CN1958198A - Plant reduction method for preparing silver Nano granules and gold Nano granules - Google Patents
Plant reduction method for preparing silver Nano granules and gold Nano granules Download PDFInfo
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- 239000010931 gold Substances 0.000 title claims abstract description 41
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 38
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 25
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 14
- 239000004332 silver Substances 0.000 title claims abstract description 14
- 239000008187 granular material Substances 0.000 title 2
- 239000002105 nanoparticle Substances 0.000 claims abstract description 37
- 241000723346 Cinnamomum camphora Species 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 21
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims abstract description 17
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 241000196324 Embryophyta Species 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 10
- 229960000846 camphor Drugs 0.000 claims abstract description 9
- 229930008380 camphor Natural products 0.000 claims abstract description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims 4
- 239000002245 particle Substances 0.000 abstract description 16
- 239000000243 solution Substances 0.000 abstract description 12
- 238000002156 mixing Methods 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 3
- 239000002082 metal nanoparticle Substances 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 241000723347 Cinnamomum Species 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 235000017803 cinnamon Nutrition 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000000813 microbial effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 244000144927 Aloe barbadensis Species 0.000 description 1
- 235000002961 Aloe barbadensis Nutrition 0.000 description 1
- 240000004784 Cymbopogon citratus Species 0.000 description 1
- 235000017897 Cymbopogon citratus Nutrition 0.000 description 1
- 240000005636 Dryobalanops aromatica Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 241000208152 Geranium Species 0.000 description 1
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 1
- 229910004042 HAuCl4 Inorganic materials 0.000 description 1
- 240000004658 Medicago sativa Species 0.000 description 1
- 235000017587 Medicago sativa ssp. sativa Nutrition 0.000 description 1
- 240000004584 Tamarindus indica Species 0.000 description 1
- 235000004298 Tamarindus indica Nutrition 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 235000011399 aloe vera Nutrition 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
植物还原法制备银纳米颗粒和金纳米颗粒，涉及一种银纳米颗粒和金纳米颗粒。提供一种在温和条件下利用植物树叶将Ag+、Au3+分别还原成银纳米颗粒和金纳米颗粒的新方法。银纳米颗粒制备方法其步骤为：取0.01～10.0g的芳樟树叶干粉和100ml硝酸银溶液混合，在15～60℃温度下反应，即制得银纳米颗粒。金纳米颗粒制备方法其步骤为：取0.01～10.0g的芳樟树叶干粉和100ml氯金酸溶液混合，在15～60℃温度下反应，即制得金纳米颗粒。工艺简单，不需要除硝酸银或氯金酸以外的添加剂，所制得的纳米级的银颗粒和金颗粒在水溶液中具有很好的分散性和稳定性，容易形成金属纳米颗粒溶胶。The preparation of silver nanoparticles and gold nanoparticles by a plant reduction method relates to a silver nanoparticle and a gold nanoparticle. A new method for reducing Ag + and Au 3+ into silver nanoparticles and gold nanoparticles by using plant leaves under mild conditions is provided. The preparation method of silver nanoparticles comprises the steps of: mixing 0.01-10.0 g of dry powder of camphor leaves and 100 ml of silver nitrate solution, and reacting at a temperature of 15-60 DEG C to obtain silver nanoparticles. The preparation method of the gold nanoparticles comprises the steps of: taking 0.01-10.0 g of dry powder of camphor leaves and mixing 100 ml of chloroauric acid solution, and reacting at a temperature of 15-60 DEG C to obtain the gold nanoparticles. The process is simple, no additives other than silver nitrate or chloroauric acid are needed, the prepared nano-scale silver particles and gold particles have good dispersion and stability in aqueous solution, and it is easy to form metal nano particle sol.
Description
技术领域technical field
本发明涉及一种银纳米颗粒和金纳米颗粒，尤其是涉及一种采用植物还原法制备银纳米颗粒和金纳米颗粒的方法。The invention relates to a silver nanoparticle and a gold nanoparticle, in particular to a method for preparing the silver nanoparticle and the gold nanoparticle by a plant reduction method.
