CN106334515B - 一种利用功能化磁性四氧化三铁吸附镉离子的方法 - Google Patents
一种利用功能化磁性四氧化三铁吸附镉离子的方法 Download PDFInfo
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229940056319 ferrosoferric oxide Drugs 0.000 title claims abstract description 43
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 40
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 19
- 238000010521 absorption reaction Methods 0.000 claims abstract description 19
- 238000003795 desorption Methods 0.000 claims abstract description 11
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003463 adsorbent Substances 0.000 claims abstract description 8
- 238000007306 functionalization reaction Methods 0.000 claims abstract description 3
- 230000002194 synthesizing effect Effects 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 8
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- FHUDAMLDXFJHJE-UHFFFAOYSA-N 1,1,1-trifluoropropan-2-one Chemical compound CC(=O)C(F)(F)F FHUDAMLDXFJHJE-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
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- 150000002505 iron Chemical class 0.000 claims description 5
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- 239000000126 substance Substances 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
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- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 claims 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 9
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- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种利用功能化磁性四氧化三铁吸附镉离子的方法。该方法以功能化磁性四氧化三铁为吸附材料吸附重金属镉离子。主要技术特征是:首先合成磁性四氧化三铁,并对其进行功能化,得到功能化磁性四氧化三铁,在一定的条件下,功能化磁性四氧化三铁对Cd2+的最大吸附量为1000mg/g,甚至更高,吸附后的功能化磁性四氧化三铁用一定浓度的HCl即可解吸附,解吸率达95.26%。再生功能化磁性四氧化三铁二次吸附的最大吸附容量为920.4mg/g。
Description
技术领域
