CN106944002A - 一种端基炔化合物改性硅胶的制备及汞离子吸附的应用 - Google Patents
一种端基炔化合物改性硅胶的制备及汞离子吸附的应用 Download PDFInfo
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Abstract
本发明公开一种端基炔化合物改性硅胶的制备及汞离子吸附的应用,利用氨丙基三甲氧基硅烷作为偶联剂,将炔基接枝到硅胶表面,合成一种端基炔化合物改性硅胶,这种单层的末端炔基修饰的硅胶不仅比传统硅胶有更好的汞离子吸附效率,而且在制造过程中使用的硅胶更少,应用于处理含有汞离子废水时处理时间短,过程中不会对环境造成污染。其制备过程简单,实验条件温和,使用的原料价格相对低廉,成本较低,可规模化应用于含有汞离子废水的处理。
Description
技术领域
本发明涉及重金属离子污水处理领域,尤其涉及一种端基炔化合物改性硅胶的制备及汞离子吸附的应用。
背景技术
汞被认为是最有害的污染物之一,因为随着环境的污染,它可以积累在生物组织中,这一过程称为生物积累。汞的排放常见于油漆、纸浆、肥料、炼油等工业生产过程中。通常利用化学沉淀凝固法、离子交换法、超滤法、反渗透法和电解法等方法用于去除废水中的汞离子,这些方法所采用的固体材料吸附剂被认为是最可靠的方便和简单的。许多多孔材料可被用作于吸附剂,例如粉煤灰、高炉矿渣、天然材料壳聚糖和活性炭等。活性炭是应用最广泛的吸附剂,但其被规模运用于污水处理时是非常昂贵的,因此寻找可代替的廉价吸附剂是非常有意义的。
有文献使用硅胶微/纳米颗粒去除废水中的重金属离子(Y. Yang, A.-M. Jonas,L. Dusan, Sci. Technol. Adv. Mater. 13 (2012), 015008-1–015008-11),虽然硅胶微/纳米颗粒具有良好的多孔结构,可以提高硅胶对镉离子的吸附率,但这样的成本同样很高。末端炔基可作为氢键受体与多种金属离子结合,实验人员在玻璃盘喷涂一层功能化末端炔基络合Ag的膜作为抗菌表面,结果证明这种抗菌表面比传统抗菌表面具有更为高效和广谱性的抗菌特点(M.N. Tahir, D. Jeong, H. Kim, J.-H. Yu, E. Cho, S. Jung,Bull. Korean Chem. Soc. 35 (2014) 39.),这种抗菌表面使用的材料很少,但却具有很好的抗菌效果,节约了成本。
鉴于上述背景技术,本发明利用氨丙基三甲氧基硅烷作为偶联剂,将炔基接枝到硅胶表面,合成一种端基炔化合物改性硅胶,作为廉价的汞离子吸附剂,这种单层的末端炔基修饰的硅胶具有有效的汞离子吸附效果,可规模化应用于含有汞离子废水的处理。
发明内容
本发明所要解决的技术问题是提供一种端基炔化合物改性硅胶的制备及汞离子吸附的应用。
实现本发明目的的解决方案为:所述的一种端基炔化合物改性硅胶的制备及汞离子吸附的应用,如下:
(1)在一个500 mL三口烧瓶中分别加入10-12 g硅胶60粉末Si60,然后将三口烧瓶置于真空干燥箱在135 ℃温度下真空干燥24 h,取出三口烧瓶并装上安装温度计、分水器和冷凝管,然后向三口烧瓶中加入2.45-2.55 mL的3-氨丙基三甲氧基硅烷作为偶联剂,之后再加入100 mL甲醇,磁力搅拌,升温至回流温度,并维持此温度24 h至反应终点,进行减压过滤和70 ℃下真空干燥,得到表面连有氨基的硅胶颗粒Si-NH2;
(2)在一个250 mL烧杯中加入步骤(1)所得的5.1-5.3 g Si-NH2,将烧杯放在42 ℃的水浴锅中,然后向烧杯中分别加入2-2.5 mL三乙胺和15-20 mL二氯甲烷,磁力搅拌0.5 h,接着再加入1-1.5 mL氯戊炔,磁力搅拌6 h至反应终点,进行减压过滤和70 ℃下真空干燥,得到的表面接枝炔化合物的硅胶颗粒,即端基炔化合物改性硅胶Si-NH-Py;
(3)一种端基炔化合物改性硅胶在处理含有汞离子废水中的应用,在废水池中通入含有汞离子的废水,调节废水的pH = 7,然后投入步骤(2)中的Si-NH-Py,匀速搅拌废水0.5h,然后将废水通入沉淀池静置6 h,之后排出处理完毕的水,即完成对含有汞离子的废水的处理。
所述步骤(3)中端基炔化合物改性硅胶对应废水体积加入的剂量为3-5 g/L,其中废水中汞离子浓度应小于250 mg/L。
本发明与现有技术相比,其有益效果是:
(1)本发明的端基炔化合物改性硅胶应用于处理含有汞离子废水,对50-200 mg/L的汞离子溶液的吸附率均大于92%,对汞离子的平均吸附率是未改性硅胶吸附剂的3倍;
(2)本发明的端基炔化合物改性硅胶由于独特的炔基官能团修饰在硅表面,使用很少的单层硅胶即可有效吸附汞离子,硅胶的用量比传统硅胶吸附剂更少,成本更低,经济性能好,可规模应用于含有汞离子废水的处理;