背景技术Background technique
银纳米颗粒因其独特的理化性质在工业生产的许多领域中有着广泛的应用，如银一直是乙烯环氧化催化剂的主要成分；单质银具有很强的杀菌能力，而将负载的银制备成纳米级的颗粒后，其杀菌活性得到了很大的提高。金纳米颗粒以其独特的光学和电学性质、良好的稳定性、小尺寸和表面效应以及独特的生物亲和性，使其在生化免疫等领域显示了潜在的应用价值。银纳米颗粒和金纳米颗粒的制备方法一直以物理和化学方法为主，尽管国内外对这两种方法的研究较为充分，工艺技术也较为成熟，但它们存在着生产成本较高和易污染环境等缺点。另外，近年来，随着一些微生物被证实在温和条件下，具有还原金属离子的能力，人们意识到可以利用微生物还原法来制备金属纳米颗粒。虽然微生物还原法能够克服传统化学法和物理法生产成本较高、易污染环境等缺点，但是，在利用微生物还原法制备银纳米颗粒和金纳米颗粒的过程中，还原速度较慢，不利于工业化过程的开发，有时需要加入酸类和碱类等添加剂，以加快生物还原反应速度；另外，微生物的培养过程较为麻烦，容易引起染菌。近年来，有报道利用植物提取物合成银纳米颗粒和金纳米颗粒，如利用紫花苜蓿活植物或生物质合成金或银纳米颗粒(1、J.Nanopart.Res.，1999，1，397；2、Nano Lett.，2002，2，397；3、Langmuir，2003，19，1357.)利用天竺葵煮液还原制备金或银纳米颗粒(1、J.Mater.Chem.，2003，13，1822；2、Biotechnol.Prog.，2003，9，1627.)利用柠檬香草煮液合成三角片状金纳米颗粒(Nat.Mater.，2004，3，482.)利用罗望子叶提取物合成三角片状金纳米颗粒(Synth.React.Inorg.Met.-Org.Nano-Metal Chem.，2005，35，19.)利用库拉索芦荟的煮液还原AuCl4 -，获得高产率的三角片状金纳米颗粒(Biotechnol.Prog.，2006，22，577.)。在常温下，利用植物树叶生物质或煮液能将Ag+、Au3+分别还原成银纳米颗粒和金纳米颗粒，其还原速度以及所制得的纳米颗粒可与传统制备方法相媲美，因而不仅能够克服上述传统化学法和物理法的缺点，还能够克服微生物还原法存在的缺点。Silver nanoparticles are widely used in many fields of industrial production because of their unique physical and chemical properties. For example, silver has always been the main component of ethylene epoxidation catalysts; elemental silver has a strong bactericidal ability, and the loaded silver is prepared into After adding nanometer particles, its bactericidal activity has been greatly improved. With its unique optical and electrical properties, good stability, small size and surface effect, and unique biological affinity, gold nanoparticles have shown potential application value in the fields of biochemical immunity and so on. The preparation methods of silver nanoparticles and gold nanoparticles have always been based on physical and chemical methods. Although the research on these two methods is relatively sufficient at home and abroad, and the technology is relatively mature, they have high production costs and are prone to pollute the environment. and other shortcomings. In addition, in recent years, as some microorganisms have been confirmed to have the ability to reduce metal ions under mild conditions, people have realized that metal nanoparticles can be prepared by using microbial reduction methods. Although the microbial reduction method can overcome the shortcomings of traditional chemical and physical methods such as high production costs and easy pollution of the environment, the reduction speed is slow in the process of preparing silver nanoparticles and gold nanoparticles by using microbial reduction methods, which is not conducive to industrialization. In the development of the process, it is sometimes necessary to add additives such as acids and alkalis to speed up the biological reduction reaction; in addition, the cultivation process of microorganisms is cumbersome and easily causes bacterial contamination. In recent years, it has been reported to utilize plant extracts to synthesize silver nanoparticles and gold nanoparticles, such as utilizing alfalfa living plants or biomass to synthesize gold or silver nanoparticles (1, J.Nanopart.Res., 1999, 1, 397; 2 , Nano Lett., 2002, 2, 397; 3, Langmuir, 2003, 19, 1357.) Utilize the reduction of geranium boiling liquid to prepare gold or silver nanoparticles (1, J.Mater.Chem., 2003, 13, 1822; 2 , Biotechnol.Prog., 2003, 9, 1627.) Utilize lemongrass boiling liquid to synthesize triangular sheet-shaped gold nanoparticles (Nat.Mater., 2004, 3, 482.) Utilize tamarind leaf extract to synthesize triangular sheet-shaped gold nanoparticles Particles (Synth.React.Inorg.Met.-Org.Nano-Metal Chem., 2005, 35, 19.) use the cooking liquid of Aloe vera to reduce AuCl 4 - , and obtain high-yield triangular sheet-shaped gold nanoparticles ( Biotechnol. Prog., 2006, 22, 577.). At room temperature, Ag + and Au 3+ can be reduced to silver nanoparticles and gold nanoparticles respectively by using plant leaf biomass or cooking liquid, and the reduction speed and the prepared nanoparticles are comparable to the traditional preparation methods, so Not only can overcome the shortcomings of the above-mentioned traditional chemical method and physical method, but also can overcome the shortcomings of the microbial reduction method.
