CN114644334B - 一种高效去除重金属污染物的多层氮掺碳材料的制备方法 - Google Patents
一种高效去除重金属污染物的多层氮掺碳材料的制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 52
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 claims abstract description 26
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical compound [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims abstract description 26
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
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- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000012300 argon atmosphere Substances 0.000 claims 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 30
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- 239000000463 material Substances 0.000 abstract description 7
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- 229910052786 argon Inorganic materials 0.000 abstract description 6
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- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000004140 cleaning Methods 0.000 abstract 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 abstract 2
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- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
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Abstract
本发明公开了一种高效去除重金属污染物的多层氮掺碳材料的制备方法。其制备步骤包括:1)将2‑甲基咪唑和硝酸锌以4mmol:1mmol的比例分别溶解于40ml甲醇溶液中,超声处理10‑15min,分别搅拌10‑15min,然后将以上两溶液混合,混合液搅拌20‑30min;2)将入1)中处理后的溶液,在90℃下加热6h,后用甲醇和超纯水清洗后2‑3遍后烘干制得ZIF‑8粉末;4)将3)中制备好的材料,经超声处理均匀分散在饱和的NaCl溶液中,期间连续加入混合溶液体积20‑40%的乙醇,后在80℃下烘干制得ZIF‑8@NaCl晶体;5)置于管式炉中氩气保护条件下,在750‑850℃分别加热3h,用超纯水清洗去除复合物中NaCl后制得多层氮掺碳材料(h‑NC)。该材料结构性能稳定强,对重金属污染物的去除效率高、且易于再生大大延长了其使用寿命。
Description
技术领域
本发明涉及吸附材料技术领域,具体的说,尤其涉及一种去除重金属污染物的MOFs衍生的多层氮掺碳材料的制备方法。
背景技术
水中重金属污染对人类和生态系统具有高毒性,特别是镉(Cd)离子的持续排放和生物累积效应,对生态环境产生致命的影响,甚至危害人类生命。为了解决这一问题,吸附法因其成本低、操作简单、环保等显著优点受到关注。因此,寻找具有结构稳定、成本低、高选择性的碳基吸附剂材料用于有效的Cd2+去除势在必行。
发明内容
本发明的目的在于提供一种高效去除水体中重金属污染物的碳基材料,该材料具有稳定的结构性能,较高的吸附性能,并且能够进行多个周期循环使用。
本发明的目的是通过以下技术方案实现的:
高效去除水体中重金属污染物的MOFs衍生的多层氮掺碳材料由以下方法制备而成:
1)首先,制备ZIF-8粉末。以4mmol:1mmol称取2-甲基咪唑粉末和六水合硝酸锌,分别溶解于40ml甲醇中,超声处理10-15min,搅拌10-15min,后将两溶液混合,搅拌20-30min,后将混合液倒入100ml水热釜中,在90℃下加热6h,用甲醇和超纯水清洗2-3遍,烘干制得ZIF-8粉末。
2)然后,制备ZIF-8@NaCl。将制得的ZIF-8粉末溶于饱和的NaCl溶液(NaCl:超纯水=3.6g:10ml)中,超声处理10min,期间连续加入混合溶液体积20-40%的乙醇发生NaCl再结晶,在80℃下烘干制得ZIF-8@NaCl晶体。
3)接着,制备h-NC。将ZIF-8@NaCl晶体,在氩气保护条件下于管式炉中烧制3h,烧制温度750-850℃,用超纯水洗去NaCl后烘干制得h-NC材料。
4)最后,重金属去除。将在不同温度制成的多层氮掺碳材料,在30℃,pH=7下,对浓度为0.4-300mg L-1的Cd2+进行去除,根据Langmuir曲线拟合得到相应的最大吸附量。
