CN115318243A - 一种磁性除磷颗粒吸附材料及其制备方法和应用 - Google Patents
一种磁性除磷颗粒吸附材料及其制备方法和应用 Download PDFInfo
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 239000011574 phosphorus Substances 0.000 title claims abstract description 101
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 101
- 239000000463 material Substances 0.000 title claims abstract description 78
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 57
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 39
- 239000002245 particle Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 20
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 20
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 19
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000004927 clay Substances 0.000 claims abstract description 7
- 230000005389 magnetism Effects 0.000 claims abstract description 6
- 238000007885 magnetic separation Methods 0.000 claims abstract description 4
- 229910021536 Zeolite Inorganic materials 0.000 claims description 8
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 8
- 239000010457 zeolite Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 239000000440 bentonite Substances 0.000 claims description 5
- 229910000278 bentonite Inorganic materials 0.000 claims description 5
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 229960000892 attapulgite Drugs 0.000 claims description 4
- 229910052625 palygorskite Inorganic materials 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 239000004113 Sepiolite Substances 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 229910052624 sepiolite Inorganic materials 0.000 claims description 2
- 235000019355 sepiolite Nutrition 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000008239 natural water Substances 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 13
- 239000000243 solution Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000013049 sediment Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052746 lanthanum Inorganic materials 0.000 description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 239000005422 algal bloom Substances 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000012851 eutrophication Methods 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- DJFBJKSMACBYBD-UHFFFAOYSA-N phosphane;hydrate Chemical compound O.P DJFBJKSMACBYBD-UHFFFAOYSA-N 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 2
