臺灣博碩士論文加值系統

揮發性有機化合物及甲醛，常存於建材製造或裝修工程中所使用之建材、塗料及接著劑等，於室內造成甲醛逸散0.11~2.11 ppm，遠高於WHO室內管制標準0.08 ppm，雖隨時間甲醛會緩慢下降，其致癌風險為可接受致癌風險 (10-6) 之100~1000倍，且其逸散釋放期達3~15年，成為室內空氣污染的隱形殺手。台灣屬高溫高濕環境，使用吸附劑會有再脫附的問題，利用二氧化鈦為觸媒，可分解有害的有機物成無害物質，達到淨化大氣功能。因此本研究以溶膠凝膠法製備鋅鐵二氧化鈦及覆膜於椰殼活性碳、煤質活性碳及天然沸石等質材，以期延長吸附材生命週期並改善室內空氣品質，進行基本性質分析、BET-比表面積及孔隙體積分析、掃描式電子顯微鏡表面結構觀察、能量發散光譜儀元素分析、X射線繞射分析、水氣等溫吸脫附、水及甲醛之動力吸脫附實驗，甲醛氣袋吸附及光催化實驗。探討鋅鐵共摻二氧化鈦覆膜活性碳及沸石對甲醛之去除。
在SEM觀察，塊狀表面含片狀的二氧化鈦存在明顯的銳鈦礦(25.28o)及金紅石礦 (27.42o) 特徵峯，然而同樣是塊狀但含不規則碎屑的鋅鐵二氧化鈦其波峰極弱；其對甲醛吸附移除量相近分別為0.086及0.084 g kg-1
，但二氧化鈦在捕蚊燈及日光下的光解移除量在2小時內分別為0.104及0.111 g kg-1，而鋅鐵二氧化鈦在24小時為0.108及0.091 g kg-1。顯示鋅鐵添加破壞二氧化鈦形成銳鈦礦及金紅石晶相結構，降低對甲醛的光催化分解作用及速率。
有機質以絲狀層層相疊的椰殼活性碳最高為98.2%，而含層狀深溝的煤質為56.7%，EDS分析，其表面碳原子分別為94.2%及90.7%，且其對水的等溫吸脫附屬於IUPAC所分類的第V型，低濕度下吸附量低，提高濕度吸附量大幅增加，於45%~75%RH有遲滯現象，屬於微孔或中孔吸附劑。沸石類似於IUPAC所分類的第Ⅱ型，單層吸附後，隨濕度提高多層吸附發生，且為H4型有狹長縫狀孔隙，此與SEM圖相吻合。10%RH質材對甲醛的氣袋吸附 (氣袋實驗) 移除量，椰殼及煤質為0.097 g kg-1、天然沸石0.025 g kg-1；而在75%RH則分別為0.417 g kg-1、0.419 g kg-1及0.166 g kg-1，顯示空氣濕度的提升有助質材對甲醛的吸附。而質材間的吸附差異應來自BET-比表面積的差異，因椰殼684 m2 g-1 (微孔佔83%) ，煤質761m2 g-1 (微孔佔58%) ，沸石最低為34.9 m2 g-1，炭材具較大的非極性表面，尤其是椰殼有較多的微孔表面。
二氧化鈦覆膜易造成質材微孔損失而鋅鐵二氧化鈦覆膜易填塞於質材孔洞造成微孔及中大孔的減少，造成BET-比表面積下降愈明顯，如椰殼覆膜二氧化鈦及鋅鐵二氧化鈦分別為664及398 m2 g-1，對甲醛的吸附降為0.366和0.361g kg-1；而煤質則分別為584及512 m2 g-1，對甲醛的吸附為0.351和0.339 g kg-1；至於沸石為38及22 m2 g-1，對甲醛則為0.186和0.187 g kg-1，顯示覆膜造成質材BET-比表面積降低也降低對甲醛的吸附。
在XRD分析中，煤質及椰殼覆二氧化鈦皆有銳鈦礦晶相存在，而鋅鐵二氧化鈦覆膜未發現，至於沸石皆出現25.76°及27.86°特徵峯。由SEM圖像，二氧化鈦覆膜在質材表面覆蓋一明顯的二氧化鈦層，造成煤質表面Ti/C為1.86，椰殼0.19，而沸石Ti/SiO2為0.10；鋅鐵二氧化鈦覆膜椰殼為0.02及煤質0.01，而沸石Ti/SiO2為0.02；可見鋅鐵的添加降低二氧化鈦在質材的覆蓋效果。在日光及捕蚊燈下，對甲醛光解量，二氧化鈦覆膜煤質 (0.073及0.112 g kg-1) 、椰殼 (0.033及0.067 g kg-1) 及沸石 (0.101及0.203 g kg-1) 皆較鋅鐵二氧化鈦覆膜煤質 (0.042及0.091 g kg-1) 、椰殼 (0.039及0.052 g kg-1) 及沸石 (0.093及0.119 g kg-1) 佳，且在捕蚊燈下的效果皆較日光佳，其中二氧化鈦覆膜沸石因甲醛量足夠隨時間仍持續進行光催化分解作用，因此其光解量為所有覆膜質材中效果最佳，顯示二氧化鈦的光解持續性是可期的。光解後各氣袋的二氧化碳濃度 (50-360 ppm) 皆有上升，在捕蚊燈下二氧化碳濃度 (185-360 ppm) 增加量較日光燈下 (50-150 ppm) 高。

