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研究生：	藍韋盛 Lan, Wei-Sheng
論文名稱：	雙氧水對化學沉降處理高濃度含硼廢水影響之研究 Effect of Hydrogen Peroxide on the Treatment of High Boron Concentration Wastewater by Chemical Precipitation Method
指導教授：	黃耀輝 Huang, Yao-Hui
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2012
畢業學年度：	100
語文別：	英文
論文頁數：	80
中文關鍵詞：	雙氧水、化學沉降、含硼廢水
外文關鍵詞：	hydrogen peroxide, precipitation, boron removal
相關次數：	點閱：86 下載：1
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硼是生物體不可或缺的微量營養素之一，但高濃度的硼除了會對人體產生輕則嘔吐重則休克死亡等各種症狀，亦會讓植物生長不良造成農業減產。故世界衛生組織(WHO)以及歐盟(EU)規範飲用水硼濃度不得超過0.3mg-B/L；行政院環保署放流水標準則為1 mg-B/L。
電混凝(EC)是針對高濃度含硼廢水的新興方法，比起傳統化學混凝法，其雖然能夠有效地降低廢液中的硼（去除率約大於80％），但缺點是其所需要的藥劑量過多、耗能且處理後依然遠超出法規標準。因此本研究以硼酸、硼砂和偏硼酸鈉(1000 mg-B/L)為目標，探討新的改善方法。
本研究先探討不同氧化劑氧化含硼廢液的能力並先輔以Ca做化學沉澱，結果顯示雙氧水為本實驗中的最佳氧化劑，其硼去除率可達80%，並且氧化pH值並不影響雙氧水結果(即雙氧水無論在酸、鹼、中性下都能發揮氧化功效)。接者以II A族(Mg、Ca、Sr、Ba)做為混凝劑並在不同混凝pH值下的除硼效果，實驗結果顯示隨著pH值上升硼去除率亦逐漸上升並在pH>9趨近於穩定。並且，混凝結果約是Ba>Ca=Sr>Mg，其去除率分別為98%(Ba)、87%(Ca)、86%(Sr)、42%(Mg)。
本研究亦嘗試探討動力機制，依據實驗結果發現氧化、混凝的反應速度非常快速，沉澱後的5分鐘至720分鐘硼濃度並無顯著變化，可說明生成的汙泥並不會再度溶解。而本實驗最佳化條件約是H2O2/B莫耳比1.5；Ba/B莫爾比0.75；混凝pH值9，在此操作條件下硼去除率可高達98%。同時根據X光水平繞射分析儀(XRD)之分析，生成的汙泥中有過硼酸鋇的結晶顆粒。因此若能回收過硼酸鋇結晶將可達到汙泥的資源化。
綜合言之，本研究選擇適當的氧化劑使之形成過硼酸，後續再加入適宜的混凝劑，藉此大幅降低廢水中的硼離子濃度（去除率>98％）。不只改良了傳統化學混凝法除硼效果不佳（去除率<15％）的缺點，並優於新興的電混凝法（去除率>80％）。

Boron is one of trace nutrient the human beings demand. However, high concentrated boron in the environment is harmful for the organism. In biological field, high concentration of boron causes poor growth of plant. Therefore, both World Health Organization (WHO) and European Union (EU) have set up a standard of 0.3 mg-B/L in drinking water. In Taiwan, EPA legislated for limiting the industry effluent lower than 1 mg-B/L.
Electrocoagulation method (EC) is newly in disposal of the high concentrated boron wastewater. In contrast, although the chemical precipitation has lower efficiency on boron removal than EC, the cost effect and energy consumption have it still popular in real water management. In preliminary test, perborate which is the oxidation state of boron compounds can be reduced by chemical precipitation directly using Ca coagulant. Thus, this work aimed at exploring a novel chemical precipitation preconditioning with an oxidation process for managing the target boron compounds, including boric acid, metaorate, borax and perborate, in a concentration of 1000 mg-B/L.
In oxidation stage, the hydrogen peroxide was an effective oxidant for pretreating the boron compounds. The efficiency of hydrogen peroxide could lead to around 80 % boron removal, which was independent of solution pH. In chemical precipitation stage, the effects of II A group cations, including Mg, Ca, Sr, and Ba, and solution pH were assessed to achieve high boron removal. The experimental results suggested that the efficiency for coagulating the oxidized boron compounds were 98 %, 87 %, 86%, and 42 % using Ba, Ca, Sr, and Mg coagulants, respectively. Meanwhile, the precipitation tended to highest level of 98% boron removal under the optimal chemical dosages, adopting the molar ratio of H2O2 to boron around 1.5 and Ba to boron around 0.75, and pH higher than 9 as well. Afterward, the precipitation of oxidized boron compounds by barium has proven to produce the crystallized power of BaB2O4(OH)4 phase, which can be seen as a recoverable resource.
This work has demonstrated a potential oxidation-chemical precipitation process for resolving the defects of traditional chemical precipitation on boron removal (< 15 %). By pretreating with a suitable oxidant, then precipitation using effective cations, the relatively higher boron removal (98 %) than the new electrocoagulation method (80 %) has been attained.

