CN106582535A - 一种改性二氧化硅纳米颗粒吸附剂、制备方法及其应用 - Google Patents
一种改性二氧化硅纳米颗粒吸附剂、制备方法及其应用 Download PDFInfo
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Abstract
本发明涉及一种改性二氧化硅纳米颗粒吸附剂、制备方法及其应用,属于纳米材料制备技术领域。首先将纳米二氧化硅颗粒和3‑缩水甘油基氧基丙基三甲氧基硅烷混合均匀,然后加入到无水乙醇溶液中,回流反应后离心分离,取出固体物质,产物标记为GPTMS‑SNPs;将GPTMS‑SNPs加入到无水乙醇溶液中,加入聚乙烯亚胺,回流反应后离心分离得到的产物标记为PEI‑SNPs;将PEI‑SNPs加入到二甲基甲酰胺中,加入氯乙酰氯,回流反应后离心分离取出固体物质,记为CAC‑SNPs;将乙醇和水混合均匀得到混合溶液,将CAC‑SNPs加入到混合溶液中,然后加入3‑氨基‑5‑巯基‑1,2,4‑三氮唑,回流反应离心分离,得到最终改性二氧化硅纳米颗粒吸附剂。本方法原材料廉价,制备工艺简单,易与水溶液分离,具有高吸附性且可循环使用。
Description
技术领域
本发明涉及一种改性二氧化硅纳米颗粒吸附剂、制备方法及其应用,属于纳米材料制备技术领域。
背景技术
随着重金属有毒重金属工业废水污染已成为一个严重的世界性问题。重金属是不能进行生物降解的,因此它们能稳定循环存在于生态系统和食物链中,重金属的富集使得食物链顶端生物所受到的污染程度急剧增加。在众多重金属中,银是一种贵金属和非常有用的原料。由于其良好的可塑性、延展性、导热性、光敏性和抗菌性能,银被广泛应用于各种工业领域中,包括电镀、催化剂、摄影、医疗、铸币、电子电器和金属合金产业,进而导致银资源的相对短缺。与此同时,银在人体内的浓度达到一定程度,会引发各种疾病和突发病,如高血压、肝肾病、行为变化、学习障碍等。因此,从工业废水中有效的去除和回收银离子已成为一个亟待解决的问题。而今,人们已陆续开发出各种将银离子从工业废水中去除回收的方法,包括吸附法、离子交换、浊点萃取、液液萃取和膜技术等,由于高吸附量、低成本、操作简单和节约时间等特点,吸附法被认为是最有效的方法。许多材料已经被研究用于吸附剂,如纳米二氧化硅、活性炭、沸石、树脂、工农业废弃物等。其中,二氧化硅纳米材料由于具有高比表面积、成本廉价、易于合成改性、绿色环保等优点,是吸附剂材料的理想之选。
发明内容
针对上述现有技术存在的问题及不足,本发明提供一种改性二氧化硅纳米颗粒吸附剂、制备方法及其应用。该改性二氧化硅纳米颗粒吸附剂可以吸附水溶液中的银离子;本方法原材料廉价,制备工艺简单,易与水溶液分离,具有高吸附性且可循环使用。本发明通过以下技术方案实现。
一种改性二氧化硅纳米颗粒吸附剂,结构式为:
,式中为二氧化硅纳米颗粒。
一种改性二氧化硅纳米颗粒吸附剂的制备方法,其具体步骤如下:
(1)首先按照液固比为3:1~5:1ml/g将纳米二氧化硅颗粒和3-缩水甘油基氧基丙基三甲氧基硅烷混合均匀,然后按照纳米二氧化硅颗粒与无水乙醇溶液液固比为15:1~17:1ml/g加入到无水乙醇溶液中,在60~70℃条件下回流反应20~30h后离心分离,取出固体物质用无水乙醇洗涤,真空干燥后得到的产物标记为GPTMS-SNPs;
(2)按照液固比为12:1~14:1ml/g将步骤(1)得到的GPTMS-SNPs加入到无水乙醇溶液中,然后按照聚乙烯亚胺与GPTMS-SNPs的质量比为1:10~1:20加入聚乙烯亚胺,在65~75℃回流反应25~35h后离心分离,取出固体物质用无水乙醇洗涤后真空干燥,得到的产物标记为PEI-SNPs;
