CN111254707A - 一种负载Fe-MOF的活性炭纤维材料的制备方法 - Google Patents
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Abstract
本发明公开了一种负载Fe‑MOF的活性炭纤维材料的制备方法,本发明将高比表面积、高孔隙率且孔体积和孔径可调的Fe‑MOF负载在活性碳纤维上制成功能纤维材料,该方法工艺简单,操作方便,原料成本低,综合利用活性炭纤维及Fe‑MOF的优良性能,对印染废水中高浓度有机染料具有优异的脱色效果;将Fe‑MOF负载到活性炭纤维上,可以解决粉末状Fe‑MOF在废水处理中难回收再利用的困难,具有广阔的应用前景。
Description
技术领域
本发明涉及污水处理技术领域,具体为一种负载Fe-MOF的活性炭纤维材料的制备方法。
背景技术
随着现代工业的迅速发展,产生了大量有毒有害的污染物,严重威胁着人类赖以生存的生态系统和人类的生存发展空间。目前人们在去除环境污染物方面已经做了很多努力,并发展了多种环境污染治理技术。印染行业作为纺织工业重要的组成部分,是纺织品生产链中产品深加工、提升品质、功能和价值的重要环节,是高附加值服装面料、家用纺织品和产业用纺织品等产业的重要技术支撑。但印染废水量大,污染重,是典型的难处理的有机废水,尤其是色度高。
活性炭纤维是一种高效的吸附材料,其比表面积大,内部有着大量相互贯通复杂的微孔结构。活性炭纤维耐高温、耐腐蚀,化学稳定性好,适应性强,无论污染物质是微量级还是高浓度,都可采用活性炭纤维进行吸附处理,达到满意效果,在很多领域中可广泛应用。目前市售的活性炭纤维以微孔为主,这就限制了其在大分子吸附领域的应用,特别是在液相吸附领域的应用。
金属有机框架材料(MOFs)是一类由有机配体和金属离子通过自组装形成具有周期性网络结构的材料。与传统的无机材料相比,MOFs具有比表面积高、孔形状规则、稳定性良好、孔道尺寸可调节等优点,利用MOFs吸附去除环境污染物的研究受到人们的广泛关注,其中Fe-MOFs用于环境治理中去除水中有机污染物的研究有很多,Fe-MOF大多以吸附剂、催化剂的方式应用于有机污染物的去除。虽然其性能优异,但存在着易团聚,不易回收等缺点。CN108607610A一种可磁回收的Fe-MOF光催化剂的制备方法及其应用,利用材料具有一定的磁性,使材料可以回收重复利用,但必须通过外加磁场来实现分离回收。
为解决上述问题,本发明将Fe-MOF负载到活性炭纤维上,制得的功能材料既具有Fe-MOF和活性炭纤维的优良性能,又可解决Fe-MOF粉体材料负载困难和回收利用不易等问题,而且该方法简单便捷,可大范围批量生产,在污水处理方面具有广阔的应用前景。
发明内容
本发明的目的在于提供一种负载Fe-MOF的活性炭纤维材料的制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:一种负载Fe-MOF的活性炭纤维材料的制备方法,包括以下步骤:
A、活性碳纤维预处理;
B、活性碳纤维上原位生长Fe-MOF。
优选的,所述步骤A具体方法为:活性碳纤维先用95-100℃热水煮10-15min,除去纤维上残留的水溶性杂质,然后将活性碳纤维浸入丙酮中超声10-15min,进一步除去纤维上残留的油性杂质,再用蒸馏水清洗3次,烘干后备用。
优选的,所述步骤B具体方法为:
a.将4-6mmol均苯三甲酸加入到15-20mL 1M NaOH溶液中,超声5-10min,得到溶液A;
b.将0.3-0.5g经过预处理的活性炭纤维加入到溶液A中,超声5-10min;
c.将6-8mmol七水合硫酸亚铁加入到50-60mL蒸馏水中,超声5-10min,得到B溶液;
d.将B溶液缓慢滴加至浸有活性碳纤维的A溶液中,室温搅拌,反应20-24h,反应结束后将活性炭纤维取出,用水清洗,烘干。
优选的,所述的活性炭纤维为活性炭纤维布或粘。
优选的,烘干温度为70-80℃,时间为15-25min。
优选的,水洗后烘干温度为80-90℃,时间为18-28min。
优选的,所述步骤d中搅拌速率为250-350rpm。
与现有技术相比,本发明的有益效果是:本发明将高比表面积、高孔隙率且孔体积和孔径可调的Fe-MOF负载在活性碳纤维上制成功能纤维材料,该方法工艺简单,操作方便,原料成本低,综合利用活性炭纤维及Fe-MOF的优良性能,对印染废水中高浓度有机染料具有优异的脱色效果;将Fe-MOF负载到活性炭纤维上,可以解决粉末状Fe-MOF在废水处理中难回收再利用的困难,具有广阔的应用前景。
附图说明