CONTENTS
摘要	I
Abstract	III
誌謝	V
CONTENTS	VI
LIST OF TABLES	VIII
LIST OF FIGURES	IX
Chapter 1 Introduction	1
1.1 Background	1
1.2 Objective	2
Chapter 2 Literature Review	3
2.1 The natural distribution of boron	3
2.2 The various usages of boron	4
2.3 Source of high boron concentration wastewater	6
2.3.1 Optoelectronic wastewater	6
2.3.2 Byproduct of sodium borohydride hydrolysis	8
2.4 Chemical and physical properties of boron	10
2.4.1 Introduction of boron	10
2.4.2 Boron oxides compounds	10
2.5 Toxic of boron	14
2.6 Methods of boron removal	17
2.6.1 Chemical precipitation	17
2.6.2 Reverse osmosis	18
2.6.3 Electrodialysis	19
2.6.4 Adsorption	20
2.6.5 Ion exchange resins	21
2.6.6 Layered double hydroxide	22
2.6.7 Electrocoagulation	23
Chapter 3 Experimental Methods	32
3.1 Framework of the Experiment	32
3.2 Materials and Analytical Methods	34
3.2.1 Materials	34
3.2.2 Analytical Methods	36
3.2.2.1 Hydrogen peroxide concentration	36
3.2.2.2 Boron and Barium concentration	37
3.2.2.3 Sludge analyze-XRD	39
3.2.2.4 Sludge analyze-SEM	41
3.2.2.5 Sludge analyze-EDS	43
3.2.2.6 Sludge analyze-NMR	45
3.3 Experimental apparatus and procedures	46
3.3.1 Experimental apparatus	46
3.3.2 Experimental procedures	48
3.3.3	Target pollutants	49
Chapter 4 Results and Discussion	50
4.1 Chemical precipitation	50
4.2 Oxidation of boron acid	52
4.2.1 Effect of oxidants on boric acid removal using chemical precipitation	52
4.2.2 Oxidation of boron compounds by hydrogen peroxide	55
4.3 Effects of coagulant and pH on boric acid removal using chemical precipitation	57
4.4 Stability of boron precipitation	59
4.5 Precipitation parameters: H2O2 and barium dosages	61
4.5.1 Optimal hydrogen peroxide dosage	61
4.6 Characterization of precipitates	68
4.6.1	XRD	68
4.6.2 SEM and EDS	71
4.7 The feasibility of oxidation-chemical precipitation process as comparing with the traditional precipitation methods	72
Chapter 5 Conclusion	73
Reference	75






LIST OF TABLES
Table 2. 1 Characteristics of the industrial wastewater [73]	8
Table 2. 2 Acid equilibrium constants of common acids	11
Table 2. 3 the polymerization of monomeric species	12
Table 2. 4  Boron tolerance limits for agricultural crops	15
Table 2. 5  Advantages and disadvantages of reverse osmosis	19
Table 2. 6 Commercially available boron selective resins[78]	21
Table 2. 7  Literature of boron removal	25
Table 4. 1 Physical data of hydrogen peroxide and sodium peroxide	54
Table 4. 2  Boron removal efficiencies at various pH values using Mg, Ca, Sr, and Ba for precipitation (boron compound=boric acid, molar ratio H2O2/B=3, molar ratio metal ion/B=1)	59
Table 4. 3 Effects of molar ratio of hydrogen peroxide to boric acid on boron removal by chemical precipitation (molar ratio Ba/B=1, precipitation pH=10, [B]i=1000 mg-B/L)	63
Table 4. 4 Effects of molar ratio of hydrogen peroxide to borax on boron removal by chemical precipitation (molar ratio Ba/B=1, precipitation pH=10, [B]i=1000 mg-B/L)	63
Table 4. 5 Effects of molar ratio of hydrogen peroxide to sodium metaborate on boron removal by chemical precipitation (molar ratio Ba/B=1, precipitation pH=10, [B]i=1000 mg-B/L)	64
Table 4. 6 Effects of molar ratio of barium to boron on boron removal by chemical precipitation (molar ratio H2O2/B=3, precipitation pH=10, [B]i=1000 mg-B/L)	66
Table 4. 7 Effects of molar ratio of barium to boron on boron removal by chemical precipitation (molar ratio H2O2/B=3, precipitation pH=10, [B]i=1000 mg-B/L)	67
Table 4. 8 Effects of molar ratio of barium to boron on boron removal by chemical precipitation (molar ratio H2O2/B=3, precipitation pH=10, [B]i=1000 mg-B/L)	67
Table 4. 9 The atom ratio of barium, boron, and oxygen	72


