TWI683698B - Packed tower with composite filler - Google Patents
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本發明有關於一種複合型填充材料的填充塔,且特別是包括氧化劑去除觸媒及觸媒再生劑的複合型填充材料的填充塔。 The invention relates to a packed tower of composite packing materials, and in particular to a packed tower of composite packing materials including an oxidant removing catalyst and a catalyst regenerant.
填充塔是化工生產中常使用的傳質設備,主要由圓柱形的塔體和設置在塔內的填充材料所組成,常用於過濾、吸收、蒸餾、萃取等。然而,在化工生產過程中,常會添加氧化劑作反應,待反應完成後,殘留的氧化劑卻難以去除。 A packed tower is a mass transfer device commonly used in chemical production. It is mainly composed of a cylindrical tower body and a packing material installed in the tower. It is often used for filtration, absorption, distillation, extraction, etc. However, in the chemical production process, oxidants are often added for reaction. After the reaction is completed, the residual oxidants are difficult to remove.
此外,汽機車燃燒廢氣產生的氧化物、工廠廢氣以及含有化學物質的煙霧與陽光進行的化學反應後,產生的環境臭氧汙染物也是一種難以去除的氧化劑。由於臭氧反應活性遠遠比氧氣強,屬於強氧化劑,對動植物及許多結構材料如塑膠、橡膠均有害。 In addition, after the chemical reaction between the oxides produced by the combustion of exhaust gas from the locomotives, factory exhaust gas and smoke containing chemical substances and sunlight, the resulting environmental ozone pollutants are also an oxidant that is difficult to remove. Ozone is far more reactive than oxygen and is a strong oxidant. It is harmful to animals and plants and many structural materials such as plastic and rubber.
因此,開發一種可以有效去除液相或氣相的氧化劑成分之填充塔,可應用在化工生產製程或生活環境中,為目前相關產業共同努力的目標。 Therefore, the development of a packed tower that can effectively remove oxidant components in the liquid or gas phase can be applied in the chemical production process or living environment, and is the goal of joint efforts of related industries.
本發明是一種複合型填充材料的填充塔,利用括氧化劑去除觸媒處理氧化劑,且利用觸媒再生劑活化並再生氧化劑去除觸媒,以有效去除氧化劑。本發明包括以下方面。 The invention is a packed tower of composite packing material, which uses oxidizer to remove catalyst to process oxidant, and uses catalyst regenerator to activate and regenerate oxidant to remove catalyst to effectively remove oxidant. The present invention includes the following aspects.
依據本發明之一方面提供一種填充塔,包括至少一塔體及一複合型填充材料。塔體具有一過濾流體入口及一過濾流體出口。複合型填充材料,承載於塔體中,用以去除液相或氣相中的氧化劑。複合型填充材料包括第一氧化劑去除觸媒用以處理氧化劑。觸媒再生劑用以活化第一氧化劑去除觸媒。 According to one aspect of the present invention, a packed tower is provided, which includes at least a tower body and a composite packing material. The tower body has a filtered fluid inlet and a filtered fluid outlet. The composite packing material is carried in the tower body to remove the oxidant in the liquid or gas phase. The composite filler material includes a first oxidant removal catalyst to treat the oxidant. The catalyst regeneration agent is used to activate the first oxidant to remove the catalyst.
10、20、30‧‧‧填充塔 10, 20, 30‧‧‧ packed tower
100、200、300‧‧‧塔體 100, 200, 300 ‧‧‧ tower
102‧‧‧複合型填充材料 102‧‧‧Composite filling material
202、204、302、304、306‧‧‧填充層 202, 204, 302, 304, 306‧‧‧filling layer
F‧‧‧過濾流體入口 F‧‧‧Fluid inlet
O‧‧‧過濾流體出口 O‧‧‧filtered fluid outlet
圖1繪示依照本發明一實施例之單一填充層的填充塔示意圖。 FIG. 1 is a schematic diagram of a packed tower with a single packed layer according to an embodiment of the invention.
圖2繪示依照本發明一實施例之雙層填充層的填充塔示意圖。 FIG. 2 is a schematic diagram of a packed tower with double-layer filling layers according to an embodiment of the invention.
