隨著工業快速發展導致放流水中氟離子濃度逐漸上升，使得環境逐漸無法負荷，該議題不僅影響水中及陸生動物，更會進一步汙染水源問題。全球國家為了保護環境及人民健康也各自訂定氟放流水標準，平均訂定氟濃度限制需小於15 mg/L。但透過前期調查得知，目前技術皆於處理氟濃度介於100-1,000 mg /L，並且無視二次汙染物議題。由於上述現況本研究重新評估現有之除氟技術，並且認為沉澱技術於高濃度仍為最佳可行方案。但伴隨沉澱技術產生之議題則會產生大量汙泥，由於高含水量特性，導致處理成本亦隨之居高不下。有鑑於汙泥高含水率研發出顆粒輔助沉澱(ballast-assisted precipitation) 及流體化床結晶 (fluidized-bed crystallization) 技術來降低副產物之含水率。吾等團隊透過第三代流體化床均質結晶 (Fluidized bed homogeneous crystallization) 技術來降低體積並產生高純度之CaF2。然而近20年透過鈣進行氟之去除並未成功，目前只能產生出大量不可被去除之懸浮固體。因此本研究透過化學沉降、顆粒輔助沉澱和流體化床結晶三種不同化學沉降法比較，最終選定利用流體化床均質結晶進行除氟。

研究使用混凝沉澱來進行氟化物去除及回收。研究參數為初始濃度100到10,000 mg/L及酸鹼值2.0-11.0進行研究分析。 研究結果呈現化學混凝法在100到10,000 mg/L的氟初始濃度可有效去除氟，但缺點是會產生懸浮於溶液中的細微固體。為了避免該議題產生，本研究搭配顆粒輔助沉澱進行初始濃度4000 ppm F- 500毫升的合成廢水進行研究。

前期調查重點在於不同沉澱劑(鋁、鈣、鎂、鋯及鐵)資料收集。並且從廢水中回收之材料(碳酸鈣及磷酸氫鈣)與事業固體廢棄物 (氧化鋁、 鐵氧化物及二氧化矽) 亦為具有潛力之穩流劑。

不同沉澱劑於得最佳除氟酸鹼值也有所不同。由研究結果顯示鈣作為沉澱劑除氟效果最佳，其次依序為鐵>鋁>鋯>鎂。且用於顆粒輔助沉澱之回收材料或事業固體廢棄物中，碳酸鈣除氟效果最佳，其次依序為氧化鋁>磷酸氫鈣>二氧化矽及鐵氧化物。方解石不斷為穩流劑，同時亦能提供額外鈣離子作為沉澱劑。此外其相關性可符合二皆方程(r2=0.8763到0.9999) ， 係數用於評估參數之顯著性(pH>[Ca]/2[F] >穩流劑量) 。

進一步探討廢水中其他成分影響，因此於原先合成廢水初始濃度4000 ppm F-添加2000 ppm陰離子(硝酸根、磷酸鹽及硫酸根)進行探討。透過反應曲面法中Box-Benkhen模式進行[Ca]/2[F]、穩流劑量及pH參數探討對於氟及磷酸鹽去除。研究結果顯示[Ca]/2[F]為最重要之參數，即使在具有高濃度陰離子條件下於最佳條件氟化物和磷酸鹽的最重要參數。 即使在極端陰離子濃度下,最佳條件 ([Ca]/2[F] = 1.0,穩流劑量= 10.0, pH = 3.79 ± 0.13)去除率仍高達98%，與預測結果差異甚大。通常於酸性環境(pH =2.0-6.0) 有機率導致鈣離子於氟離子無法沉澱，但氟化鈣則不會有此現象。該研究當中，透過回收產生之方解石會降低穩流劑重量，但卻可作為磷酸鹽之吸附劑。此外在酸性環境 (pH =2.0-6.0) 有利於溶解沉澱，也是除氟其中一項機制。其中流體化床造粒過程需要極低之初始進流並且不施加回流以利於顆粒之形成。

透過流體化床回收顆粒尺寸分布小於0.2 mm，由於其重量相對較重因此通常無法到突破口，因此紀錄床高僅約12.5公分。透過觀察初始氟濃度為450 mg/L於最佳條件下總結晶率及去除率皆可達到98%去除效果。並於7天內將氟化物濃度降至低於15 mg F-/L。研究最後雖仍無法得到回收均質結晶，但改善流體化床結晶系統提高總去除率及結晶率。透過氧化鋁作為擔體處理初始濃度3600 mg F-/L使得總去除率及結晶率達到95%。此外靜床高從30公分膨脹至50公分，但含水率約50%且仍以細粉為主。