Volatile organic compounds and formaldehyde are common in building materials, paint and adhesive agent, which can cause formaldehyde to emit 0.11~2.11 ppm which is higher than the WHO indoor control standard (0.8 ppm), used for making building materials and fixing up a building. Although as time goes on formaldehyde will slowly decrease, the risk at causing cancer is 100~1000 times higher than the acceptable risk (10-6). Moreover, since its releasing period lasts for 3 to 15 years, it becomes invisible killer of indoor air pollution. Taiwan is a hot and humid place. There may be the problem of desorption when using adsorbents. However, the use of titanium dioxide as a catalyst can degrade harmful organics into harmless substances and purify air. Therefore, this study focuses on preparing zinc and iron co-doped titanium dioxide and sol-gel titanium coating coconut shell activated carbon, coal activated carbon and natural zeolite etc, in order to extend the life cycle of the adsorptive materials and improve indoor air quality. The properties of materials, specific surface area and porosity, surface structure image and element composition with scanning electron microscope (SEM) and energy dispersive spectrometer (EDS), X-ray diffraction, the water isotherms and kinetics, kinetics of formaldehyde, adsorption and photolysis of formaldehyde airbag experiments. To explore zinc and iron co-doped titanium dioxide coated activated carbon and zeolite on the removal of formaldehyde.
The result shows that with the SEM, titanium dioxide whose block surface contains sheets has obvious characteristic peaks of anatase (25.28o) and rutile (27.42o). Otherwise, zinc and iron co-doped titanium dioxide whose block surface contains random pieces has very weak peaks. But the formaldehyde adsorption of removal for them is close and is 0.086 and 0.084 g kg-1 respectively. Under the irradiation of mosquito and fluorescent lamp for 2 hours, the removal of formaldehyde for titanium dioxide is 0.104 and 0.111 g kg-1 respectively. Besides, under the irradiation of them for 4 and 24 hours, the removal for zinc and iron co-doped titanium dioxide is 0.113 and 0.091 g kg-1 respectively. It demonstrates that adding zinc and iron to titanium dioxide destroys the phenomenon of titanium dioxide forming anatase and rutile crystal structure, which reduces the effect and rate of photolytic degradation for formaldehyde.
The organic matter for layer-by-layer and filamentous coconut shell activated carbon is 98.2%. And it with coal activated carbon of layered- groove accounts for 56.7%. With EDS analysis, the superficial carbon atoms is 94.2% and 90.7% respectively. The isotherms of water on activated carbon are classified as the V-type in IUPAC. The adsorption amount of water in low humidity is low, and adsorption amount increased significantly when raising the humidity. What’s more it has hysteresis at 45% ~ 75% RH, which means it belongs to micro-porous or meso-porous adsorbent. Zeolites are similar typeⅡ in IUPAC classification multilayer adsorption occurs with increasing humidity after monolayer adsorption. And their H4 type has narrow slit-like pores, which is consistent with the SEM image. In 10% RH airbag experiments, the remove of adsorption on coconut shell activated carbon and coal activated carbon is 0.097 g kg-1 and that of natural zeolite is 0.025 g kg-1. And for these materials in 75% RH, the remove