TWI404566B - 用於水處理之吸附床 - Google Patents
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- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- B01J2220/42—Materials comprising a mixture of inorganic materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/50—Aspects relating to the use of sorbent or filter aid materials
- B01J2220/56—Use in the form of a bed
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/06—Contaminated groundwater or leachate
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
Description
本發明係關於用於水處理之吸附床。
地下水污染,且特別是砷污染,為全世界所面對的問題。許多種用於從水和其他水溶液移除污染物的方法已經被開發出。常用的技術包括化學凝結/沉澱法、膜分離法、和吸附法。例如,美國專利案第6,994,792號揭露包括含水氧化鐵之吸附材料。不過,替代性吸附材料和吸附床將有用於水處理。
本發明所要解決的問題為提供可用於水處理的替代性吸附床。
本發明提供包括含水氧化鐵和碳酸鈣材料之吸附床;該吸附床具有第一部分及第二部份,該第一部份具有35至50重量%的鐵含量和1至10重量%的鈣含量,及該第二部分具有0.5至5重量%的鐵含量和30至40重量%的鈣含量。
百分比為重量百分比(“重量%(wt%)”);溫度為℃,除非另有不同規定,例如,體積百分比(體積%(vol%))和元素百分比都是以乾量基準(dry basis)計算。“碳酸鈣材料”為含有至少50%碳酸鈣,或者至少85%碳酸鈣,或者至少90%碳酸鈣者;於某些具體實施例中,最大碳酸鈣含量為97%。含有碳酸鈣的材料之例子包括,例如,石灰石、文石(aragonite)、六方方解石(vaterite)、大理石、白雲石(dolomite)和珊瑚(coral)。此等材料常含有可變量的矽石、黏土、粉砂、和砂;且取決於其形成方法,可能為結晶質、碎屑狀、顆粒狀或塊狀者。方解石、石英、白雲石或重晶石(barite)的晶體可能在岩石中排列成小腔洞。於本發明某些具體實施例中,碳酸鈣材料為具有10至100微米,或者從30至70微米的平均粒子尺寸之石灰石粉末。於某些具體實施例中,該材料包括石灰石碎片,較佳地為在從100微米至10毫米,或者從100至800微米,或者從150微米至500微米的範圍內。
術語“含水氧化物”或“氧(氫氧)化物(oxyhydroxide)”係指稱從高pH值的水沉澱出的鐵化合物之混合物。含水氧化物可為鐵的氧化物及/或氫氧化物。彼等的結構可為非晶形或結晶形。可用於本發明中的鐵氧化物之例子包括,例如,非晶形式與結晶形式,包括針鐵礦(goethite)、纖鐵礦(lepidocrocite)、施氏礦(schwertmannite)、四方纖鐵礦(akaganeite)、六方纖鐵礦(feroxybyte)、水鐵礦(ferrihydrite)、赤鐵礦(hematite)、磁鐵礦(magnetite)、磁赤鐵礦(maghemite)、方鐵礦(wustite)、稀烴瀝青(bernalite)和綠銹(green rusts)。典型地,鐵的含水氧化物係經由添加鹼水溶液,將鐵鹽水溶液的pH值增加到高於3,較佳為自5至7而形成。於本發明某些具體實施例中,用於本發明吸附床的吸附劑係經由將碳酸鈣材料的粒子與鐵化合物組合,得到經鐵塗覆的粒子而製成。