 
LIST OF FIGURES
Figure 2. 1 The distribution of boric acid and borate in seawater	3
Figure 2. 2 Boron application industries	4
Figure 2. 3 Structure of polarizer	6
Figure 2. 4 Process of manufacturing polarizer	7
Figure 2. 5 The aqueous borate ions species as a function of pH	13
Figure 2. 6 Osmosis and reverse osmosis	18
Figure 2. 7 Diagram used for electrodialysis	20
Figure 2. 8  Structural formula of N-methyl-D-glucamine[78]	22
Figure 2. 9  LDHs structure and boron removal schemes[79]	23
Figure 2. 10 Electrocoagulation reactor used to remove boron from aqueous solutions	24
Figure 3. 1 The schematic diagram of this study	32
Figure 3. 2 Calibration curve of the H2O2 concentration	36
Figure 3. 3 Inductively Coupled Plasma Optical Emission Spectrometer ( ICP-OES)	37
Figure 3. 4 X-ray diffraction analyzer (XRD)	39
Figure 3. 5 Scanning Electron Microscope (SEM)	41
Figure 3. 6 Structure of Scanning Electron Microscope	42
Figure 3. 7 Energy Dispersive Spectrometer ( EDS)	43
Figure 3. 8 Nuclear magnetic resonance ( NMR)	45
Figure 3. 9 Jar-test ( type：JT-6S)	46
Figure 3. 10 Experimental photos	48
Figure 4. 1 Effect of Ca/B molar ratio on the removals of boric acid, borax, sodium metaborate and perborate by chemical precipitation ([B]i=1000 mg/L, precipitation pH=10)	51
Figure 4. 2  Effect of different oxidants and pH values (boron compound=boric acid, coagulant=Ca, molar ratio Ca/B=1, precipitation pH=10)	53
Figure 4. 3 Dependence of the degree of polymerization and composition of perborates；m is molar ratio of H_2 O_2/B(OH)_4^- [76]	56
Figure 4. 4 boron removals as a function of pH values for Mg, Ca, Sr, and Ba coagulants (boron compound=boric acid, molar ratio H2O2/B=3, molar ratio coagulant/B=1)	58
Figure 4. 5 Effect of duration of precipitation process on the boron removal (boron compound=boric acid, molar ratio H2O2/B=3, molar ratio Ba/B=1)	60
Figure 4. 6 Effect of H2O2/B molar ratio on boron removal by chemical precipitation (molar ratio Ba/B=1, precipitation pH=10)	62
Figure 4. 7 Effect of Ba/B molar ratio on boron removal by chemical precipitation (molar ratio H2O2/B=3, precipitation pH=10, [B]i=1000 mg-B/L)	65
Figure 4. 8 Structure of cyclic dimer of perborate	68
Figure 4. 9  XRD analytical results (a) borax Na2B4O5(OH)4 + H2O2 + BaCl2 (b)perborate NaBO3+ BaCl2 , comparing with the standard pattern of BaB2O4(OH)4	69
Figure 4. 10 XRD analytical results (c) metaborate NaBO2 + H2O2 + BaCl2 (d) boric acid B(OH)3 + H2O2 + BaCl2	70
Figure 4. 11(a) NaBO2 + H2O2 + BaCl2 (b) Na2B4O5(OH)4 + H2O2 + BaCl2(a) B(OH)3 + H2O2 + BaCl2	71


                                    

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