所述一种高效去除重金属污染物的双碳结构的氮掺碳材料的制备方法,其特征在于:本发明采用NaCl为模板,以ZIF-8为基础碳材料烧制而成,以此改变了氮掺碳材料的微观结构,同时影响氮掺碳材料中的元素含量,从而影响其稳定性和吸附性能。由于NaCl的盐密封作用,其发生分解作用时中间产物被困在氯化钠中,启动原位自组装过程,进一步碳化和除盐后合成双碳分层纳米结构,有利于活性吸附剂与污染物之间的化学相互作用。
本发明要解决的第二个问题是,探究烧制的不同温度,对氮掺碳材料结构和对重金属污染物的吸附性能的影响。一种能高效去除重金属污染物的制备方法,这是本技术的关键所在。因此,在保证氮掺碳材料的结构稳定性和良好吸附性能的前提下,作为优选,本发明通过以下方法制备:
将ZIF-8@NaCl晶体,在氩气保护条件下于管式炉中烧制3h,烧制温度800℃。
本发明的优点如下:本发明通过合理地控制材料烧制时间,得到稳定的三维碳纳米多面体@纳米片结构,并得到合理的碳、氮元素比,从而增加了吸附剂与污染物之间的化学作用,提高了对污染物的去除效率。另一方面,氮掺碳材料的比表面积增大,并存在微孔,大大增加了吸附剂与污染物的接触面积,从而提高了对污染物的去除效果。
附图说明
图1为本发明中材料合成示意图。
图2为吸附效果图。
图3为h-NC-750的(a)TEM低倍图和(b)TEM高倍图;h-NC-800的(c)TEM低倍图和(d)TEM高倍图;h-NC-850的(e)TEM低倍图和(f)TEM高倍图。
具体实施方式
下面结合附图和实例对本发明进行说明。
实施案例1
如图1所示,本发明中h-NC-750制备时碳化的温度为750℃。图3a-b所示为TEM低倍图和TEM高倍图。其具体制备方法如下:
1)称取3.28g的2-甲基咪唑和2.98g的六水合硝酸锌,分别溶解于40ml甲醇中,超声处理10min,搅拌15min,后将两溶液混合,搅拌30min;
2)将1)中混合液倒入100ml水热釜中,在90℃下加热6h,用甲醇和超纯水清洗2遍,烘干制得ZIF-8粉末;
3)取0.8g ZIF-8粉末放入饱和的NaCl溶液(7.2gNaCl溶于20ml超纯水)中,超声处理10min,期间连续加入6ml乙醇,后在80℃下烘干制得ZIF-8@NaCl晶体;
4)将ZIF-8@NaCl晶体,在氩气保护条件下,在管式炉中烧制3h,烧制温度为750℃;
5)通过离心、过滤,用超纯水洗去NaCl后,烘干制得h-NC-750;
6)由此制备的h-NC-750比表面积较小,为1270m2/g,结构紧实,并且结构不稳定,呈非晶态;
7)同时其在30℃,pH=7条件下,对Cd2+的最大吸附量为317mg g-1。
实施案例2
如图1所示,本发明中h-NC-800制备时碳化的温度为800℃。图3c-d所示为TEM低倍图和TEM高倍图。其具体制备方法如下:
1)称取3.28g的2-甲基咪唑和2.98g的六水合硝酸锌,分别溶解于40ml甲醇中,超声处理10min,搅拌15min,后将两溶液混合,搅拌30min;
2)将1)中混合液倒入100ml水热釜中,在90℃下加热6h,用甲醇和超纯水清洗2遍,烘干制得ZIF-8粉末;
3)取0.8g ZIF-8粉末放入饱和的NaCl溶液(7.2gNaCl溶于20ml超纯水)中,超声处理10min,期间连续加入6ml乙醇,后在80℃下烘干制得ZIF-8@NaCl晶体;
4)将ZIF-8@NaCl晶体,在氩气保护条件下,在管式炉中烧制3h,烧制温度为800℃;
5)通过离心、过滤,用超纯水洗去NaCl后,烘干制得h-NC-800;
6)由此制备的h-NC-800的比表面积比h-NC-750稍小,为1174m2/g,并且结构稳定有序;
7)同时其在30℃,pH=7条件下,对Cd2+的最大吸附量为356mg g-1,与h-NC-750相比提高近10%。
实施案例3
如图1所示,本发明中h-NC-850制备时碳化的温度为850℃。图3e-f所示为TEM低倍图和TEM高倍图。具体的制备方法如下:
1)称取3.28g的2-甲基咪唑和2.98g的六水合硝酸锌,分别溶解于40ml甲醇中,超声处理10min,搅拌15min,后将两溶液混合,搅拌30min;
2)将1)中混合液倒入100ml水热釜中,在90℃下加热6h,用甲醇和超纯水清洗2遍,烘干制得ZIF-8粉末;
3)取0.8g ZIF-8粉末放入饱和的NaCl溶液(7.2gNaCl溶于20ml超纯水)中,超声处理10min,期间连续加入6ml乙醇,后在80℃下烘干制得ZIF-8@NaCl晶体;
4)将ZIF-8@NaCl晶体,在氩气保护条件下,在管式炉中烧制3h,烧制温度为850℃;
5)通过离心、过滤,用超纯水洗去NaCl后,烘干制得h-NC-850;
6)由此制备得到纳米晶态的h-NC-850,其比表面积相比最小,为1037m2/g,且平面间距更清晰;
7)同时其在30℃,pH=7条件下,对Cd2+的最大吸附量为240mg g-1。
Claims (4)
1.一种高效去除重金属污染物多层氮掺碳材料的制备方法,其特征在于,步骤如下:
将ZIF-8经超声处理均匀分散于饱和的NaCl溶液中得到混合溶液,期间连续加入混合溶液体积20-40%的乙醇,然后在 80℃下烘干制得ZIF-8@NaCl晶体;
将ZIF-8@NaCl晶体置于管式炉中,在氩气氛围下,烧制3h,温度控制在750-850℃,然后用超纯水洗去NaCl,烘干制得h-NC。
2.根据权利要求1中所述的制备方法,其特征在于:在管式炉中烧制时温度设为800℃。
3.根据权利要求1中所述的制备方法,其特征在于:0.8g ZIF-8粉末放入饱和的NaCl溶液,NaCl溶液采用7.2gNaCl溶于20ml超纯水。
4.按照权利要求1中所述的方法所制备的h-NC在pH=5-9范围内下对镉离子进行去除的用途。
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