图1为本发明负载Fe-MOF的活性碳纤维在黑暗条件下对活性黑KN-B染料溶液的脱色效果图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
请参阅图1,本发明提供一种技术方案:一种负载Fe-MOF的活性炭纤维材料的制备方法,包括以下步骤:
A、活性碳纤维预处理;
B、活性碳纤维上原位生长Fe-MOF。
本发明中,步骤A具体方法为:活性碳纤维先用95-100℃热水煮10-15min,除去纤维上残留的水溶性杂质,然后将活性碳纤维浸入丙酮中超声10-15min,进一步除去纤维上残留的油性杂质,再用蒸馏水清洗3次,烘干后备用,烘干温度为70-80℃,时间为15-25min。
本发明中,步骤B具体方法为:
a.将4-6mmol均苯三甲酸加入到15-20mL 1M NaOH溶液中,超声5-10min,得到溶液A;
b.将0.3-0.5g经过预处理的活性炭纤维加入到溶液A中,超声5-10min;
c.将6-8mmol七水合硫酸亚铁加入到50-60mL蒸馏水中,超声5-10min,得到B溶液;
d.将B溶液缓慢滴加至浸有活性碳纤维的A溶液中,室温搅拌,搅拌速率为250-350rpm,反应20-24h,反应结束后将活性炭纤维取出,用水清洗,烘干;水洗后烘干温度为80-90℃,时间为18min-28min。
本发明中,活性炭纤维为活性炭纤维布或粘。
实施例1:
一种负载Fe-MOF的活性碳纤维布的制备方法,具体步骤如下:
(1)活性碳纤维布的预处理:活性碳纤维布先用95℃热水煮10min,除去纤维上残留的水溶性杂质,然后将活性碳纤维浸入丙酮中超声10min,进一步除去纤维上残留的油性杂质,再用蒸馏水清洗3次,烘干后备用。
(2)活性碳纤维上原位生长Fe-MOF:将4mmol均苯三甲酸加入到15mL 1M NaOH溶液中,超声5min,得到溶液A;将0.3g经过预处理的活性炭纤维布加入到溶液A中,超声5min;将6mmol七水合硫酸亚铁加入到50mL蒸馏水中,超声5min,得到B溶液;将B溶液缓慢滴加至浸有活性碳纤维布的A溶液中,室温搅拌,反应20h,反应结束后将活性炭纤维布取出,用水清洗,烘干。
为了考察所制备的活性炭纤维材料的吸附性能,选择活性黑KN-B染料为研究对象,测定其在黑暗条件下对染料的吸附性能,测试条件为0.25g活性炭纤维材料,对50mL质量浓度为50mg/L的活性黑KN-B染料溶液在室温下吸附2h,每隔0.5h,测定溶液的吸光度。根据下列公式计算染料的降解率:
式中,A0为脱色前染液的吸光度;A1为脱色后染液的吸光度。
所制得的活性炭纤维布对活性黑KN-B染料溶液的脱色率测试结果如图1所示。从图1中可以看出,在黑暗下吸附2h后,负载Fe-MOF的活性碳纤维布比未负载Fe-MOF的活性碳纤维对活性黑KN-B溶液的脱色率提高了48%,负载Fe-MOF的活性碳纤维脱色率达到84%,说明负载Fe-MOF的活性碳纤维具有更好的脱色效果。
为了考察所制备的活性炭纤维材料的光催化性能,测试0.25g活性炭纤维材料,在1000W氙灯照射下,对50mL添加了15uL H2O2的浓度为50mg/L的活性黑KN-B染料溶液在室温下处理15min,测试结果脱色率大于99%。
实施例2:
一种负载Fe-MOF的活性碳纤维布的制备方法,具体步骤如下:
(1)活性碳纤维布的预处理:活性碳纤维布先用95℃热水煮10min,除去纤维上残留的水溶性杂质,然后将活性碳纤维浸入丙酮中超声10min,进一步除去纤维上残留的油性杂质,再用蒸馏水清洗3次,烘干后备用。
(2)活性碳纤维上原位生长Fe-MOF:将5mmol均苯三甲酸加入到15mL 1M NaOH溶液中,超声5min,得到溶液A;将0.3g经过预处理的活性炭纤维布加入到溶液A中,超声5min;将7mmol七水合硫酸亚铁加入到50mL蒸馏水中,超声10min,得到B溶液;将B溶液缓慢滴加至浸有活性碳纤维布的A溶液中,室温搅拌,反应24h,反应结束后将活性炭纤维布取出,用水清洗,烘干。
为了考察所制备的活性炭纤维材料的吸附性能,选择活性黑KN-B染料为研究对象,测定其在黑暗条件下对染料的吸附性能,测试条件为0.25g活性炭纤维材料,对50mL质量浓度为50mg/L的活性黑KN-B染料溶液在室温下吸附2h,每隔0.5h,测定溶液的吸光度。根据下列公式计算染料的降解率:
式中,A0为脱色前染液的吸光度;A1为脱色后染液的吸光度。
所制得的活性炭纤维布对活性黑KN-B染料溶液的脱色率测试结果如图1所示。从图1中可以看出,在黑暗下吸附2h后,负载Fe-MOF的活性碳纤维布比未负载Fe-MOF的活性碳纤维对活性黑KN-B溶液的脱色率提高了54%,负载Fe-MOF的活性碳纤维脱色率达到90%,说明负载Fe-MOF的活性碳纤维具有更好的脱色效果。