圖3繪示依照本發明一實施例之三層填充層的填充塔示意圖。 FIG. 3 is a schematic diagram of a packed tower with three packed layers according to an embodiment of the invention.
請參照圖1,其繪示依照本發明一實施例之單一填充層的填充塔示意圖。如圖1所示,填充塔10包括一塔體100及一複合型填充材料102。塔體100具有一過濾流體入口F及一過濾流體出口O。複合型填充材料102,承載於塔體100中,用以去除液相或氣相中的氧化劑。複合型填充材料102堆疊方式包括整齊堆疊、隨機堆疊、依照不同粒徑分層排列或不同粒徑混合填充。塔體100的長寬比可以為0.1-1.5(直徑/高度),較佳地為1.0-1.5。
Please refer to FIG. 1, which illustrates a schematic diagram of a packed tower with a single packed layer according to an embodiment of the invention. As shown in FIG. 1, the packed
於一實施例中,複合型填充材料102包括第一氧化劑去除觸媒及觸媒再生劑。第一氧化劑去除觸媒為氧化劑捕捉或分解材料,可用以處理例如
是濃度較高的氧化劑,透過結構物性可初步去除氧化劑等雜質,再透過化性反性可處理濃度例如50ppm-10000ppm之氧化劑,反應速率為k[氧化劑濃度] n [催化劑濃度] m ,且5>n,m>0。其中,依據使用的催化材料,可能有不同的反應途徑,不同的反應途徑會影響反應速率級數及/或速率常數k值。第一氧化劑去除觸媒去除的氧化劑的反應速率與氧化劑去除觸媒的材料尺寸、多孔材質的孔徑有關。第一氧化劑去除觸媒可以為單一材料或複數材料的組合,具有降低氧化劑活化能,並催化反應進行。具體而言,可催化一個或多個反應路徑,達到整體反應速率的提升。化性處理的方式,是利用氧化劑去除觸媒表面進行吸附或結合之氧化劑,藉此提供氧化劑不同反應路徑,此案例為提供低活化能路徑以提高氧化劑分解速率。氧化劑去除觸媒的活化與再生乃採用觸媒再生劑或其他再生或是活化程序例如熱處理或添加還原劑。
In one embodiment, the
於一實施例中,第一氧化劑去除觸媒可吸附或分解選自於臭氧、氧氣、雙氧水、氯酸鹽、過氯酸鹽、重鉻酸鉀、過錳酸鉀及過氧化物所構成的群組,例如是由碳(活性碳、椰殼炭、木炭、煤炭及改質碳)使用比涵蓋5%~99%或較佳地為10%~80%或最佳為30%~75%。矽(含量涵蓋5%~99% or 10%~80% or 15%~60%)、氧化鋁(含量5%~99%或較佳地為10%~95%或最佳的為30%~90%)、天然礦石(例如沸石)、錳、鐵、鉑、鈀、釕、釩、鉻、鈷、銅及鎳所構成的群組,其中錳、鐵、鉑、鈀、釕、釩、鉻、鈷、銅及鎳之金屬含量0.5%~80%或較佳地為1%~70%或最佳為1%~50%、,且包括其氧化型態。觸媒再生劑例如是選擇自上述材料(碳、石英砂、矽、氧化鋁、天然礦石(例如沸石)、錳、鐵、鉑、鈀、釕、釩、鉻、鈷、銅及鎳所構成的群組)之基材,且含有二氧化七錳或過錳酸鉀或是氧化鐵等具有較高氧化電位之成分所構成的群組。 In one embodiment, the first oxidant removal catalyst can adsorb or decompose selected from ozone, oxygen, hydrogen peroxide, chlorate, perchlorate, potassium dichromate, potassium permanganate and peroxide Group, for example, the use ratio of carbon (activated carbon, coconut shell charcoal, charcoal, coal and modified carbon) covers 5% to 99% or preferably 10% to 80% or optimally 30% to 75% . Silicon (content covers 5%~99% or 10%~80% or 15%~60%), alumina (content 5%~99% or preferably 10%~95% or optimally 30%~ 90%), natural ore (such as zeolite), manganese, iron, platinum, palladium, ruthenium, vanadium, chromium, cobalt, copper, and nickel, of which manganese, iron, platinum, palladium, ruthenium, vanadium, chromium , Cobalt, copper and nickel metal content 0.5% ~ 80% or preferably 1% ~ 70% or most preferably 1% ~ 50%, and including its oxidation type. The catalyst regenerant is selected from the above materials (carbon, quartz sand, silicon, alumina, natural ore (e.g. zeolite), manganese, iron, platinum, palladium, ruthenium, vanadium, chromium, cobalt, copper and nickel Group), and contains a group consisting of components with higher oxidation potential such as heptamanganese dioxide, potassium permanganate or iron oxide.
