CN110540243B - 无定型羟基氧化铁的制备方法及吸附有机物后的回收方法 - Google Patents
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- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 10
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- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 3
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract description 10
- 229910002588 FeOOH Inorganic materials 0.000 abstract description 9
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- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 3
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- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 3
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- 125000004122 cyclic group Chemical group 0.000 description 1
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- 229910001385 heavy metal Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
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- 239000006228 supernatant Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B82—NANOTECHNOLOGY
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Abstract
本发明公开了一种无定型羟基氧化铁的制备方法及吸附有机物后的回收方法,本发明提高无定型羟基氧化铁的制备效率,由于所采用的制备原料为氯化铁,其中的铁为三价铁,而非传统的氯化亚铁或硫酸亚铁,避免了制备过程中的氧化流程,使无定型羟基氧化铁的制备效率大幅提高。吸附有机物后的羟基氧化铁得到有效回收利用,经过煅烧后获得具有光催化效果的纳米α氧化铁,由于有机物的存在,使得所制得的纳米氧化铁,其晶粒比直接由无定型羟基氧化铁制备的纳米氧化铁更细,表面具有更多的活性点,催化效果更好。
Description
技术领域
本发明涉及印染废水有机物降解领域,尤其涉及一种无定型羟基氧化铁的制备方法及吸附有机物后的回收方法。
背景技术
目前国内生产羟基氧化铁主要采用以硫酸亚铁和碳酸钠或碳酸氢铵为原料,按比例混合后,在加热状态下,通入空气氧化,经洗涤、过滤制成产品。该工艺采用空气氧化法,反应速度慢,生产效率低。
无定型羟基氧化铁广泛用于脱硫剂、重金属脱除剂、污水处理剂。其对有机废水的脱除主要是物理吸附,并没有分解有机物,吸附过有机物的羟基氧化铁,再次利用时,其吸附效率急剧降低。
发明内容
本发明针对羟基氧化铁制备效率低,无定型羟基氧化铁吸附有机物后循环利用困难的问题,本发明提供了一种无定型羟基氧化铁的制备方法及吸附有机物后的回收方法,该方法以氯化铁为原料制备无定型羟基氧化铁,无需氧化流程,效率高;吸附有机物后的羟基氧化铁经煅烧获得具有光催化性能的纳米氧化铁,可以用于光催化讲解有机物。
本发明通过以下技术方案来实现上述目的:
本发明一种无定型羟基氧化铁的制备方法及吸附有机物后的回收方法,其特征在于:将煤油、司盘80、吐温80和蒸馏水按照质量比为:20:10:10:1的比例配成微乳相,搅拌至透明待用;加入氯化铁粉末,氯化铁粉末与蒸馏水的质量比为1-4:1,其充分搅拌至粉末完全溶解,加入氢氧化钠颗粒,氢氧化钠与氯化铁的摩尔比为1:1,加热至80℃~90℃反应30分钟后停止加热,离心获得沉淀,用无水乙醇洗涤2次,用蒸馏水洗涤2次,干燥后得到无定型羟基氧化铁。
