CN103785854A - Method for utilizing sodium alginate to compound nanogold in environment-friendly mode - Google Patents
Method for utilizing sodium alginate to compound nanogold in environment-friendly mode Download PDFInfo
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- CN103785854A CN103785854A CN201410038653.9A CN201410038653A CN103785854A CN 103785854 A CN103785854 A CN 103785854A CN 201410038653 A CN201410038653 A CN 201410038653A CN 103785854 A CN103785854 A CN 103785854A
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Abstract
The invention relates to a method utilizing sodium alginate to compound nanogold in an environment-friendly mode. The method comprises the steps of preparing chloroauric acid solution and sodium alginate solution, wherein the chloroauric acid solution and the sodium alginate solution are different in concentration; mixing the chloroauric acid solution and the sodium alginate solution, and obtaining pre-reaction drive body solution through magnetic stirring and even mixing, wherein the concentration of the chloroauric acid solution in the mixed solution is 10-2-10-4mol/L, and the mass percent concentration of the sodium alginate solution in the mixed solution is 0.5%-5%; placing the pre-reaction drive body solution obtained in the last step in a constant-temperature water bath pot, wherein the temperature is controlled at 20 DEG C-80 DEG C, the reaction time is controlled in 5-10 minutes, and the grain size of the controllable nanogold is 5-100nm. The method conforms to the advocated green chemistry requirement, uses reproducible biomass resource sodium alginate as reducing agents and stabilizers, does not need introduction of other chemical reagents, and is simple in technology, convenient to operate, and low in energy consumption. Moreover, the obtained nanogold is controllable in shape and size, even in dispersion, free of agglomeration and high in productivity.
Description
Technical field
The invention belongs to metal nano material preparing technical field, in particular, the present invention relates to a kind of method of utilizing the green synthesis of nano gold of sodium alginate.
Background technology
Nm of gold and compound thereof have the performances such as skin effect, quantum size effect, optical effect because of it makes it have extensively potential application prospect in Industrial Catalysis, biological medicine, bioanalysis chemistry, food security fast detecting, optical probe, sensor aspect numerous.The preparation method of nm of gold mainly contains physical vapor evaporation agglutination, sputtering method, laser high-temperature combustion method, mechanical milling method, electrochemical process, liquid phase chemical reduction method and photo-induction inducing defecation by enema and suppository etc. at present.Wherein, liquid phase chemical reduction method, because its equipment is simple, easy to operate, pattern and size are controlled etc., and feature becomes the main method that low cost is prepared nm of gold.But most chemical methods need to be introduced more chemical reagent, exist production cost higher, and may bring the problems such as certain environmental pollution.
Sodium alginate (sodium alginate, be called for short SA) be the class natural polysaccharide being present in brown algae, be polymerized by (1-4) glycosidic bond by beta-D-mannuronic acid (M) and α-L-guluronic acid (G), it is a kind of water soluble polymer, nontoxic, nonirritant, be renewable resource abundant in ocean, there is good biocompatibility, thereby to be recognized be one of the most rising biodegradable macromolecular material.In addition, spin in industry at seal, sodium alginate can be used as the dyeing auxiliaries of reactive dye, is best sizing agent and the printing paste of modern dyeing industry, has been widely used in the stamp of the various fabrics such as cotton, hair, silk, nylon.In food industry, as thickener, stabilizing agent, emulsifying agent, in medical industry, can make dental impression silica material, styptic sponge used, hemostatic gauze, hemostasis film, scalds gauze, spraying styptic etc.
Hydrothermal Synthesis is the emerging in recent years method of preparing nano particle.Hydro-thermal method, is called again hydrothermal method, refers in sealed pressure vessel, and take water as solvent, under the condition of high temperature (100 ℃ of >), high pressure (> 9.81MPa), the method for research, rapidoprint.The nano particle purity prepared by hydro-thermal method is high, narrow diameter distribution, good dispersion, reunion degree is low, crystal formation good, and composition is pure, and hydro-thermal method preparation process pollute little, cost is low, be applicable to industrialization produces.The patent No. is a kind of method that the patent of CN 10056388C discloses polyacrylic acid Synthesized by Hydrothermal Method gold, after being dissolved in to water, polyacrylic acid adds chlorauric acid solution, obtain reaction precursor liquid solution, gained precursor solution is poured in autoclave, at 100 ~ 200 ℃, react 40min ~ 4h, cooling rear centrifugal, washing, obtains nm of gold.But this patent is to react under HTHP, and utilize be that technical grade polyacrylic acid is reducing agent, increased industrialization cost, in addition, nano Au particle particle diameter prepared by this invention is larger, is 100 ~ 200nm, has limited the scope of nm of gold Follow-up Industryization application.