第一氧化劑去除觸媒及觸媒再生劑的比例,可依據所欲去除的氧化劑種類及濃度作調配,比例為0.1:1~99:1。進一步來說,當所欲去除的氧化劑為雙氧水時,第一氧化劑去除觸媒及觸媒再生劑的比例為1:1~99:1的區間有較佳的反應性,但第一氧化劑去除觸媒及觸媒再生劑的比例在4:1時,具有最佳的使用條件。於另一實施例中,當處理之氧化劑溶液pH小於7時,雙氧水濃度8000ppm的情況下,第一氧化劑去除觸媒及觸媒再生劑的比例在1:1~9:1,具有最佳的使用壽命。當處理之氧化劑溶液pH大於7時,雙氧水濃度8000ppm的情況下,第一氧化劑去除觸媒及觸媒再生劑的比例在0.5:1~6:1,具有最佳的使用壽命。 The ratio of the first oxidant to remove the catalyst and the catalyst regenerant can be adjusted according to the type and concentration of the oxidant to be removed. The ratio is 0.1:1~99:1. Further, when the oxidant to be removed is hydrogen peroxide, the ratio of the first oxidant removal catalyst and the catalyst regeneration agent is in the range of 1:1 to 99:1, but the first oxidant removes the catalyst. When the ratio of media and catalyst regenerator is 4:1, it has the best use conditions. In another embodiment, when the pH of the treated oxidant solution is less than 7, and the hydrogen peroxide concentration is 8000 ppm, the ratio of the first oxidant to remove the catalyst and the catalyst regenerator is 1:1 to 9:1, which has the best Service life. When the pH of the treated oxidant solution is greater than 7, and the hydrogen peroxide concentration is 8000 ppm, the ratio of the first oxidant to remove the catalyst and the catalyst regenerator is 0.5:1~6:1, which has the best service life.
當填充塔的高度約為110公分(cm),且處理之氧化劑溶液pH介於4-10時,雙氧水去除效率的實驗數據如表1所示。實施例A及B的雙氧水去除濾達到100%,已經測不到雙氧水的殘留。實施例C的雙氧水去除濾達99%,顯見本發明之實施例所提供的複合型填充材料具有極佳的去除效果。 When the height of the packed tower is about 110 centimeters (cm) and the pH of the treated oxidant solution is between 4-10, the experimental data of hydrogen peroxide removal efficiency is shown in Table 1. The hydrogen peroxide removal filtration of Examples A and B reaches 100%, and the residual hydrogen peroxide has not been detected. The hydrogen peroxide removal filtration of Example C is up to 99%. It is obvious that the composite filling material provided by the embodiment of the present invention has an excellent removal effect.