为了考察所制备的活性炭纤维材料的光催化性能,测试0.25g活性炭纤维材料,在1000W氙灯照射下,对50mL添加了15uL H2O2的浓度为50mg/L的活性黑KN-B染料溶液在室温下处理15min,测试结果脱色率大于99%。
实施例3:
一种负载Fe-MOF的活性碳纤维粘的制备方法,具体步骤如下:
(1)活性碳纤维粘的预处理:活性碳纤维粘先用100℃热水煮15min,除去纤维上残留的水溶性杂质,然后将活性碳纤维浸入丙酮中超声15min,进一步除去纤维上残留的油性杂质,再用蒸馏水清洗3次,烘干后备用。
(2)活性碳纤维上原位生长Fe-MOF:将6mmol均苯三甲酸加入到20mL 1M NaOH溶液中,超声10min,得到溶液A;将0.5g经过预处理的活性炭纤维粘加入到溶液A中,超声10min;将8mmol七水合硫酸亚铁加入到60mL蒸馏水中,超声10min,得到B溶液;将B溶液缓慢滴加至浸有活性碳纤维布的A溶液中,室温搅拌,反应24h,反应结束后将活性炭纤维粘取出,用水清洗,烘干。
为了考察所制备的活性炭纤维材料的吸附性能,选择活性黑KN-B染料为研究对象,测定其在黑暗条件下对染料的吸附性能,测试条件为0.25g活性炭纤维材料,对50mL质量浓度为50mg/L的活性黑KN-B染料溶液在室温下吸附2h,每隔0.5h,测定溶液的吸光度。根据下列公式计算染料的降解率:
式中,A0为脱色前染液的吸光度;A1为脱色后染液的吸光度。
所制得的活性炭纤维布对活性黑KN-B染料溶液的脱色率测试结果如图1所示。从图1中可以看出,在黑暗下吸附2h后,负载Fe-MOF的活性碳纤维布比未负载Fe-MOF的活性碳纤维对活性黑KN-B溶液的脱色率提高了51%,负载Fe-MOF的活性碳纤维脱色率达到87%,说明负载Fe-MOF的活性碳纤维具有更好的脱色效果。
为了考察所制备的活性炭纤维材料的光催化性能,测试0.25g活性炭纤维材料,在1000W氙灯照射下,对50mL添加了15uL H2O2的浓度为50mg/L的活性黑KN-B染料溶液在室温下处理15min,测试结果脱色率大于99%。
综上所述,本发明将高比表面积、高孔隙率且孔体积和孔径可调的Fe-MOF负载在活性碳纤维上制成功能纤维材料,该方法工艺简单,操作方便,原料成本低,综合利用活性炭纤维及Fe-MOF的优良性能,对印染废水中高浓度有机染料具有优异的脱色效果;将Fe-MOF负载到活性炭纤维上,可以解决粉末状Fe-MOF在废水处理中难回收再利用的困难,具有广阔的应用前景。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (7)
1.一种负载Fe-MOF的活性炭纤维材料的制备方法,其特征在于:包括以下步骤:
A、活性碳纤维预处理;
B、活性碳纤维上原位生长Fe-MOF。
2.根据权利要求1所述的一种负载Fe-MOF的活性炭纤维材料的制备方法,其特征在于:所述步骤A具体方法为:活性碳纤维先用95-100℃热水煮10-15min,除去纤维上残留的水溶性杂质,然后将活性碳纤维浸入丙酮中超声10-15min,进一步除去纤维上残留的油性杂质,再用蒸馏水清洗3次,烘干后备用。
3.根据权利要求1所述的一种负载Fe-MOF的活性炭纤维材料的制备方法,其特征在于:所述步骤B具体方法为:
a.将4-6mmol均苯三甲酸加入到15-20mL 1M NaOH溶液中,超声5-10min,得到溶液A;
b.将0.3-0.5g经过预处理的活性炭纤维加入到溶液A中,超声5-10min;
c.将6-8mmol七水合硫酸亚铁加入到50-60mL蒸馏水中,超声5-10min,得到B溶液;
d.将B溶液缓慢滴加至浸有活性碳纤维的A溶液中,室温搅拌,反应20-24h,反应结束后将活性炭纤维取出,用水清洗,烘干。
4.根据权利要求1所述的一种负载Fe-MOF的活性炭纤维材料的制备方法,其特征在于:所述的活性炭纤维为活性炭纤维布或粘。
5.根据权利要求2所述的一种负载Fe-MOF的活性炭纤维材料的制备方法,其特征在于:烘干温度为70-80℃,时间为15-25min。
6.根据权利要求3所述的一种负载Fe-MOF的活性炭纤维材料的制备方法,其特征在于:水洗后烘干温度为80-90℃,时间为18-28min。
7.根据权利要求3所述的一种负载Fe-MOF的活性炭纤维材料的制备方法,其特征在于:所述步骤d中搅拌速率为250-350rpm。
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