is 0.417 g kg-1, 0.419 g kg-1 and 0.166 g kg-1 respectively. It shows raising humidity enhance the adsorption of formaldehyde for these materials. The difference of adsorption among these materials may come from the difference of their BET-specific surface area. The BET-specific surface area of coconut shell activated carbon is 684 m2 g-1 (83% porous); coal activated carbon is 761m2 g-1 (58% porous), and zeolite has minimum of 34.9 m2 g-1. Activated carbon processes larger non-polar surfaces, especially coconut shell activated carbon, it has more micro-porous surface.
Coating titanium dioxide can easily lead to the loss of material micro-porous and coating zinc and iron co-doped titanium dioxide cause it to jam in the material pores and give rise to the reduction of meso-pores, macro-pores and micro-pores, which can result in BET-specific surface area decreasing more obviously. For example, the BET-specific surface area of coconut shell activated carbon coated titanium dioxide and zinc and iron co-doped titanium dioxide is 664 and 398 m2 g-1 respectively, and the adsorption of formaldehyde for them reduces to 0.366 and 0.361g kg-1 respectively, coal activated carbon is 584 and 512 m2 g-1 respectively, and the adsorption of formaldehyde for them is 0.351 and 0.339 g kg-1 respectively. Zeolite is 38 and 22 m2 g-1 respectively, and the adsorption of formaldehyde for them is 0.186 and 0.187 g kg-1 respectively. They display that coating results in not only reduction of material BET-specific surface area but also reduction of formaldehyde adsorption.
In the XRD analysis, titanium dioxide coated coal activated carbon and coconut shell activated carbon both process anatase crystalline, but zinc and iron co-doped titanium dioxide coated doesn’t, zeolite has characteristic peaks of 25.76° and 27.86°. By the SEM image, with thick coating titanium dioxide, the Ti/C of coal activated carbon surface is 1.86; that of coconut shell activated carbon is 0.19 and Ti/SiO2 of zeolite is 0.10. With coating zinc and iron co-doped titanium dioxide, the Ti/C of coconut shell activated carbon is 0.02, coal activated carbon is 0.01 and the Ti/SiO2 of zeolite is 0.02. The addition of zinc and iron reduces the coating effects of titanium dioxide. Under the irradiation of fluorescent (24hr) and mosquito lamp (6hr), the photolytic amount of formaldehyde for titanium dioxide coated coal activated carbon (0.073 and 0.112 g kg-1), coconut shell activated carbon (0.033 and 0.067 g kg-1) and zeolite (0.101 and 0.203 g kg-1 ) are all higher than that for zinc and iron co-doped titanium oxide coated coal activated carbon (0.042 and 0.091 g kg-1), coconut shell activated carbon (0.039 and 0.052 g kg-1) and zeolite (0.093 and 0.119 g kg-1). Furthermore, the effect under the irradiation of mosquito lamp is better than that under the irradiation of fluorescent. Because titanium dioxide coated zeolite is in sufficient amount of formaldehyde, it continues its photolytic degradation as time goes on. Consequently, the photolytic amount for it is the most among these materials, which indicates that the photolysis continuity of titanium dioxide can be expected. The concentration of carbon dioxide (50-360 ppm) in each airbag increases after photolysis. The addition of concentration of carbon dioxide under the irradiation of mosquito lamp (180-360) is more than under the irradiation of fluorescent lamp (50-150 ppm).