於一實施例中,複合型填充材料102還包括一第二氧化劑去除觸媒,用以處理濃度介於10ppm-4000ppm之氧化劑,第二氧化劑去除觸媒的反應速率及氧化劑處理濃度,與其選用成分比例、孔洞大小以及顆粒大小有關。舉
例來說,用小粒徑具有較大孔洞可有助於提高氧化劑接觸材料表面進行吸附與去除,其反應副產物例如氧氣停留於空隙內部時間縮短將有利於提高單位時間的反應,反應速率為k[氧化劑濃度] a [催化劑濃度] b ,其中5>a,b>0。其中,依據使用的催化材料,可能有不同的反應途徑,不同的反應途徑會影響反應速率級數及/或速率常數k值。第二氧化劑去除觸媒去除氧化劑的反應速率與氧化劑去除觸媒的材料尺寸、多孔材質的孔徑有關。觸媒再生劑可用以還原(活化或再生)第一氧化劑去除觸媒及第二氧化劑去除觸媒,使得反覆使用致使第一氧化劑去除觸媒及第二氧化劑去除觸媒老化或失效時,透過再生劑的還原,可以回復第一氧化劑去除觸媒及第二氧化劑去除觸媒活性,而不需要自填充塔10取出第一氧化劑去除觸媒及第二氧化劑去除觸媒或置換,以提高填充塔10的使用壽命。
In one embodiment, the
於一實施例中,第一氧化劑去除觸媒與第二氧化劑去除觸媒兩者皆會在任意濃度之氧化劑進行反應,但第一氧化劑去除觸媒與第二氧化劑去除觸媒的材料設計(例如結構強度、孔隙大小等)不同,而可在不同濃度下展現不同的真實反應速率。例如,第一氧化劑去除觸媒(A材料)可以選用結構堅硬適合直接接觸高濃度氧化劑之材質,惟其孔洞因反應後產生之副產物佔據而降低整體的反應效能,使得處理後的氧化劑從10000ppm下降至4000ppm,此時利用可選用結構相較A材料脆弱但具有質量較輕或是顆粒較小之優勢的B材料作為第二氧化劑去除觸媒,繼續處理殘餘的氧化劑。 In one embodiment, both the first oxidant removal catalyst and the second oxidant removal catalyst will react at any concentration of oxidant, but the material design of the first oxidant removal catalyst and the second oxidant removal catalyst (e.g. Structural strength, pore size, etc.) are different, and can exhibit different true reaction rates at different concentrations. For example, the first oxidant removal catalyst (A material) can be made of a material with a hard structure suitable for direct contact with high concentration of oxidant, but its pores are reduced due to the by-products generated after the reaction and the overall reaction performance is reduced, so that the treated oxidant drops from 10000ppm Up to 4000ppm, at this time, the optional B material, which is weaker than the A material but has the advantage of lighter weight or smaller particles, is used as the second oxidant to remove the catalyst and continue to process the residual oxidant.
於一實施例中,複合型填充材料,可包括第一氧化劑去除觸媒及第二氧化劑去除觸媒,係選自於由碳、石英砂、矽、氧化鋁、天然礦石(例如沸石)、錳、鐵、鉑、鈀、釕、釩、鉻、鈷、銅及鎳所構成的群組,上述材料可為 細沙狀、顆粒狀、球狀、不規則狀、磚形、板式、柱狀、蜂巢狀、多孔材料之任一種形式或不同形狀之組合。且複合型填充材料為顆粒狀或球狀且具有粒徑或直徑0.5mm~10cm,或複合型填充材料為為磚形、板式或柱狀且具有邊長0.1mm~100cm。複合型填充材料除可作為觸媒以處理氧化劑之外,本身也可能具有物性的過濾效果,依據填充材料的尺寸、粒徑或結構,可除去1μm以上的微粒雜質。 In an embodiment, the composite filler material may include a first oxidant removal catalyst and a second oxidant removal catalyst, selected from carbon, quartz sand, silicon, alumina, natural ore (such as zeolite), manganese , Iron, platinum, palladium, ruthenium, vanadium, chromium, cobalt, copper and nickel, the above materials can be Fine sand, granular, spherical, irregular, brick, plate, column, honeycomb, porous material in any form or combination of different shapes. And the composite filling material is granular or spherical and has a particle size or diameter of 0.5 mm to 10 cm, or the composite filling material is brick, plate or column and has a side length of 0.1 mm to 100 cm. In addition to being used as a catalyst to treat oxidants, the composite filler may also have a physical filtering effect. Depending on the size, particle size or structure of the filler, it can remove particulate impurities above 1 μm.
於一實施例中,填充塔可以包括複數個塔體彼此串聯設置,設置的方式可以依據實際過濾的氧化劑種類作調整,同時可根據各填充塔出口氧化劑濃度調整合適組成,例如第一填充塔雙氧水濃度為8000ppm去除後殘餘小於4000ppm,則第二填充塔可選用高佔比之第二氧化劑去除觸媒配比進行雙氧水去除。 In an embodiment, the packed tower may include a plurality of tower bodies arranged in series with each other, and the setting mode may be adjusted according to the type of oxidant actually filtered, and at the same time, a suitable composition may be adjusted according to the concentration of the oxidant at the outlet of each packed tower, for example, hydrogen peroxide in the first packed tower After the concentration is 8000ppm, the residual is less than 4000ppm, then the second packed tower can choose the high proportion of the second oxidant to remove the catalyst ratio for hydrogen peroxide removal.
