CN112452310B - 一种氮掺杂碳吸附剂及其制备方法和对有机染料的吸附应用 - Google Patents
一种氮掺杂碳吸附剂及其制备方法和对有机染料的吸附应用 Download PDFInfo
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Abstract
本发明涉及有机染料污水处理技术领域,公开了一种氮掺杂碳吸附剂及其制备方法和对有机染料的吸附应用。所述的氮掺杂碳吸附剂的制备包括以下步骤:以柠檬酸铵和葡萄糖酸锌小分子为单体,通过自下而上方法在100~250℃的高压反应釜中进行水热碳化反应0.5~24h,待反应结束后,自然降至室温,将反应液离心处理,将所得沉淀进行洗涤,最后对沉淀进行干燥处理,得到氮掺杂碳吸附剂。本发明制备工艺简单易行、经济、绿色环保、重复性好,所制备的氮掺杂碳吸附剂,具有良好的水分散性,可用于有机染料亚甲基蓝和活性蓝19的吸附应用,具有较高的吸附性能。
Description
技术领域
本发明涉及有机染料污水处理技术领域,涉及一种氮掺杂碳吸附剂及其制备方法和对有机染料的吸附应用。
背景技术
随着城市化和工业化的快速发展,水资源污染和洁净水短缺的问题日益突出。其中人工染料污染是导致洁净水短缺的重要原因之一。我们日常生活中很多与染料息息相关,它无处不在,其中包括衣服、车子、和房子等等。在我国,每年的污水排放量逐年增加,已经接近4.0×1010t,其中有一半来自工业废水,而且工业废水有接近30%来自纺织和印染行业。而这些废水中含有大量的毒性大且不易降解的有机染料污染物。有机染料的污染源主要来自纺织、纤维、塑料、皮革、油漆、造纸、印染、和涂层等工业废水,这些行业在生产过程中都需要大量排放工业废水,正常情况下1吨工业废水可能会污染20吨左右的水体环境。当前,染料废水的排放量越来越大,由于受到资金和技术条件的制约,治理率和治理合格率却越来越低。有机染料废水得不到应有的治理或治理排放不达标直接排放到大自然中,会严重损害水资源、土壤以及相关的生物,从而危害人类健康。因此,对有机染料废水进行有效处理对生态平衡至关重要。
有机染料污染物种类繁多,具有结构复杂、色度大、毒性强、且难以降解等特点,导致有机染料废水处理的难度的难度大大增加,另一方面也引起了广大科研工作者的高度重视。当前,用于有机染料的废水处理技术和相关报道主要包括吸附、膜过滤、电凝、离子交换云点萃取、化学氧化、光解等多种工艺技术。其中,吸附由于其广泛的适用性、设计的简单性、方便性、成本效益和废旧材料的再生而成为去除有机染料的最适用的技术之一。然而,作为广泛应用于水处理的常用吸附剂、活性炭和碳纳米管在实践中相对昂贵,并且难以分离回收。另一方面,大部分合成的用于有机染料吸附的碳材料通常需要高温煅烧,对于环境具有一定的危害性。因此,对于吸附应用而言,仍然需要寻求经济,高效,可持续,绿色的吸附剂。
发明内容
本发明针对当前吸附剂价格昂贵,合成成本高,制备工艺不环保等不利于有机染料污水吸附处理工艺的发展,通过一种简单、有效、环保的方法合成氮掺杂碳吸附剂的,并应用于有机染料的吸附应用。
本发明的第一个目的是提供一种氮掺杂碳吸附剂的制备方法,该氮掺杂碳吸附剂是由葡萄糖酸锌和柠檬酸铵通过水热碳化制备而成,包括以下步骤:
将柠檬酸铵和葡萄糖酸锌加入到反应罐中,加入水性溶剂使其完全溶解,将所得反应体系放置于烘箱中,加热至反应温度进行反应,然后自然降至室温,将反应生成的产物进行纯化,即得到所述的氮掺杂碳吸附剂。