本发明属于工业污水处理领域,具体地说,利用功能化磁性四氧化三铁处理工业生产过程中形成的含镉离子废水。
背景技术
环境中镉的主要污染来源是:铅锌矿的开采、选矿和冶炼过程中产生的废水和废气;合金钢的生产和加工过程;电镀镉的生产废水,染料、农药、油漆、玻璃、陶瓷、照像材料等生产和加工过程。植物吸收富集于土壤中的镉,可使农作物中镉含量增高。水生动物吸收富集于水中的镉,可使动物体中镉含量升高。人体的镉中毒主要是通过消化道与呼吸道摄取被镉污染的水、食物、空气而引起的。镉在人体积蓄作用,潜伏期可长达10~30年。据报道,当水中镉超过0.2mg/L时,居民长期饮水和从食物中摄取含镉物质,可引起“骨痛病”。目前,目前,处理重金属污染常用的方法有化学沉淀法、容积萃取法、膜分离法、离子交换法和吸附法等。吸附法是处理重金属污染的有效途径之一。然而,吸附后的分离也是限制吸附法发展的关键问题,磁性材料的出现有效的解决了该问题。磁性四氧化三铁应用于重金属污染物的吸附成为一新的研究热点,然而目前的应用过程中,吸附量和其再生仍然是制约其应用的瓶颈。本发明合成了2-噻吩甲酰三氟丙酮功能化的磁性四氧化三铁,并将其用于吸附重金属镉离子的吸附。镉离子首先和功能化磁性四氧化三铁表面的小分子发生作用。功能化磁性四氧化三铁表面吸附镉后表面带有部分正电荷,OH-又被吸附至表面,形成了层层组装的吸附,功能化磁性四氧化三铁对镉的吸附量为1000mg/g,甚至更高,再生容易,可用于含镉废水的处理,具有广阔的应用前景。
发明内容
本发明的目的是提供一种利用功能化磁性四氧化三铁吸附镉离子的方法。特征在于该方法具有以下工艺步骤:
(1) 按照二价铁与三价铁的物质的量之比1:1~2:3,将二价铁盐(FeCl2)和三价铁盐(FeCl3·6H2O)混合溶液至三口烧瓶中,置于70 ~80℃恒温水浴锅中,剧烈搅拌,在氮气气氛下,恒压漏斗中逐滴加入浓氨水,使体系的pH ≥10,剧烈搅拌50~70min后,采用磁分离分离沉淀物,用蒸馏水反复洗涤沉淀物直至中性,在60下真空干燥后,研磨即得磁性四氧化三铁;
(2) 称取1~2g 十六烷基三甲基溴化铵溶解于100mL去离子水,加入0.8~1.2g 磁性四氧化三铁置于250mL锥形瓶中,置于70~80 ℃在恒温水浴振荡器中加热震荡10~12h。后将溶液自然冷却至室温磁分离操作并用去离子水洗涤,只至用AgNO3检测无色。置于真空干燥箱中60℃真空干燥,研磨得到产物1;
(3) 称取0.2~0.3g 2-噻吩甲酰三氟丙酮充分溶解于100mL无水乙醇中,将(2)中得到的产物1置于溶液置于2-噻吩甲酰三氟丙酮乙醇溶液中,放置在恒温水浴振荡器中,60℃搅拌30~40min,后取出继续静置老化30~50min。老化完成在磁性作用下先用无水乙醇清洗2~3次,然后用去离子水继续清洗2~3次后磁分离,60℃真空干燥,研磨得到最终产物功能化磁性四氧化三铁;
(4) 吸附:移取10.00mg/mLCd2+溶液10.00~20.00mL放入100mL锥形瓶中,加入10mL蒸馏水,加入0.1g~0.2g步骤(3)合成的功能化磁性四氧化三铁,摇匀,边摇边逐滴加入1mol/LNaOH溶液,采用磁分离分离吸附后吸附剂,用酸度计准确测量磁分离后溶液的pH8.60~12.00,并取清夜,用原子吸收法测定镉;
(5) 解吸附:将步骤(4)中吸附Cd2+后的功能化磁性四氧化三铁磁分离后,弃去上层溶液,加入40mL~80mL0.1mol/LHCl溶液,充分摇匀,磁分离,用蒸馏水洗涤,滤液定容,稀释,用原子吸收法测定镉,磁分离后的固体为再生的功能化磁性四氧化三铁;
(6)再吸附:移取10.00mg/mLCd2+溶液10.00~20.00mL放入含有步骤(5)中再生的功能化磁性四氧化三铁的100mL锥形瓶中,加入10mL蒸馏水,摇匀,边摇边逐滴加入1mol/LNaOH溶液,采用磁分离分离吸附后吸附剂,用酸度计准确测量磁分离后溶液的pH8.60~12.00,并取清夜,用原子吸收法测定镉。
本发明的有益成果
(1) 本发明中功能化磁性四氧化三铁的合成方法简单,经济,重现性强,环境污染小。
(2)本发明采用功能化磁性四氧化三铁吸附镉,吸附性能优良,吸附量可达1000mg/g,且可实现磁分离。