The present invention utilizes hydro-thermal reaction system, only utilize occurring in nature sodium alginate renewable and easy degraded under normal temperature or low temperature, to reduce gold ion, do not adopt other any reducing agents, prepare the controlled nm of gold of pattern and size, the method energy-saving and environment friendly, does not also have the relevant report about this respect at present.
Summary of the invention
The deficiency existing for overcoming prior art, for new way is opened up in the preparation of nm of gold, the object of the present invention is to provide the green synthetic method of a kind of nm of gold, using reproducible biomass resource sodium alginate as reducing agent and stabilizing agent, without introducing other chemical reagent, and technique is simple, easy to operate, energy consumption is low, the nano Au particle obtaining varies in color, size is controlled, be uniformly dispersed, nothing is reunited, productive rate is high.
For achieving the above object, the technical solution used in the present invention is as follows: a kind of method of utilizing the green synthesis of nano gold of sodium alginate, comprises the steps:
1) gold chloride (HAuCl of preparation variable concentrations
4) solution and sodium alginate (SA) solution;
2) chlorauric acid solution described in step 1) is mixed by a certain percentage with sodium alginate soln, magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in thermostat water bath, after isothermal reaction certain hour, collect products therefrom, the particle diameter of controlled preparation nm of gold is 5-100nm.
Preferably, step 2) gold chloride (HAuCl in described mixed liquor
4) molar concentration is 10
-2-10
-4mol/L.
Preferably, step 2) mass percent concentration of sodium alginate (SA) is 0.5%-5% in described mixed liquor.
Preferably, the temperature of isothermal reaction is 20 ~ 80 ℃ described in step 3), and the reaction time is 5-30min.
Preferably, described sodium alginate preferably extracts from marine alga or sea-tangle.
Compared with prior art, synthetic method of the present invention has the following advantages: the chemical reagent that (1) the present invention uses is few, sodium alginate had both played the effect of reducing agent in synthetic reaction, also play the effect of stabilizing agent and dispersant, without re-using other any reduction, stable, dispersion reagent, therefore the method industrialization cost is low; (2) sodium alginate is the resource of the renewable and easy degraded of occurring in nature, and whole synthetic reaction does not produce any pollution, meets " Green Chemistry " requirement of advocating; (3) the inventive method, without high-temperature high-pressure reaction kettle, can be reacted at ambient temperature, and low energy environmental protection can also be by regulating reaction temperature to carry out Reaction time shorten; (4) the inventive method technique is simple, easy to operate, and the particle diameter of nm of gold is controlled, and the GRR of product is high, is conducive to expanding production; (5) the inventive method is controlled the color of nm of gold by controlling the particle diameter of synthetic nm of gold, and the nanogold particle particle diameter of preparation is little, and good dispersion and narrow diameter distribution, reunion degree are low, good stability, is conducive to Follow-up Industryization application.
Accompanying drawing explanation
Fig. 1 is nm of gold and the uv-visible absorption spectroscopy figure thereof that embodiment 1 makes.In Fig. 1, abscissa is wavelength (nm), and ordinate is absorbance, and maximum absorption band is 521nm.
Fig. 2 is nm of gold and the uv-visible absorption spectroscopy figure thereof that embodiment 3 makes.In Fig. 2, abscissa is wavelength (nm), and ordinate is absorbance, and maximum absorption band is 532nm.
Fig. 3 is nm of gold and the uv-visible absorption spectroscopy figure thereof that embodiment 5 makes.In Fig. 3, abscissa is wavelength (nm), and ordinate is absorbance, and maximum absorption band is 544nm.
Fig. 4 is the nano Au particle transmission electron microscope picture that embodiment 1 makes.In Fig. 4, scale is 20nm.
The specific embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described in further detail, but protection scope of the present invention is not limited to this:
Embodiment 1
A kind of method of utilizing the green synthesis of nano gold of sodium alginate of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of preparation variable concentrations;
2) chlorauric acid solution is mixed with sodium alginate soln, the gold chloride concentration in mixed liquor is 10
-4mol/L, the mass percent concentration of sodium alginate is 0.5%, magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 20 ℃ of thermostat water baths and react 30min, collect products therefrom, the nm of gold obtaining for pink, particle size range is distributed between 5 ~ 20nm.
Embodiment 2
A kind of method of utilizing the green synthesis of nano gold of sodium alginate of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of preparation variable concentrations;
2) chlorauric acid solution is mixed with sodium alginate soln, the gold chloride concentration in mixed liquor is 10
-3mol/L, the mass percent concentration of sodium alginate is 5%, magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 60 ℃ of thermostat water baths and react 20min, collect products therefrom, the nm of gold obtaining for pink, particle size range is distributed between 5 ~ 20nm.