优选的,所述的柠檬酸铵和葡萄糖酸锌的质量比为1:20~20:1;
所述的柠檬酸铵与水性溶剂的质量体积比为1g柠檬酸铵:10~200mL水性溶剂。
优选的,所述的水性溶剂为去离子水或氨水溶液。
优选的,所述的氨水溶液中氨的质量分数为5%~25%。
优选的,所述的反应温度为100~250℃,所述的反应时间为0.5~24h。
优选的,所述的纯化步骤为:将所得反应产物进行离心,除去上清液,并用去离子水洗涤,直至离心上清液为澄清无色,将离心后固体进行干燥。
本发明的氮掺杂碳吸附剂是通过将葡萄糖酸锌和柠檬酸铵经水热碳化而得,无需高温煅烧即可得到多孔结构的氮掺杂碳材料,其具有类似活性碳的较高的表面积,从而具有良好的染料吸附性能,同时碳掺杂碳吸附剂表面含有较多羧基、氨基、正负电中心等,对于含有正电或负电分子的有机染料具有良好的静电吸附、氢键作用,从而有效提高对有机染料的吸附作用。此外,本发明具有原料来源丰富、价廉、制备工艺简单易行,不产生有毒气体等优势,具有绿色环保、经济易行等特点,是在吸附应用领域具有更好的应用。
本发明的第二个目的是提供一种由上述的制备方法制备得到的氮掺杂碳吸附剂。
本发明的第三个目的是提供上述的氮掺杂碳吸附剂在吸附有机染料中的应用。
优选的,所述的有机染料为亚甲基蓝和/或活性蓝19。
优选的,将本发明制得的氮掺杂碳吸附剂应用于吸附有机染料亚甲基蓝和活性蓝19的步骤为:
将一定量氮掺杂碳吸附剂加入到一定浓度的亚甲基蓝或活性蓝19的水溶液中,超声分散,然后置于一定温度和震荡速度下进行吸附反应,于不同时间点取样离心,取上清液分别采用紫外可见分光光度计测定664nm和626nm的吸收值,并计算氮掺杂碳吸附剂分别对亚甲基蓝和活性蓝19的吸附量。
作为本发明的进一步改进,所述的有机染料(亚甲基蓝或活性蓝19)水溶液的浓度为10~100μg/mL,氮掺杂碳吸附剂的用量为0.1~2mg/mL,吸附温度为15~65℃,吸附时间为5~4320min,震荡速度100~300r/min。
与现有技术相比,本发明具有如下有益效果:
(1)本发明的氮掺杂碳吸附剂是采用柠檬酸铵和葡萄糖酸锌小分子单体作为原料通过水热碳化一步制备而得,原料来源丰富、价廉,反应条件温和,制备工艺具有简单易行、绿色环保、经济的特点。
(2)本发明的氮掺杂碳吸附剂无需高温煅烧即可得到类似活性炭的多孔结构材料,对亚甲基蓝和活性蓝19的有机染料具有良好的吸附活性。
(3)本发明提供的氮掺杂碳吸附剂表面具有大量的氨基、羧基官能团,大大增加了其亲水性,并提高了正负电荷中心,从而使其对具有相反电荷的亚甲基蓝或活性蓝19具有良好的吸附能力。
附图说明
图1为实施例1中制得的氮掺杂碳吸附剂的透射电子显微镜(TEM)图。
图2为实施例1中制得的氮掺杂碳吸附剂的红外光谱(FT-IR)图。
图3为实施例1中制得的氮掺杂碳吸附剂的X射线衍射(XRD)谱图。
图4为氮掺杂碳吸附剂对亚甲基蓝(MB)的吸附应用。
图5为氮掺杂碳吸附剂对活性蓝19(RB19)的吸附应用。
具体实施方式
以下实施例是对本发明的进一步说明,而不是对本发明的限制。
实施例1
一种氮掺杂碳吸附剂的制备方法,包括以下步骤:分别称取2.3g柠檬酸铵、1.2g葡萄糖酸锌加入到100mL聚四氟乙烯反应罐中,并向其中加入50mL去离子水使固体完全溶解,然后进于高压釜中并置于烘箱中,将反应温度升至180℃反应3h,然后自然降至室温,将所得反应产物于10000rpm下离心10min,除去上清液,并用去离子水洗至上清液无色,并将所得固体干燥,即得氮掺杂碳吸附剂。
