CN106512921A - 一种改性二氧化硅纳米颗粒、制备方法及其应用 - Google Patents
一种改性二氧化硅纳米颗粒、制备方法及其应用 Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 38
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000010931 gold Substances 0.000 claims abstract description 30
- 229910052737 gold Inorganic materials 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
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- 238000000926 separation method Methods 0.000 claims abstract description 20
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 12
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims abstract description 11
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims abstract description 11
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 238000005119 centrifugation Methods 0.000 claims description 13
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 10
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
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- -1 gold ions Chemical class 0.000 abstract description 21
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- 238000010992 reflux Methods 0.000 abstract 2
- 238000001291 vacuum drying Methods 0.000 abstract 2
- YLDIJCRKMDUKEJ-UHFFFAOYSA-M 2-but-2-enoyloxyethyl(trimethyl)azanium chloride Chemical compound [Cl-].CC=CC(=O)OCC[N+](C)(C)C YLDIJCRKMDUKEJ-UHFFFAOYSA-M 0.000 abstract 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract 1
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- 239000000243 solution Substances 0.000 description 28
- 238000010521 absorption reaction Methods 0.000 description 13
- 238000001179 sorption measurement Methods 0.000 description 10
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
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Abstract
本发明涉及一种改性二氧化硅纳米颗粒、制备方法及其应用,属于纳米材料制备技术领域。将纳米二氧化硅颗粒与3‑氯丙基三乙氧基硅烷混合后,加入到无水乙醇溶液中,然后再加入氨水,回流反应后液固分离,取出固体物质用无水乙醇洗涤离心分离后真空干燥,将得到的产物标记为GPTS‑SNPs;将得到的GPTS‑SNPs加入到二甲基甲酰胺溶液中,加入甲基丙烯酰氧乙基三甲基氯化铵、4,4‑联吡啶和CuCl,回流反应后液固分离,取出固体物质用二甲基甲酰胺溶液洗涤离心分离后真空干燥,得到最终改性二氧化硅纳米颗粒,标记为CHClN‑SNPs。该改性二氧化硅纳米颗粒可用作吸附剂,吸附酸性浸出液中的金离子,材料成本低,工艺制备简单,易与水溶液分离,具有高吸附性且可重复使用。
Description
技术领域
本发明涉及一种改性二氧化硅纳米颗粒、制备方法及其应用,属于纳米材料制备技术领域。
背景技术