Embodiment 3
A kind of method of utilizing the green synthesis of nano gold of sodium alginate of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of preparation variable concentrations;
2) chlorauric acid solution is mixed with sodium alginate soln, the gold chloride concentration in mixed liquor is 10
-3mol/L, the mass percent concentration of sodium alginate is 1%, magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 60 ℃ of thermostat water baths and react 20min, collect products therefrom, the nm of gold obtaining is aubergine, particle size range is distributed between 20 ~ 60nm.
Embodiment 4
A kind of method of utilizing the green synthesis of nano gold of sodium alginate of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of preparation variable concentrations;
2) chlorauric acid solution is mixed with sodium alginate soln, the gold chloride concentration in mixed liquor is 10
-2mol/L, the mass percent concentration of sodium alginate is 5%, magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 80 ℃ of thermostat water baths and react 10min, collect products therefrom, the nm of gold obtaining is aubergine, particle size range is distributed between 20 ~ 60nm.
Embodiment 5
A kind of method of utilizing the green synthesis of nano gold of sodium alginate of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of preparation variable concentrations;
2) chlorauric acid solution is mixed with sodium alginate soln, the gold chloride concentration in mixed liquor is 10
-2mol/L, the mass percent concentration of sodium alginate is 2.5%, magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 40 ℃ of thermostat water baths and react 10min, collect products therefrom, the nm of gold obtaining is purple, particle size range is distributed between 60 ~ 100nm.
Embodiment 6
A kind of method of utilizing the green synthesis of nano gold of sodium alginate of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of preparation variable concentrations;
2) chlorauric acid solution is mixed with sodium alginate soln, the gold chloride concentration in mixed liquor is 10
-3mol/L, the mass percent concentration of sodium alginate is 0.5%, magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 80 ℃ of thermostat water baths and react 5min, collect products therefrom, the nm of gold obtaining is purple, particle size range is distributed between 60 ~ 100nm.
Claims (5)
1. a method of utilizing the green synthesis of nano gold of sodium alginate, comprises the steps:
1) gold chloride (HAuCl of preparation variable concentrations
4) solution and sodium alginate (SA) solution;
2) chlorauric acid solution described in step 1) is mixed by a certain percentage with sodium alginate soln, magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in thermostat water bath, after isothermal reaction certain hour, collect products therefrom, the particle diameter of controlled preparation nm of gold is 5-100nm.
2. a kind of utilize the green synthesis of nano gold of sodium alginate according to described in claim 1 method, is characterized in that: described step 2) gold chloride (HAuCl in mixed liquor
4) concentration is 10
-2-10
-4mol/L.
3. a kind of utilize the green synthesis of nano gold of sodium alginate according to described in claim 1 or 2 method, is characterized in that: described step 2) mass percent concentration of sodium alginate (SA) is 0.5%-5% in mixed liquor.
4. according to a kind of method of utilizing the green synthesis of nano gold of sodium alginate described in claim 1 or 2, it is characterized in that: in described step 3), the temperature of isothermal reaction is 20 ~ 80 ℃, the reaction time is 5-30min.
5. a kind of utilize the green synthesis of nano gold of sodium alginate according to described in claim 4 method, is characterized in that: described step 2) in the sodium alginate that adds be preferably from marine alga or sea-tangle and extract.
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Cited By (5)
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|---|---|---|---|---|
| CN104858448A (en) * | 2015-05-11 | 2015-08-26 | 华南理工大学 | Green synthesis method for nanogold in lignin solution |
| CN105618786A (en) * | 2016-01-22 | 2016-06-01 | 青岛大学 | Preparation method for cage-shaped nanometer gold-silver alloy suitable for being used as organic dye catalyst |
| CN108746658A (en) * | 2018-05-24 | 2018-11-06 | 西安理工大学 | A kind of preparation method of the algal polysaccharides nanogold particle with antibacterial activity |
| CN110055619A (en) * | 2019-05-07 | 2019-07-26 | 湖北大学 | The preparation method and application of nano combined fluorescent fiber |
| CN111000797A (en) * | 2020-01-06 | 2020-04-14 | 湖北大学 | Preparation method and application of gold nanoparticle in-situ growth type sodium alginate nanogel |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108746658A (en) * | 2018-05-24 | 2018-11-06 | 西安理工大学 | A kind of preparation method of the algal polysaccharides nanogold particle with antibacterial activity |
| CN110055619A (en) * | 2019-05-07 | 2019-07-26 | 湖北大学 | The preparation method and application of nano combined fluorescent fiber |
| CN110055619B (en) * | 2019-05-07 | 2021-09-28 | 湖北大学 | Preparation method and application of nano composite fluorescent fiber |
| CN111000797A (en) * | 2020-01-06 | 2020-04-14 | 湖北大学 | Preparation method and application of gold nanoparticle in-situ growth type sodium alginate nanogel |
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