CN104014813B - A kind of preparation method of the nano-Au solution based on Ago-Gel - Google Patents
A kind of preparation method of the nano-Au solution based on Ago-Gel Download PDFInfo
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- 238000001069 Raman spectroscopy Methods 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
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Abstract
本发明公开了一种基于琼脂糖凝胶的纳米金溶液的制备方法，包括以下步骤：(1)在水中加入琼脂糖凝胶，加热得澄清均匀的琼脂糖溶液；(2)在琼脂糖溶液中加入氯金酸溶液，恒温搅拌均匀，将混合溶液常温放置，得纳米金凝胶；(3)将步骤(2)得到的纳米金凝胶进行冷冻干燥去除凝胶，洗涤后得纳米金溶液。所述纳米金溶液由纳米金颗粒均匀分散在水中形成，所述纳米金颗粒尺寸均匀，平均粒径为1～10nm。本发明涉及的制备工艺简单易行，使用的还原剂为琼脂糖凝胶，常见无毒，制得的纳米金颗粒尺寸均匀可控，粒径小，且不易发生团聚。本方法在纳米金的制备领域中具有重要的实际应用价值。
The invention discloses a preparation method of nano-gold solution based on agarose gel, which comprises the following steps: (1) adding agarose gel into water, and heating to obtain a clear and uniform agarose solution; (2) adding the agarose solution to the agarose solution Add chloroauric acid solution to the mixture, stir at a constant temperature, place the mixed solution at room temperature to obtain a nano-gold gel; (3) freeze-dry the nano-gold gel obtained in step (2) to remove the gel, and obtain a nano-gold solution after washing . The nano-gold solution is formed by uniformly dispersing the nano-gold particles in water, the size of the nano-gold particles is uniform, and the average particle diameter is 1-10 nm. The preparation process involved in the present invention is simple and easy, and the reducing agent used is agarose gel, which is common and non-toxic, and the prepared nano-gold particles have a uniform and controllable size, a small particle size, and are not prone to agglomeration. The method has important practical application value in the field of preparation of nano gold.
Description
技术领域technical field
本发明涉及一种基于琼脂糖凝胶的纳米金溶液的制备方法。The invention relates to a preparation method of agarose gel-based nano gold solution.
背景技术Background technique
纳米金由于具备量子尺寸效应、宏观量子隧道效应和表面效应等诸多特殊性质，广泛应用于电化学探针、光学探针、DNA检测、生化分析、催化剂、溶胶、植物保护和拉曼散射等领域。Gold nanoparticles are widely used in electrochemical probes, optical probes, DNA detection, biochemical analysis, catalysts, sols, plant protection, and Raman scattering due to their special properties such as quantum size effects, macroscopic quantum tunneling effects, and surface effects. .
小尺寸纳米金具有较高的比表面积以及较大的电荷密度，催化活性较高，实际应用前景比大尺寸的纳米金大。目前，合成小尺寸纳米金的条件苛刻，步骤繁琐，所用试剂较多。黄德欢等[CN1663714A]以水合肼为还原剂，并以聚乙烯吡咯烷酮和十二烷基硫酸钠为添加剂制备得到纳米金溶液；董守安等[CN1554503A]以丙酮为还原剂并添加聚乙烯醇等保护剂制备得到纳米金粒子。目前报道的制备法中除还原剂外往往需要引入其它添加剂，如分散剂，稳定剂、保护剂或絮凝剂等，并可能使用毒性较大、污染严重的有机溶剂，不利于进行广泛应用。Small-sized gold nanoparticles have higher specific surface area and higher charge density, higher catalytic activity, and have greater practical application prospects than large-sized gold nanoparticles. At present, the conditions for synthesizing small-sized gold nanoparticles are harsh, the steps are cumbersome, and many reagents are used. [CN1663714A] such as Huang Dehuan take hydrazine hydrate as reducing agent, and prepare nano-gold solution with polyvinylpyrrolidone and sodium lauryl sulfate as additives; Preparation of gold nanoparticles. In addition to the reducing agent, other additives, such as dispersant, stabilizer, protective agent or flocculant, etc. need to be introduced in the preparation methods reported so far, and organic solvents with high toxicity and serious pollution may be used, which is not conducive to wide application.