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 calcium hydroxide modified zeolite Chemical class 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B01J2/14—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in rotating dishes or pans
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Abstract
本发明提供了一种磁性除磷颗粒吸附材料的制备方法,该材料的原料包括天然粘土、氢氧化钙和四氧化三铁,这三种材料按一定比例混合并用圆盘造粒机进行造粒即可得磁性除磷颗粒吸附材料。该材料对水体兼具极强的磷吸附能力和磁性,磁分离效果好,便于磷吸附饱和后移出水生态***。该材料受pH值影响小,可以用于天然水体、黑臭水体及城市污水除磷。本发明制备工艺简单,制得的磁性除磷颗粒吸附材料的原材料来源广泛、成本低、除磷效果好、易于回收且回收率高,环保无二次污染。
Description
技术领域
本发明属于水污染治理领域,涉及一种用于富营养化水体治理材料及其制备方法和应用,具体涉及一种磁性除磷颗粒吸附材料及其制备方法和应用。
背景技术
受人类活动和气候变化共同影响,湖泊富营养化和藻类水华仍是未来相当长一段时间内的水生态环境问题。因此,水体富营养化治理和藻类水华防控技术的研发、应用是必不可少的。磷是水生态***中主要限制因子,是驱动藻类水华爆发的关键因素,降低水体磷负荷是水体富营养化治理的重要方法,也是藻类水华防控的常规手段。
吸附法具有高效、经济和简便易行等优势,广泛应用于富营养化水体磷治理中。传统的除磷吸附材料主要是铝、铁、钙等金属盐类,这些金属阳离子类都能跟水体磷酸根结合,形成沉淀物质,从而将水体或沉积物活性磷转化为难溶的惰性磷。此外,铁盐和铝盐具有很强的絮凝作用,通过絮凝作用将水体的有机磷或颗粒态磷絮凝沉降到湖底,以降低水体总磷含量。虽然基于铝、铁、钙等金属盐类制成吸附或絮凝材料能有效降低水体磷含量,但这只是暂时将磷以较为稳定的形态封存在沉积物中,没有将磷彻底移除水生态***,这种稳定形态的磷在条件适宜情况下还有被释放的风险;而且吸附材料磷吸附饱和后就失去了吸附效果,长期滞留在沉积物中有可能存在二次污染问题。因此,迫切希望寻求制备一种成本低、生态安全性高、吸附饱和后能够被移除水生态***,彻底降低水体和沉积物磷负荷的高效除磷材料。
目前,国内外比较知名的除磷吸附材料均基于稀有元素镧改性粘土矿物,如广泛应用的锁磷剂华中科技大学发明了一项镧改性磁性膨润土除磷材料(CN110548490 B),虽然该材料在适宜条件下对水体磷去除效果好,且易于回收。但该材料受pH值影响大,在酸性条件下除磷效果显著降低。此外,作为一种稀有金属元素,生态风险高,且镧价格逐年上升等是限制其大规模使用的关键因素。氢氧化钙广泛用于养殖水体清塘,对水生态影响较小、价格便宜,且能与水体活性磷结合形成磷灰石沉淀,因此广泛应用于各种水体除磷中。有研究表明,氢氧化钙改性沸石受pH值影响较小,在酸碱和碱性条件下均能与磷反应。因此基于钙负载磁性絮凝剂的应用前景更广阔。
发明内容
为了解决上述问题,本发明的目的在于提供一种成本低、生态安全性高、能够通过磁分离技术将吸附饱和后的吸附材料移出水生态***外的磁性除磷颗粒吸附材料及其制备方法,该制备方法工艺简单,制备出的磁性除磷吸附材料对磷的吸附能力强,且磁性强、回收率高,无二次污染。
本发明的另一目的在于提供一种氢氧化钙改性粘土负载四氧化三铁磁性除磷吸附材料。
本发明还提供一种富营养化水体除磷治理方法。
为了实现上述目的,本发明提供一种磁性除磷颗粒吸附材料及其制备方法,该制备方法包括以下步骤:
(1)将天然粘土、四氧化三铁和氢氧化钙碾磨,过300目筛;
(2)取天然粘土6-8份,四氧化三铁1-2份,氢氧化钙粉末1-2份,这三种材料在圆盘造粒机中以1200r/s的速度快速搅拌2min,使其充分混合;
(3)充分混合后加入适量的水,将圆盘造粒机速度调到1200r/s,利用紊流混合原理造粒得到磁性除磷吸附材料;该造粒过程操作简单、可快速高效的在较短时间内制备出所需要的颗粒;
(4)将造粒得到的磁性除磷吸附材料烘干后过筛,得到粒径在1-5mm范围内不同粒径的磁性除磷颗粒吸附材料。
优选地,所述天然粘土包括但不限于:沸石、凹凸棒土、膨润土、海泡石等的一种或几种按任意比例混合。
优选地,其原料按照重量份包括:氢氧化钙1份,四氧化三铁1份,沸石8份;或其原料按照重量份包括:氢氧化钙1份,四氧化三铁1份,凹凸棒土8份;或其原料按照重量份包括:氢氧化钙1份,四氧化三铁1份,膨润土8份。优选地,制备得到的磁性除磷颗粒吸附材料兼具磁性和高效的磷吸附能力。
优选地,将氢氧化钙、四氧化三铁和沸石按特定比例混合并造粒即可。
优选地,混合造粒后45至65℃烘干。
优选地,制备得到的磁性除磷颗粒吸附材料兼具磁性和高效的磷吸附能力。
