CN103978223B - A kind of method utilizing Cortex Eucommiae water extract green syt nanometer gold - Google Patents
A kind of method utilizing Cortex Eucommiae water extract green syt nanometer gold Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000010931 gold Substances 0.000 title claims abstract description 40
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 39
- 239000000284 extract Substances 0.000 title claims abstract description 31
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 27
- 241000208688 Eucommia Species 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000000703 high-speed centrifugation Methods 0.000 claims description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims 4
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims 1
- 241000208689 Eucommia ulmoides Species 0.000 abstract description 18
- 239000002253 acid Substances 0.000 abstract description 12
- 239000000203 mixture Substances 0.000 abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract description 6
- 239000007791 liquid phase Substances 0.000 abstract description 5
- 239000003223 protective agent Substances 0.000 abstract description 4
- 241000196324 Embryophyta Species 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 10
- 230000035484 reaction time Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 206010067482 No adverse event Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- -1 gold ions Chemical class 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
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- 238000004544 sputter deposition Methods 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
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Abstract
本发明公开了一种利用杜仲水提取物绿色合成纳米金的方法，按照以下步骤进行：将杜仲洗净，60℃干燥，粉碎成粉末；称取20mg杜仲粉末于烧杯中，加入100mg水，置于恒温80℃水浴锅中30分钟，过滤；将所得溶液高速离心分离，得到杜仲水提取物；将氯金酸溶液与杜仲水提取物混合均匀，置于恒温水浴锅中反应，得到纳米金粒子。本发明的有益效果是提供一种温和条件下在液相中利用植物水提取物为还原剂和保护剂制备金纳米的方法,不会对环境和人体产生危害。
The invention discloses a method for synthesizing nano-gold greenly by using eucommia water extract, which is carried out according to the following steps: wash the eucommia ulmoides, dry at 60°C, and pulverize into powder; weigh 20 mg of eucommia ulmoides powder into a beaker, add 100 mg of water, place Put it in a water bath at a constant temperature of 80°C for 30 minutes, filter; centrifuge the obtained solution at high speed to obtain the water extract of Eucommia; mix the chloroauric acid solution and the water extract of Eucommia evenly, and place it in a constant temperature water bath for reaction to obtain gold nanoparticles . The beneficial effect of the present invention is to provide a method for preparing gold nanometers in a liquid phase using plant water extracts as a reducing agent and a protective agent under mild conditions, which will not cause harm to the environment and human body.
Description
技术领域technical field
本发明属于纳米材料制备技术领域，涉及一种利用杜仲水提取物绿色合成纳米金的方法。The invention belongs to the technical field of nanometer material preparation and relates to a method for green synthesis of nanometer gold by using Eucommia ulmoides water extract.
背景技术Background technique
现有化学法生产金纳米材料需要加入多种化学试剂，因此制备过程中对环境和人体产生危害，并且成本过高。The existing chemical method to produce gold nanomaterials needs to add a variety of chemical reagents, so the preparation process is harmful to the environment and human body, and the cost is too high.
纳米金及其复合物因其具有表面效应、量子尺寸效应、光学效应等性能使其在工业催化、生物医药、生物分析化学、食品安全快速检测、光学探针、传感器等众多方面有着广泛潜在的应用前景。目前纳米金的制备方法主要有物理气相蒸发凝集法、溅射法、激光高温燃烧法、机械研磨法、电化学法、液相化学还原法以及光诱导法等。其中，液相化学还原法，因其设备简单，操作方便，形貌和尺寸可控等特点成为低成本制备纳米金的主要方法。但是多数化学法需要引入较多化学试剂，存在生产成本较高，而且可能带来一定的环境污染等问题。Due to their surface effect, quantum size effect, optical effect and other properties, gold nanoparticles and their composites have extensive potential in many aspects such as industrial catalysis, biomedicine, bioanalytical chemistry, food safety rapid detection, optical probes, sensors, etc. Application prospect. At present, the preparation methods of nano gold mainly include physical vapor phase evaporation condensation method, sputtering method, laser high temperature combustion method, mechanical grinding method, electrochemical method, liquid phase chemical reduction method and light induction method. Among them, the liquid-phase chemical reduction method has become the main method for preparing nano-gold at low cost because of its simple equipment, convenient operation, and controllable shape and size. However, most chemical methods need to introduce more chemical reagents, which have high production costs and may cause certain environmental pollution and other problems.