因此，进一步寻找工艺简单，所用原料常见无毒的小尺寸纳米金的制备方法，具有重要的实际意义。Therefore, it is of great practical significance to further find a preparation method of small-sized gold nanoparticles with simple process and common non-toxic raw materials.
发明内容Contents of the invention
本发明的目的在于，提供一种工艺简单，所用原料对环境友好的纳米金制备方法，采用所述方法制得的纳米金颗粒尺寸可控，粒径很小，且不易发生团聚。The purpose of the present invention is to provide a method for preparing nano-gold with simple process and environmentally friendly raw materials. The size of nano-gold particles prepared by the method is controllable, the particle size is small, and it is not easy to agglomerate.
为实现上述目的，本发明采用的技术方案为：To achieve the above object, the technical solution adopted in the present invention is:
一种基于琼脂糖凝胶的纳米金溶液的制备方法，包括以下步骤：A kind of preparation method based on the nano gold solution of agarose gel, comprises the following steps:
(1)在水中加入琼脂糖凝胶，置于水浴箱中加热，得澄清均匀的琼脂糖溶液；(1) Add agarose gel into water, place in a water bath and heat to obtain a clear and uniform agarose solution;
(2)在琼脂糖溶液中加入氯金酸溶液，恒温搅拌均匀，在此过程中，琼脂糖富含的羟基将氯金酸中的金离子还原成金粒子，将混合溶液常温放置，金粒子镶嵌在逐渐形成的琼脂糖凝胶的内部空腔中，得纳米金凝胶；(2) Add chloroauric acid solution to the agarose solution, and stir evenly at a constant temperature. During this process, the rich hydroxyl groups in the agarose reduce the gold ions in the chloroauric acid to gold particles, and the mixed solution is placed at room temperature, and the gold particles are inlaid In the inner cavity of the gradually formed agarose gel, a nano-gold gel is obtained;
(3)将步骤(2)得到的纳米金凝胶进行冷冻干燥去除凝胶，洗涤得所述纳米金溶液。(3) freeze-drying the nano-gold gel obtained in step (2) to remove the gel, and washing to obtain the nano-gold solution.
所述步骤(1)中的水为超纯水。The water in the step (1) is ultrapure water.
所述琼脂糖溶液中加入氯金酸溶液后，琼脂糖在得到的混合溶液中的浓度为0.08～0.15g/mL。所述氯金酸溶液的浓度为0.02～2.5mM。After the chloroauric acid solution is added to the agarose solution, the concentration of the agarose in the obtained mixed solution is 0.08-0.15 g/mL. The concentration of the chloroauric acid solution is 0.02-2.5mM.
所述琼脂糖溶液与氯金酸溶液体积比为(1～9):1。The volume ratio of the agarose solution to the chloroauric acid solution is (1-9):1.
所述恒温搅拌温度为80～100℃，恒温搅拌时间为3～5min，常温温度为20～30℃，常温放置时间为1～15d。The constant temperature stirring temperature is 80-100° C., the constant temperature stirring time is 3-5 minutes, the normal temperature is 20-30° C., and the normal temperature storage time is 1-15 days.
所述的洗涤步骤是用超纯水洗涤3次。The washing step is to wash 3 times with ultrapure water.
所述的纳米金溶液由纳米金颗粒均匀分散在水中形成，纳米金颗粒尺寸均匀，粒径很小，平均粒径为1～10nm。The nano-gold solution is formed by uniformly dispersing the nano-gold particles in water, and the nano-gold particles are uniform in size and small in size, with an average particle size of 1-10 nm.
纳米金颗粒的尺寸可控，通过调节琼脂糖的浓度以控制凝胶的内部空腔大小来实现。The size of gold nanoparticles can be controlled by adjusting the concentration of agarose to control the size of the inner cavity of the gel.