发明内容Contents of the invention
本发明旨在提供一种在温和条件下利用植物树叶将Ag+、Au3+分别还原成银纳米颗粒和金纳米颗粒的新方法。The present invention aims to provide a new method for reducing Ag + and Au 3+ into silver nanoparticles and gold nanoparticles by using plant leaves under mild conditions.
本发明所述的银纳米颗粒制备方法其步骤为：取0.01～10.0g的芳樟树叶干粉和100ml硝酸银溶液混合，在15～60℃温度下反应，即制得银纳米颗粒。The preparation method of silver nanoparticles in the present invention comprises the following steps: mixing 0.01-10.0 g of dry powder of camphor leaves and 100 ml of silver nitrate solution, and reacting at a temperature of 15-60 DEG C to obtain silver nanoparticles.
所述的芳樟树叶干粉和硝酸银溶液混合的反应时间最好为24～120h。硝酸银溶液的浓度最好为0.01mM～10M。The reaction time for mixing the dry powder of camphor leaves and the silver nitrate solution is preferably 24-120 hours. The concentration of the silver nitrate solution is preferably 0.01mM-10M.
本发明所述的金纳米颗粒制备方法其步骤为：取0.01～10.0g的芳樟树叶干粉和100ml氯金酸溶液混合，在15～60℃温度下反应，即制得金纳米颗粒。The preparation method of gold nanoparticles in the present invention comprises the steps of: mixing 0.01-10.0 g of cinnamomum camphora leaf dry powder with 100 ml of chloroauric acid solution, and reacting at a temperature of 15-60° C. to obtain gold nanoparticles.
所述的芳樟树叶干粉和氯金酸溶液混合的反应时间最好为1～6h。氯金酸溶液的浓度最好为0.01mM～10M。The reaction time for mixing the dry powder of camphor leaves and the chloroauric acid solution is preferably 1 to 6 hours. The concentration of the chloroauric acid solution is preferably 0.01mM-10M.
本发明所述的纳米银颗粒和纳米金颗粒其Ag+和Au3+是通过芳樟树叶干粉还原，所得银纳米颗粒的粒径在10～100nm，三角片状金纳米颗粒的边长在25～150nm，球形金纳米颗粒的粒径在5～40nm。The Ag + and Au3 + of the nano-silver particle and nano-gold particle described in the present invention are reduced by the dry powder of cinnamon camphor leaves, and the particle diameter of the gained silver nano-particle is 10～100nm, and the side length of the triangular flaky gold nano-particle is 25 ~150nm, the particle size of spherical gold nanoparticles is 5~40nm.
本发明所采用的植物树叶为芳樟叶干粉不同于已有的报道。芳樟叶干粉的制备利用在40～100℃将新鲜芳樟叶烘干，或者在室外将新鲜芳樟叶晒干，或者在10～40℃温度下利用空气对流让新鲜芳樟叶自然风干。接着利用手工研磨或机械研磨的方法，将干芳樟叶制成芳樟叶干微细粉。The plant leaf that the present invention adopts is cinnamon camphor leaf dry powder and is different from existing report. The dry powder of cinnamon leaves is dried by drying the fresh cinnamon leaves at 40-100 DEG C, or drying the fresh cinnamon camphor leaves outdoors, or using air convection to let the fresh cinnamon camphor leaves dry naturally at a temperature of 10-40 DEG C. Then, the dry cinnamon leaves are made into fine powder of cinnamon leaves by manual grinding or mechanical grinding.
本发明的工艺简单，不需要除硝酸银或氯金酸以外的添加剂，所制得的纳米级的银颗粒和金颗粒在水溶液中具有很好的分散性和稳定性，容易形成金属纳米颗粒溶胶。The process of the present invention is simple, does not need additives other than silver nitrate or chloroauric acid, and the prepared nano-scale silver particles and gold particles have good dispersibility and stability in aqueous solution, and it is easy to form metal nano-particle sol .