於一實施例中,複合型填充材料的填充層,也可以依照需求,使用不同尺寸的材料混和填充、間隔填充設置。 In one embodiment, the filling layer of the composite filling material can also be mixed and spaced by using materials of different sizes according to requirements.
圖2-3分別繪示依照本發明一實施例之雙層及三層填充層的填充塔示意圖。請參考圖2,填充塔20包括塔體200、第一填充層202、第二填充層204,承載於塔體200中,用以去除液相或氣相中的氧化劑。塔體200具有一過濾流體入口F及一過濾流體出口O。各層的堆疊方式包括整齊堆疊、隨機堆疊、依照不同粒徑分層排列或不同粒徑混合填充。第一填充層202的材質可為第一氧化劑去除觸媒及第二氧化劑去除觸媒任一者或兩者混合,且第二填充層204的材質可為第一氧化劑去除觸媒及第二氧化劑去除觸媒任一者或兩者混合。並且,第一填充層202及第二填充層204的材質可以相同或不同,第一氧化劑去除觸媒及
第二氧化劑去除觸媒的材質選擇已如前所述,容此不再贅述。於一實施例中,第一填充層202的材料尺寸小於第二填充層204的材料尺寸。
FIG. 2-3 are schematic diagrams of packed towers with double and triple packed layers according to an embodiment of the invention, respectively. Referring to FIG. 2, the packed
請參考圖3,填充塔30包括塔體300、第一填充層302、第二填充層304、第三填充層306,承載於塔體300中,用以去除液相或氣相中的氧化劑。塔體300具有一過濾流體入口F及一過濾流體出口O。各層的堆疊方式包括整齊堆疊、隨機堆疊、依照不同粒徑分層排列或不同粒徑混合填充。第一填充層302、第二填充層304及第三填充層306的材質,分別可為第一氧化劑去除觸媒及第二氧化劑去除觸媒任一者或兩者混合,且第一填充層302、第二填充層304及第三填充層306的材質可以相同或不同,第一氧化劑去除觸媒及第二氧化劑去除觸媒的材質選擇已如前所述,容此不再贅述。於一實施例中,第一填充層302的材料尺寸小於第二填充層304的材料尺寸,且第二填充層304的材料尺寸小於第三填充層306的材料尺寸。
Referring to FIG. 3, the packed
於一實施例中,複合型填充材料的材質為多孔材質,可以增加表面積,提高處理氧化劑的效率。由過濾流體入口F向過濾流體出口O的方向,多孔複合型填充材料的尺寸由小至大排列,使得越接近過濾流體入口F之塔體上部填充的多孔複合型填充材料尺寸較小,例如尺寸為0.6mm~1.5mm第一氧化劑去除觸媒,可先初步濾除3μm以上的微粒,且與氧化劑反應時,待處理的氧化劑會滲入多孔材質地孔洞並被吸附或於內部反應,粒徑越小時反應產生的氣體自材料孔洞內部逸散出來的路徑最短且滯留時間也較短,反應速率最快,可減少氣體膨脹撐開孔洞而造成材料結構破壞。越接近過濾流體出口O的塔體下部填充的多孔複合型填充材料尺寸較大,例如尺寸為1mm~10mm之第二氧化劑去除觸媒,與氧化劑反應時的氣體逸散路徑較長,反應速率最慢。如此一來,可 以在第一階段先處理高濃度的氧化劑,並可降低氧化劑的濃度,當流體進入再進入第二階段處理低濃度的氧化劑,即當過濾流體進入塔體中後段去除殘餘氧化劑時,因為所需處理的氧化劑減少,避免中大顆粒直接處理高濃度氧化劑時,因為氧化劑進入孔洞內反應產氣,破壞多孔複合型填充材料的結構。 In an embodiment, the composite filler material is porous, which can increase the surface area and improve the efficiency of processing the oxidant. From the direction of the filter fluid inlet F to the direction of the filter fluid outlet O, the size of the porous composite packing material is arranged from small to large, so that the size of the porous composite packing material filled closer to the upper part of the tower of the filter fluid inlet F is smaller, for example, the size The first oxidant is 0.6mm~1.5mm to remove the catalyst. The particles above 3μm can be preliminarily filtered out. When reacting with the oxidant, the oxidant to be treated will infiltrate into the pores of the porous material and be adsorbed or react internally. The gas generated during the hour reaction has the shortest path to escape from the inside of the material pores and the residence time is also short, and the reaction rate is the fastest, which can reduce the gas expansion and expand the pores to cause damage to the material structure. The porous composite packing material filled in the lower part of the tower closer to the filter fluid outlet O is larger in size, for example, the second oxidant with a size of 1 mm to 10 mm removes the catalyst, the gas escape path when reacting with the oxidant is longer, and the reaction rate is the most slow. In this way, can In the first stage, the high concentration of oxidant can be treated first, and the concentration of oxidant can be reduced. When the fluid enters and then enters the second stage, the low concentration of oxidant is processed, that is, when the filtered fluid enters the tower body to remove residual oxidant, because Reduced oxidant treatment, avoiding medium and large particles when directly processing high concentration oxidant, because the oxidant enters the hole to react to produce gas, destroying the structure of the porous composite filling material.
