CN114871426B - 一种介孔氧化铝原位包覆纳米银材料、制备方法及应用 - Google Patents
一种介孔氧化铝原位包覆纳米银材料、制备方法及应用 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 8
- 239000001509 sodium citrate Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims 3
- 229910052709 silver Inorganic materials 0.000 abstract description 16
- 239000004332 silver Substances 0.000 abstract description 16
- -1 silver ions Chemical class 0.000 abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 230000003115 biocidal effect Effects 0.000 abstract description 2
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- 239000002270 dispersing agent Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
本发明公布了一种介孔氧化铝原位包覆纳米银的制备方法。通过将银离子和还原剂预先置于氧化铝凝胶孔隙中，然后通过加热启动还原反应和凝胶老化同时进行，将银离子原位还原成纳米银，并固化于氧化铝凝胶网络孔隙中，由于氧化铝凝胶中介孔孔隙的限域效应，得到的纳米银尺寸小于介孔氧化铝孔径的尺寸，获得的介孔氧化铝原位包覆纳米银材料用于抗菌防霉，除异味等领域。
Description
技术领域
本发明属于新材料技术领域，具体涉及一种抗菌材料及制备方法。
背景技术
银是一种高效广谱抗菌剂，低至1ppm浓度的银，就能杀灭数百种细菌。银作为抗菌剂使用，有两种形式，一种是银离子，另一种是纳米银。银离子很不稳定，容易被光或是还原剂还原，如沾到人的皮肤上会留下黑斑，清洗不掉，需要一两周时间颜色才能随着皮肤的新陈代谢而消失。另外银离子还容易和水中普遍存在的氯离子反应，氯化银难溶于水，且见光容易分解为银。因为银离子的不稳定，容易变色等限制了银离子的应用范围。纳米银是尺寸在纳米尺度的颗粒状银，或是纳米银线，用作抗菌剂的纳米银主要是指颗粒状银。纳米银是用量最大的纳米材料之一，制备纳米银的方法常用的主要是液相还原法例如多元醇法、生物质提取物还原法、葡萄糖和柠檬酸钠还原法等多种。液相还原法的优点是工艺简单，容易放大生产。但是也存在一些缺点，通常纳米银的粒径越小抗菌活性越好，但是液相还原法制备的纳米银，粒径分布宽，纳米银粒径在25纳米以上，粒径较大，难以获得粒径均一，5纳米左右小尺寸纳米银。且在液相还原法中普遍使用PVP等表面活性剂作为分散剂，分散剂的使用影响纳米银释放有效的抗菌活性银离子，为了起到杀菌作用，不得不提高纳米银的浓度和用量，造成废水中银离子含量超过0.1ppm国家标准的范围。另外制备的纳米银普遍存在在体系中稳定性差，易团聚沉降，容易被氧化，游离的纳米银颗粒对生物体有潜在危害。
发明内容
本发明的目的在于提供一种介孔氧化铝原位包覆纳米银材料、制备方法及应用，解决上述的分散剂的使用影响抗菌活性，游离的纳米银颗粒对生物体有潜在危害的问题。
为实现上述目的，本发明的技术方案为：
一种介孔氧化铝原位包覆纳米银材料的制备方法：将一定量硝酸银溶于10～40wt％的酸性铝溶胶中，其中铝溶胶中氧化铝的粒径为5～30nm，溶解后得到银离子含量为100～10000ppm的混合液，再向其中加入柠檬酸钠形成凝胶，将上述凝胶置于60℃～95℃的温度的水浴锅中加热24小时，再经过烘干得到介孔氧化铝原位包覆纳米银材料。
本发明的介孔氧化铝原位包覆纳米银材料应用于抗菌防霉除异味等领域。
本发明有益的技术效果：柠檬酸钠充当还原剂和凝胶促进剂的双重作用，制备过程简单，减少了引入试剂的种类，无游离的颗粒纳米银释放，安全环保，银离子可以稳定释放，没有使用分散剂粉体抗菌活性高。
