CN104014813A - Nanogold solution preparing method based on sepharose gel - Google Patents
Nanogold solution preparing method based on sepharose gel Download PDFInfo
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Abstract
The invention discloses a nanogold solution preparing method based on sepharose gel. The method comprises the following steps that firstly, the sepharose gel is added into water and heated to obtain a clarification sepharose solution; secondly, a chloroauric acid solution is added into the sepharose solution and stirred evenly at the constant temperature, and the mixed solution is placed at the normal temperature to obtain the nanogold sepharose gel; thirdly, the nanogold sepharose gel obtained in the second step is dried in a freezing mode, the gel is removed, and the nanogold solution is obtained after washing. The nanogold solution is formed by evenly scattering nanogold particles in water, the sizes of the nanogold particles are even, and the average particle diameter ranges from 1 nm to 10 nm. The preparing technology is simple and practical, the applied reducing agent is the sepharose gel which is common and non-toxic, the sizes of the obtained nanogold particles are even and controllable, the grain diameter is small, and the nanogold particles are not prone to being aggregated. The nanogold solution preparing method has very important actual application value in the nanogold preparing field.
Description
Technical field
The present invention relates to a kind of preparation method of the nano-Au solution based on Ago-Gel.
Background technology
Nm of gold, owing to possessing many special natures such as quantum size effect, macro quanta tunnel effect and skin effect, is widely used in the fields such as electrochemical probe, optical probe, DNA detection, biochemical analysis, catalyst, colloidal sol, plant protection and Raman scattering.
Small size nm of gold has higher specific area and larger charge density, and catalytic activity is higher, and actual application prospect is larger than large-sized nm of gold.At present, the condition harshness of synthetic small size nm of gold, complex steps, agents useful for same is more.Huang Dehuans etc. [CN 1663714A] are taking hydrazine hydrate as reducing agent, and prepare nano-Au solution taking polyvinylpyrrolidone and lauryl sodium sulfate as additive; Dong Shouan etc. [CN 1554503A] are taking acetone as reducing agent and add the protective agents such as polyvinyl alcohol and prepare nano Au particle.In the preparation method of report, except reducing agent, often need to introduce other additive at present, as dispersant, stabilizing agent, protective agent or flocculant etc., and may use larger, the with serious pollution organic solvent of toxicity, be unfavorable for carrying out extensive use.
Therefore, further find technique simple, the preparation method of raw materials used common nontoxic small size nm of gold, has important practical significance.
Summary of the invention
The object of the invention is to, provide a kind of technique simple, raw materials used environment amenable nm of gold preparation method, the nanogold particle size that adopts described method to make is controlled, and particle diameter is very little, and is difficult for reuniting.
For achieving the above object, the technical solution used in the present invention is:
A preparation method for nano-Au solution based on Ago-Gel, comprises the following steps:
(1) in water, add Ago-Gel, be placed in water bath and heat, must clarify uniform agarose solution;
(2) in agarose solution, add chlorauric acid solution, constant temperature stirs, in this process, the gold ion in gold chloride is reduced into gold particle by the hydroxyl that agarose is rich in, mixed solution normal temperature is placed, gold particle is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, washs to obtain described nano-Au solution.
Water in described step (1) is ultra-pure water.
In described agarose solution, add after chlorauric acid solution, the concentration of agarose in the mixed solution obtaining is 0.08～0.15g/mL.The concentration of described chlorauric acid solution is 0.02～2.5mM.
Described agarose solution and chlorauric acid solution volume ratio are (1～9): 1.
Described constant temperature whipping temp is 80～100 DEG C, and constant temperature mixing time is 3～5min, and normal temperature temperature is 20～30 DEG C, and normal temperature standing time is 1～15d.
Described washing step is with ultra-pure water washing 3 times.
Described nano-Au solution is dispersed in water and is formed by nanogold particle, nanogold particle size uniform, and particle diameter is very little, and average grain diameter is 1～10nm.
The size of nanogold particle is controlled, realizes with the internal cavities size of controlling gel by the concentration that regulates agarose.
Compared with prior art, the invention has the beneficial effects as follows:
(1) preparation technology of the present invention is simple, and agarose had not only been made reducing agent but also used as stabilizers in preparation process, without introducing other reducing agents or additive, safety non-toxic.
(2) Ago-Gel is better to the compatibility of nanogold particle, has solved the chemical reagent problem poor to nanogold particle compatibility in other preparation methods.
(3) internal cavities of Ago-Gel can be controlled the size of nanogold particle and prevent that nano Au particle from reuniting.
(4) in preparation process, adopt cryodesiccated method to remove gel, remove gel without heating or calcining.In the product that freeze drying obtains, impurity content is few, washs and can effectively remove impurity, without increasing the complicated deimpurity step of going with ultra-pure water.