优选地,制备得到的磁性除磷颗粒吸附材料在富营养化水体中吸附饱和后可通过磁分离技术回收该材料,以防止该材料的二次污染。
优选地,制备得到的磁性除磷颗粒吸附材料在水体pH为3-11的较宽范围内均具有良好的除磷能力。
优选地,制备得到的磁性除磷颗粒吸附材料在水体除磷领域中应用。
本发明以我国储量丰富,价格低廉的天然粘土、熟石灰(氢氧化钙)和四氧化三铁为原料,制备工艺简单,不涉及液相沉淀/还原,成本低廉,制备得到的磁性除磷吸附材料磁性强,易于回收,可有效避免吸附材料在沉积物滞留而导致的二次污染问题。
本发明有益效果在于本发明提供了一种磁性除磷颗粒吸附材料及其制备方法,该制备方法工艺简单,制备的磁性除磷颗粒吸附材料磁性强、对富营养化水体磷具有极强的吸附性能,且易于回收,绿色环保。
附图说明
图1为本发明所制备的磁性除磷吸附材料及磁吸效果图;
图2所示为磁性除磷吸附材料添加量与磷去除率的关系图;
图3所示为不同pH条件下磁性除磷吸附材料与磷去除率的关系图。
具体实施方式
下述实施案例中所使用的实验方法如无特殊说明,均为常规办法。
下述实施案例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施案例1磁性除磷吸附材料的制备
将沸石、氢氧化钙和四氧化三铁粉碎,过300目筛。称取300目沸石4kg,300目氢氧化钙0.5kg,300目四氧化三铁0.5kg,加入至圆盘造粒机中以1200rpm的速度快速搅拌2min,使其充分混合。混合后,加水1.5L,将转子转速调为1200rpm,造粒盘转速为50rpm,运行2min既为磁性除磷吸附材料,将制得的磁性除磷吸附材料在65℃恒温鼓风干燥箱烘干48h,烘干后,筛选粒径2-3mm的磁性除磷吸附材料,装入塑料瓶中密封备用。
实施案例2磁性除磷吸附材料对水体中磷的吸附去除效果及回收情况
采用磷酸二氢钾配制磷浓度为5mg/L的溶液,采用0.1mol/L的HCl溶液和0.1mol/L的NaOH溶液调节pH至7。然后按0.15、0.3、0.6、1.2、2.4g/L称取实施案例1制备的磁性除磷吸附材料添加至250mL磷溶液中,设置3个重复,放置到摇床上;摇床设置参数为200rpm,24h。最后采用0.45μm玻璃纤维滤膜过滤,测定原液磷含量和吸附后磷含量并计算不同添加量下磁性除磷吸附材料添的去除率。结果发现,当添加量达到0.6g/L时,磷的去除率达到79%,此时磷的吸附量最高,为6mg/g;添加量为1.2和2.4g/L时,磷的去除率达到97%以上,磷的吸附量分别为4和2mg/g。
实施案例3pH值对磁性除磷吸附材料吸附水体磷的影响
采用磷酸二氢钾配制磷浓度为5mg/L的溶液,采用0.1mol/L的HCl溶液和0.1mol/L的NaOH溶液分别调节pH为3、5、7、9、11。然后称取100mg左右实施例1制备的磁性除磷吸附材料添加至250mL磷溶液中,设置3个重复,放置到摇床上;摇床设置参数为200rpm,24h。最后采用0.45μm玻璃纤维滤膜过滤反应液,测定原液磷含量和吸附后磷含量并计算不同pH值下磁性除磷吸附材料的去除率。结果发现,该pH值对该磁性吸附材料影响较小,pH值在3-11范围内,吸附材料去除率差异不大,均能维持在90%以上。
Claims (9)
1.一种磁性除磷颗粒吸附材料的制备方法,其特征在于:该制备方法包括以下步骤:
(1)将天然粘土、四氧化三铁和氢氧化钙碾磨,过300目筛;
(2)取天然粘土6-8份,四氧化三铁1-2份,氢氧化钙粉末1-2份,这三种材料在圆盘造粒机中以1200r/s的速度快速搅拌2min,使其充分混合;
(3)充分混合后加入适量的水,将圆盘造粒机速度调到1200r/s,利用紊流混合原理造粒得到磁性除磷吸附材料;该造粒过程操作简单、可快速高效的在较短时间内制备出所需要的颗粒;
(4)将造粒得到的磁性除磷吸附材料烘干后过筛,得到粒径在1-5mm范围内不同粒径的磁性除磷颗粒吸附材料。
2.根据权利要求1所述的一种磁性除磷颗粒吸附材料的制备方法,其特征在于:天然粘土主要为沸石、凹凸棒土、膨润土、海泡石。
3.根据权利要求2所述的一种磁性除磷颗粒吸附材料的制备方法,其特征在于:其原料按照重量份包括:氢氧化钙1份,四氧化三铁1份,沸石8份;或其原料按照重量份包括:氢氧化钙1份,四氧化三铁1份,凹凸棒土8份;或其原料按照重量份包括:氢氧化钙1份,四氧化三铁1份,膨润土8份。
4.根据权利要求1所述的一种磁性除磷颗粒吸附材料的制备方法,其特征在于:将氢氧化钙、四氧化三铁和沸石按特定比例混合并造粒即可。
5.根据权利要求1所述的一种磁性除磷颗粒吸附材料的制备方法,其特征在于:混合造粒后45至65℃烘干。
6.根据权利要求1所述的一种磁性除磷颗粒吸附材料的制备方法,其特征在于:制备得到的磁性除磷颗粒吸附材料兼具磁性和高效的磷吸附能力。
7.根据权利要求1所述的一种磁性除磷颗粒吸附材料的制备方法,其特征在于:制备得到的磁性除磷颗粒吸附材料在富营养化水体中吸附饱和后可通过磁分离技术回收该材料,以防止该材料的二次污染。
8.根据权利1要求所述的一种磁性除磷颗粒吸附材料的制备方法,其特征在于:制备得到的磁性除磷颗粒吸附材料在水体pH为3-11的较宽范围内均具有良好的除磷能力。
9.根据权利要求1所述的一种磁性除磷颗粒吸附材料的制备方法,其特征在于,制备得到的磁性除磷颗粒吸附材料在水体除磷领域中应用。
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