与现有技术相比，本发明的有益效果是：Compared with prior art, the beneficial effect of the present invention is:
(1)本发明制备工艺简单，琼脂糖在制备过程中既作还原剂又作稳定剂，无需引入其他还原剂或添加剂，安全无毒。(1) The preparation process of the present invention is simple, and the agarose is used as both a reducing agent and a stabilizing agent in the preparation process, without introducing other reducing agents or additives, and is safe and non-toxic.
(2)琼脂糖凝胶对纳米金颗粒的相容性较好，解决了其他制备方法中化学试剂对纳米金颗粒相容性差的问题。(2) The compatibility of the agarose gel to the gold nanoparticles is better, which solves the problem of poor compatibility of chemical reagents to the gold nanoparticles in other preparation methods.
(3)琼脂糖凝胶的内部空腔可控制纳米金颗粒的尺寸并防止纳米金粒子发生团聚。(3) The inner cavity of the agarose gel can control the size of the gold nanoparticles and prevent the aggregation of the gold nanoparticles.
(4)制备过程中，采用冷冻干燥的方法去除凝胶，无需进行加热或煅烧来去除凝胶。冷冻干燥得到的产物中杂质含量少，用超纯水进行洗涤即可有效去除杂质，无需增加复杂的去除杂质的步骤。(4) During the preparation process, the gel is removed by freeze-drying, without heating or calcining to remove the gel. The product obtained by freeze-drying has less impurity content, and the impurity can be effectively removed by washing with ultrapure water, without adding complicated steps for removing impurities.
(5)制得的纳米金溶液中纳米金颗粒的尺寸均匀，粒径很小，达几个纳米，稳定性好，不易发生团聚。(5) The size of the nano-gold particles in the prepared nano-gold solution is uniform, the particle size is very small, up to several nanometers, the stability is good, and it is difficult to agglomerate.
(6)制得的纳米金溶液以水为溶剂，来源简单、廉价、无毒，使得到的纳米金溶液使用安全、存储方便。(6) The prepared nano-gold solution uses water as a solvent, and the source is simple, cheap and non-toxic, so that the obtained nano-gold solution is safe to use and convenient to store.
附图说明Description of drawings
下面结合附图对本发明作进一步说明，附图中：The present invention will be further described below in conjunction with accompanying drawing, in the accompanying drawing:
图1为本发明实施例1中制得的纳米金溶液中纳米金颗粒的紫外-可见吸收光谱图。FIG. 1 is an ultraviolet-visible absorption spectrum diagram of nano-gold particles in a nano-gold solution prepared in Example 1 of the present invention.
图2为本发明实施例1中制得的纳米金溶液中纳米金颗粒的透射电镜图图。Fig. 2 is a transmission electron micrograph of gold nanoparticles in a gold nano solution prepared in Example 1 of the present invention.
图3为本发明实施例1中制得的纳米金溶液中纳米金颗粒的粒度分布图。FIG. 3 is a particle size distribution diagram of gold nanoparticles in the gold nanoparticles solution prepared in Example 1 of the present invention.
图4为本发明实施例2中制得的纳米金溶液中纳米金颗粒的紫外-可见吸收光谱图。Fig. 4 is an ultraviolet-visible absorption spectrum diagram of the nano-gold particles in the nano-gold solution prepared in Example 2 of the present invention.
图5为本发明实施例2中制得的纳米金溶液中纳米金颗粒的透射电镜图图。Fig. 5 is a transmission electron micrograph of gold nanoparticles in a gold nano solution prepared in Example 2 of the present invention.
图6为本发明实施例2中制得的纳米金溶液中纳米金颗粒的粒度分布图。FIG. 6 is a particle size distribution diagram of gold nanoparticles in a gold nano solution prepared in Example 2 of the present invention.
具体实施方式detailed description
为使本发明的目的、技术方案及优点更加清楚明白，下面结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.
下述实施例中所使用的材料、试剂等如无特别说明，均可从商业途径中得到。The materials and reagents used in the following examples can be obtained from commercial sources unless otherwise specified.
下述实施例中通过紫外-可见分光光度计(TU-1901双光束紫外可见分光光度计)检测样品特征吸收峰。In the following examples, the characteristic absorption peaks of samples were detected by a UV-Vis spectrophotometer (TU-1901 double-beam UV-Vis spectrophotometer).
