硼的污染隨著人類的發展而日益嚴重，其中高達80%經由河川進入海洋的硼與人類活動有關，而主要污染表面水的硼來源包含採礦、油氣探勘、燃煤火力發電與各式工業生產所排出的廢水，考量到硼元素對於人類、植物與動物的毒性，台灣環保署針對硼所制定的排放水標準為5 mg-B/L。儘管許多除硼技術已被陸續開發，包含硼選擇性螯合樹脂、混凝程序、電混凝程序、薄膜程序與傳統沉澱技術，高濃度含硼廢水的處理仍存在技術障礙，故催生了能在常溫常壓下操作的化學過氧沉澱程序(Chemical oxo-precipitation, COP)。COP技術利用雙氧水將硼酸轉換為過硼酸根，再以鹼土金屬沉澱劑產生難溶性的過硼酸鹽達成硼的去除，其中使用鋇鹽為沉澱劑的鋇系COP效果尤佳，其能在15分鐘內將硼濃度自1000 mg-B/L去除至30 mg-B/L，並在適當條件下能於4小時內進一步削減至3 mg-B/L，此二度除硼現象乃來自於沉澱物過硼酸鋇(Barium perborate, BaPB)的相轉換。然而鋇系COP至今仍有許多尚未了解的現象與性質，例如BaPB沉澱的熱力學、相轉換的途徑與BaPB的晶體成長。
本研究旨在深入研究鋇系COP之原理，並根據之設計適當程序以妥善處理含硼溶液。首先，吾人以平衡實驗法求得非晶質過硼酸鋇(A-BaPB, Ba(B(OH)3OOH)2)與結晶性過硼酸鋇(C-BaPB, BaB(OH)2(OO)2B(OH)2)的溶解度積(Ksp)分別為10-8.40 及10-9.53，根據Ksp所建構的熱力學平衡溶解度模組顯示A-BaPB的溶解度約為C-BaPB的十倍，此顯著的溶解度差異為驅動BaPB相轉換之關鍵，此外鋇系COP的殘餘硼濃度可透過此模組進行預測。第二部分的研究著重於開發針對回收A-BaPB的流體化床結晶技術(Fluidized-bed crystallization, FBC)，以在連續操作模式獲得顆粒狀產物、減少汙泥產量，FBC的除硼率受到A-BaPB的平衡濃度所限制，顆粒化率則受到流體化床底部之過飽和度所控制，此過飽和度與操作pH、進料濃度、加藥量與回流比例有關，故吾人提出一套根據過飽和度的演算法預測回收A-BaPB的FBC之除硼率與顆粒化率。第三部分的目的為研究C-BaPB的晶體成長與應用，粉末晶種成長實驗顯示C-BaPB的晶體成長機制受pH影響，其中以pH 9與10為最快，可在60分鐘內達到約90%的去除率([B]0 = 4 mM (43 mg-B/L), 晶種量= 3 g/L)；吾人進一步透過表面改質程序，將以FBC合成的A-BaPB顆粒之表面物種轉換為C-BaPB以獲得粒狀晶種，藉此實現以連續模式操作的C-BaPB之 FBC單元，可針對合成的A-BaPB的FBC出流水達到89.9%的去除率與87.7%的結晶率([B]in = 4.5 mM (50 mg-B/L), [Per]in = 31.9 mM, [Ba]in = 13.2 mM, [NaCl] = 33 mM, pHin = 10.02, U = 6 m/h, HRT = 12 min, 晶種總面積 = 205 m2)。最終，串聯回收A-BaPB與C-BaPB的FBC處理程序被證實能妥善處理高濃度含硼溶液([B]0 = 46 mM (500 mg-B/L))，第一道A-BaPB的FBC可達到79.8%去除率與74.7%顆粒化率，而第二道C-BaPB的FBC則獲得89.0%之去除率，總體而言，此新穎串聯程序可達到97.8%之去除率與97.4%之結晶率。

The human activities have perturbed the global boron cycle significantly. The anthropogenic emission of boron to the surface water accounted for 80% of the total river flux to the sea. Therefore, the boron-containing streams produced in oil/gas extraction, mining activities, coal-fired power plants, and manufacturing must be treated properly. Although boron is an essential micronutrient for organisms, elevated exposure is detrimental. The Environmental Protection Administration of Taiwan regulated an effluent standard of boron as 5 mg-B/L, while the standards vary from 1.5 to 10 mg-B/L in other countries. Despite that many methods have been developed for boron removal, chemical oxo-precipitation (COP) is the sole method that is capable of treating solutions with high boron content (1000 mg-B/L) at room temperature. However, the fundamentals of the solubility, phase transition, and crystal growth of BaPBs were still unclear, which hinders the full implementation of barium-based COP.
This research aims to fill the knowledge and technology gaps in barium-based COP. Firstly, the solubility products (Ksp) of the amorphous BaPB (A-BaPB, Ba(B(OH)3OOH)2) and the crystalline BaPB (C-BaPB, BaB(OH)2(OO)2B(OH)2) were experimentally determined to be 10-8.40 and 10-9.53, respectively. The thermodynamic model that was built based on Ksp confirmed that A-BaPB is 10-fold soluble than C-BaPB, which drove the phase transformation through the dissolution-precipitation route. The model managed to predict the residual boron level of barium-based COP in the published literature. Secondly, the barium-based COP was operated in a fluidized-bed crystallizer (FBC) so that the aqueous boron could be recovered as on the supports as A-BaPB continuously. While the removal of boron was subject to the equilibrium solubility of A-BaPB, the crystallization ratio was governed by the supersaturation ratio of the mixture at the bottom of the reactor, which was related to pH, reflux ratio, input concentration of boron, and dosages of hydrogen peroxide and barium. Therefore, an algorithm based on the supersaturation ratio was developed to predict the total removal and crystallization ratio. The FBC of A-BaPB achieved 85.1% of boron removal and 83.7% of crystallization ratio under the following condition: [B]0 = 46 mM (500 mg-B/L), surface loading = 1.45 kg-B/(m2•h), [H2O2]0/[B]0 = 1.5, [Ba]0/[B]0 = 0.8, pHE = 10.0, U = 20 m/h, reflux ratio = 0.8. Thirdly, the crystal growth of C-BaPB was studied and engineered. The crystal growth rate of C-BaPB powder at pH 9 and 10 followed a parabolic relation with the relative supersaturation (S-1), suggesting that the rate-limiting step was surface spiral growth. For the ease of implementation, granular C-BaPB seeds were acquired by modifying the BaPB granules in a closed system for 5 days, during which the surface of the granules transformed from A-BaPB to C-BaPB. Therefore, the crystal growth of granular C-BaPB seeds could be performed continuously in a FBC, achieving 89.9% of boron removal and 87.7% of crystallization ratio from the synthetic effluent of FBC of A-BaPB ([B]in = 4.5 mM (50 mg-B/L), [Per]in = 31.9 mM, [Ba]in = 13.2 mM, [NaCl] = 33 mM, pHin = 10.02, U = 6 m/h, HRT = 6.5 min, total surface area = 205 m2). Ultimately, a hybrid system that integrates two FBCs for the subsequent crystallization of A-BaPB and C-BaPB was demonstrated to treat the concentrated boric acid solution (500 mg-B/L). The integrated system enabled 97.8% of boron removal and 97.4% of crystallization ratio, producing an effluent with a boron level as low as 7.8 mg-B/L.

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