此外,可以透過逆洗的方式,亦即,將塔體反置並以清潔液由過濾流體出口O往過濾流體入口F的方向沖洗,可以沖去小顆粒及攔阻的雜質,藉以去除髒污,可延長填充塔的使用壽命。此外,當填充塔使用一段時間,可以直接透過過塔體上部(濾流體入口F區域)補充各種粒徑的複合型填充材料,再透過快速逆洗舉床,可以重新排列以獲得從過濾流體入口F至過濾流體出口O的方向,由小至大排列的複合型填充材料。如有多孔複合型填充材料破損而變成小尺寸顆粒時,也可以透過逆洗作重新排列,回補中上層的填充區域,作為小尺寸多孔複合型填充材料的補充。上述逆洗的實施例,適用於填充塔具有兩層以上的填充層之結構。 In addition, it can be cleaned by backwashing, that is, by inverting the tower and washing it with cleaning fluid from the filter fluid outlet O to the filter fluid inlet F, small particles and blocked impurities can be washed away to remove dirt, The service life of the packed tower can be extended. In addition, when the packed tower is used for a period of time, it can directly supplement the composite packing materials of various particle sizes through the upper part of the tower body (the area of the filter fluid inlet F), and then through the rapid backwashing bed, it can be rearranged to obtain the filter fluid inlet From F to the direction of the filter fluid outlet O, the composite filling materials are arranged from small to large. If the porous composite filler material is damaged and becomes small-sized particles, it can also be rearranged through backwashing to supplement the filling area of the upper and middle layers to supplement the small-sized porous composite filler material. The above embodiment of backwashing is applicable to the structure in which the packed tower has two or more packed layers.
綜上所述,藉由複合型填充材料的填充塔,利用氧化劑去除觸媒處理氧化劑,且利用觸媒再生劑活化並再生氧化劑去除觸媒,可以有效地去除液相或氣相中的氧化劑,還可過濾超過雜質微粒,去除濾達80%-100%。 In summary, through the packed tower of the composite packing material, the oxidant is used to remove the catalyst to treat the oxidant, and the catalyst regenerant is used to activate and regenerate the oxidant to remove the catalyst, which can effectively remove the oxidant in the liquid phase or gas phase. It can also filter particles that exceed impurities, removing filtration up to 80%-100%.
10‧‧‧填充塔 10‧‧‧packed tower
100‧‧‧塔體 100‧‧‧ Tower
102‧‧‧複合型填充材料 102‧‧‧Composite filling material
F‧‧‧過濾流體入口 F‧‧‧Fluid inlet
O‧‧‧過濾流體出口 O‧‧‧filtered fluid outlet
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TW200902454A (en) * | 2007-03-16 | 2009-01-16 | Kurita Water Ind Ltd | Method and apparatus for organic matter removal |
TW200904762A (en) * | 2007-07-18 | 2009-02-01 | Taiwan Environment Scient Co Ltd | Chemical oxidation method for remediating organic pollutants in the environment |
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