附图说明
图1为本发明实施例1介孔氧化铝包覆纳米银材料的XRD图；
图2本发明实施例1介孔氧化铝包覆纳米银材料的eds能谱
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，显而易见仍然属于本发明保护的范围。
实施例1：
将一定量硝酸银溶于10wt％的酸性铝溶胶中得到银离子含量为100ppm的混合液，再向其中加入柠檬酸钠形成凝胶，将上述凝胶置于60℃的温度的水浴锅中加热24小时，再经过烘干得到介孔氧化铝原位包覆纳米银材料。
实施例2：
将一定量硝酸银溶于30wt％的酸性铝溶胶中得到银离子含量为1000ppm的混合液，再向其中加入柠檬酸钠形成凝胶，将上述凝胶置于70℃的温度的水浴锅中加热24小时，再经过烘干得到介孔氧化铝原位包覆纳米银材料。
实施例3：
将一定量硝酸银溶于35wt％的酸性铝溶胶中得到银离子含量为5000ppm的混合液，再向其中加入柠檬酸钠形成凝胶，将上述凝胶置于80℃的温度的水浴锅中加热24小时，再经过烘干得到介孔氧化铝原位包覆纳米银材料。
实施例4：
将一定量硝酸银溶于40wt％的酸性铝溶胶中得到银离子含量为10000ppm的混合液，再向其中加入柠檬酸钠形成凝胶，将上述凝胶置于95℃的温度的水浴锅中加热24小时，再经过烘干得到介孔氧化铝原位包覆纳米银材料。
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 (3)
1.一种介孔氧化铝原位包覆纳米银的制备方法，其特征在于：包括如下步骤：将硝酸银溶于酸性铝溶胶中得到的混合液，再向其中加入柠檬酸钠形成凝胶，将上述凝胶置于水浴锅中加热24小时，再经过烘干得到介孔氧化铝原位包覆纳米银材料；
其中，所述酸性铝溶胶中氧化铝的粒径大小为5～30nm。
2.根据权利要求1所述的介孔氧化铝原位包覆纳米银的制备方法，其特征在于：所述混合液中银离子含量为100～10000ppm。
3.根据权利要求1所述的介孔氧化铝原位包覆纳米银的制备方法，其特征在于：所述酸性铝溶胶的氧化铝含量为10～40wt％。
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| CN1623897A (zh) * | 2004-11-19 | 2005-06-08 | 中国乐凯胶片集团公司 | 载纳米银的二氧化硅制备方法 |
| JP2006169208A (ja) * | 2004-12-20 | 2006-06-29 | Ets:Kk | 抗菌性に優れた銀微粒子担持体 |
| CN1792508A (zh) * | 2005-11-25 | 2006-06-28 | 华南理工大学 | 以无机金属氧化物为载体的纳米银及其制备方法 |
| CN104226374A (zh) * | 2014-09-05 | 2014-12-24 | 天津大学 | 一种负载型氧化物包覆金属核壳催化剂及其制备方法 |
| CN104923215A (zh) * | 2015-05-07 | 2015-09-23 | 中国石油大学(北京) | 担载贵金属的有序介孔氧化铝材料及其合成方法与应用 |
| WO2016192242A1 (zh) * | 2015-05-29 | 2016-12-08 | 厦门大学 | 一种可控壳层隔绝银纳米粒子的合成方法 |
| CN105217749A (zh) * | 2015-07-03 | 2016-01-06 | 何素梅 | 一种负载纳米银的吸附载体及其制备方法 |
| CN107096529A (zh) * | 2017-04-12 | 2017-08-29 | 浙江大学 | 一种极小粒径纳米银负载的石墨烯气凝胶及其制备方法和应用 |
| CN107159212A (zh) * | 2017-05-08 | 2017-09-15 | 上海大学 | 纳米金属颗粒负载于介孔γ‑氧化铝复合材料的制备方法 |
| CN114050239A (zh) * | 2021-10-28 | 2022-02-15 | 复旦大学 | 一种银纳米晶修饰的介孔金属氧化物复合材料及制备方法 |
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