含碳酸鈣的材料之粒子可經由添加鹼到裝有該等粒子和鐵鹽水溶液(較佳者氯化鐵(III),pH值低於3)之反應器中,而用含水氧化物予以塗覆。塗層的平均厚度為從5至50微米。含碳酸鈣的材料之覆蓋可為完全或部分。於本發明某些具體實施例中,經鐵塗覆的粒子之表面積為從20至80平方米/公克,且其孔徑為由BET測孔儀(BET porosimetry)所測量之20至50。於本發明某些具體實施例中,將過多的水從經塗覆的粒子排出,且將彼等乾燥以達到從2至30%,或者從2至15%的濕氣含量。於本發明某些具體實施例中,碳酸鈣材料係與亞鐵(鐵(II))鹽的溶液接觸,且然後與氧化劑接觸以在碳酸鈣材料上面產生含水氧化鐵(III)的沉澱。適當的氧化劑包括,例如,過氧化物、過錳酸鹽和二氧化錳。
較佳地,新製備的經鐵塗覆之粒子以乾量基準計算的鐵含量為從1%至50%。於本發明某些具體實施例中,鐵含量為至少2%,或者至少3%,或者至少4%。於某些具體實施例中,鐵含量為不多於25%,或者不多於15%,或者不多於10%,或者不多於8%。
於本發明某些具體實施例中,吸附床係經由用經鐵塗覆的碳酸鈣材料裝填該床,然後通過小的上流而擴展該床,及使其沉澱而製成。該床的擴展步驟可重複數次。較佳地,該床係經擴展到其原有體積的1.5至3倍,或者從1.5至2.5倍。擴展步驟在該床內產生密度梯度,在床的底部具有較密的部分而在該底部之上方具有較不密的部分。於本發明某些具體實施例中,床係經由添加一份材料到該床,接著添加另一份材料而產生。於此方法中,較密的部分可在床的底部或在床的頂部。
於本發明某些具體實施例中,第一部分構成床的30至95體積%且第二部分構成床的5至70體積%。或者,第一部分構成床的30至70體積%且第二部分構成床的30至70體積%,或者第一部分構成床的35至65體積%且第二部分構成床的35至65體積%。於本發明某些具體實施例中,第一部分的粒子尺寸範圍為從30至200微米且第二部分的粒子尺寸範圍為從125至2000微米。或者,第一部分的粒子尺寸範圍為50至180微米。或者,第二部分的粒子尺寸範圍為從50至750微米,或者從100至450微米。於某些具體實施例中,第一部分具有至少38重量%,或者至少40重量%的鐵含量;而鈣含量為至少2重量%,或者至少3重量%,或者至少4重量%,鐵含量為不大於48重量%,或者不大於46重量%;且鈣含量為不大於9重量%,或者不大於8重量%,或者不大於7重量%。於某些具體實施例中,第二部分具有至少0.8重量%,或者至少1重量%的鐵含量;而鈣含量為至少32重量%,或者至少34重量%;鐵含量為不大於3重量%;鈣含量為不大於39重量%,或者不大於38重量%。於某些具體實施例中,第一部分的BET表面積為從150至300平方米/公克且第二部分的BET表面積為從1至10平方米/公克。
本發明進一步有關用以從水移除砷之方法,係藉由使本發明之吸附床接觸含砷的水。該方法可從水溶液,諸如水、水系液體、和其他液體移除污染物。可被移除的污染物包括,但不限於:砷、硝酸鹽、矽石、過氯酸鹽、磷酸鹽、氯化物、氟化物、銅、鈾、錳、汞、鎳、鉻、硒、鎘、鐵、鋅、鈷、鉛、鋁、鋇、鉍、銻、鉻酸鹽和氰化物。該方法特別可應用於從水移除砷。於水中,砷主要以兩種氧化態存在:砷酸鹽(As(V))和亞砷酸鹽(As(III))。在水中低pH值下的砷酸鹽結構為H3
AsO4
且亞砷酸鹽的結構為H3
AsO3
。砷酸鹽最普遍存在於含氧水(地面水)中。水中As的濃度範圍通常在百萬份之幾(“ppm”)與低量之十億份之幾(“ppb”)之間。較佳者,第一部分係位於第二部分之上且床中的水流係向下。
較佳者,以每分鐘通過床的床體積(bed volumes)(“BV”)來算流速,係從0.01至15,或者從0.1至6,或者從0.5至4。