(3)按照液固比为12:1~14:1ml/g将步骤(2)得到的PEI-SNPs加入到二甲基甲酰胺中,再按照氯乙酰氯与PEI-SNPs的液固比为6:1~8:1ml/g加入氯乙酰氯,在75~85℃回流反应后离心分离25~35h,取出固体物质用二甲基甲酰胺洗涤后真空干燥,得到的产物标记为CAC-SNPs;
(4)将乙醇和水按照体积比为1:1混合均匀得到混合溶液,按照液固比为30:1~40:1ml/g将步骤(3)得到的CAC-SNPs加入到混合溶液中,然后按照3-氨基-5-巯基-1,2,4-三氮唑与CAC-SNPs的质量比为1:1.5~1:2.5加入3-氨基-5-巯基-1,2,4-三氮唑,在75~85℃条件下回流反应30~40h后离心分离,取出固体物质用蒸馏水洗涤后真空干燥,得到最终改性二氧化硅纳米颗粒吸附剂,标记为ATT-SNPs。
一种改性二氧化硅纳米颗粒吸附剂作为银离子吸附剂的应用。
上述的有机试剂和无机试剂都为市购的分析纯。
本发明制备得到的吸附剂主要用于吸附废水中的银离子,与现有技术相比,具有如下优点:
(1)对银离子的吸附量高,可用于工业废水中银离子的去除与回收。
(2)本发明的改性方法简单、成本较低。
(3)本发明的改性二氧化硅纳米颗粒无毒无害,理化性能稳定,易于分离,可循环使用,不造成二次污染。
(4)具有广泛的应用价值和经济价值。
具体实施方式
下面结合具体实施方式,对本发明作进一步说明。
实施例1
该改性二氧化硅纳米颗粒吸附剂,结构式为:
,式中为纳米二氧化硅颗粒。
该改性二氧化硅纳米颗粒吸附剂的制备方法,其具体步骤如下:
(1)首先按照液固比为3:1ml/g将纳米二氧化硅颗粒和3-缩水甘油基氧基丙基三甲氧基硅烷混合均匀,然后按照纳米二氧化硅颗粒与无水乙醇溶液液固比为15:1ml/g加入到无水乙醇溶液中,在60℃条件下回流反应20h后离心分离,取出固体物质用无水乙醇洗涤,真空干燥后得到的产物标记为GPTMS-SNPs;
(2)按照液固比为12:1ml/g将步骤(1)得到的GPTMS-SNPs加入到无水乙醇溶液中,然后按照聚乙烯亚胺与GPTMS-SNPs的质量比为1:10加入聚乙烯亚胺,在65℃回流反应25h后离心分离,取出固体物质用无水乙醇洗涤后真空干燥,得到的产物标记为PEI-SNPs;
(3)按照液固比为12:1ml/g将步骤(2)得到的PEI-SNPs加入到二甲基甲酰胺中,再按照氯乙酰氯与PEI-SNPs的液固比为6:1ml/g加入氯乙酰氯,在75℃回流反应后离心分离25h,取出固体物质用二甲基甲酰胺洗涤后真空干燥,得到的产物标记为CAC-SNPs;
(4)将乙醇和水按照体积比为1:1混合均匀得到混合溶液,按照液固比为30:1ml/g将步骤(3)得到的CAC-SNPs加入到混合溶液中,然后按照3-氨基-5-巯基-1,2,4-三氮唑与CAC-SNPs的质量比为1:1.5加入3-氨基-5-巯基-1,2,4-三氮唑,在75℃条件下回流反应30h后离心分离,取出固体物质用蒸馏水洗涤后真空干燥,得到最终改性二氧化硅纳米颗粒吸附剂,标记为ATT-SNPs。
吸附银离子性能测定:
取20mgATT-SNPs吸附剂投入初始浓度为100mg/L的银离子溶液中震荡吸附2h后,离心分离吸附剂,用ICP-OES测定滤液中剩余银离子浓度为14.4mg/L,吸附率为85.6%。将吸附过银离子的吸附剂在硫脲溶液(10wt%)中搅拌洗涤4h,然后用蒸馏水洗涤3次,最后将吸附剂在50℃下真空干燥24h。取上述吸附剂20mg投入初始浓度为100mg/L的银离子溶液中震荡吸附2h后,离心分离吸附剂,用ICP-OES测定滤液中剩余银离子浓度为14.9mg/L,吸附率为85.1%。说明本发明的改性二氧化硅纳米颗粒ATT-SNPs是可重复使用。
