CN106430396B - 一种选择性纳米吸附剂和氧族桥联铁絮凝剂制备方法及其协同净水应用 - Google Patents
一种选择性纳米吸附剂和氧族桥联铁絮凝剂制备方法及其协同净水应用 Download PDFInfo
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- 229910001868 water Inorganic materials 0.000 title claims abstract description 49
- 239000003463 adsorbent Substances 0.000 title claims abstract description 18
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- 150000001787 chalcogens Chemical group 0.000 title claims abstract description 13
- 238000000746 purification Methods 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000009286 beneficial effect Effects 0.000 claims abstract description 12
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 8
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011575 calcium Substances 0.000 claims abstract description 7
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 6
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 28
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- 239000000243 solution Substances 0.000 claims description 10
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 9
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
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- 239000000654 additive Substances 0.000 claims description 6
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- HJKYXKSLRZKNSI-UHFFFAOYSA-I pentapotassium;hydrogen sulfate;oxido sulfate;sulfuric acid Chemical compound [K+].[K+].[K+].[K+].[K+].OS([O-])(=O)=O.[O-]S([O-])(=O)=O.OS(=O)(=O)O[O-].OS(=O)(=O)O[O-] HJKYXKSLRZKNSI-UHFFFAOYSA-I 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- -1 sulfate radical Chemical class 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 239000002250 absorbent Substances 0.000 claims description 3
- 230000002745 absorbent Effects 0.000 claims description 3
- 159000000013 aluminium salts Chemical class 0.000 claims description 3
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
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- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