下述实施例中通过透射电电子显微镜(JEM-2100)观测样品形貌。In the following examples, the morphology of the samples was observed by a transmission electron microscope (JEM-2100).
下述实施例中通过粒度仪(动态光散射仪/电位仪PSSNicomp380)观测样品粒度分布。In the following examples, the particle size distribution of samples was observed by a particle size analyzer (dynamic light scattering meter/potentiometer PSSNicomp380).
实施例1：Example 1:
一种基于琼脂糖凝胶的纳米金溶液的制备方法，包含以下步骤：A kind of preparation method of the nano gold solution based on agarose gel, comprises the following steps:
(1)称取1.5g琼脂糖凝胶加入9mL超纯水中，将混合液置于水浴箱中加热，搅拌直至混合液变澄清透明，得均匀的琼脂糖溶液；(1) Weigh 1.5 g of agarose gel and add it to 9 mL of ultrapure water, heat the mixed solution in a water bath, and stir until the mixed solution becomes clear and transparent to obtain a uniform agarose solution;
(2)在配制的琼脂糖溶液中加入1mL浓度为2.5mM的氯金酸溶液，在100℃下恒温搅拌5min，在此过程中琼脂糖富含的羟基将氯金酸中的金离子还原得到金粒子。将混合溶液置于25℃放置15d，得到的金粒子镶嵌在逐渐形成的琼脂糖凝胶的内部空腔中，得纳米金凝胶；(2) Add 1mL of chloroauric acid solution with a concentration of 2.5mM to the prepared agarose solution, and stir at a constant temperature at 100°C for 5min. During this process, the rich hydroxyl groups in the agarose reduce the gold ions in the chloroauric acid to obtain gold particles. Place the mixed solution at 25°C for 15 days, and the obtained gold particles are embedded in the inner cavity of the gradually formed agarose gel to obtain nano-gold gel;
(3)将步骤(2)得到的纳米金凝胶进行冷冻干燥去除凝胶，再用超纯水进行洗涤3次，得所述纳米金溶液。(3) Freeze-dry the nano-gold gel obtained in step (2) to remove the gel, and then wash with ultrapure water for 3 times to obtain the nano-gold solution.
本实施例所得到的产物中的颗粒经紫外-可见分光光度计分析确定为纳米金颗粒，其紫外-可见吸收光谱图见图1。透射电镜结果表明，得到产物中的颗粒呈球状，其SEM图见图2。采用粒度仪对产物中颗粒的粒度分布状态进行分析，结果表明，颗粒尺寸主要分布在2～5nm，平均粒径为3nm，其粒度分布图见图3。The particles in the product obtained in this example were determined to be gold nanoparticles by ultraviolet-visible spectrophotometer analysis, and its ultraviolet-visible absorption spectrum is shown in FIG. 1 . The results of transmission electron microscopy showed that the particles in the obtained product were spherical, and the SEM image thereof was shown in FIG. 2 . The particle size distribution of the particles in the product was analyzed by a particle size analyzer. The results showed that the particle size was mainly distributed in the range of 2 to 5 nm, with an average particle size of 3 nm. The particle size distribution diagram is shown in Figure 3.
实施例2：Example 2:
一种基于琼脂糖凝胶的纳米金溶液的制备方法，包含以下步骤：A kind of preparation method of the nano gold solution based on agarose gel, comprises the following steps:
(1)称取1.5g琼脂糖凝胶加入5mL超纯水中，将混合液置于水浴箱中加热，搅拌直至混合液变澄清透明，得均匀的琼脂糖溶液；(1) Weigh 1.5 g of agarose gel and add it to 5 mL of ultrapure water, heat the mixed solution in a water bath, and stir until the mixed solution becomes clear and transparent to obtain a uniform agarose solution;
(2)在配制的琼脂糖溶液中加入5mL浓度为0.02mM的氯金酸溶液，在90℃下恒温搅拌4min，在此过程中琼脂糖富含的羟基将氯金酸中的金离子还原得到金粒子。将混合溶液置于20℃放置15d，得到的金粒子镶嵌在逐渐形成的琼脂糖凝胶的内部空腔中，得纳米金凝胶；(2) Add 5mL of chloroauric acid solution with a concentration of 0.02mM to the prepared agarose solution, and stir at a constant temperature of 90°C for 4 minutes. During this process, the rich hydroxyl groups in the agarose reduce the gold ions in the chloroauric acid to obtain gold particles. Place the mixed solution at 20°C for 15 days, and the obtained gold particles are embedded in the inner cavity of the gradually formed agarose gel to obtain nano-gold gel;
(3)将步骤(2)得到的纳米金凝胶进行冷冻干燥去除凝胶，再用超纯水进行洗涤3次，得所述纳米金溶液。(3) Freeze-dry the nano-gold gel obtained in step (2) to remove the gel, and then wash with ultrapure water for 3 times to obtain the nano-gold solution.
