臺灣博碩士論文加值系統

都市廢水經污水處理所產生下水污泥，含大量易腐敗有機物，隨意棄置會造成環境及公共衛生問題，根據中華民國九十九年版污水下水道統計要覽所載，目前下水污泥大多採焚化與掩埋方式處理，由於部分下水污泥會藉焚化方式形成污泥焚化灰，因此下水污泥與污泥焚化灰為本研究之主要研究對象。此外花蓮縣主要的產業尚包括造紙業與石材加工業，故紙漿污泥與石材污泥亦為研究對象。本研究旨在開發污泥之資源化技術，研究目標分為低溫共燒技術製備輕質骨材與表面改質技術製備染料吸附劑兩部分，以期能擴展污泥之再利用用途進而促進污泥資源化。
在眾多污泥處置技術中，以燒結法形成輕質骨材，因同時具有再利用與減少天然建材消耗之優點而備受重視。但燒製輕質骨材需要使污泥形成熔融玻璃相，燒製溫度多超過1000 oC能量消耗大，製造成本高。為解決此缺點，本研究藉添加硼酸(H3BO3)與碳酸鈉(Na2CO3)等低熔點物質做為助熔劑與污泥進行低溫共燒，使污泥燒製溫度降低。透過骨材之吸水率、視孔隙率、體密度、抗壓強度、健性等試驗以了解不同實驗條件對骨材性質的影響。
依本研究實驗規劃，下水污泥先以SiO2調質，使SiO2/Al2O3=4:1。當H3BO3為助熔劑時，需再添加調質污泥3 wt%之CaO以消除骨材黑心現象。H3BO3添加量為調質污泥之13 wt%，在400 oC持溫0.5 hr，850 oC持溫1 hr可得抗壓強度最高之輕質骨材，其吸水率、視孔隙率、體密度、抗壓強度分別為3.88 %、3.93 %、1.05 g/cm3、29.7 Mpa。以Na2CO3為助熔劑時，添加量為調質污泥之16 wt%，以400 oC持溫0.5 hr，900 oC持溫1 hr亦可得抗壓強度最強之輕質骨材，其前述之四項參數試驗結果分別為1.36 %、1.7 %、1.26 g/cm3、27.7 MPa。
污泥灰為下水污泥先經過900 oC灼燒1小時後形成。如同下水污泥，污泥灰先以SiO2調質，使SiO2/Al2O3=4:1再進行燒製實驗。以H3BO3為助熔劑時，最佳燒製方式：H3BO3添加量為調質污泥灰22 wt%，以900 oC持溫15 min可得高抗壓輕質骨材，其四項參數試驗結果分別為5.43 %、5.15 %、0.97 g/cm3與29.2 Mpa。調質污泥灰添加22 wt%之Na2CO3為助熔劑，以900 oC持溫0.5 hr可得抗壓強度高之輕質骨材，其四項參數試驗結果分別為1.42 %、1.64 %、1.17 g/cm3及88.4 MPa。
紙漿污泥含矽量較低，先以SiO2調質，使濕污泥中含SiO2為13 wt%。添加調質污泥18 wt%之H3BO3為助熔劑，以890 oC持溫30 min可得低吸水率之輕質骨材，其前述之四項參數分別為4.64 %、2.77 %、及0.6 g/cm3、13.2 MPa。
石材污泥最佳之燒製條件為：添加污泥15 wt%之H3BO3為助熔劑，850 oC持溫15 min可得輕質骨材，其吸水率、視孔隙率、體密度及抗壓強度分別為0.21 %、0.35 %、1.67 g/cm3 及66.94 MPa。
除了輕質骨材資源化，本實驗第二部在於吸附劑資源化技術開發，選定下水污泥，污泥灰與紙漿污泥為實驗對象，選擇之離子性染料為陽離子性染料亞甲基藍(Methylene Blue，MB)及陰離子性染料普施安紅(Procion Red MX-5B，PR)。下水污泥具有含富氧官能基之有機物而可成為水體中污染物之吸附材料。為使污泥具有陰陽離子性染料的吸附能力，並且提升污泥過濾效率，本實驗利用水熱法將Fe3O4合成於污泥顆粒表面，一方面作為離子性染料之吸附位，另一方面透過Fe3O4之結晶顆粒改善污泥之過濾特性。實驗結果顯示，鐵氧磁體化污泥對MB與PR兩種染料的理想吸附pH分別為6與3，其吸附模式滿足Langmuir equation，經計算所得之最大吸附量分別為25.06 mg/g與18.83 mg/g。依動力學實驗結果，符合pseudo-second-order動力學模型，其吸附活化能分別為42.78 kJ/mol (MB)與32.69 kJ/mol (PR)。鐵氧磁體結晶合成於污泥顆粒表面，可大幅改善污泥之過濾效率，透過過濾阻抗實驗量測結果，污泥之過濾阻抗值，由1.34×107 s2/g降至0.08×107 s2/g以下。
相較於下水污泥，由於污泥灰經過熱處理程序，有機物均氧化為二氧化碳氣體逸失，故污泥灰顆粒缺少含官能基之有機物質幫助吸附，因此本實驗將污泥灰進行鐵氧磁體化，利用Fe3O4作為活性吸附位而使其能資源化形成離子性染料吸附材料。由於鐵氧磁體其顆粒界達電位在酸性環境具正值，在鹼性環境中則為負值，故可藉靜電引力對離子性染料產生吸附。實驗結果顯示，在鹼性環境中對MB的吸附效果較佳，反之酸性中對PR吸附效果較好，符合界達電位之結果。等溫吸附結果符合Langmuir equation，動力學上符合pseudo-second-order模型，計算所得之最大吸附量分別是22.27 mg/g (針對MB)，28.8 mg/g (針對PR)，其吸附活化能則分別為61.7 kJ/mol 與9.07 kJ/mol。
紙漿污泥含有大量纖維及其他有機化合物，可藉由熱解法使污泥形成活性碳,作為染料之吸附劑。故本實驗藉紙漿污泥在氮氣氛中熱解成為活性碳而製備染料吸附劑。實驗條件為在氮氣氛下，於600 oC熱解1 hr，樣品以1M HCl水洗後再以蒸餾水水洗，烘乾形成活性碳吸附劑。依吸附實驗結果，紙漿污泥製備之活性碳符合Langmuir equation及pseudo-second-order模型。其對MB與PR之最大吸附量分別為119.1 mg/L及65.8 mg/L，其吸附活化能則為8.66 kJ/mol及2.47 kJ/mol。

