CN109701496B - 氧化石墨烯复合材料、其制备方法及应用 - Google Patents
氧化石墨烯复合材料、其制备方法及应用 Download PDFInfo
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Abstract
本发明提供一种氧化石墨烯复合材料的制备方法,包括如下步骤:在无机弱碱的存在下,经分散处理的氧化石墨烯与L‑精氨酸,在常温下反应,然得到氧化石墨烯复合材料。本发明还公开了所述方法制得的氧化石墨烯复合材料。本发明还公开了所述氧化石墨烯复合材料吸附Cr(VI)的应用。本发明工艺,制备条件温和,步骤简单,且制备的氧化石墨烯复合材料展示出来良好的Cr(VI)吸附性能。
Description
技术领域
本发明涉及化学领域,尤其涉及一种对Cr(VI)离子具有吸附作用的氧化石墨烯复合材料、其制备方法及应用。
背景技术
重金属通常以单质或化合物形式存在于自然界中,对生态和人类健康威胁较小;但是近年来随着对金属矿物的过度开发,产生了含有大量金属离子的工业废水。
以铬为例,铬是生物体所需的微量元素和工业领域的战略性元素之一,在自然界中,铬主要以铬铁矿(FeCr2O4)和铬铅矿(PbCrO4)的形式存在,其主要用于冶金工业、化妆品原料、皮革、工业色素等领域。然而,这些工业生产引起了严重的环境污染,比如水体中的铬污染。众所周知,Cr(VI)的毒性远大于Cr(III),Cr(VI)是一种易被人体吸收的致癌物;人体吸入这种高毒性的六价铬离子后,轻者可能引起皮肤过敏,重者可能会导致遗传性基因缺陷或者引起癌症。水体被铬污染直接威胁着人类的生命健康,因此,有效地从工业废水中除去Cr(VI)已经成为一个严重的急需解决的问题。
近年来,研究者们对Cr(VI)的移除方法已经做了很多研究,主要包括化学沉淀法,离子交换法,电解法以及吸附法等。其中,吸附法由于原料易得,操作简便,成本低,Cr(VI)除去率高等优点被广泛运用。然而,常用的吸附剂如活性炭,生物吸附剂、玉米秸秆、吸附树脂、沸石吸附、黏土吸附和二氧化硅吸附等,但这些吸附剂在铬离子移除方面都存在一定限制。因此,开发新型有效的 Cr(VI)吸附剂仍旧是需要解决的问题。
有鉴于此,需要提供一种改进的能够吸附Cr(VI)的L-精氨酸/氧化石墨烯复合材料、制备方法及应用。
发明内容
本发明的目的在于提供一种对Cr(VI)离子具有吸附作用的L-精氨酸/氧化石墨烯复合材料、制备方法及应用。
为达到上述目的,本发明提供如下技术方案:一种L-精氨酸/氧化石墨烯复合材料的制备方法,包括如下步骤:S1:将氧化石墨烯加入到四氢呋喃中,分散得到氧化石墨烯的四氢呋喃分散液;S2:向氧化石墨烯的四氢呋喃分散液中加入L-精氨酸、碳酸钾粉末和去离子水,常温下搅拌24h;S3:用水洗涤若干次,干燥后得到L-精氨酸/氧化石墨烯复合材料。
作为本发明的进一步改进,氧化石墨烯的四氢呋喃分散液中,氧化石墨烯的浓度为0.5mg/mL~5mg/mL。
作为本发明的进一步改进,步骤S1具体为:在200W超声波清洗器中超声分散1h,得到氧化石墨烯的四氢呋喃分散液。
作为本发明的进一步改进,步骤S2中,各组分加入比例为:氧化石墨烯:L-精氨酸:碳酸钾:去离子水为:1g~1.5g:3g:0.5g~0.75g:5mL~7.5mL。
作为本发明的进一步改进,步骤S2中,各组分加入比例为:氧化石墨烯与L-精氨酸的用量比例是1g~1.5g:3g;氧化石墨烯与碳酸钾用量比例是1g:0.5g;碳酸钾和去离子水用量比例是1g:10mL。
作为本发明的进一步改进,步骤S3中,干燥过程具体为产物在60℃条件下真空干燥10h~15h。
为达到上述目的,本发明还提供由上述L-精氨酸/氧化石墨烯复合材料的制备方法制备的L-精氨酸/氧化石墨烯复合材料。
为达到上述目的,本发明还提供一种L-精氨酸/氧化石墨烯复合材料对溶液中Cr(VI)离子进行吸附的应用。