对本实施例1得到的氮掺杂碳吸附剂进行透射电子显微镜(TEM)测试,所得到的TEM图如图1所示。由图1可知,所制备的氮掺杂碳吸附剂具有圆形的片状结构。此外,圆形的氮掺杂碳吸附剂粒径在4.5~4.8μm范围内,同样具有类二维结构。TEM结果说明了本实施例得到的氮掺杂碳吸附剂具有不同于已报道的用于有机染料吸附的碳吸附剂的结构,属于新型氮掺杂碳吸附剂。
对本实施例1得到的氮掺杂碳吸附剂进行红外光谱(FT-IR)测试,所得FT-IR如图2所示。由图2可知,谱图在3411和3217cm-1有吸收峰,分别为-OH和N-H的伸缩振动峰,2356、1635和1382cm-1处的特征峰分别为C≡N、C=O和C=N的伸缩振动吸收峰。这些官能团表明氮掺杂碳吸附剂表面具有丰富的羧基、氨基等亲水性基团,同时亦证明氮元素成功掺杂到吸附剂结构中。
对本实施例1得到的氮掺杂碳吸附剂进行X射线衍射光谱(XRD)测试,所得XRD谱图如图3所示。由图3可知,在2θ=~26.76°处有一尖衍射峰,对应(002)位面,表明其具有石墨结构。
实施例2
一种氮掺杂碳吸附剂的制备方法,包括以下步骤:分别称取0.1g柠檬酸铵、2g葡萄糖酸锌加入到50mL聚四氟乙烯反应罐中,并向其中加入20mL质量分数为25%氨水溶液使固体完全溶解,然后进于高压釜中并置于烘箱中,将反应温度升至150℃反应5h,然后自然降至室温,将所得反应产物于10000rpm下离心10min,除去上清液,并用去离子水洗至上清液无色,并将所得固体干燥,即得氮掺杂碳吸附剂。
实施例3
一种氮掺杂碳吸附剂的制备方法,包括以下步骤:分别称取2g柠檬酸铵、0.1g葡萄糖酸锌加入到50mL聚四氟乙烯反应罐中,并向其中加入20mL去离子水使固体完全溶解,然后进于高压釜中并置于烘箱中,将反应温度升至100℃反应24h,然后自然降至室温,将所得反应产物于10000rpm下离心10min,除去上清液,并用去离子水洗至上清液无色,并将所得固体干燥,即得氮掺杂碳吸附剂。
实施例4
一种氮掺杂碳吸附剂的制备方法,包括以下步骤:分别称取3g柠檬酸铵、1.5g葡萄糖酸锌加入到100mL聚四氟乙烯反应罐中,并向其中加入60mL质量分数为5%的氨水溶液使固体完全溶解,然后进于高压釜中并置于烘箱中,将反应温度升至100℃反应24h,然后自然降至室温,将所得反应产物于10000rpm下离心10min,除去上清液,并用去离子水洗至上清液无色,并将所得固体干燥,即得氮掺杂碳吸附剂。
应用实例1
(1)将50mg实施例1制备的氮掺杂碳吸附剂加入到100mL浓度为50μg/mL的亚甲基蓝水溶液中,超声分散2min,然后于25℃、200r/min条件下振荡,并于不同时间点取样,离心,取上清液,采用紫外分光光度计进行测定不同处理时间点的亚甲基蓝的吸收光谱变化情况,在664nm波长处测定吸光度,并计算氮掺杂碳吸附剂对亚甲基蓝的吸附量(Qe),结果见图4。
(2)将50mg实施例2制备的氮掺杂碳吸附剂加入到100mL浓度为50μg/mL的亚甲基蓝水溶液中,超声分散2min,然后于25℃、200r/min条件下振荡,并于不同时间点取样,离心,取上清液,采用紫外分光光度计进行测定处理不同时间点的亚甲基蓝的吸收光谱变化情况,在664nm波长处测定吸光度,并计算氮掺杂碳吸附剂对亚甲基蓝的吸附量(Qe),结果见图4。