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- 150000002500 ions Chemical class 0.000 claims description 2
- FPNCFEPWJLGURZ-UHFFFAOYSA-L iron(2+);sulfite Chemical compound [Fe+2].[O-]S([O-])=O FPNCFEPWJLGURZ-UHFFFAOYSA-L 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
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- 230000002045 lasting effect Effects 0.000 claims 1
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 5
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- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 abstract description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 abstract description 3
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
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- 229910052787 antimony Inorganic materials 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
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- 239000004021 humic acid Substances 0.000 description 2
- 150000002505 iron Chemical class 0.000 description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
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- 229910021529 ammonia Inorganic materials 0.000 description 1
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Classifications
-
- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Water Treatment By Sorption (AREA)
Abstract
本发明属于水净化领域,提供了一种选择性纳米吸附剂和氧族桥联铁絮凝剂的协同净水方法。本发明的多羟基氧硫酸铁吸附剂材料具有良好的吸附性能,同时具有良好的选择性,制备的絮凝剂材料具有新生态的桥联基团,反应活性位点更多,具有高分子量克服传统絮凝剂的局限性,且其操作方便、无污染。应用合成的吸附剂和絮凝剂材料,通过吸附协同混凝技术联用,实现选择性的去除有害元素砷、铬、钒等同时保护有益元素锶、钙等,实现净水同时保护有益元素,达到矿泉水指标的出水产品。
Description
技术领域
本发明属于水净化领域,涉及一种选择性纳米吸附剂和絮凝剂的吸附-混凝协同净水方法,实现水资源利用率和制备优质矿泉水的一种方法。
背景技术
水是人类最基本的生存资源。虽然地球上71%为水所覆盖,但其中可供人类利用的淡水资源仅占其中的0.7%左右。然而,随着经济的不断发展,环境问题也逐渐凸显,同时造成水污染问题也更加突出,近十年来水污染突发事件次数的频繁,中国环境状况表明,近年来的环境事件中有50%的比例为水污染有关,仅在2013年上半年曝光的水污染事件中,就有16件河流水污染事件,8件地下水污染事件,平均每个月有4件,这频率己不得不引起重视。目前的饮用矿泉水源于是地下水在地层深处经长期与围岩相互作用、溶蚀岩石中的矿物质而形成,水质中不仅含有钙、镁、锌、硒、碘等营养元素,还含有锂、锶等微量元素,但同时未经处理的水源水中也会存在一些对人体健康产生危害的物质,例如钼、汞、砷和铬等无机物还有有微污染和重污染的有机污染物等,因此需要一种具有选择性的吸附剂材料在处理有害元素的同时保护营养元素。