作为本发明的进一步改进,L-精氨酸/氧化石墨烯复合材料对溶液中Cr(VI)离子进行吸附具体为:准确称取3mg的L-精氨酸/氧化石墨烯复合材料作为吸附剂加入到pH介于1~6之间的10mL, 0.5mmol/L~2mmol/L的Cr(VI)离子的溶液中,15℃~30℃恒温搅拌反应0h~24h,过滤得到澄清的溶液,然后利用紫外可见分光光度计检测澄清溶液的吸光度,最后计算出L-精氨酸/氧化石墨烯复合材料对Cr(VI)离子的除去率。
作为本发明的进一步改进,过滤过程具体为:利用220nm微孔滤膜滤出吸附剂得到澄清的溶液
本发明的有益效果在于:本发明的L-精氨酸/氧化石墨烯复合材料的制备方法,通过反应在氧化石墨烯表面接枝L-精氨酸,制备条件温和,步骤简单,且制备的L-精氨酸/氧化石墨烯复合材料展示出来良好的Cr(VI)吸附性能。
附图说明
图1为本发明一种L-精氨酸/氧化石墨烯复合材料的制备方法的反应路线图。
图2是图1所示的L-精氨酸/氧化石墨烯复合材料、L-精氨酸原料及氧化石墨烯原料的红外光谱图。
具体实施方式
下面结合附图和实施例,对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明,但不用来限制本发明的范围。
请参见图1,为本发明的L-精氨酸/ 氧化石墨烯复合材料的制备方法。该方法以石墨烯或氧化石墨烯为基础,在氧化石墨烯上接枝L-精氨酸,形成具有吸附Cr(VI)作用的L-精氨酸/ 氧化石墨烯复合材料。利用石墨烯本身具有大的比表面积,大的π共轭结构和稳定性将其作为基体。选用可以提供孤对电子的氨基的L-精氨酸,在酸性条件下可被质子化带正电,进而可通过静电吸附作用吸附酸性条件下的Cr(VI)离子。另外,L-精氨酸作为一种环境友好型化合物,在Cr(VI)离子吸附过程中不会对水体造成二次污染。
其中,氧化石墨烯可以采用经典的Hummer方法制备,冷冻干燥得到;也可以直接购买获得。L-精氨酸通过直接购买获得。
L-精氨酸/氧化石墨烯复合材料的制备方法包括如下步骤:
S1:将氧化石墨烯加入到四氢呋喃中,分散得到氧化石墨烯的四氢呋喃分散液;S2:向氧化石墨烯的四氢呋喃分散液中加入L-精氨酸、碳酸钾粉末和去离子水,常温下搅拌24h;S3:用水洗涤若干次,干燥后得到L-精氨酸/氧化石墨烯复合材料。
步骤S1具体为:在200W超声波清洗器中超声分散1h,得到氧化石墨烯的四氢呋喃分散液;另外,其氧化石墨烯的浓度为0.5mg/mL~5mg/mL。
步骤S2中,各组分加入量为:氧化石墨烯:L-精氨酸:碳酸钾:去离子水为:1g~1.5g:3g:0.5g~0.75g:5mL~7.5mL。优选地,石墨烯与L-精氨酸的用量比例是1g~1.5g:3g;氧化石墨烯与碳酸钾用量比例是1g:0.5g;碳酸钾和去离子水用量比例是1g:10mL。
步骤S3中,干燥过程具体为产物在60℃条件下真空干燥10h~15h。
以下将以几个具体的实施例说明L-精氨酸/氧化石墨烯复合材料的制备方法:
实施例一,S1:将100mg氧化石墨烯加入到50mL的四氢呋喃中,在200W超声波清洗器中超声分散1h,得到氧化石墨烯的四氢呋喃分散液;S2:向氧化石墨烯的四氢呋喃分散液中加入0.3g的L-精氨酸、0.05g的碳酸钾粉末和0.5mL去离子水,25℃条件下搅拌24h;S3:最后用水洗涤3次,产物60℃真空干燥12h得到L-精氨酸/氧化石墨烯复合材料。
由上述制备方法获得的L-精氨酸/氧化石墨烯复合材料,通过傅立叶变换红外光谱(FT-IR)测定样品的结构。测试条件为:波长范围为4000~400cm-1,分辨率为4,扫描次数为32;L-精氨酸/氧化石墨烯复合材料、氧化石墨烯原料、L-精氨酸原料均采用溴化钾压片的方法测试。测试结果如图2所示,说明我们成功地在氧化石墨烯表面接枝了L-精氨酸,制备了L-精氨酸/氧化石墨烯复合材料。
实施例二,S1:将25mg氧化石墨烯加入到50mL的四氢呋喃中,在200W超声波清洗器中超声分散1h,得到氧化石墨烯的四氢呋喃分散液;S2:向氧化石墨烯的四氢呋喃分散液中加入0.3g的L-精氨酸、12.5mg的碳酸钾粉末和0.125mL去离子水,25℃条件下搅拌24h;S3:最后用水洗涤3次,产物60℃真空干燥12h得到L-精氨酸/氧化石墨烯复合材料。