实施例2
该改性二氧化硅纳米颗粒吸附剂,结构式为:
,式中为二氧化硅纳米颗粒。
该改性二氧化硅纳米颗粒吸附剂的制备方法,其具体步骤如下:
(1)首先按照液固比为4:1ml/g将纳米二氧化硅颗粒和3-缩水甘油基氧基丙基三甲氧基硅烷混合均匀,然后按照纳米二氧化硅颗粒与无水乙醇溶液液固比为16:1ml/g加入到无水乙醇溶液中,在65℃条件下回流反应25h后离心分离,取出固体物质用无水乙醇洗涤,真空干燥后得到的产物标记为GPTMS-SNPs;
(2)按照液固比为13:1ml/g将步骤(1)得到的GPTMS-SNPs加入到无水乙醇溶液中,然后按照聚乙烯亚胺与GPTMS-SNPs的质量比为1:15加入聚乙烯亚胺,在70℃回流反应30h后离心分离,取出固体物质用无水乙醇洗涤后真空干燥,得到的产物标记为PEI-SNPs;
(3)按照液固比为13:1ml/g将步骤(2)得到的PEI-SNPs加入到二甲基甲酰胺中,再按照氯乙酰氯与PEI-SNPs的液固比为7:1ml/g加入氯乙酰氯,在80℃回流反应后离心分离30h,取出固体物质用二甲基甲酰胺洗涤后真空干燥,得到的产物标记为CAC-SNPs;
(4)将乙醇和水按照体积比为1:1混合均匀得到混合溶液,按照液固比为35:1ml/g将步骤(3)得到的CAC-SNPs加入到混合溶液中,然后按照3-氨基-5-巯基-1,2,4-三氮唑与CAC-SNPs的质量比为1:2加入3-氨基-5-巯基-1,2,4-三氮唑,在80℃条件下回流反应35h后离心分离,取出固体物质用蒸馏水洗涤后真空干燥,得到最终改性二氧化硅纳米颗粒吸附剂,标记为ATT-SNPs。
吸附银离子性能测定:
取20mgATT-SNPs吸附剂投入初始浓度为100mg/L的银离子溶液中震荡吸附2h后,离心分离吸附剂,用ICP-OES测定滤液中剩余银离子浓度为10.2mg/L,吸附率为89.8%。将吸附过银离子的吸附剂在硫脲溶液(10wt%)中搅拌洗涤4h,然后用蒸馏水洗涤3次,最后将吸附剂在50℃下真空干燥24h。取上述吸附剂20mg投入初始浓度为100mg/L的银离子溶液中震荡吸附2h后,离心分离吸附剂,用ICP-OES测定滤液中剩余银离子浓度为10.7mg/L,吸附率为89.3%。说明本发明的改性二氧化硅纳米颗粒ATT-SNPs是可重复使用。
实施例3
该改性二氧化硅纳米颗粒吸附剂,结构式为:
,式中为二氧化硅纳米颗粒。
该改性二氧化硅纳米颗粒吸附剂的制备方法,其具体步骤如下:
(1)首先按照液固比为5:1ml/g将纳米二氧化硅颗粒和3-缩水甘油基氧基丙基三甲氧基硅烷混合均匀,然后按照纳米二氧化硅颗粒与无水乙醇溶液液固比为17:1ml/g加入到无水乙醇溶液中,在70℃条件下回流反应30h后离心分离,取出固体物质用无水乙醇洗涤,真空干燥后得到的产物标记为GPTMS-SNPs;
(2)按照液固比为14:1ml/g将步骤(1)得到的GPTMS-SNPs加入到无水乙醇溶液中,然后按照聚乙烯亚胺与GPTMS-SNPs的质量比为1:20加入聚乙烯亚胺,在75℃回流反应35h后离心分离,取出固体物质用无水乙醇洗涤后真空干燥,得到的产物标记为PEI-SNPs;
(3)按照液固比为14:1ml/g将步骤(2)得到的PEI-SNPs加入到二甲基甲酰胺中,再按照氯乙酰氯与PEI-SNPs的液固比为8:1ml/g加入氯乙酰氯,在85℃回流反应后离心分离35h,取出固体物质用二甲基甲酰胺洗涤后真空干燥,得到的产物标记为CAC-SNPs;