(3)本发明的端基炔化合物改性硅胶合成条件温和,使用原料价格相对低廉,应用在汞离子废水时操作简单,处理时间短,过程中不会对环境造成污染。
附图说明
图1为硅胶60粉末、实施例1步骤(1)所得的Si-NH2和实施例1步骤(2)所得的Si-NH-Py对不同浓度汞离子溶液中汞离子的吸附率。
具体实施方式
实施例1
(1)在一个500 mL三口烧瓶中分别加入10 g硅胶60粉末Si60,然后将三口烧瓶置于真空干燥箱在135 ℃温度下真空干燥24 h,取出三口烧瓶并装上安装温度计、分水器和冷凝管,然后向三口烧瓶中加入2.55 mL的3-氨丙基三甲氧基硅烷作为偶联剂,之后再加入100mL甲醇,磁力搅拌,升温至回流温度,并维持此温度24 h至反应终点,进行减压过滤和70 ℃下真空干燥,得到表面连有氨基的硅胶颗粒Si-NH2;
(2)在一个250 mL烧杯中加入步骤(1)所得的5.3 g Si-NH2,将烧杯放在42 ℃的水浴锅中,然后向烧杯中分别加入2.5 mL三乙胺和15-20 mL二氯甲烷,磁力搅拌0.5 h,接着再加入1-1.5 mL氯戊炔,磁力搅拌6 h至反应终点,进行减压过滤和70 ℃下真空干燥,得到的表面接枝炔化合物的硅胶颗粒,即端基炔化合物改性硅胶Si-NH-Py;
(3)一种端基炔化合物改性硅胶在处理含有汞离子废水中的应用:在废水池中通入含有汞离子的废水,调节废水的pH = 7,然后投入步骤(2)中的Si-NH-Py,改性硅胶对应废水体积加入的剂量为3 g/L,其中废水中汞离子浓度为135 ppm,匀速搅拌废水0.5 h,然后将废水通入沉淀池静置6 h,之后排出处理完毕的水,即完成对含有汞离子的废水的处理。
实施例2
分别取实施例1步骤(1)使用的Si60、实施例1步骤(1)所得的Si-NH2和实施例1步骤(2)所得的Si-NH-Py,作为吸附剂用于测试汞离子离子的吸附率:
实验采用HgCl2配成汞离子浓度为50-500 mg/L 的溶液,溶液汞离子浓度分别为50mg/L、100 mg/L、150 mg/L、200 mg/L、250 mg/L、300 mg/L、350 mg/L、400 mg/L、450 mg/L、500 mg/L。将实施例1步骤(1)使用的Si60、实施例1步骤(1)所得的Si-NH2和实施例1步骤(2)所得的Si-NH-Py作为吸附剂分别对上述10种不同浓度的溶液做吸附测试实验,其中每组实验所加入吸附剂的质量皆为0.1 g,测试溶液的体积为100 mL,加入吸附剂后震荡2 h,过滤出吸附剂后测各烧杯中剩余汞离子的含量,测得每组实验中所用吸附剂对汞离子的吸附率(见图1)。
实验结果表明:本发明的Si-NH-Py对汞离子具有良好的吸附效果,加入的剂量仅为3 g/L,对50-200 mg/L的汞离子溶液的吸附率均大于92%,对250-500 mg/L的汞离子溶液的吸附率均大于81%; Si-NH2对汞离子吸附率比较未改性的Si60没有明显提高,而本发明的端基炔化合物改性硅胶对汞离子的平均吸附率是未改性Si60的3倍以上,可见对硅胶增强改性起作用的是端基炔化合物。
Claims (2)
1.一种端基炔化合物改性硅胶的制备及汞离子吸附的应用,其特征在于,包括如下步骤:
(1)在一个500 mL三口烧瓶中分别加入10-12 g硅胶60粉末Si60,然后将三口烧瓶置于真空干燥箱在135 ℃温度下真空干燥24 h,取出三口烧瓶并装上安装温度计、分水器和冷凝管,然后向三口烧瓶中加入2.45-2.55 mL的3-氨丙基三甲氧基硅烷作为偶联剂,之后再加入100 mL甲醇,磁力搅拌,升温至回流温度,并维持此温度24 h至反应终点,进行减压过滤和70 ℃下真空干燥,得到表面连有氨基的硅胶颗粒Si-NH2;
(2)在一个250 mL烧杯中加入步骤(1)所得的5.1-5.3 g Si-NH2,将烧杯放在42 ℃的水浴锅中,然后向烧杯中分别加入2-2.5 mL三乙胺和15-20 mL二氯甲烷,磁力搅拌0.5 h,接着再加入1-1.5 mL氯戊炔,磁力搅拌6 h至反应终点,进行减压过滤和70 ℃下真空干燥,得到的表面接枝炔化合物的硅胶颗粒,即端基炔化合物改性硅胶Si-NH-Py;
(3)一种端基炔化合物改性硅胶在处理含有汞离子废水中的应用:在废水池中通入含有汞离子的废水,调节废水的pH = 7,然后投入步骤(2)中的Si-NH-Py,匀速搅拌废水0.5h,然后将废水通入沉淀池静置6 h,之后排出处理完毕的水,即完成对含有汞离子的废水的处理。
2.根据权利要求1所述的端基炔化合物改性硅胶在处理含有汞离子废水中的应用,其特征在于,所述步骤(3)中端基炔化合物改性硅胶对应废水体积加入的剂量为3-5 g/L,其中废水中汞离子浓度应小于250 mg/L。
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