Sewage sludge is produced by urban waste water treatment. Because of the perishable organic substances, sludge disposal without advanced treatment can produce public health problem. Lightweight aggregate synthesized with sewage sludge is a feasible method for sludge recycling and natural constructive materials saving, but the sintering temperature is always over 1000 oC to form melting glassy phase and large energy is consumed. This study focused on adding some low melting point compounds (H3BO3 and Na2CO3) as flux in order to lower the sintering temperature of artificial aggregates. Water adsorption, apparent porosity, bulk density, compressive strength, and soundness test were applied to evaluate the effect of experiment condition on the characteristics of synthetic aggregates. In addition, there were three other wastes which were used as raw materials for aggregates synthesis in this study, including sludge ash derived from sewage sludge, paper sludge and stone manufacturing sludge. As a result, all these industrial waste could be transformed to lightweight aggregates by thermal treatment and the characteristics of these aggregates were different in a reasonable range.
According to the experimental design, sewage sludge was adjusted by adding SiO2 to make the SiO2/Al2O3 ratio of the conditioned sludge up to 4. When the flux of H3BO3 was used, 3 wt% of conditioned sludge of CaO was added to prevent the occurrence of black core phenomenon. Conditioned sewage sludge mixed with 13 wt% H3BO3 and 3 wt% CaO were heated at 400 oC for 0.5 hr and 850 oC for 1hr was followed to get highest compressive strength aggregate. The values of four primary parameters of aggregate (including water adsorption, apparent porosity, bulk density and compressive strength) were 3.88 %, 3.93 %, 1.05 g/cm3, 29.7 MPa. The flux was Na2CO3, the highest value of compressive strength of aggregates were got when sludge mixed with 16 wt% Na2CO3 and sintered at 400 oC for 0.5 hr; 900 oC for 1 hr. The values of the four primary parameters of aggregates are 1.36 %, 1.7 %, 1.26 g/cm3, and 27.7 MPa.
Sewage sludge ash was also adjusted by adding SiO2 and the ratio of SiO2/Al2O3 was 4. The identical dosages of both H3BO3 and Na2CO3 were 22 wt% of conditioned ash. When the flux was H3BO3, the synthetic aggregates with high compressive strength were sintered at 900 oC for 15 min. When the flux was Na2CO3, the aggregates with higher compressive strength were sintered at 900 oC for 0.5 hr. The values of the four primary parameters of aggregates mentioned above were 5.43 %、5.15 %、0.97 g/cm3、29.2 MPa and 1.42 %、1.64 %、1.17 g/cm3、88.4 MPa respectively.
Because the content of Si of paper sludge was too low, SiO2 was added to make the SiO2 content up to 12 wt% of the wet paper sludge. The dosage of H3BO3 was 18 wt% of the conditioned paper sludge and the sintering program was 890 oC for 30 min. The aggregates synthesized with this procedure have the lower water adsorption and the values of the four primary parameters of aggregates are 4.64 %, 2.77 %, 0.6 g/cm3, and 13.2 MPa.