(3)本发明中功能化磁性四氧化三铁再生性能好,吸附后的磁性四氧化三铁解吸方便,成本低,可重复利用。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外还应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明做各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1 (1) 按照二价铁与三价铁的物质的量之比1:1,将二价铁盐(FeCl2)和三价铁盐(FeCl3·6H2O)混合溶液至三口烧瓶中,置于70 ~80℃恒温水浴锅中,剧烈搅拌,在氮气气氛下,恒压漏斗中逐滴加入浓氨水,使体系的pH ≥10,剧烈搅拌50~70min后,采用磁分离分离沉淀物,用蒸馏水反复洗涤沉淀物直至中性,在60下真空干燥后,研磨即得磁性四氧化三铁;
(2) 称取1g 十六烷基三甲基溴化铵溶解于100mL去离子水,加入0.8g 磁性四氧化三铁置于250mL锥形瓶中,置于70 ℃在恒温水浴振荡器中加热震荡10h。后将溶液自然冷却至室温磁分离操作并用去离子水洗涤,只至用AgNO3检测无色。置于真空干燥箱中60℃真空干燥,研磨得到产物1;
(3) 称取0.2g 2-噻吩甲酰三氟丙酮充分溶解于100mL无水乙醇中,将(2)中得到的产物1置于溶液置于2-噻吩甲酰三氟丙酮乙醇溶液中,放置在恒温水浴振荡器中,60℃搅拌30min,后取出继续静置老化30min。老化完成在磁性作用下先用无水乙醇清洗2~3次,然后用去离子水继续清洗2~3次后磁分离,60℃真空干燥,研磨得到最终产物功能化磁性四氧化三铁。
实施例2 (1) 按照二价铁与三价铁的物质的量之比4:5,将二价铁盐(FeCl2)和三价铁盐(FeCl3·6H2O)混合溶液至三口烧瓶中,置于75℃恒温水浴锅中,剧烈搅拌,在氮气气氛下,恒压漏斗中逐滴加入浓氨水,使体系的pH ≥10,剧烈搅拌60min后,采用磁分离分离沉淀物,用蒸馏水反复洗涤沉淀物直至中性,在60下真空干燥后,研磨即得磁性四氧化三铁;
(2) 称取1.5g 十六烷基三甲基溴化铵溶解于100mL去离子水,加入1.0g 磁性四氧化三铁置于250mL锥形瓶中,置于75℃在恒温水浴振荡器中加热震荡11h。后将溶液自然冷却至室温磁分离操作并用去离子水洗涤,只至用AgNO3检测无色。置于真空干燥箱中60℃真空干燥,研磨得到产物1;
(3) 称取0.25g 2-噻吩甲酰三氟丙酮充分溶解于100mL无水乙醇中,将(2)中得到的产物1置于溶液置于2-噻吩甲酰三氟丙酮乙醇溶液中,放置在恒温水浴振荡器中,60℃搅拌40min,后取出继续静置老化50min。老化完成在磁性作用下先用无水乙醇清洗2~3次,然后用去离子水继续清洗2~3次后磁分离,60℃真空干燥,研磨得到最终产物功能化磁性四氧化三铁。
实施例3 移取10.00mg/mLCd2+溶液10.00~20.00mL放入100mL锥形瓶中,加入10mL蒸馏水,加入0.1g功能化磁性四氧化三铁,摇匀,边摇边逐滴加入1mol/LNaOH溶液,采用磁分离分离吸附后吸附剂,用酸度计准确测量磁分离后溶液的pH8.60,并取清夜,用原子吸收法测定镉,经计算得0.1g功能化磁性四氧化三铁吸附了0.09925g镉,吸附量为0.9925g/g,吸附率为99.25%。
实施例4 移取10.00mg/mLCd2+溶液10.00~20.00mL放入100mL锥形瓶中,加入10mL蒸馏水,加入0.1g功能化磁性四氧化三铁,摇匀,边摇边逐滴加入1mol/LNaOH溶液,采用磁分离分离吸附后吸附剂,用酸度计准确测量磁分离后溶液的pH11.0,并取清夜,用原子吸收法测定镉,未检出镉离子,经计算得0.1g功能化磁性四氧化三铁吸附了0.1000g镉,吸附量为1.000g/g,吸附率为100.0%。
实施例5 解吸附:将0.1g功能化磁性四氧化三铁吸附10.00mL10.00mg/mLCd2+溶液后的功能化磁性四氧化三铁磁分离后,弃去上层溶液,加入40mL0.1mol/LHCl溶液,充分摇匀,磁分离,用蒸馏水洗涤,滤液定容,稀释,用原子吸收法测定镉,结果93.19%的Cd2+被解析下来。