摘 要.............................................I
Abstract.........................................IV
誌 謝..........................................VIII
目錄..............................................IX
表目錄...........................................XIII
圖目錄............................................ XV
第1章 前言..........................................1
1.1 研究緣起………………………………… ………………….1
1.2 研究目的...................................2
第2章 文獻回顧.......................................3
2.1 室內空氣品質問題.............................3
2.2 室內空氣污染物...............................3
2.3 甲醛特性及危害...............................5
2.3.1甲醛物化性質.............................5
2.3.2甲醛用途................................5
2.3.3甲醛危害................................6
2.3.4 室內甲醛的逸散、累積及控制................7
2.4 室内甲醛污染控制.............................10
2.5吸附機制及其應用 ...........................11
2.5.1吸附機制................................11
2.5.2吸附模式...............................12
2.5.3等溫吸附曲線............................12
2.5.4 遲滯迴路...............................13
2.5.5 吸附劑................................14
2.5.5.1 活性碳..........................16
2.5.5.2 沸石............................17
2.6 光觸媒原理及種類.............................19
2.7二氧化鈦.....................................20
2.7.1二氧化鈦結構.............................20
2.7.2光催化反應機制...........................22
2.7.3二氧化鈦光催化之改良......................24
2.7.4二氧化鈦製備方式.........................25
2.7.5二氧化鈦改質結合吸附劑....................27
第3章 材料與方法 ...................................28
3.1 吸附質.....................................28
3.2 吸附劑.....................................28
3.2.1 質材前處理.............................28
3.3 光觸媒之製備 ...........................29
3.3.1 二氧化鈦及鋅鐵共摻二氧化鈦粉末之製備.......29
3.3.2 二氧化鈦覆膜之製備......................30
3.3.3 鋅鐵共摻二氧化鈦覆膜之製備...............30
3.4 質材基本性質分析.............................33
3.4.1 酸鹼值測定.............................33
3.4.2 總體密度及顆粒密度測定...................33
3.4.3 有機質及灰份測定........................34
3.5 質材比表面積及孔隙分析........................34
3.6 質材表面結構與元素分析........................34
3.7 X射線繞射分析...............................35
3.8 微量天平吸附實驗.............................36
3.8.1 水氣之等溫吸脫附實驗.....................37
3.8.2 水及甲醛之動力吸脫附實驗..................37
3.9 甲醛光催化實驗...............................38
3.9.1甲醛溶液及檢量線製備......................38
3.9.2 質材吸附及光催化實驗.....................38
3.9.2.1 質材吸附實驗......................39
3.9.2.2 二氧化鈦粉末吸附及光解實驗..........39
3.9.2.3 二氧化鈦覆膜質材吸附及光解實驗.......39
第4章 結果與討論.......................................42
4.1質材基本性質...................................42
4.2 質材比表面積及孔隙分析.........................44
4.3質材表面結構與元素分析..........................46
4.3.1質材表面結構分析..........................46
4.3.2質材元素分析.............................52
4.4 X射線繞射分析................................54
4.5 質材對水氣之等溫吸脫附.........................58
4.6 水氣及甲醛之動力吸脫附.........................60
4.7 甲醛的吸附及光催化............................63
4.7.1 質材對甲醛的吸附.........................63
4.7.2 光觸媒粉末對甲醛的光解....................63
4.7.3 覆膜質材對甲醛的吸附及光解.................64
4.7.4 二氧化碳測定.............................65
第5章 結論與建議........................................73
5.1 結論.........................................73
5.2 建議.........................................74
第6章 參考文獻..........................................75
作者簡介...............................................81