Lightweight aggregates can be produced from stone manufacturing sludge with 15 wt% of H3BO3. The sintering program was set for 850 oC 15 min. The water adsorption, apparent porosity, bulk density and compressive strength of the aggregates were 0.21 %, 0.35 %, and 1.67 g/cm3 and 66.9 MPa.
Sewage sludge, sewage sludge ash and paper sludge were investigated to be adsorbent for Methylene Blue (MB, cationic dye) and Procion Red MX-5B (PR, ionic dye). Sewage sludge contained organic compounds with oxygen-rich functional group (such as humic substances) which can adsorb pollutants in the water. In order to improve the adsorption ability and filtration efficiency of sewage sludge, Fe3O4 was synthesized on the sewage sludge by hydrothermal method. Fe3O4 can not only act as an adsorptive site for ionic dye, but also decrease the specific resistance of sewage sludge by crystallization. The experimental results showed that ideal pH for modified magnetic sewage sludge to adsorb MB and PR were 6 and 3, and the isotherm adsorption was fitted well to Langmuir equation. The maximum adsorption capacity for MB and PR were 25.06 and 18.83 mg/g. Pseudo-first-order and pseudo-second-order models were utilized to realize the kinetic adsorption of MB and PR. The adsorption data of both dyes were fitted pseudo-second-order model well and the activation energy of MB and PR adsorption were 42.78 kJ/mol and 32.69 kJ/mol, respectively. The crystalline of Fe3O4 synthesized on sewage sludge improved the filtration efficiency of modified magnetic adsorbent and the filtration resistance was decreased from 1.34×107 s2/g to less than 0.08×107 s2/g.
Different from sewage sludge, sludge ash was under thermal treatment and the organic compounds were oxidized to CO2 so that sludge ash particle possessed no organic functional group on the surface. In this study, ferrite process was also conducted on sludge ash and Fe3O4 can act as adsorptive site for ionic dyes because Fe3O4 can provide electrostatic attraction to ionic dyes. The zeta potential of Fe3O4 was positive in acid and anionic dye can be adsorbed. Similarly, that was negative in alkali solution and cationic dye can be adsorbed. As the result of adsorption, MB was well adsorbed in pH 9 and that for PR was 2.7 which corresponded to the zeta potential of modified magnetic sludge ash. The isotherm adsorption and kinetic adsorption of MB and PR were also investigated. For isotherm adsorption, the results were fitted Langmuir equation well and the maximum adsorption capacities of MB and PR were 22.27 mg/g and 28.8 mg/g. For kinetic adsorption, pseudo-first-order and pseudo-second-order models were utilized to examine the adsorption behavior and the results were fitted pseudo-second-order models well. The activation energy calculated from Arrhenius equation was 61.7 kJ/mol for MB and 9.07 kJ/mol for PR.
Owing to paper sludge contained large amount of organic compounds such as fibers and lignin, it could be pyrolyzed to form activated carbon for dye adsorption. In this study, paper sludge was pyrolyzed under nitrogen atmosphere at 600 oC 1 hr. Then, sample was washed with 1 M HCl and DI water, and dried in an oven. The zeta potential measurement of adsorbent showed that the isoelectric point of paper sludge derived activated carbon was around 3 which meant PR should be adsorbed well below pH 3 and that of MB was in neutral or alkali solution. The effect of pH on adsorption, isotherm adsorption and kinetic adsorption were examined to realize the adsorption behavior of paper sludge derived activated carbon. The results of adsorption in different pH condition were conformed to the results of zeta potential. The data of isotherm adsorption experiment revealed that the adsorption behavior can be described by Langmuir equation well and the maximum adsorption capacities of MB and PR were 119.1 mg/L and 65.8 mg/L. Kinetic adsorption revealed that the adsorption of two dyes were fitted pseudo-second-order model well, and the activation energy of MB and PR adsorption were 8.66 and 2.47 kJ/mol.