目前水处理的絮凝剂主要分为无机絮凝剂和有机絮凝剂两大类,其中无机絮凝剂因为其用量少,无二次污染和反应迅速等优点被广泛的应用。其中主要的无机絮凝剂主要分为无机小分子絮凝剂和无机高分子絮凝剂两大类,无机低分子絮凝剂可直接或配成水溶液投入到废水处理设备中,其优点是价格便宜,但在水处理过程中存在一些较严重的问题,如凝聚速度慢,形成的絮状物小,且具有强腐蚀性,净水效果不理想,因此,无机絮凝剂已逐渐被无机高分子絮凝剂所取代。朱富坤等人采用水热法制备了一种新的无机高分子絮凝剂—纳米聚合硫酸铁(PFS)絮凝剂,对镇江段长江水样进行了絮凝实验,结果表明,在PFS的投加量为COD去除率和浊度去除率分别达到了80.8%、90.3%,比传统的聚丙烯酰胺絮凝剂具有更好的CODCr去除率和除浊性能。Joo等人研究了无机铁盐、铝盐复合高分子絮凝剂对当地燃料厂排放的含活性燃料废水的絮凝性能,结果表明色度去除率接近100%。Moussas等人研究了聚硅酸硫酸铁与非改性铁基絮凝剂对高岭土—腐植酸悬浮液的絮凝效果,结果表明,聚硅酸硫酸铁絮凝剂比非改性的铁基絮凝剂具有更好的絮凝性能,尤其是在磷离子的去除方面。但是无机高分子絮凝剂的反应时间比较长,活性位点反应活性较小,需要一定的助凝剂的配合使用。
吸附剂材料因为其稳定性好、粒度可控和容易去除等优点被广泛的作为助凝剂使用,目前应用的吸附剂有炭类吸附剂、腐殖酸类吸附剂、矿物吸附剂、高分子吸附剂生物吸附剂以及工业废物吸附剂等。哈尔滨工业大学的范延臻等研究应用硝酸根改性生物碳材料可以明显的提高吸附剂材料的吸附效果。伍喜庆等以硫脲和甲醛为主要原料对活性炭进行了改性,实验表明改性活性炭对金的吸附容量比一般活性炭强得多。但是生物碳材料作为广性吸附剂材料对水体系中的所有元素都会吸附去除,无法实现对营养元素的保护。肖文香应用改性介孔二氧化硅实现了对铅的选择性吸附。釜山国立大学的Aneesh Mathew等人应用改性的分子筛材料实现了对Hg2+的选择性的吸附,但是存在吸附量的限制问题。综上,很少有吸附剂材料可以实现现则性吸附去除有害元素而保护能源元素。
本发明针对以上问题,合成一种具有选择性纳米吸附剂材料和一种,针对于污染水源水,去除有害元素砷、铬等的同时保护营养元素钙、锶等,实现最终出水具有矿泉水水质指标。
发明内容
本发明针对现有技术的不足,对含有有害元素的水源水处理,提出的一种选择性吸附剂和具有高活性的氧族桥联铁絮凝剂用于净水的方法,同时应用制备的材料,通过吸附混凝协同处理具有有害元素的水源水,在去除有害元素砷、铬、钒等同时保护有益元素锶、钙等,实现净水同时保护有益元素,达到矿泉水指标的出水产品。
本发明的技术方案:
一种选择性纳米吸附剂和氧族桥联铁絮凝剂用于净水的方法,步骤如下:
(1)多羟基氧铁盐选择性吸附剂
在N2保护的状态下,将亚硫酸铁配置成溶液,搅拌均匀,保持N2保护氛围,用双氧水将二价铁氧化为三价铁,同时提供活性桥联羟基氧自由基基团,按照三价铁与二价铁摩尔比为3-0.5:1加入双氧水控制Fe/O=6/8;待不在有气泡产生后加入添加剂亚硝酸钠,亚硝酸钠的加入量与总混合溶液的体积比为0.1-5:1000,搅拌均匀;控制温度在45-70℃持续搅拌30-90min并加入催化剂,催化剂的加入量与总混合溶液的体积比为1-10:1000;加入碱液调节pH为3-5,并继续N2保护搅拌30-90min;升高温度到80-95℃反应40-120min;停止搅拌,撤去N2进行陈化,陈化时间为1-10h;过滤后得到固体浆料,搅拌均匀,密封保存;
所述的催化剂为溶解性铝盐;
所述的碱液为氨水、氢氧化钠、氢氧化钙中的一种或两种以上混合;
(2)氧族桥联聚合氯化铁絮凝剂
在N2保护的状态下,将氯化亚铁配置成溶液,搅拌均匀,将二价铁氧化为三价铁,氧化方法选择单过硫酸氢钾和双氧水联用的氧化方法;先加入单过硫酸氢钾,将二价铁总量的1/10-20氧化为三价铁同时生成新生态的硫酸根,搅拌5-30min;再加入双氧水氧化剩余的二价铁,搅拌5-30min;待不在有气泡产生后加入添加剂亚硝酸钠,亚硝酸钠的加入量与总混合溶液的体积比为0.1-5:1000,搅拌均匀;控制温度在45-70℃持续搅拌30-90min,调节pH为0.5-3;停止搅拌,陈化时间为1-10h,搅拌均匀。
按照浓度为5-100ppm向含有有害元素如砷、钒、锑等重金属离子和锶、钙等有益元素的水源中加入选择性纳米吸附剂和氧族桥联铁絮凝剂,快速搅拌5-30min,慢速搅拌30-120min,反应结束后过滤得净化水,并保持有益元素。
本发明的多羟基氧硫酸铁吸附剂材料具有良好的吸附性能,同时具有良好的选择性,制备的絮凝剂材料具有新生态的桥联基团,反应活性位点更多,具有高分子量克服传统絮凝剂的局限性,且其操作方便、无污染。应用合成的吸附剂和絮凝剂材料,通过吸附协同混凝技术联用,实现选择性的去除有害元素砷、铬、钒等同时保护有益元素锶、钙等,实现净水同时保护有益元素,达到矿泉水指标的出水产品。
附图说明
图1是选择性纳米吸附剂材料扫描电镜图。
图2是选择性纳米吸附剂材料粒度分布图。