黄金是一种兼具商品和货币双重属性的特殊产品,在应对金融危机、保障国家经济安全中具有不可替代的作用。我国黄金的生产原料来源于黄金矿山、有色金属工业副产物,其中矿山产金占据较大比例,2014年达到368.364吨,占全国总产量的81.53%。不论是在金的分析测定还是在其湿法冶炼过程中,对金的分离富集都是必不可少的。吸附分离富集法由于选择性好、操作简单等特点而普遍受到重视。目前应用较广泛的吸附剂有纳米二氧化硅、活性炭、聚氨酯泡沫塑料、螯合树脂等。为了适应各种目的和要求,人们研究开发新型吸附剂的努力从未间断过。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、制备方法及其应用。该改性二氧化硅纳米颗粒可用作吸附剂,吸附酸性浸出液中的金离子,材料成本低,工艺制备简单,易与水溶液分离,具有高吸附性且可重复使用。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,其结构式为:
,式中为纳米二氧化硅颗粒。
一种改性二氧化硅纳米颗粒的制备方法,其具体步骤如下:
(1)将纳米二氧化硅颗粒与3-氯丙基三乙氧基硅烷混合后,加入到无水乙醇溶液中,然后再加入氨水,回流反应后液固分离,取出固体物质用无水乙醇洗涤离心分离后真空干燥,将得到的产物标记为GPTS-SNPs;
(2)将步骤(1)得到的GPTS-SNPs加入到二甲基甲酰胺溶液中,加入甲基丙烯酰氧乙基三甲基氯化铵、4,4-联吡啶和CuCl,回流反应后液固分离,取出固体物质用二甲基甲酰胺溶液洗涤离心分离后真空干燥,得到最终改性二氧化硅纳米颗粒,标记为CHClN-SNPs。
所述步骤(1)中3-氯丙基三乙氧基硅烷与纳米二氧化硅颗粒液固比为2:1~4:1ml/g,无水乙醇溶液与纳米二氧化硅颗粒液固比为15:1~17:1ml/g,氨水与纳米二氧化硅颗粒液固比为1:1.2~1:1.3ml/g。
所述步骤(2)中二甲基甲酰胺溶液与GPTS-SNPs液固比为35:1~45:1ml/g,甲基丙烯酰氧乙基三甲基氯化铵与GPTS-SNPs液固比为4:1~6:1ml/g,4,4-联吡啶与GPTS-SNPs的质量比为1:15~1:25,CuCl与GPTS-SNPs的质量比为1:35~1:45。
所述步骤(1)中在60~70℃条件下回流反应20~30h。
所述步骤(2)中在65~75℃条件下回流反应30~40h。
该改性二氧化硅纳米颗粒能在酸性浸出液中吸附分离金的应用。
上述的有机试剂和无机试剂都为市购的分析纯。
本发明制备得到的改性二氧化硅纳米颗粒吸附剂主要用于从酸性浸出液中吸附分离金离子,与现有技术相比,具有如下优点:
(1)对金离子有较高的吸附量。
(2)本发明的制备方法简捷、成本较低。
(3)本发明的二氧化硅纳米颗粒吸附剂无毒无害,性能稳定,易于分离,可重复利用,对环境不造成二次污染。
(4)具有较好的应用与经济价值。
综上所述,本发明的吸附分离金的二氧化硅纳米颗粒CHClN-SNPs在金离子的吸附分离方面具有很大的潜力。
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,其结构式为:
,式中为纳米二氧化硅颗粒。
该改性二氧化硅纳米颗粒的制备方法,其具体步骤如下:
(1)将液固比为2:1ml/g纳米二氧化硅颗粒与3-氯丙基三乙氧基硅烷混合后,按照无水乙醇溶液与纳米二氧化硅颗粒液固比为15:1ml/g加入到无水乙醇溶液中,然后按照氨水与纳米二氧化硅颗粒液固比为1:1.2ml/g再加入氨水,在60℃条件下回流反应20h后液固分离,取出固体物质用无水乙醇洗涤离心分离后真空干燥,将得到的产物标记为GPTS-SNPs;
(2)按照液固比为35:1ml/g将步骤(1)得到的GPTS-SNPs加入到二甲基甲酰胺溶液中,加入甲基丙烯酰氧乙基三甲基氯化铵、4,4-联吡啶和CuCl,其中甲基丙烯酰氧乙基三甲基氯化铵与GPTS-SNPs液固比为4:1ml/g,4,4-联吡啶与GPTS-SNPs的质量比为1:15,CuCl与GPTS-SNPs的质量比为1:35,在65℃的条件下回流反应30h后液固分离,取出固体物质用二甲基甲酰胺溶液洗涤离心分离后真空干燥,得到最终改性二氧化硅纳米颗粒,标记为CHClN-SNPs。
吸附金离子性能测定:
取20mgCHClN-SNPs吸附剂投入初始浓度为100mg/L的金离子溶液中震荡吸附1h后,离心分离吸附剂,用ICP-OES测定滤液中剩余金离子浓度为24.4mg/L,吸附率为75.6%。将吸附过金离子的吸附剂在硫脲溶液(10wt%)中搅拌洗涤3h,然后用蒸馏水洗涤4次,最后将吸附剂在60℃下真空干燥12h。取上述吸附剂20mg投入初始浓度为100mg/L的金离子溶液中震荡吸附1h后,离心分离吸附剂,用ICP-OES测定滤液中剩余金离子浓度为25.6mg/L,吸附率为77.4%。说明本发明的吸附分离金的二氧化硅纳米颗粒CHClN-SNPs可循环利用。
实施例2
该改性二氧化硅纳米颗粒,其结构式为:
,式中为纳米二氧化硅颗粒。
该改性二氧化硅纳米颗粒的制备方法,其具体步骤如下:
(1)将液固比为3:1ml/g纳米二氧化硅颗粒与3-氯丙基三乙氧基硅烷混合后,按照无水乙醇溶液与纳米二氧化硅颗粒液固比为16:1ml/g加入到无水乙醇溶液中,然后按照氨水与纳米二氧化硅颗粒液固比为1:1.3ml/g再加入氨水,在65℃条件下回流反应25h后液固分离,取出固体物质用无水乙醇洗涤离心分离后真空干燥,将得到的产物标记为GPTS-SNPs;