中文摘要 I
ABSTRACT V
目錄 IX
表目錄 XV
圖目錄 XVII
第一章 緒論 1
1-1前言 1
1-1-1污泥輕質骨材資源化技術 2
1-1-1-1 下水污泥製備輕質骨材 4
1-1-1-2 下水污泥灰製備輕質骨材 5
1-1-1-3紙漿污泥燒製陶瓷材料 6
1-1-1-4石材污泥燒製陶瓷材料 7
1-1-2污泥之吸附劑資源化技術 8
1-1-2-1下水污泥製備吸附劑 8
1-1-2-2污泥灰製備吸附劑 10
1-1-2-3 紙漿污泥製備吸附劑 11
1-2研究動機與目的 12
1-3研究架構 13
第二章 理論基礎 15
2-1低溫共燒技術 15
2-2 表面改質技術 16
2-2-1鐵氧磁體化 16
2-2-2 熱解技術 17
2-3 染料吸附研究 18
2-3-1 等溫吸附模型 18
2-3-2 吸附動力學 20
第三章 實驗材料與方法 23
3-1實驗樣品與藥劑 23
3-2低溫共燒製備輕質骨材 25
3-2-1污泥特性分析 25
3-2-2輕質骨材燒製 26
3-2-2-1 下水污泥燒製輕質骨材 26
3-2-2-2污泥灰燒製輕質骨材 27
3-2-2-3紙漿污泥燒製輕質骨材 29
3-2-2-4石材污泥燒製輕質骨材 30
3-2-3骨材特性試驗 31
3-2-3-1吸水率、體密度、視孔隙率試驗 31
3-2-3-2抗壓強度試驗 31
3-2-3-3健性試驗 32
3-3表面改質製備染料吸附劑 32
3-3-1吸附劑性質分析方法 32
3-3-2下水污泥鐵氧磁體化 33
3-3-3污泥灰鐵氧磁體化 35
3-3-4紙漿污泥熱解 37
3-3-5離子性染料濃度及吸附量測定 39
3-3-6溶液化學需氧量(COD)測定 39
3-3-7吸附活化能 40
3-3-8過濾阻抗實驗 40
第四章 低溫共燒製備輕質骨材 43
4-1下水污泥製備輕質骨材 43
4-1-1下水污泥特性分析 43
4-1-2以H3BO3為助熔劑進行輕質骨材製備 45
4-1-2-1過篩條件對骨材性質影響 45
4-1-2-2骨材黑心現象探討 46
4-1-2-3 H3BO3添加量對骨材性質影響 48
4-1-2-4燒製溫度對骨材性質影響 49
4-1-2-5持溫時間對骨材性質影響 52
4-1-3以Na2CO3為助熔劑進行輕質骨材製備 56
4-1-3-1過篩條件對骨材性質影響 56
4-1-3-2 Na2CO3添加量對骨材性質影響 58
4-1-3-3燒製溫度對骨材性質影響 59
4-1-3-4持溫時間對骨材性質影響 61
4-2下水污泥灰製備輕質骨材 64
4-2-1下水污泥灰特性分析 64
4-2-2以H3BO3為助熔劑進行輕質骨材製備 64
4-2-2-1過篩條件對骨材性質影響 64
4-2-2-2 H3BO3添加量對骨材性質影響 65
4-2-2-3燒製溫度對骨材性質影響 67
4-2-2-4持溫時間對骨材性質影響 70
4-2-3以Na2CO3為助熔劑進行輕質骨材製備 72
4-2-3-1過篩條件對骨材性質影響 72
4-2-3-2 Na2CO3添加量對骨材性質影響 73
4-2-3-3燒製溫度對骨材性質影響 75
4-2-3-4持溫時間對骨材性質影響 77
4-3紙漿污泥製備輕質骨材 79
4-3-1紙漿污泥特性分析 79
4-3-2以H3BO3作為助熔劑燒製輕質骨材 80
4-3-3燒製溫度對骨材性質影響 81
4-3-4 H3BO3添加量對骨材性質影響 83
4-3-5持溫時間對骨材性質影響 85
4-3-6紙漿污泥燒製輕質骨材之效益評估 87
4-4石材污泥製備輕質骨材 89
4-4-1石材污泥特性分析 89
4-4-2 H3BO3添加量對骨材性質影響 90
4-4-3燒製溫度對骨材性質影響 92
4-4-4 持溫時間對骨材性質影響 93
第五章 表面改質製備吸附劑 95
5-1下水污泥製備離子性染料吸附劑 95
5-1-1 下水污泥吸附劑性質 95
5-1-2 溶液pH對染料吸附之影響 99
5-1-3等溫吸附 104
5-1-4吸附動力學 106
5-1-5過濾阻抗實驗 107
5-2污泥灰製備離子性染料吸附劑 109
5-2-1 污泥灰鐵氧磁體化 109
5-2-2溶液pH對染料吸附之影響 111
5-2-3等溫吸附 115
5-2-4吸附動力學 117
5-3 紙漿污泥製備離子性染料吸附劑 118
5-3-1 紙漿污泥熱解 118
5-3-2 溶液pH對染料吸附之影響 120
5-3-3等溫吸附 123
5-3-4 吸附動力學 125
第六章 總結論與建議 127
6-1 低溫共燒輕質骨材結論 127
6-2 污泥表面改質吸附劑 131
6-3 建議 133
參考文獻 135

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