本实施例所得到的产物中的颗粒通过紫外-可见分光光度计分析确定为纳米金颗粒，其紫外-可见吸收光谱图见图4。透射电镜结果表明，得到产物中的颗粒呈球状，其SEM图见图5。采用粒度仪对产物中颗粒的粒度分布状态进行分析，结果表明，颗粒尺寸主要分布在2～5nm，平均粒径为2.9nm，其粒度分布图见图6。The particles in the product obtained in this example were determined to be gold nanoparticles by ultraviolet-visible spectrophotometer analysis, and its ultraviolet-visible absorption spectrum is shown in FIG. 4 . The results of transmission electron microscopy showed that the particles in the obtained product were spherical, and the SEM image thereof is shown in FIG. 5 . The particle size distribution of the particles in the product was analyzed by a particle size analyzer. The results showed that the particle size was mainly distributed in the range of 2-5nm, with an average particle size of 2.9nm. The particle size distribution diagram is shown in Figure 6.
实施例3：Example 3:
一种基于琼脂糖凝胶的纳米金溶液的制备方法，包含以下步骤：A kind of preparation method of the nano gold solution based on agarose gel, comprises the following steps:
(1)称取0.8g琼脂糖凝胶加入8.5mL超纯水中，将混合液置于水浴箱中加热，并搅拌直至混合液变澄清透明，得均匀的琼脂糖溶液；(1) Weigh 0.8 g of agarose gel and add it to 8.5 mL of ultrapure water, heat the mixed solution in a water bath, and stir until the mixed solution becomes clear and transparent to obtain a uniform agarose solution;
(2)在配制的琼脂糖溶液中加入1.5mL浓度为2.5mM的氯金酸溶液，在80℃下恒温搅拌5min，在此过程中琼脂糖富含的羟基将氯金酸中的金离子还原得到金粒子。将混合溶液置于30℃放置8d，得到的金粒子镶嵌在逐渐形成的琼脂糖凝胶的内部空腔中，得纳米金凝胶；(2) Add 1.5 mL of chloroauric acid solution with a concentration of 2.5mM to the prepared agarose solution, and stir at a constant temperature of 80°C for 5 minutes. During this process, the rich hydroxyl groups in the agarose will reduce the gold ions in the chloroauric acid get gold particles. Place the mixed solution at 30°C for 8 days, and the obtained gold particles are embedded in the inner cavity of the gradually formed agarose gel to obtain nano-gold gel;
(3)将步骤(2)得到的纳米金凝胶进行冷冻干燥去除凝胶，再用超纯水进行洗涤3次，得所述纳米金溶液。(3) Freeze-dry the nano-gold gel obtained in step (2) to remove the gel, and then wash with ultrapure water for 3 times to obtain the nano-gold solution.
制得的纳米金溶液中，纳米金颗粒尺寸主要分布在7～10nm，平均粒径为8.3nm。In the prepared nano-gold solution, the size of the nano-gold particles is mainly distributed in the range of 7-10 nm, and the average particle size is 8.3 nm.