(3)将50mg实施例3制备的氮掺杂碳吸附剂加入到100mL浓度为50μg/mL的亚甲基蓝水溶液中,超声分散2min,然后于25℃、200r/min条件下振荡,并于不同时间点取样,离心,取上清液,采用紫外分光光度计进行测定处理不同时间点的亚甲基蓝的吸收光谱变化情况,在664nm波长处测定吸光度,并计算氮掺杂碳吸附剂对亚甲基蓝的吸附量(Qe),结果见图4。
吸附量(Qe)的计算公式为:
a.A0/At=C0/Ct(A为吸光度,C为吸附质溶液浓度;A0和At分别表示在初始时间和t时间时吸附质溶液的吸光度,C0和Ct分别表示在初始时间和t时间时吸附质溶液的浓度)
b.Qe=(C0-Ct)×V/W(V表示吸附质溶液的体积,W表示吸附剂的质量)。
应用实例2
(1)将40mg实施例1制备的氮掺杂碳吸附剂加入到100mL含有50μg/mL的活性蓝19水溶液中,超声分散2min,然后于25℃、180r/min条件下振荡,并于不同时间点取样,离心,取上清液,采用紫外分光光度计进行测定处理不同时间点的活性蓝19的吸收光谱变化情况,在626nm波长处测定吸光度,并计算氮掺杂碳吸附剂对活性蓝19的吸附量(Qe),结果见图5。
(2)将40mg实施例2制备的氮掺杂碳吸附剂加入到100mL含有50μg/mL的活性蓝19水溶液中,超声分散2min,然后于25℃、180r/min条件下振荡,并于不同时间点取样,离心,取上清液,采用紫外分光光度计进行测定处理不同时间点的活性蓝19的吸收光谱变化情况,在626nm波长处测定吸光度,并计算氮掺杂碳吸附剂对活性蓝19的吸附量(Qe),结果见图5。
(3)将40mg实施例3制备的氮掺杂碳吸附剂加入到100mL含有50μg/mL的活性蓝19水溶液中,超声分散2min,然后于25℃、180r/min条件下振荡,并于不同时间点取样,离心,取上清液,采用紫外分光光度计进行测定处理不同时间点的活性蓝19的吸收光谱变化情况,在626nm波长处测定吸光度,并计算氮掺杂碳吸附剂对活性蓝19的吸附量(Qe),结果见图5。
以上仅是本发明的优选实施方式,应当指出的是,上述优选实施方式不应视为对本发明的限制,本发明的保护范围应当以权利要求所限定的范围为准。对于本技术领域的普通技术人员来说,在不脱离本发明的精神和范围内,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (3)
1.一种氮掺杂碳吸附剂在吸附有机染料中的应用,其特征在于,包括以下步骤:将柠檬酸铵和葡萄糖酸锌加入到反应罐中,加入水性溶剂使其完全溶解,将所得反应体系放置于烘箱中,加热至反应温度进行反应,然后自然降至室温,将反应生成的产物进行纯化,即得到所述的氮掺杂碳吸附剂;
所述的柠檬酸铵和葡萄糖酸锌的质量比为1:20~20:1;所述的柠檬酸铵与水性溶剂的质量体积比为1g柠檬酸铵:10~200mL水性溶剂;
所述的水性溶剂为去离子水或氨水溶液;所述的氨水溶液中氨的质量分数为5%~25%;
所述的反应温度为100~250℃,所述的反应时间为0.5~24 h;
所述的有机染料为亚甲基蓝和/或活性蓝19。
2.根据权利要求1所述的氮掺杂碳吸附剂在吸附有机染料中的应用,其特征在于,所述的纯化步骤为:将所得反应产物进行离心,除去上清液,并用去离子水洗涤,直至离心上清液为澄清无色,将离心后固体进行干燥。
3.一种如权利要求1所述应用中的氮掺杂碳吸附剂。
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