表2-1 常見的室內空氣污染物及其對健康的影響..................4

表2-2 甲醛濃度對人體之影響................................6

表2-3 甲醛濃度與暴露時間對人體健康之影響....................7

表2.4 各國室內甲醛管制標準或建議值.........................9

表2-5 物理吸附與化學吸附之特性............................11

表2-6 常用吸附劑之比表面積...............................15

表2-7 工業上常用的吸附劑特性比較..........................15

表2-8 浸漬前後對甲醛溶液蒸氣與水蒸汽的靜態吸附量.............16

表2-9 浸漬前後預吸附水蒸氣後對甲醛溶液蒸氣的靜態吸附量........17

表2-10 甲醛濃度和活性碳的淨化效率.........................17

表2-11 不同觸媒製備方法之優缺點...........................26

表3-1 實驗藥品.........................................30

表3-2 攜帶式甲醛分析儀基本資料............................37

表4-1 質材基本性質......................................43

表4-2 質材比表面積及孔隙分析..............................45

表4-3 質材元素分析......................................53

表4-4 質材不同濕度下對水的吸附量...........................60

表4-5 質材在11%RH對水及甲醛的動力吸脫附量...................63

表4-6質材在60%RH對水及甲醛的動力吸脫附量....................63

表4-7 光解後二氧化碳濃度變化...............................72

圖2-1 六種型態之吸附曲線..................................12

圖2-2 遲滯迴路..........................................14

圖2-3 常用光觸媒材料之能隙值..............................20

圖2-4 銳鈦礦及金紅石結構.................................21

圖2- 5 二氧化鈦相圖.....................................22

圖2-6光催化反應機制圖....................................23

圖2-7 吸附劑與光觸媒結合示意圖............................27

圖3-1 三種0.5~1.0 nm質材外觀............................29

圖3-2光觸媒覆膜質材之外觀................................31

圖3-3光觸媒製備流程圖...................................32

圖3-4 微量天平系統圖....................................36

圖3-5 甲醛檢量線.......................................38

圖3-6氣袋光催化實驗流程圖................................41

圖4-1二氧化鈦之SEM圖....................................47

圖4-2鋅鐵共摻二氧化鈦之SEM圖.............................47

圖4-3椰殼活性碳之SEM圖..................................48

圖4-4煤質活性碳之SEM圖..................................48

圖4-5二氧化鈦覆膜椰殼活性碳之SEM圖........................49

圖4-6二氧化鈦覆膜煤質活性碳之SEM圖........................49

圖4-7鋅鐵共摻二氧化鈦覆膜椰殼活性碳之SEM圖.................50

圖4-8鋅鐵共摻二氧化鈦覆膜煤質活性碳之SEM圖.................50

圖4-9 天然沸石之SEM圖..................................51

圖4-10 二氧化鈦覆膜天然沸石之SEM圖.......................51

圖4-11 鋅鐵共摻二氧化鈦覆膜天然沸石之SEM圖.................51

圖4-12 銳鈦礦標準圖譜...................................54

圖4-13 金紅石標準圖譜...................................55

圖4-14 光觸媒XRD圖.....................................55

圖4-15 不同覆膜椰殼活性碳XRD圖...........................56

圖4-16 不同覆膜煤質活性碳XRD圖...........................56

圖4-17 不同覆膜天然沸石XRD圖.............................57

圖4-18 天然沸石XRD圖....................................57

圖4-19 質材對水的等溫吸脫附曲線...........................59

圖4-20 質材在11%RH對水的動力吸脫附曲線....................61

圖4-21 質材在11%RH對甲醛的動力吸脫附曲線...................61

圖4-22 質材在60%RH對水的動力吸脫附曲線....................62

圖4-23 質材在60%RH對甲醛的動力吸脫附曲線..................62

圖4-24 質材吸附甲醛之濃度變化............................66

圖4-25 質材吸附甲醛之移除率..............................66

圖4-26質材吸附甲醛之移除量...............................67

圖4-27 二氧化鈦粉末光解甲醛之濃度變化.....................67

圖4-28 二氧化鈦粉末光解甲醛之移除率.......................68

圖4-29 二氧化鈦粉末光解甲醛之移除量.......................68

圖4-30在日光燈下質材對甲醛吸附及光解之濃度變化..............69

圖4-31在日光燈下質材對甲醛吸附及光解之移除率................69

圖4-32在日光燈下質材對甲醛吸附及光解之移除量................70

圖4-33在捕蚊燈下質材對甲醛吸附及光解之濃度變化..............70

圖4-34在捕蚊燈下質材對甲醛吸附及光解之移除率................71

圖4-35在捕蚊燈下質材對甲醛吸附及光解之移除量................71

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