesizing porous materials from incineration ash and slag in the embodiment of the present invention mainly includes seven major steps.
首先,執行步驟(a),提供一焚化灰渣(Incineration ash)。在本實施例中,該焚化灰渣為底渣(Bottom ash)、飛灰(Fly ash)或其組合,端看焚化廠或相關業者所提供之焚化灰渣而定,本發明並不加以限制。接著執行步驟(b),調整該焚化灰渣中矽化合物及鋁化合物的一矽鋁比值,再執行步驟(c),加入一鹼活化劑混合攪拌,並進行一鹼熔反應。First, perform step (a) to provide an incineration ash. In this embodiment, the incineration ash is Bottom ash, Fly ash, or a combination thereof, depending on the incineration ash provided by the incineration plant or related industry, and the present invention is not limited . Then, step (b) is performed to adjust the ratio of silicon to aluminum of the silicon compound and aluminum compound in the incineration ash, and then step (c) is performed to add an alkali activator to mix and stir, and perform an alkali melting reaction.
在本實施例之步驟(b)-(c)中,所述的矽鋁比值介於10-40之間,最佳為10、20或40;其調整方式係透過焚化灰渣中回收矽化合物與鋁化合物,並調整適當的矽、鋁莫耳比例。而鹼活化劑可以採用鹼性物質,如氫氧化鈉(NaOH)、氫氧化鉀(KOH)、碳酸鈉(Na2 CO3 )或其組合,以固定鹼灰比1.5的方式加入並均勻混合。In steps (b)-(c) of this embodiment, the ratio of silicon to aluminum is between 10-40, preferably 10, 20 or 40; the adjustment method is to recover silicon compounds from incineration ash It is compounded with aluminum, and the ratio of silicon to aluminum molar is adjusted appropriately. The alkali activator can be an alkali substance, such as sodium hydroxide (NaOH), potassium hydroxide (KOH), sodium carbonate (Na 2 CO 3 ), or a combination thereof, which is added in a fixed alkali-to-ash ratio of 1.5 and mixed uniformly.
至於鹼熔反應中會調整適當的液體固體比例,以利下個步驟使用;在本步驟中,推薦調整的液體固體比值可介於100-200之間,且又以100、150或200為佳。而本步驟鹼熔反應所採用的反應硬體為高溫爐,反應時間可介於20-80分鐘之間,反應溫度則可介於攝氏溫度200-800度之間。在本步驟中,最佳的鹼熔反應溫度及時間依序為攝氏溫度400-600度反應40-60分鐘。As for the alkali fusion reaction, the appropriate liquid-to-solid ratio will be adjusted to facilitate the use in the next step; in this step, the recommended liquid-to-solid ratio can be adjusted between 100-200, and 100, 150 or 200 is better. . The reaction hardware used in the alkali fusion reaction in this step is a high-temperature furnace, the reaction time can be between 20-80 minutes, and the reaction temperature can be between 200-800 degrees Celsius. In this step, the optimal alkali fusion reaction temperature and time are 400-600 degrees Celsius for 40-60 minutes in order.
接著執行步驟(d),進行一水解反應後分離為一固體及一水解溶液。本實施例中,水解反應所採用的參數為攝氏溫度105度下反應24小時,反應結束後冷卻降溫,並去除殘留不溶解的物質。Then, step (d) is performed, a hydrolysis reaction is performed and then separated into a solid and a hydrolysis solution. In this embodiment, the parameter used in the hydrolysis reaction is a reaction at 105 degrees Celsius for 24 hours. After the reaction is completed, the temperature is cooled down and the remaining insoluble substances are removed.
再執行步驟(e),將該水解溶液加入一調整液後攪拌形成一前驅液。本實施例之步驟(e)中,調整液包含一硫酸,且所述硫酸的體積莫耳濃度為1 M。調整液中更包含總溶液(即調整液和水解溶液的總和)重量百分比濃度1.2%的溴化十六烷基三甲銨(Cetyltrimethylammonium bromide, CTAB)溶液。最後,在本實施例之步驟(d)中,透過硫酸將該前驅液之pH值調整至8-12。Then perform step (e), add the hydrolysis solution to an adjustment solution and stir to form a precursor solution. In step (e) of this embodiment, the adjustment solution contains a sulfuric acid, and the volumetric molar concentration of the sulfuric acid is 1 M. The adjustment solution further includes a Cetyltrimethylammonium bromide (CTAB) solution with a concentration of 1.2% by weight of the total solution (that is, the sum of the adjustment solution and the hydrolysis solution). Finally, in step (d) of this embodiment, the pH value of the precursor solution is adjusted to 8-12 through sulfuric acid.