將400克具有212至710微米尺寸範圍的石灰石粒子充添到旋轉反應器內。於反應器中充添400毫升的去離子水。逐漸地,在20分鐘內添加800毫升的氯化鐵溶液(40%重量/體積(w/v))。在室溫下攪拌混合物35分鐘。於3分鐘內加入1200毫升的15%(重量/重量(w/w))之NaOH且攪拌混合物10分鐘。於60分鐘後將pH值維持在4至9範圍內。用25升的水進行水洗直到流出液變成透明為止。最後pH值為7.2。將該批料排出且在55℃下烤箱烘乾24小時。介質中的濕氣含量為低於10重量%且予以裝填。
從該批料採取一份樣品,在110℃下乾燥24小時以供示性用。粒子尺寸測量給出50至180微米和212至710微米的雙峰(bimodal)粒子尺寸分布。經由酸浸提(acid digest)之介質測得%-Fe為9重量%,而酸浸提之鐵是用ICP測量。據報告有45平方米/公克之BET表面積。
將400克具有212至710微米尺寸範圍的石灰石粒子充添到旋轉反應器內。於反應器充添400毫升的去離子水。逐漸地,在20分鐘內添加800毫升的氯化鐵溶液(40%重量/體積)。在室溫下攪拌混合物35分鐘。於3分鐘內加入1200毫升的15%(重量/重量)之NaOH且攪拌混合物10分鐘。於60分鐘後將pH值維持在4至9範圍內。用25升的水進行水洗直到流出液變成透明為止。最後pH值為7.2。將該批料排出,在布赫納漏斗(Buchher funnel)上乾燥且予以裝填。該介質的濕氣含量為高於20%。
從該批料採取一份樣品,在110℃乾燥24小時以供示性用。粒子尺寸測量給出50至180微米和212至710微米的雙峰粒子尺寸分布。經由酸浸提之介質測得%-Fe為9重量%,而酸浸提之鐵是用ICP測量。據報告有45平方米/公克之BET表面積。
將400克具有212至355微米尺寸範圍的石灰石粒子充添到旋轉反應器內。於反應器充添400毫升的去離子水。逐漸地,在20分鐘內添加800毫升的氯化鐵溶液(40%重量/體積)。在室溫下攪拌混合物35分鐘。於3分鐘內加入1200毫升的15%(重量/重量)之NaOH且攪拌混合物10分鐘。於60分鐘後將pH值維持在4至9範圍內。用25升的水進行水洗直到流出液變成透明為止。最後pH值為7.2。將該批料排出且在55℃下烤箱烘乾24小時。介質中的濕氣含量為低於10重量%。
從該批料採取一份樣品,在110℃乾燥24小時以供示性用。粒子尺寸測量給出50至190微米和212至355微米的雙峰粒子尺寸分布。經由酸浸提之介質測得%-Fe為18重量%,而酸浸提之鐵是用ICP測量。據報告有75平方米/公克之BET表面積。
將從實施例1得到的8毫升之乾燥介質充添到管柱內(10毫米之內直徑與17毫升之總容積)。透過泵經由向上流以1毫升/分鐘的低流速用水充添17毫升之管柱以溼潤介質而無明顯擴展床。
將從實施例2得到的8毫升經布赫納乾燥之介質充添到管柱內(10毫米之內直徑與17毫升之總容積)。透過泵經由向上流以1毫升/分鐘的低流速用水充添17毫升之管柱以濕潤介質而無明顯擴展床。
將從實施例1得到的8毫升之乾燥介質充添到管柱內(10毫米之內直徑與17毫升之總容積)。透過泵經由向上流以2毫升/分鐘的低流速用水充添17毫升之管柱以濕潤介質。將流速增加以擴展床到16毫升,之後停止水流。讓介質沉澱且在5分鐘後重複該程序。將此最後步驟重複7次。得到兩層。底層的體積%為57%而頂層為43%。頂層的ICP分析顯示其為43.5%的鐵與6.5%的鈣,而底層為1%的鐵與37.6%的鈣,全部都是以乾量基準計算。
將從實施例3得到的8毫升之乾燥介質充添到管柱內(10毫米之內直徑與17毫升之總容積)。透過泵經由向上流以2毫升/分鐘的低流速用水充添17毫升之管柱以濕潤介質。將流速增加以擴展床到16毫升,之後停止水流。讓介質沉澱且在5分鐘後重複該程序。將此最後步驟重複7次。得到兩層。底層的體積%為44%而頂層為56%。頂層的ICP分析顯示其為45.2%的鐵與5.5%的鈣,而底層為2%的鐵與36.7%的鈣,全部都是以乾量基準計算。
之後使用得自實施例4至6之含有8毫升介質的管柱進行砷移除。製備含有100ppb砷,pH值7.6,20ppm矽石之砷溶液。所用流速為呈下流型態5毫升/分鐘。於不同的時間採取樣品且測定在失效時通過管柱的床體積(BV)數。失效情況經認定是在洗出液中的砷濃度達到10ppb(飲用水MCL標準(Drinking Water MCL Standard))時發生。