本发明利用水热反应体系，仅利用自然界中可再生的杜仲水提取物在温和反应条件下还原金离子，未采用其他任何还原剂，制备出了形貌和尺寸可控的纳米金，该方法绿色节能环保，目前还没有关于这方面的相关报道。The present invention utilizes a hydrothermal reaction system to reduce gold ions under mild reaction conditions by using only renewable eucommia water extracts in nature, without using any other reducing agent, and prepares nano-gold with controllable morphology and size. The method Green energy saving and environmental protection, there is no relevant report on this aspect.
发明内容Contents of the invention
本发明的目的在于提供一种利用杜仲水提取物绿色合成纳米金的方法，解决了现有化学法生产金纳米材料需要加入多种化学试剂，因此制备过程中对环境和人体产生危害的问题。The purpose of the present invention is to provide a green method for synthesizing nano-gold by using eucommia water extract, which solves the problem that various chemical reagents need to be added in the production of gold nano-materials in the existing chemical method, so the problem of harm to the environment and human body during the preparation process is solved.
本发明所采用的技术方案是按照以下步骤进行：The technical scheme adopted in the present invention is to carry out according to the following steps:
步骤1：将杜仲洗净，60℃干燥，粉碎成粉末；Step 1: Wash Eucommia ulmoides, dry at 60°C, and pulverize into powder;
步骤2：称取20mg杜仲粉末于烧杯中，加入100mg水，置于恒温80℃水浴锅中30分钟，过滤；Step 2: Weigh 20mg of Eucommia powder into a beaker, add 100mg of water, place in a water bath at a constant temperature of 80°C for 30 minutes, and filter;
步骤3：将所得溶液高速离心分离，得到杜仲水提取物；Step 3: centrifuging the obtained solution at high speed to obtain the water extract of Eucommia ulmoides;
步骤4：将氯金酸溶液与杜仲水提取物混合均匀，置于恒温水浴锅中反应，得到纳米金粒子。Step 4: mix the chloroauric acid solution and the Eucommia ulmoides water extract evenly, place them in a constant temperature water bath for reaction, and obtain nano gold particles.
进一步，步骤3中高速离心12000r/min；所述步骤4中混合液中的氯金酸浓度为10-2-10-4mol/L。Further, high-speed centrifugation at 12000 r/min in step 3; the concentration of chloroauric acid in the mixed solution in step 4 is 10 -2 -10 -4 mol/L.
进一步，步骤4中恒温反应的温度为20～60℃，反应时间为5-30min。Further, the temperature of the constant temperature reaction in step 4 is 20-60° C., and the reaction time is 5-30 min.
进一步，步骤1中杜仲指杜仲皮和杜仲叶。Further, in step 1, Eucommia refers to Eucommia bark and Eucommia leaves.
本发明的有益效果是提供一种温和条件下在液相中利用植物水提取物为还原剂和保护剂制备金纳米的方法,不会对环境和人体产生危害。The beneficial effect of the present invention is to provide a method for preparing gold nanometers in a liquid phase using plant water extracts as a reducing agent and a protective agent under mild conditions, which will not cause harm to the environment and human body.
附图说明Description of drawings
图1是实施例1制得的纳米金及其紫外-可见光吸收光谱图；Fig. 1 is the nano-gold that embodiment 1 makes and ultraviolet-visible light absorption spectrogram thereof;
图2是实施例1制得的纳米金粒子透射电镜图片；Fig. 2 is the gold nanoparticle transmission electron microscope picture that embodiment 1 makes;
图3是实施例1制得的纳米金粒子的粒径分布图。3 is a particle size distribution diagram of the gold nanoparticles prepared in Example 1.
具体实施方式detailed description
下面结合附图和具体实施方式对本发明进行详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.