实施例三,S1:将250mg氧化石墨烯加入到50mL的四氢呋喃中,在200W超声波清洗器中超声分散1h,得到氧化石墨烯的四氢呋喃分散液;S2:向氧化石墨烯的四氢呋喃分散液中加入0.3g的L-精氨酸、125mg的碳酸钾粉末和1.25mL去离子水,25℃条件下搅拌24h;S3:最后用水洗涤3次,产物60℃真空干燥12h得到L-精氨酸/氧化石墨烯复合材料。
通过傅立叶变换红外光谱(FT-IR)测定实施例二和实施例三获得的样品结构,也表明成功地在氧化石墨烯表面接枝了L-精氨酸,制备了L-精氨酸/氧化石墨烯复合材料。
本发明的L-精氨酸/氧化石墨烯对溶液中Cr(VI)离子进行吸附的应用,具体为:准确称取3mg的L-精氨酸/氧化石墨烯复合材料作为吸附剂加入到pH介于1~6之间的10mL,0.5mmol/L~2mmol/L的Cr(VI)离子的溶液中,15℃~30℃恒温搅拌反应0h~24h,过滤得到澄清的溶液,然后利用紫外可见分光光度计检测澄清溶液的吸光度,最后计算出L-精氨酸/氧化石墨烯复合材料对Cr(VI)离子的除去率。
过滤过程具体为:利用220nm微孔滤膜滤出吸附剂得到澄清的溶液,然后利用紫外可见分光光度计检测澄清溶液的吸光度。
以下将以实施例1获得的L-精氨酸/氧化石墨烯复合材料的应用实施例,说明本发明的L-精氨酸/氧化石墨烯复合材料吸附铬的用途。
准确称取3mg的L-精氨酸/氧化石墨烯复合材料加入到pH=3.00的10mL,1mmol/L的Cr(VI)离子的溶液中,25℃恒温搅拌反应12h,利用220nm微孔滤膜滤出吸附剂得到澄清的溶液,然后利用紫外可见分光光度计检测澄清溶液的吸光度并计算Cr(VI)含量在处理前后的含量变化,从而计算出L-精氨酸/氧化石墨烯复合材料对Cr(VI)的吸附量及溶液中Cr(VI)的除去率。同时,采用没有修饰的氧化石墨烯作为对比例,采用同样的方法对同一份工业废水进行处理。结果如下表所示:
样品名称 | Cr(VI)吸附量(mg/g) | Cr(VI)除去率 |
氧化石墨烯 | 19.8 | 11.42% |
L-精氨酸/氧化石墨烯复合材料 | 158.5 | 91.46% |
由上述表格可知,L-精氨酸/氧化石墨烯复合材料对Cr(VI)离子的吸附效果良好;含Cr(VI)离子废水在采用本发明的L-精氨酸/氧化石墨烯复合材料处理后,溶液中Cr(VI)离子的除去率为90%以上。
经过大量实验证明,L-精氨酸/氧化石墨烯复合材料相对铬含量比越高,吸附去除铬的效率越高。
综上所述:本发明的L-精氨酸/氧化石墨烯复合材料的制备方法,通过反应在氧化石墨烯表面接枝L-精氨酸,制备条件温和,步骤简单,且制备的L-精氨酸/氧化石墨烯复合材料展示出来良好的Cr(VI)吸附性能,对溶液中Cr(VI)离子的除去率为90%以上。
以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (6)
1.氧化石墨烯复合材料的制备方法,其特征是,包括如下步骤:
S1:将氧化石墨烯加入到四氢呋喃中,分散得到氧化石墨烯的四氢呋喃分散液;
S2:向氧化石墨烯的四氢呋喃分散液中加入L-精氨酸、碳酸钾粉末和去离子水,常温下搅拌24h;
S3:用水洗涤若干次,干燥后得到氧化石墨烯复合材料;
所述氧化石墨烯与L-精氨酸的用量比例是0.25:3g、2.5g:3g或1g:3g,所述氧化石墨烯与碳酸钾的用量比例是1g:0.5g。
2.如权利要求1所述的制备方法,其特征是,所述碳酸钾与反应体系中水的用量比例是1g:10mL,所述氧化石墨烯与L-精氨酸的用量比例是0.25:3g或2.5g:3g。
3.如任一在先权利要求所述的制备方法,其特征是,所述氧化石墨烯的四氢呋喃分散液中,氧化石墨烯的浓度为0.5mg/mL-5mg/mL。
4.如权利要求3所述的制备方法,其特征是,所述氧化石墨烯的浓度为2mg/mL。
5.一种由任意一项在先权利要求所述的制备方法制备得到的氧化石墨烯复合材料。
6.一种前一权利要求所述的氧化石墨烯复合材料对溶液中六价Cr离子进行吸附的应用。
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