關鍵詞: 氟化物;化學沉降; 顆粒輔助沉澱; 流體化床結晶; 流體化床均質結晶

Excessive and industrial advances have increased fluoride quantity in the effluents. However, the environmental carrying capacity for fluoride is relatively slim immediately affecting both aquatic and terrestrial animals while its transport can further contaminate the water source. To protect the public and the environment, different environmental agencies globally set their respective effluent standard restricting F- concentration to 15 mg/L as the median value. However, various processes from previous investigations have mostly been limited in treating 100-1,000 mg F-/L with secondary pollution commonly overlooked. Re-assessing the available defluoridation technologies, chemical precipitation has still been the most feasible among the technologies, especially extremely high fluoride concentrations. However, conventional precipitation has its inherent drawback of producing an enormous amount of sludge causing high operational costs using functional space due to high moisture content. Second-generation technologies have been developed ballast-assisted precipitation and fluidized-bed heterogeneous crystallization using seed to catalyze the reaction and the latter to reduce moisture content. A third-generation technology, fluidized-bed homogenous crystallization, has been attempted by our research group to reduce space requirements and increase the economic potential of CaF2 with high purity. However, for the past 20 years, fluidized-bed homogenous crystallization for defluoridation using calcium has not been successful only producing highly non-settleable suspended solids. Thus, this study re-examines different chemical precipitation strategies such as conventional coagulation-flocculation, ballasted precipitation, and fluidized-bed heterogeneous crystallization ultimately anticipating defluoridation by fluidized-bed homogenous crystallization.

In this study, fluoride removal through chemical precipitation was initially investigated using conventional coagulation-flocculation and fluidized-bed homogeneous crystallization. Parameters such as a wide range of initial concentrations from 100 to10,000 mg/L and pH 2.0-11.0 under conventional coagulation-flocculation were varied and analyzed. Results showed that chemical precipitation could effectively remove fluoride even at very high fluoride concentrations ranging from 1,000 to 10,000 mg/L. However, drawbacks were high turbidity linked to non-settleable solids.

To overcome these drawbacks, the ballast precipitation was simulated under a laboratory scale with a volume of 500-mL containing synthetic wastewater (4,000 ppm F-). The preliminary investigations focused on the comparison of different precipitants previously reported (Al, Ca, Mg, Zr, and Fe). Moreover, the recovered materials from wastewater treatment (CaCO3 and CaHPO4) and discarded industrial solid waste (Al2O3, FeOOH, and SiO2) have been investigated as potential ballast. Optimum defluoridation using different precipitants was also found at different pH. The results showed that Ca remained the most feasible precipitant with the highest defluoridation efficiency (Ca>Fe>Al>Zr>Mg). Meanwhile, among the discarded and recovered materials use for ballast CaCO3 demonstrated the highest defluoridation efficiency (CaCO3>Al2O3>CaHPO4>SiO2>Fe2O3). Calcite did not only act as ballast but also a precipitant by providing additional calcium ions through leaching. The defluoridation by ballasted precipitation could efficiently remove fluoride by 99% and reduced turbidity by >90%. Moreover, the parameter correlation could be fitted in a quadratic equation (r2 from 0.8763 to 0.9999). The coefficients were used to estimate the significance of each parameter (showing pH > Ca/2F ratio > ballast dosage).

To further explore the effects of other components in wastewater, the simulated wastewater contained 4,000 ppm F introducing 2,000 ppm of co-anions (NO3-, PO43-, and SO42-). Critical factors such as molar ratio (Ca/2F), ballast dosage (g/L), and pH were subjected to Box-Benkhen Design, a response surface methodology to simultaneously treat F- and PO43-. Generally, the critical factors were all statistically significant with the molar ratio as the most significant parameter for both fluoride and phosphate removal. Even at extreme anion concentrations, the optimum condition (molar ratio = 1.0, ballast dosage =10.0, and pH = 3.79 ± 0.13) still reached a high removal efficiency about 98% with marginal error from predicted total removal. The range of the prevailing acidic pH (2.0-6.0) presumably deterred the potential precipitation of Ca with other anions but still proceed with CaF2 precipitation. In this study, the unrefined size of the recovered calcite might reduce its potential capacity as ballast but could act as an adsorbent for phosphate. Moreover, low pH induced dissolution favoring precipitation, the main defluoridation mechanism.

Alternatively, in the fluidized-bed granulation process, an initial very low flow without recirculation flow was required to initiate particle formation. The predominant size of the recovered particle was <0.2 mm which was relatively heavy atypically not reaching the upper region of the reactor with the highest recorded static bed height only about 12.50 cm. Under the observed optimum condition with an initial fluoride concentration of 450 mg/L, both total removal and crystallization ratio could reach ~98% efficiency lowering fluoride concentration to <15.0 mg F-/L within 7 days. Finally, although the heterogeneous crystallization was not obtained it resulted in a modified FBHC system resulting in high total removal and crystallization ratio treating an initial tank concentration of about 3,600 mg F-/L lead total removal and crystallization ratio about 95% using alumina as bed support. Moreover, this had already exceeded a typical bed height of 30 cm reaching about 50 cm. static bed height. However, moisture content at this condition aggravated moisture content ~50% which was still dominated by fines.

Keywords: Fluoride; Chemical Precipitation; Ballasted Precipitation; Fluidized-Bed Crystallization; Fluidized-Bed Homogenous Crystallization

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