包括以下步骤：(1)杜仲水提取物的制备：将杜仲洗净，60℃干燥，粉碎成粉末。称取20mg杜仲粉末于烧杯中，加入100mg水，置于恒温80℃水浴锅中30分钟，过滤，可用滤纸，将所得溶液高速离心(12000r/min)分离，得到杜仲水提取物；(2)将氯金酸溶液与杜仲水提取物混合，混合液中的氯金酸浓度为10-2-10-4mol/L，混合均匀后，置于恒温水浴锅中，温度控制在20℃-60℃，反应时间控制在5-30min，可控制备，控制不同的温度和反应时间，改变氯金酸的浓度，可以获得不同粒径的纳米金粒子，可制得的纳米金的粒径为5-60nm。The method comprises the following steps: (1) preparation of the Eucommia water extract: washing the Eucommia ulmoides, drying at 60° C., and pulverizing into powder. Weigh 20 mg of Eucommia powder into a beaker, add 100 mg of water, place in a constant temperature 80°C water bath for 30 minutes, filter, and use filter paper to separate the obtained solution by high-speed centrifugation (12000r/min) to obtain Eucommia water extract; (2) Mix the chloroauric acid solution with the Eucommia ulmoides water extract, the concentration of chloroauric acid in the mixture is 10 -2 -10 -4 mol/L, after mixing evenly, put it in a constant temperature water bath, and the temperature is controlled at 20°C-60°C ℃, the reaction time is controlled at 5-30min, controllable preparation, controlling different temperatures and reaction times, changing the concentration of chloroauric acid, can obtain nano-gold particles with different particle sizes, and the particle size of the prepared nano-gold is 5 -60nm.
本发明解决的技术问题在于提供一种温和条件下在液相中利用植物水提取物为还原剂和保护剂制备金纳米的方法,该方法简单易行,条件温和,具有环境友好，产量大且结构明晰等特点。The technical problem solved by the present invention is to provide a method for preparing gold nanometers using plant water extracts as a reducing agent and a protective agent in a liquid phase under mild conditions. Features such as clear structure.
杜仲水提取物中多酚作为还原剂，不需要加入其它化学试剂，对环境和生物没有毒害作用,弥补了现有化学法生产金纳米材料的不足，杜仲胶作为保护剂，可以有效控制金纳米产物的形貌。本反应体系简单，配制方便,条件温和,如用于生产,可大大节约成本。The polyphenols in Eucommia ulmoides water extract are used as reducing agents, no need to add other chemical reagents, and have no toxic effects on the environment and organisms, making up for the shortcomings of existing chemical methods for producing gold nanomaterials. Eucommia gum, as a protective agent, can effectively control gold nanomaterials. The shape of the product. The reaction system is simple, easy to prepare, mild conditions, and can greatly save costs if used in production.
下面列举具体实施例对本发明进行说明：List specific embodiment below and illustrate the present invention:
实施例1：本实施例的一种利用杜仲水提取物绿色合成纳米金的方法，其具体步骤如下：Embodiment 1: A kind of method of utilizing Eucommia ulmoides water extract green synthesis nano-gold of the present embodiment, its specific steps are as follows:
步骤1：将杜仲洗净，60℃干燥，粉碎成粉末；Step 1: Wash Eucommia ulmoides, dry at 60°C, and pulverize into powder;
步骤2：称取20mg杜仲粉末于烧杯中，加入100mg水，置于恒温80℃水浴锅中30分钟，过滤；Step 2: Weigh 20mg of Eucommia powder into a beaker, add 100mg of water, place in a water bath at a constant temperature of 80°C for 30 minutes, and filter;
步骤3：将所得溶液高速离心12000r/min分离，得到杜仲水提取物；Step 3: centrifuging the obtained solution at a high speed of 12000r/min to obtain the Eucommia water extract;
步骤4：将氯金酸溶液与杜仲水提取物混合，混合液中的氯金酸浓度为10-3mol/L，混合均匀后，置于恒温水浴锅中，温度控制在40℃，反应时间控制在20min，制备的纳米金的粒径为10-40nm。Step 4: Mix the chloroauric acid solution with the Eucommia ulmoides water extract, the concentration of the chloroauric acid in the mixture is 10 -3 mol/L, after mixing evenly, put it in a constant temperature water bath, the temperature is controlled at 40°C, and the reaction time is Controlled at 20min, the particle size of the prepared nano gold is 10-40nm.