(5) size uniform of nanogold particle in the nano-Au solution making, particle diameter is very little, reaches several nanometers, good stability, difficult reunion.
(6) nano-Au solution making is taking water as solvent, and source is simple, cheap, nontoxic, makes the nano-Au solution obtaining use safety, convenient storage.
Brief description of the drawings
Below in conjunction with accompanying drawing, the invention will be further described, in accompanying drawing:
Fig. 1 is the uv-visible absorption spectra figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope picture figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 1.
Fig. 3 is the particle size distribution figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 1.
Fig. 4 is the uv-visible absorption spectra figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 2.
Fig. 5 is the transmission electron microscope picture figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 2.
Fig. 6 is the particle size distribution figure of nanogold particle in the nano-Au solution making in the embodiment of the present invention 2.
Detailed description of the invention
For making object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The material, the reagent etc. that in following embodiment, use if no special instructions, obtain in all can be from commercial channels.
In following embodiment, detect sample characteristic absworption peak by ultraviolet-visible spectrophotometer (TU-1901 dual-beam ultraviolet-uisible spectrophotometer).
In following embodiment by transmission electricity electron microscope (JEM-2100) observing samples pattern.
In following embodiment, pass through particle size analyzer (dynamic light scattering/potentiometer PSS Nicomp380) observing samples size distribution.
Embodiment 1:
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 1.5g Ago-Gel and add in 9mL ultra-pure water, mixed liquor is placed in to water bath and heats, stir until mixed liquor becomes clear, obtain uniform agarose solution;
(2) in the agarose solution of preparation, adding 1mL concentration is the chlorauric acid solution of 2.5mM, and at 100 DEG C, constant temperature stirs 5min, and the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process.Mixed solution is placed in to 25 DEG C and places 15d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water, obtains described nano-Au solution.
Particle in the product that the present embodiment obtains is nanogold particle through ultraviolet-visible spectrophotometer Analysis deterrmination, and its uv-visible absorption spectra figure is shown in Fig. 1.Transmission electron microscope results shows, the particle obtaining in product is spherical, and its SEM figure is shown in Fig. 2.Adopt particle size analyzer to analyze the size distribution state of particle in product, result shows, particle size is mainly distributed in 2～5nm, and average grain diameter is 3nm, and its particle size distribution figure is shown in Fig. 3.
Embodiment 2:
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 1.5g Ago-Gel and add in 5mL ultra-pure water, mixed liquor is placed in to water bath and heats, stir until mixed liquor becomes clear, obtain uniform agarose solution;
(2) in the agarose solution of preparation, adding 5mL concentration is the chlorauric acid solution of 0.02mM, and at 90 DEG C, constant temperature stirs 4min, and the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process.Mixed solution is placed in to 20 DEG C and places 15d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water, obtains described nano-Au solution.
Particle in the product that the present embodiment obtains is nanogold particle by ultraviolet-visible spectrophotometer Analysis deterrmination, and its uv-visible absorption spectra figure is shown in Fig. 4.Transmission electron microscope results shows, the particle obtaining in product is spherical, and its SEM figure is shown in Fig. 5.Adopt particle size analyzer to analyze the size distribution state of particle in product, result shows, particle size is mainly distributed in 2～5nm, and average grain diameter is 2.9nm, and its particle size distribution figure is shown in Fig. 6.
Embodiment 3:
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 0.8g Ago-Gel and add in 8.5mL ultra-pure water, mixed liquor is placed in to water bath and heats, and stirring is until mixed liquor becomes clear, obtains uniform agarose solution;
(2) in the agarose solution of preparation, adding 1.5mL concentration is the chlorauric acid solution of 2.5mM, and at 80 DEG C, constant temperature stirs 5min, and the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process.Mixed solution is placed in to 30 DEG C and places 8d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water, obtains described nano-Au solution.
In the nano-Au solution making, nanogold particle size is mainly distributed in 7～10nm, and average grain diameter is 8.3nm.
Embodiment 4
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 1.0g Ago-Gel and add in 9mL ultra-pure water, mixed liquor is placed in to water bath and heats, and stirring is until mixed liquor becomes clear, obtains uniform agarose solution;
(2) in the agarose solution of preparation, adding 1mL concentration is the chlorauric acid solution of 2.5mM, and at 100 DEG C, constant temperature stirs 3min, and the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process.Mixed solution is placed in to 25 DEG C and places 15d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step (2) being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water, obtains described nano-Au solution.
In the nano-Au solution making, nanogold particle size is mainly distributed in 2～7nm, and average grain diameter is 5.2nm.