实施例4Example 4
一种基于琼脂糖凝胶的纳米金溶液的制备方法，包含以下步骤：A kind of preparation method of the nano gold solution based on agarose gel, comprises the following steps:
(1)称取1.0g琼脂糖凝胶加入9mL超纯水中，将混合液置于水浴箱中加热，并搅拌直至混合液变澄清透明，得均匀的琼脂糖溶液；(1) Weigh 1.0 g of agarose gel and add it to 9 mL of ultrapure water, heat the mixed solution in a water bath, and stir until the mixed solution becomes clear and transparent to obtain a uniform agarose solution;
(2)在配制的琼脂糖溶液中加入1mL浓度为2.5mM的氯金酸溶液，在100℃下恒温搅拌3min，在此过程中琼脂糖富含的羟基将氯金酸中的金离子还原得到金粒子。将混合溶液置于25℃放置15d，得到的金粒子镶嵌在逐渐形成的琼脂糖凝胶的内部空腔中，得纳米金凝胶；(2) Add 1mL of chloroauric acid solution with a concentration of 2.5mM to the prepared agarose solution, and stir at a constant temperature at 100°C for 3 minutes. During this process, the rich hydroxyl groups in the agarose reduce the gold ions in the chloroauric acid to obtain gold particles. Place the mixed solution at 25°C for 15 days, and the obtained gold particles are embedded in the inner cavity of the gradually formed agarose gel to obtain nano-gold gel;
(3)将步骤(2)得到的纳米金凝胶进行冷冻干燥去除凝胶，再用超纯水进行洗涤3次，得所述纳米金溶液。(3) Freeze-dry the nano-gold gel obtained in step (2) to remove the gel, and then wash with ultrapure water for 3 times to obtain the nano-gold solution.
制得的纳米金溶液中，纳米金颗粒尺寸主要分布在2～7nm，平均粒径为5.2nm。In the prepared nano-gold solution, the size of the nano-gold particles is mainly distributed in the range of 2-7 nm, and the average particle size is 5.2 nm.
实施例5：Example 5:
一种基于琼脂糖凝胶的纳米金溶液的制备方法，包含以下步骤：A kind of preparation method of the nano gold solution based on agarose gel, comprises the following steps:
(1)称取1.5g琼脂糖凝胶加入9mL超纯水中，将混合液置于水浴箱中加热，并搅拌直至混合液变澄清透明，得均匀的琼脂糖溶液；(1) Weigh 1.5 g of agarose gel and add it to 9 mL of ultrapure water, heat the mixed solution in a water bath, and stir until the mixed solution becomes clear and transparent to obtain a uniform agarose solution;
(2)在配制的琼脂糖溶液中加入1mL浓度为2.5mM的氯金酸溶液，在100℃下恒温搅拌5min，在此过程中琼脂糖富含的羟基将氯金酸中的金离子还原得到金粒子。将混合溶液置于30℃放置1d，得到的金粒子镶嵌在逐渐形成的琼脂糖凝胶的内部空腔中，得纳米金凝胶；(2) Add 1mL of chloroauric acid solution with a concentration of 2.5mM to the prepared agarose solution, and stir at a constant temperature at 100°C for 5min. During this process, the rich hydroxyl groups in the agarose reduce the gold ions in the chloroauric acid to obtain gold particles. Place the mixed solution at 30°C for 1 day, and the obtained gold particles are embedded in the inner cavity of the gradually formed agarose gel to obtain nano-gold gel;
(3)将步骤2得到的纳米金凝胶进行冷冻干燥去除凝胶，再用超纯水进行洗涤3次，得所述纳米金溶液。(3) Freeze-dry the nano-gold gel obtained in step 2 to remove the gel, and then wash with ultrapure water for 3 times to obtain the nano-gold solution.
制得的纳米金溶液中，纳米金颗粒尺寸主要分布在0.2～1.4nm，平均粒径为1nm。In the prepared nano-gold solution, the size of the nano-gold particles is mainly distributed in the range of 0.2-1.4 nm, and the average particle diameter is 1 nm.
在不违背本发明实质及精神的情况下，熟悉本领域的技术人员可能根据本发明做出各种各样的改变或变形，但这些相应的改变或变形都应属于本发明所附的权利要求的保护范围。Without departing from the essence and spirit of the present invention, those skilled in the art may make various changes or deformations according to the present invention, but these corresponding changes or deformations should belong to the appended claims of the present invention scope of protection.
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