图3是处理前后水源水中有毒元素的浓度变化。
图4是处理前后水源水中有益元素的浓度变化。
具体实施方式
以下结合附图和技术方案,进一步说明本发明的具体实施方式。
实施例1
1)称取69.5g七水合硫酸亚铁溶解到500mL水中N2保护搅拌1h得到澄清溶液。
2)在N2保护氛围和搅拌下,按照三价铁与二价铁摩尔比为3-0.5:1的比例向1)中七水合硫酸亚铁溶液加入氧化剂双氧水,双氧水加入量按照Fe/O=3/4的比例加入,搅拌反应10-100min。
3)待2)中混合溶液不再有气泡产生后加入添加剂,搅拌均匀。合成过程的添加剂为亚硝酸钠,加入量按照质量体积比为0.1-5:1000;
4)控制温度在45-70℃持续搅拌30-90min并加入催化剂;催化剂可选择溶解性铝盐,加入量按照质量体积比为1-10:1000;
5)加入碱液调节pH为3-7,并继续N2保护搅拌30-90min;合成过程中碱液可以为氨水、碳酸钠、氢氧化钠、氢氧化钙中的一种或上述的混合液;
6)升高温度到80-95℃反应40-120min;
7)停止搅拌,撤去N2进行陈化,陈化时间为1-10h;
8)向合成的液体中加入分散剂,搅拌均匀,得到具有选择性的纳米多羟基氧硫酸铁吸附剂材料,检测结果显示多羟基氧硫酸铁吸附剂材料为规则的纳米颗粒,并存在一定的团聚现象,其尺寸范围10-40nm之间。
实施例2
1)称取159g无水氯化亚铁溶解到500mL水中搅拌1h,加入4.76g单过硫酸氢钾氧化1/16的二价铁,同时生成新生态的硫酸根桥联基团,搅拌3-10min。
2)向1)中得到的混合液中加入30%的双氧水75.2mL,缓慢滴加双氧水氧化剩余的二价铁,在60℃搅拌30min。
3)向1)中得到的混合液中加入12g NaOH调节pH到3-5,并且调节新生态硫酸根与氢氧根的比例为1/3,滴加碱液过程中N2保护持续搅拌30min。
4)碱液滴加完成后,将混合液的温度升高至90℃继续反应1h,陈化10h。
5)向得到的液体中加入20mL10%PE溶液,搅拌均匀得到氧族桥联聚合氯化铁絮凝剂备用。
实施例3
1)取300mL的含有害元素的水源水水样,加入5-100ppm的实施例2中得到的选择性吸附剂材料,快速搅拌5-10min。
2)向1)中得到的混合溶液中加入5-100ppm的实施例1中制备得到的高分子絮凝剂材料,快速搅拌5-10min,慢速搅拌30min,反应结束后沉降20min,过滤后水质检测结果表明,水中的铝、砷、锑、钨、铀和钛等有害元素可以有效地去除到饮用水水平,同时水质中Sr、Zn、Ga等有益元素可以很好地保护下来,实现出水达到矿泉水的水平。
Claims (3)
1.一种选择性纳米吸附剂和氧族桥联铁絮凝剂用于净水的方法,其特征在于,步骤如下:
(1)多羟基氧铁盐选择性吸附剂
在N2保护的状态下,将亚硫酸铁配置成溶液,搅拌均匀,保持N2保护氛围,用双氧水将二价铁氧化为三价铁,同时提供活性桥联羟基氧自由基基团,按照三价铁与二价铁摩尔比为3-0.5:1加入双氧水控制Fe/O=6/8;待不在有气泡产生后加入添加剂亚硝酸钠,亚硝酸钠的加入量与总混合溶液的体积比为0.1-5:1000,搅拌均匀;控制温度在45-70℃持续搅拌30-90min并加入催化剂,催化剂的加入量与总混合溶液的体积比为1-10:1000;加入碱液调节pH为3-5,并继续N2保护搅拌30-90min;升高温度到80-95℃反应40-120min;停止搅拌,撤去N2进行陈化,陈化时间为1-10h;过滤后得到固体浆料,搅拌均匀,密封保存;
(2)氧族桥联聚合氯化铁絮凝剂
在N2保护的状态下,将氯化亚铁配置成溶液,搅拌均匀,将二价铁氧化为三价铁,氧化方法选择单过硫酸氢钾和双氧水联用的氧化方法;先加入单过硫酸氢钾,将二价铁总量的1/10-20氧化为三价铁同时生成新生态的硫酸根,搅拌5-30min;再加入双氧水氧化剩余的二价铁,搅拌5-30min;待不在有气泡产生后加入添加剂亚硝酸钠,亚硝酸钠的加入量与总混合溶液的体积比为0.1-5:1000,搅拌均匀;控制温度在45-70℃持续搅拌30-90min,调节pH为0.5-3;停止搅拌,陈化时间为1-10h,搅拌均匀;
按照浓度为5-100ppm向含有有害元素砷、钒、锑重金属离子或含有有益元素锶、钙的水源中加入多羟基氧铁盐选择性吸附剂和氧族桥联聚合氯化铁絮凝剂,快速搅拌5-30min,慢速搅拌30-120min,反应结束后过滤得净化水,并保持有益元素。
2.根据权利要求1所述的选择性纳米吸附剂和氧族桥联铁絮凝剂用于净水的方法,其特征在于,所述的催化剂为溶解性铝盐。
3.根据权利要求1或2所述的选择性纳米吸附剂和氧族桥联铁絮凝剂用于净水的方法,其特征在于,所述的碱液为氨水、氢氧化钠、氢氧化钙中的一种或两种以上混合。
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