Embodiment 5:
A preparation method for nano-Au solution based on Ago-Gel, comprises following steps:
(1) take 1.5g Ago-Gel and add in 9mL ultra-pure water, mixed liquor is placed in to water bath and heats, and stirring is until mixed liquor becomes clear, obtains uniform agarose solution;
(2) in the agarose solution of preparation, adding 1mL concentration is the chlorauric acid solution of 2.5mM, and at 100 DEG C, constant temperature stirs 5min, and the gold ion reduction in gold chloride is obtained gold particle by the hydroxyl that agarose is rich in this process.Mixed solution is placed in to 30 DEG C and places 1d, the gold particle obtaining is embedded in the internal cavities of the Ago-Gel forming gradually, obtains nm of gold gel;
(3) nm of gold gel step 2 being obtained carries out freeze drying and removes gel, then washs 3 times with ultra-pure water, obtains described nano-Au solution.
In the nano-Au solution making, nanogold particle size is mainly distributed in 0.2～1.4nm, and average grain diameter is 1nm.
Without prejudice to essence of the present invention and spirit in the situation that, those of ordinary skill in the art may make according to the present invention various changes or distortion, but these corresponding changes or distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (8)
1. a preparation method for the nano-Au solution based on Ago-Gel, comprises the following steps:
(1) in water, add Ago-Gel, heat to obtain the uniform agarose solution of clarification;
(2) in agarose solution, add chlorauric acid solution, constant temperature stirs, and obtains reaction solution, and reaction solution normal temperature is placed, and obtains nm of gold gel;
(3) the nm of gold gel obtaining is carried out to freeze drying and remove gel, after washing, obtain described nano-Au solution.
2. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that, described water is ultra-pure water.
3. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that, described agarose solution and chlorauric acid solution volume ratio are (1～9): 1.
4. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that, the concentration of described chlorauric acid solution is 0.02～2.5mM.
5. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that, in described agarose solution, adds after chlorauric acid solution, and the concentration of agarose in gained mixed solution is 0.08～0.15g/mL.
6. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, it is characterized in that, described constant temperature whipping temp is 80～100 DEG C, and constant temperature mixing time is 3～5min, normal temperature temperature is 20～30 DEG C, and normal temperature standing time is 1～15d.
7. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, is characterized in that, described washing step is with ultra-pure water washing 3 times.
8. the preparation method of a kind of nano-Au solution based on Ago-Gel according to claim 1, it is characterized in that, the nano-Au solution that described method makes is dispersed in water and is formed by nanogold particle, and nanogold particle size uniform is controlled, and average grain diameter is 1～10nm.
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Cited By (5)
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| CN106180753A (en) * | 2016-08-05 | 2016-12-07 | 武汉工程大学 | The preparation method of a kind of nano silver particles and thus obtained nano silver particles |
| CN106180752A (en) * | 2016-08-05 | 2016-12-07 | 武汉工程大学 | A kind of preparation method of dendroid silver |
| CN106346018A (en) * | 2016-09-21 | 2017-01-25 | 武汉工程大学 | Preparation method and application of agarose/nano-silver composite gel |
| CN106645135A (en) * | 2017-02-27 | 2017-05-10 | 南京七彩生物科技有限公司 | Preparation method and sensing application of gold nanorod thin film |
| CN112059200A (en) * | 2020-08-21 | 2020-12-11 | 武汉纺织大学 | Silver nanoparticles and macro-controllable preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106180753A (en) * | 2016-08-05 | 2016-12-07 | 武汉工程大学 | The preparation method of a kind of nano silver particles and thus obtained nano silver particles |
| CN106180752A (en) * | 2016-08-05 | 2016-12-07 | 武汉工程大学 | A kind of preparation method of dendroid silver |
| CN106180752B (en) * | 2016-08-05 | 2018-05-08 | 武汉工程大学 | A kind of preparation method of dendroid silver |
| CN106346018A (en) * | 2016-09-21 | 2017-01-25 | 武汉工程大学 | Preparation method and application of agarose/nano-silver composite gel |
| CN106645135A (en) * | 2017-02-27 | 2017-05-10 | 南京七彩生物科技有限公司 | Preparation method and sensing application of gold nanorod thin film |
| CN106645135B (en) * | 2017-02-27 | 2019-12-10 | 南京七彩生物科技有限公司 | preparation method of gold nanorod film and sensing application thereof |
| CN112059200A (en) * | 2020-08-21 | 2020-12-11 | 武汉纺织大学 | Silver nanoparticles and macro-controllable preparation method thereof |
| CN112059200B (en) * | 2020-08-21 | 2023-04-18 | 武汉纺织大学 | Silver nanoparticles and macro-controllable preparation method thereof |
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