具体实施方式Detailed ways
下面通过实施例对本发明作进一步说明。Below by embodiment the present invention will be further described.
实施例1Example 1
干芳樟树叶粉碎并过20目筛得芳樟树叶干粉。称取5g芳樟叶干粉，与浓度为10mM的AgNO3溶液100ml在100ml的锥形瓶中反应，反应在40℃、150r/min的水浴摇床上进行。反应118h后，用透射电镜(TEM)观察所得银溶胶，其中银纳米颗粒的形貌均为近球形，粒径绝大部分分布在50～80nm，平均粒径为64.8nm。Dried Cinnamomum camphora leaves are pulverized and sieved with 20 meshes to obtain Cinnamomum camphora leaf dry powder. Weigh 5g of dry powder of cinnamon camphor leaves, react with 100ml of AgNO3 solution with a concentration of 10mM in a 100ml Erlenmeyer flask, and the reaction is carried out on a water bath shaker at 40°C and 150r/min. After reacting for 118 hours, the obtained silver sol was observed with a transmission electron microscope (TEM), and the morphology of the silver nanoparticles was nearly spherical, most of the particle diameters were distributed in the range of 50-80nm, and the average particle diameter was 64.8nm.
实施例2Example 2
采用实施例1中的芳樟树叶干粉，称取1g芳樟叶干粉，与浓度为10mM的HAuCl4溶液100ml反应，反应温度为30℃，其它反应条件同实施例1。用透射电镜对样品进行观察金溶胶，可以看到大量的形貌清晰的三角片状金纳米颗粒，三角片状金纳米颗粒的厚度在20nm以内，边长在20～150nm，平均边长为80.0nm。Adopt the dry powder of camphor leaf in embodiment 1, take by weighing 1g dry powder of camphor leaf, be 10mM HAuCl solution 100ml reaction with concentration, reaction temperature is 30 ℃, other reaction conditions are with embodiment 1. Observing the sample gold sol with a transmission electron microscope, you can see a large number of triangular sheet-shaped gold nanoparticles with a clear shape. The thickness of the triangular sheet-shaped gold nanoparticles is within 20nm, the side length is 20-150nm, and the average side length is 80.0 nm.
实施例3Example 3
采用实施例1中的芳樟树叶干粉。称取5g芳樟叶干粉，与浓度为10mM的HAuCl4溶液100ml反应，反应温度为30℃，其它反应条件同实施例1。用透射电镜(TEM)观察金溶胶，可以观察到金纳米颗粒形貌均为球形，所得金纳米颗粒的粒径分布在10～40nm，平均粒径为23.4nm。Adopt the dry powder of Cinnamomum camphora leaf among the embodiment 1. Weigh 5g of Cinnamomum camphora leaf dry powder, and react with 100ml of 10mM HAuCl solution, the reaction temperature is 30°C, and other reaction conditions are the same as in Example 1. Observing the gold sol with a transmission electron microscope (TEM), it can be observed that the morphology of the gold nanoparticles is spherical, and the particle size distribution of the obtained gold nanoparticles is 10-40nm, with an average particle size of 23.4nm.
实施例4Example 4
采用实施例1中的芳樟树叶干粉。称取10g芳樟叶干粉，与浓度为10mM的HAuCl4溶液100ml反应，反应温度为30℃，其它反应条件同实施例1。反应1.5h后，用透射电镜(TEM)观察金溶胶，所得金纳米颗粒形貌均为球形，粒径分布在15～35nm，平均粒径为21.5nm。Adopt the dry powder of Cinnamomum camphora leaf among the embodiment 1. Weigh 10g of Cinnamomum camphora leaf dry powder, and react with 100ml of HAuCl4 solution with a concentration of 10mM, the reaction temperature is 30°C, and other reaction conditions are the same as in Example 1. After reacting for 1.5 h, the gold sol was observed with a transmission electron microscope (TEM), and the obtained gold nanoparticles were all spherical in shape, with a particle size distribution of 15-35 nm and an average particle size of 21.5 nm.
Claims (6)
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| US20050009170A1 (en) * | 2002-12-10 | 2005-01-13 | The University Of Texas System | Preparation of metal nanoparticles in plants |
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