接著將獲得的前驅液繼續進行步驟(f),將該前驅液進行一水熱合成反應並獲得一沉澱物。在本實施例步驟(f)中,該水熱合成反應所採用的方式為加蓋密封的熱水反應器。其反應時間介於12-48小時之間;而反應溫度介於攝氏溫度80-180度之間。本實施例步驟(f)所採用的最佳參數為反應溫度與時間依序為攝氏溫度105度反應24或48小時。Then, the obtained precursor liquid is continued to step (f), and the precursor liquid is subjected to a hydrothermal synthesis reaction to obtain a precipitate. In step (f) of this embodiment, the method used for the hydrothermal synthesis reaction is a hot water reactor with a cover and a seal. The reaction time is between 12-48 hours; and the reaction temperature is between 80-180 degrees Celsius. The optimal parameter used in step (f) of this embodiment is that the reaction temperature and time are 105 degrees Celsius for 24 or 48 hours in sequence.
最後透過步驟(g),將該沉澱物取出清洗後烘乾並煅燒,形成一多孔性材料。本實施例步驟(g)中,步驟(f)所獲得的沉澱物取出清洗後會進行過濾,接著煅燒的參數採用攝氏溫度450-650度作用3-6小時。Finally, through step (g), the precipitate is taken out for cleaning, dried and calcined to form a porous material. In step (g) of this embodiment, the precipitate obtained in step (f) will be filtered after being taken out and cleaned, and then the calcination parameter adopts 450-650 degrees Celsius for 3-6 hours.
本實施例最終生產出的多孔性材料為沸石(Zeolite)。請參照圖2,圖2為本發明實施例焚化灰渣合成多孔性材料的方法之最終成品圖。如圖2所示,在圖2為掃描式電子顯微鏡圖的前提下,可看出本發明實施例所合成的沸石具有高品質的特性,且可依照不同的條件參數合成出不同性質的沸石,並可應用作為吸附材料(Adsorbent)、觸媒載體(catalyst support)、耐溫材料或表面改質材料等,僅依照實施的需求調整,本發明並不加以限制。The porous material finally produced in this example is Zeolite. Please refer to FIG. 2, which is a final product diagram of the method for incineration of ash and slag to synthesize porous materials according to an embodiment of the present invention. As shown in Figure 2, under the premise that Figure 2 is a scanning electron microscope image, it can be seen that the zeolite synthesized in the embodiment of the present invention has high-quality characteristics, and zeolites with different properties can be synthesized according to different conditions and parameters. It can also be used as an adsorbent, a catalyst support, a temperature-resistant material or a surface modification material, etc. It can only be adjusted according to the requirements of the implementation, and the present invention is not limited.
惟以上所述者,僅為本發明之較佳實施例而已,當不能以此限定本發明實施之範圍,即依本發明申請專利範圍及說明內容所作之簡單變化與修飾,皆仍屬本發明涵蓋之範圍內。However, the above are only the preferred embodiments of the present invention, and should not be used to limit the scope of implementation of the present invention, that is, simple changes and modifications made in accordance with the scope of the patent application and the description of the present invention still belong to the present invention. Covered.
(a)-(g):步驟 (a)-(g): steps
圖1為本發明實施例焚化灰渣合成多孔性材料的方法之步驟流程圖。 圖2為本發明實施例焚化灰渣合成多孔性材料的方法之最終成品圖。Fig. 1 is a flow chart of steps of a method for incineration of ash to synthesize porous materials according to an embodiment of the present invention. Fig. 2 is a final product diagram of the method for incineration of ash and slag to synthesize porous materials according to an embodiment of the present invention.
(a)-(g):步驟 (a)-(g): steps
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