如图1所示为实施例1制得的纳米金及其紫外-可见光吸收光谱图.其最大吸收峰为521nm。As shown in Figure 1, it is the nano-gold prepared in Example 1 and its ultraviolet-visible light absorption spectrum. Its maximum absorption peak is 521nm.
如图2所示为实施例1制得的纳米金粒子透射电镜图片。在图2中，标尺为20nm。As shown in FIG. 2, it is a transmission electron microscope picture of the gold nanoparticles prepared in Example 1. In Figure 2, the scale bar is 20 nm.
如图3所示是实施例1制得的纳米金粒子的粒径分布图。As shown in FIG. 3 is the particle size distribution diagram of the gold nanoparticles prepared in Example 1.
实施例2：本实施例的一种利用杜仲水提取物绿色合成纳米金的方法，其具体步骤如下：Embodiment 2: A kind of method of utilizing Eucommia ulmoides water extract green synthesis nano-gold of the present embodiment, its specific steps are as follows:
步骤1：将杜仲洗净，60℃干燥，粉碎成粉末；Step 1: Wash Eucommia ulmoides, dry at 60°C, and pulverize into powder;
步骤2：称取20mg杜仲粉末于烧杯中，加入100mg水，置于恒温80℃水浴锅中30分钟，过滤；Step 2: Weigh 20mg of Eucommia powder into a beaker, add 100mg of water, place in a water bath at a constant temperature of 80°C for 30 minutes, and filter;
步骤3：将所得溶液高速离心12000r/min分离，得到杜仲水提取物；Step 3: centrifuging the obtained solution at a high speed of 12000r/min to obtain the Eucommia water extract;
步骤4：将氯金酸溶液与杜仲水提取物混合，混合液中的氯金酸浓度为10-4mol/L，混合均匀后，置于恒温水浴锅中，温度控制在20℃，反应时间控制在30min，制备的纳米金的粒径为5-20nm。Step 4: Mix the chloroauric acid solution with the Eucommia ulmoides water extract, the concentration of chloroauric acid in the mixture is 10 -4 mol/L, after mixing evenly, put it in a constant temperature water bath, the temperature is controlled at 20°C, and the reaction time is Controlled at 30min, the particle size of the prepared nano gold is 5-20nm.
实施例3：本实施例的一种利用杜仲水提取物绿色合成纳米金的方法，其具体步骤如下：Embodiment 3: A kind of method of utilizing Eucommia ulmoides water extract green synthesis nano-gold of the present embodiment, its specific steps are as follows:
步骤1：将杜仲洗净，60℃干燥，粉碎成粉末；Step 1: Wash Eucommia ulmoides, dry at 60°C, and pulverize into powder;
步骤2：称取20mg杜仲粉末于烧杯中，加入100mg水，置于恒温80℃水浴锅中30分钟，过滤；Step 2: Weigh 20mg of Eucommia powder into a beaker, add 100mg of water, place in a water bath at a constant temperature of 80°C for 30 minutes, and filter;
步骤3：将所得溶液高速离心12000r/min分离，得到杜仲水提取物；Step 3: centrifuging the obtained solution at a high speed of 12000r/min to obtain the Eucommia water extract;
步骤4：将氯金酸溶液与杜仲水提取物混合，混合液中的氯金酸浓度为10-2mol/L，混合均匀后，置于恒温水浴锅中，温度控制在60℃，反应时间控制在5min，制备的纳米金的粒径为30-60nm。Step 4: Mix the chloroauric acid solution with the Eucommia ulmoides water extract, the concentration of the chloroauric acid in the mixture is 10 -2 mol/L, after mixing evenly, place it in a constant temperature water bath, the temperature is controlled at 60°C, and the reaction time is Controlled within 5 minutes, the particle size of the prepared nano gold is 30-60nm.
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| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN103273079A (en) * | 2013-05-10 | 2013-09-04 | 安徽医科大学 | Gold nanoflower preparing method and application of gold nanoflowers |
| CN103302306A (en) * | 2013-06-19 | 2013-09-18 | 东南大学 | Method for reducing and preparing functionalized nano-silver based on polyphenol |
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