(2)按照液固比为40:1ml/g将步骤(1)得到的GPTS-SNPs加入到二甲基甲酰胺溶液中,加入甲基丙烯酰氧乙基三甲基氯化铵、4,4-联吡啶和CuCl,其中甲基丙烯酰氧乙基三甲基氯化铵与GPTS-SNPs液固比为5:1ml/g,4,4-联吡啶与GPTS-SNPs的质量比为1:20,CuCl与GPTS-SNPs的质量比为1:40,在70℃的条件下回流反应35h后液固分离,取出固体物质用二甲基甲酰胺溶液洗涤离心分离后真空干燥,得到最终改性二氧化硅纳米颗粒,标记为CHClN-SNPs。
吸附金离子性能测定:
取20mgCHClN-SNPs吸附剂投入初始浓度为100mg/L的金离子溶液中震荡吸附1h后,离心分离吸附剂,用ICP-OES测定滤液中剩余金离子浓度为19.5mg/L,吸附率为80.5%。将吸附过金离子的吸附剂在硫脲溶液(10wt%)中搅拌洗涤3 h,然后用蒸馏水洗涤4次,最后将吸附剂在60℃下真空干燥12h。取上述吸附剂20mg投入初始浓度为100mg/L的金离子溶液中震荡吸附1h后,离心分离吸附剂,用ICP-OES测定滤液中剩余金离子浓度为20.1mg/L,吸附率为79.9%。说明本发明的吸附分离金的二氧化硅纳米颗粒CHClN-SNPs可循环利用。
实施例3
该改性二氧化硅纳米颗粒,其结构式为:
,式中为纳米二氧化硅颗粒。
该改性二氧化硅纳米颗粒的制备方法,其具体步骤如下:
(1)将液固比为4:1ml/g纳米二氧化硅颗粒与3-氯丙基三乙氧基硅烷混合后,按照无水乙醇溶液与纳米二氧化硅颗粒液固比为17:1ml/g加入到无水乙醇溶液中,然后按照氨水与纳米二氧化硅颗粒液固比为1:1.3ml/g再加入氨水,在70℃条件下回流反应30h后液固分离,取出固体物质用无水乙醇洗涤离心分离后真空干燥,将得到的产物标记为GPTS-SNPs;
(2)按照液固比为45:1ml/g将步骤(1)得到的GPTS-SNPs加入到二甲基甲酰胺溶液中,加入甲基丙烯酰氧乙基三甲基氯化铵、4,4-联吡啶和CuCl,其中甲基丙烯酰氧乙基三甲基氯化铵与GPTS-SNPs液固比为6:1ml/g,4,4-联吡啶与GPTS-SNPs的质量比为1:25,CuCl与GPTS-SNPs的质量比为1:45,在75℃的条件下回流反应40h后液固分离,取出固体物质用二甲基甲酰胺溶液洗涤离心分离后真空干燥,得到最终改性二氧化硅纳米颗粒,标记为CHClN-SNPs。
吸附金离子性能测定:
取20mgCHClN-SNPs吸附剂投入初始浓度为100mg/L的金离子溶液中震荡吸附1h后,离心分离吸附剂,用ICP-OES测定滤液中剩余金离子浓度为25.6mg/L,吸附率为74.4%。将吸附过金离子的吸附剂在硫脲溶液(10wt%)中搅拌洗涤3h,然后用蒸馏水洗涤4次,最后将吸附剂在60℃下真空干燥12h。取上述吸附剂20mg投入初始浓度为100mg/L的金离子溶液中震荡吸附1h后,离心分离吸附剂,用ICP-OES测定滤液中剩余金离子浓度为25.9mg/L,吸附率为74.1%。说明本发明的吸附分离金的二氧化硅纳米颗粒CHClN-SNPs可循环利用。
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 (7)
1.一种改性二氧化硅纳米颗粒,其特征在于:其结构式为:
,式中为纳米二氧化硅颗粒。
2.一种根据权利要求1所述的改性二氧化硅纳米颗粒的制备方法,其特征在于具体步骤如下:
(1)将纳米二氧化硅颗粒与3-氯丙基三乙氧基硅烷混合后,加入到无水乙醇溶液中,然后再加入氨水,回流反应后液固分离,取出固体物质用无水乙醇洗涤离心分离后真空干燥,将得到的产物标记为GPTS-SNPs;
(2)将步骤(1)得到的GPTS-SNPs加入到二甲基甲酰胺溶液中,加入甲基丙烯酰氧乙基三甲基氯化铵、4,4-联吡啶和CuCl,回流反应后液固分离,取出固体物质用二甲基甲酰胺溶液洗涤离心分离后真空干燥,得到最终改性二氧化硅纳米颗粒,标记为CHClN-SNPs。
3.根据权利要求2所述的权利要求1所述的改性二氧化硅纳米颗粒的制备方法,其特征在于:所述步骤(1)中3-氯丙基三乙氧基硅烷与纳米二氧化硅颗粒液固比为2:1~4:1ml/g,无水乙醇溶液与纳米二氧化硅颗粒液固比为15:1~17:1ml/g,氨水与纳米二氧化硅颗粒液固比为1:1.2~1:1.3ml/g。
4.根据权利要求2所述的权利要求1所述的改性二氧化硅纳米颗粒的制备方法,其特征在于:所述步骤(2)中二甲基甲酰胺溶液与GPTS-SNPs液固比为35:1~45:1ml/g,甲基丙烯酰氧乙基三甲基氯化铵与GPTS-SNPs液固比为4:1~6:1ml/g,4,4-联吡啶与GPTS-SNPs的质量比为1:15~1:25,CuCl与GPTS-SNPs的质量比为1:35~1:45。
5.根据权利要求2所述的权利要求1所述的改性二氧化硅纳米颗粒的制备方法,其特征在于:所述步骤(1)中在60~70℃条件下回流反应20~30h。
6.根据权利要求2所述的权利要求1所述的改性二氧化硅纳米颗粒的制备方法,其特征在于:所述步骤(2)中在65~75℃条件下回流反应30~40h。
7.根据权利要求1至6任意一项所述的权利要求1所述的改性二氧化硅纳米颗粒能在酸性浸出液中吸附分离金的应用。
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