其結果呈現於下:
實施例4:2800 BV
實施例5:2850 BV
實施例6:7600 BV
實施例7:15000 BV
實施例9:As(III)和Fe(II)之同時移除
之後使用得自實施例6之含有8毫升介質的管柱進行亞砷酸鹽和鐵(II)的移除。製備含有100ppb亞砷酸鹽,pH值7.6,20ppm矽石和2ppm Fe(II)之亞砷酸鹽溶液。所用流速為由泵控制、呈下流型態之10毫升/分鐘。將21升之溶液通過管柱且於每一升之後採取樣品。所有樣品的流出液內之Fe(II)都低於0.2ppm且As(III)低於10ppb。
之後使用得自實施例6之含有8毫升介質的管柱進行重金屬:Hg、Pb和Cd的移除。使用ICP標準製備溶液以製成10公升含有250ppb之Hg、270ppb之Pb和310ppb之Cd且具有pH值4之溶液。所用流速為由泵控制、呈下流型態之5毫升/分鐘。將10公升之溶液通過管柱且於每一升之後採取樣品。流出液樣品內之所得濃度為:Hg<0.1ppb、Pb<0.2ppb且Cd<0.1ppb。
Claims (10)
- 一種包括含水氧化鐵和碳酸鈣材料之吸附床,該吸附床具有第一部分及第二部份,該第一部分具有35至50重量%的鐵含量和1至10重量%的鈣含量,及該第二部分具有0.5至5重量%的鐵含量和30至40重量%的鈣含量。
- 如申請專利範圍第1項之吸附床,其中該第一部分構成該床的30至95體積%且該第二部分構成該床的5至70體積%。
- 如申請專利範圍第2項之吸附床,其中該第一部分的BET表面積為從150至300平方米/公克且該第二部分的BET表面積為從1至10平方米/公克。
- 如申請專利範圍第3項之吸附床,其中該第一部分的粒子尺寸範圍為從30至200微米且該第二部分的粒子尺寸範圍為從125至2000微米。
- 如申請專利範圍第4項之吸附床,其中該第一部分具有40至48重量%的鐵含量及2至9重量%的鈣含量且該第二部分具有1至3重量%的鐵含量及32至39重量%的鈣含量。
- 如申請專利範圍第5項之吸附床,其中該第一部分位於該第二部分之上。
- 一種從水移除砷之方法,包括使如申請專利範圍第1項之吸附床接觸含砷之水。
- 如申請專利範圍第7項之方法,其中該第一部分構成該床的30至95體積%且該第二部分構成該床的5至70體積%;該第一部分的BET表面積為從150至300平方米/公克且該第二部分的BET表面積為從1至10平方米/公克;且該第一部分的粒子尺寸範圍為從50至200微米且該第二部分的粒子尺寸範圍為從125至2000微米。
- 如申請專利範圍第8項之方法,其中該第一部分構成該床的30至70體積%且該第二部分構成該床的30至70體積%。
- 如申請專利範圍第9項之方法,其中該第一部分位於該第二部分之上且水係向下流。
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US9580343B2 (en) | 2011-08-31 | 2017-02-28 | Prochemtech International, Inc. | Treatment of gas well production wastewaters |
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US11583846B2 (en) | 2014-11-25 | 2023-02-21 | Graver Technologies Llc | High capacity adsorbent for oxyanions and cations and method for making the same |
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