本发明一种无定型羟基氧化铁制备吸附有机物后的回收方法,其特征在于:取适量制备的无定型羟基氧化铁,加入印染废水中,充分搅拌,通过无定型羟基氧化铁的吸附作用,有效脱除印染废水中的有机物;吸收有机物后的无定型羟基氧化铁,在600~800℃下煅烧1~3小时,获得具有光催化效果的纳米氧化铁,可用于印染废水的光催化。
具体地,经过离心提取沉淀后剩余的微乳相能继续循环使用。
具体地,无定型羟基氧化铁通过物理吸附的方法脱除印染废水中的有机物。
具体地,无定型羟基氧化铁经过600~800℃煅烧所获得的纳米氧化铁为α氧化铁。
具体地,经过600~800℃的煅烧,被羟基氧化铁吸附的有机物被分解,在分解过程中部分有机物被碳化,并在进一步氧化过程中,起到细化纳米氧化铁晶粒的作用,使其表面活性点更多,光催化效果更好。
本发明的有益效果在于:
本发明是一种无定型羟基氧化铁的制备方法及吸附有机物后的回收方法,与现有技术相比,本发明提高无定型羟基氧化铁的制备效率,由于所采用的制备原料为氯化铁,其中的铁为三价铁,而非传统的氯化亚铁或硫酸亚铁,避免了制备过程中的氧化流程,使无定型羟基氧化铁的制备效率大幅提高。吸附有机物后的羟基氧化铁得到有效回收利用,经过煅烧后获得具有光催化效果的纳米α氧化铁,由于有机物的存在,使得所制得的纳米氧化铁,其晶粒比直接由无定型羟基氧化铁制备的纳米氧化铁更细,表面具有更多的活性点,催化效果更好。
附图说明
图1为所制备的无定型羟基氧化铁的XRD图;
图2为循环次数对无定型羟基氧化铁10分钟吸附脱色率的影响图;
图3为吸附过有机物后的羟基氧化铁经过700℃煅烧2小时后获得的纳米氧化铁的XRD图;
图4为纳米氧化铁紫外光催化降解甲基橙降解率曲线;
图5为纳米氧化铁模拟太阳光催化降解甲基橙降解率曲线。
具体实施方式
下面对本发明作进一步说明:
实施例1
将煤油、司盘80、吐温80和蒸馏水按照质量比为:20:10:10:1的比例配成微乳相,搅拌至透明待用;加入氯化铁粉末,氯化铁粉末与蒸馏水的质量比为1-4:1,其充分搅拌至粉末完全溶解,加入氢氧化钠颗粒,氢氧化钠与氯化铁的摩尔比为1:1,加热至80℃反应30分钟后停止加热,离心获得沉淀,用无水乙醇洗涤2次,用蒸馏水洗涤2次,干燥后得到无定型羟基氧化铁。其XRD图谱如附图1所示。
在100毫升浓度为50mg/l的甲基橙溶液中加入0.1g无定型羟基氧化铁,在避光的条件下搅拌吸附10分钟,取样,在离心机中以10000转/分钟的转速离心10分钟,脱除悬浮在溶液中的无定型羟基氧化铁粉末,取上清液,用紫外可见光分光光度计测吸光度,计算脱色率。吸附过甲基橙的无定型羟基氧化铁通过离心的方式回收,然后再相同的条件下进行第1次、第2次和第3次循环吸附实验,计算脱色率。结果如附图2所示,随着循环次数的增加,无定型羟基氧化铁的吸附效果急剧下降。
实施例2
将实施例1中吸附过甲基橙的无定型羟基氧化铁在700℃下煅烧2小时,获得纳米α羟基氧化铁,其XRD图谱如附图3所示。取100毫升浓度为20mg/l的甲基橙溶液,加入0.01g纳米α羟基氧化铁,避光搅拌1小时,加入5毫升30%的双氧水,在300nm紫外光下照射进行降解,降解率如附图4所示。
实施例3
取100毫升浓度为20mg/l的甲基橙溶液,加入0.01g实施例2所制备的纳米α羟基氧化铁,避光搅拌1小时,加入5毫升30%的双氧水,在300W氙气灯下照射进行降解,降解率如附图5所示。
以上显示和描述了本发明的基本原理和主要特征及本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (2)
1.一种无定型羟基氧化铁的制备方法,其特征在于:将煤油、司盘80、吐温80和蒸馏水按照质量比为:20:10:10:1的比例配成微乳相,搅拌至透明待用;加入氯化铁粉末,氯化铁粉末与蒸馏水的质量比为1-4:1,其充分搅拌至粉末完全溶解,加入氢氧化钠颗粒,氢氧化钠与氯化铁的摩尔比为1:1,加热至80℃~90℃反应30分钟后停止加热,离心获得沉淀,用无水乙醇洗涤2次,用蒸馏水洗涤2次,干燥后得到无定型羟基氧化铁。
2.根据权利要求1所述的无定型羟基氧化铁的制备方法,其特征在于:经过离心提取沉淀后剩余的微乳相能继续循环使用。
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