(4)将乙醇和水按照体积比为1:1混合均匀得到混合溶液,按照液固比为40:1ml/g将步骤(3)得到的CAC-SNPs加入到混合溶液中,然后按照3-氨基-5-巯基-1,2,4-三氮唑与CAC-SNPs的质量比为1:2.5加入3-氨基-5-巯基-1,2,4-三氮唑,在85℃条件下回流反应40h后离心分离,取出固体物质用蒸馏水洗涤后真空干燥,得到最终改性二氧化硅纳米颗粒吸附剂,标记为ATT-SNPs。
吸附银离子性能测定:
取20mg ATT-SNPs吸附剂投入初始浓度为100 mg/L 的银离子溶液中震荡吸附2h 后,离心分离吸附剂,用ICP-OES测定滤液中剩余银离子浓度为13.8mg/L,吸附率为86.2%。将吸附过银离子的吸附剂在硫脲溶液(10wt%)中搅拌洗涤4 h,然后用蒸馏水洗涤3次,最后将吸附剂在50℃下真空干燥24 h。取上述吸附剂20 mg 投入初始浓度为100mg/L的银离子溶液中震荡吸附2h 后,离心分离吸附剂,用ICP-OES测定滤液中剩余银离子浓度为14.1mg/L,吸附率为85.9%。说明本发明的改性二氧化硅纳米颗粒ATT-SNPs是可重复使用。
以上对本发明的具体实施方式作了详细说明,但是本发明并不限于上述实施方式,在本领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下做出各种变化。
Claims (3)
1.一种改性二氧化硅纳米颗粒吸附剂,其特征在于:结构式为:
,式中为二氧化硅纳米颗粒。
2.一种根据权利要求1所述的改性二氧化硅纳米颗粒吸附剂的制备方法,其特征在于具体步骤如下:
(1)首先按照液固比为3:1~5:1ml/g将纳米二氧化硅颗粒和3-缩水甘油基氧基丙基三甲氧基硅烷混合均匀,然后按照纳米二氧化硅颗粒与无水乙醇溶液液固比为15:1~17:1ml/g加入到无水乙醇溶液中,在60~70℃条件下回流反应20~30h后离心分离,取出固体物质用无水乙醇洗涤,真空干燥后得到的产物标记为GPTMS-SNPs;
(2)按照液固比为12:1~14:1ml/g将步骤(1)得到的GPTMS-SNPs加入到无水乙醇溶液中,然后按照聚乙烯亚胺与GPTMS-SNPs的质量比为1:10~1:20加入聚乙烯亚胺,在65~75℃回流反应25~35h后离心分离,取出固体物质用无水乙醇洗涤后真空干燥,得到的产物标记为PEI-SNPs;
(3)按照液固比为12:1~14:1ml/g将步骤(2)得到的PEI-SNPs加入到二甲基甲酰胺中,再按照氯乙酰氯与PEI-SNPs的液固比为6:1~8:1ml/g加入氯乙酰氯,在75~85℃回流反应后离心分离25~35h,取出固体物质用二甲基甲酰胺洗涤后真空干燥,得到的产物标记为CAC-SNPs;
(4)将乙醇和水按照体积比为1:1混合均匀得到混合溶液,按照液固比为30:1~40:1ml/g将步骤(3)得到的CAC-SNPs加入到混合溶液中,然后按照3-氨基-5-巯基-1,2,4-三氮唑与CAC-SNPs的质量比为1:1.5~1:2.5加入3-氨基-5-巯基-1,2,4-三氮唑,在75~85℃条件下回流反应30~40h后离心分离,取出固体物质用蒸馏水洗涤后真空干燥,得到最终改性二氧化硅纳米颗粒吸附剂,标记为ATT-SNPs。
3.一种根据权利要求1或2所述的改性二氧化硅纳米颗粒吸附剂作为银离子吸附剂的应用。
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