实施例6 解吸附:将0.1g功能化磁性四氧化三铁吸附10.00mL10.00mg/mLCd2+溶液后的功能化磁性四氧化三铁磁分离后,弃去上层溶液,加入60mL0.1mol/LHCl溶液,充分摇匀,磁分离,用蒸馏水洗涤,滤液定容,稀释,用原子吸收法测定镉,结果95.26%的Cd3+被解析下来。
实施例7 再吸附:移取10.00mg/mLCr3+溶液10.00mL放入含有再生的功能化磁性四氧化三铁的100mL锥形瓶中,加入10mL蒸馏水,摇匀,边摇边逐滴加入1mol/LNaOH溶液,采用磁分离分离吸附后吸附剂,用酸度计准确测量磁分离后溶液的pH9.50,并取清夜,用原子吸收法测定镉,测定其再吸附率为92.04%。
Claims (3)
1.一种利用功能化磁性四氧化三铁吸附镉离子的方法,其特征在于,包括以下步骤:
(1) 功能化磁性四氧化三铁的制备:首先合成磁性四氧化三铁,然后将所合成的四氧化三铁进一步功能化为功能化磁性四氧化三铁;
(2) 功能化磁性四氧化三铁吸附镉离子:将含镉离子的溶液和功能化磁性四氧化三铁混合,摇匀,逐滴加入NaOH溶液,使镉离子吸附于功能化磁性四氧化三铁表面;
(3) 解吸附和再吸附:功能化磁性四氧化三铁吸附镉离子后,逐滴加入盐酸使其解吸附,利用解吸附后的功能化磁性四氧化三铁进一步吸附镉离子;
其中,步骤(1)所述的功能化磁性四氧化三铁的制备具体如下:
① 按照二价铁与三价铁的物质的量之比1:1~2:3,将二价铁盐FeCl2和三价铁盐FeCl3·6H2O混合溶液置于三口烧瓶中,置于70~80℃恒温水浴锅中,剧烈搅拌,在氮气气氛下,恒压漏斗中逐滴加入浓氨水,使体系的pH≥10,剧烈搅拌50~70min后,采用磁分离法分离沉淀物,用蒸馏水反复洗涤沉淀物直至中性,在60℃下真空干燥后,研磨即得磁性四氧化三铁;
② 称取1~2g十六烷基三甲基溴化铵溶解于100mL去离子水,加入0.8~1.2g磁性四氧化三铁至250mL锥形瓶中,置于70~80℃恒温水浴振荡器中加热震荡10~12h,后将溶液自然冷却至室温,磁分离操作并用去离子水洗涤,直至用AgNO3检测无色,置于真空干燥箱中60℃真空干燥,研磨得到产物1;
③ 称取0.2~0.3g 2-噻吩甲酰三氟丙酮充分溶解于100mL无水乙醇中,将②中得到的产物1置于2-噻吩甲酰三氟丙酮乙醇溶液中,放置在恒温水浴振荡器中,60℃搅拌30~40min后,取出继续静置老化30~50min,老化完成在磁性作用下先用无水乙醇清洗2~3次,然后用去离子水继续清洗2~3次后磁分离,60℃真空干燥,研磨得到最终产物功能化磁性四氧化三铁。
2.根据权利要求1所述的一种利用功能化磁性四氧化三铁吸附镉离子的方法,其特征在于,步骤(2)所述的功能化磁性四氧化三铁吸附镉离子,具体有以下步骤:移取10.00mg/mL Cd2+溶液10.00~20.00mL放入100mL锥形瓶中,加入10mL蒸馏水,加入0.1g~0.2g功能化磁性四氧化三铁,摇匀,边摇边逐滴加入1mol/L NaOH溶液,采用磁分离法分离吸附后吸附剂,用酸度计准确测量磁分离后溶液的pH8.60~12.00,并取清液,用原子吸收法测定镉。
3.根据权利要求1所述的一种利用功能化磁性四氧化三铁吸附镉离子的方法,其特征在于,步骤(3)所述的解吸附和再吸附,具体有以下步骤:
(1) 解吸附:将吸附Cd2+后的功能化磁性四氧化三铁磁分离后,弃去上层溶液,加入40mL~80mL 0.1mol/L HCl溶液,充分摇匀,磁分离,用蒸馏水洗涤,滤液定容,稀释,用原子吸收法测定镉,磁分离后的固体为再生的功能化磁性四氧化三铁;
(2) 再吸附:移取10.00mg/mL Cd2+溶液10.00~20.00mL放入含有再生的功能化磁性四氧化三铁的100mL锥形瓶中,加入10mL蒸馏水,摇匀,边摇边逐滴加入1mol/L NaOH溶液,采用磁分离法分离吸附后吸附剂,用酸度计准确测量磁分离后溶液的pH8.60~12.00,并取清液,用原子吸收法测定镉。
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