CN103785854B - A kind of method utilizing sodium alginate green syt nm of gold - Google Patents
A kind of method utilizing sodium alginate green syt nm of gold Download PDFInfo
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- CN103785854B CN103785854B CN201410038653.9A CN201410038653A CN103785854B CN 103785854 B CN103785854 B CN 103785854B CN 201410038653 A CN201410038653 A CN 201410038653A CN 103785854 B CN103785854 B CN 103785854B
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- sodium alginate
- gold
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Abstract
The present invention relates to a kind of method utilizing sodium alginate green syt nm of gold, described method comprises the steps: 1) the preparation chlorauric acid solution of variable concentrations and sodium alginate soln; 2) mixed with sodium alginate soln by chlorauric acid solution, the gold chloride concentration in mixed liquor is 10
-2-10
-4mol/L, the mass percent concentration of sodium alginate is 0.5%-5%, and 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, temperature controls at 20 DEG C-80 DEG C, and the reaction time controls at 5-30min, and the particle diameter of controlled synthesis nm of gold is 5-100nm.The inventive method meets " Green Chemistry " requirement advocated, using reproducible biomass resource sodium alginate as reducing agent and stabilizing agent, without the need to introducing other chemical reagent, and technique is simple, easy to operate, energy consumption is low, the nm of gold pattern obtained and size controlled, be uniformly dispersed, soilless sticking, productive rate be high.
Description
Technical field
The invention belongs to metal nano material preparing technical field, in particular, the present invention relates to a kind of method utilizing sodium alginate green syt nm of gold.
Background technology
Nm of gold and compound thereof have because of it that performances such as skin effect, quantum size effect, optical effect make that it detects fast in Industrial Catalysis, biological medicine, bioanalytical chemistry, food security, optical probe, sensor numerous in have extensively potential application prospect.The preparation method of current nm of gold mainly contains physical vapor evaporation agglutination, sputtering method, laser high-temperature combustion method, mechanical milling method, electrochemical process, solution phase chemical reduction and light inducible etc.Wherein, solution phase chemical reduction, because its equipment is simple, easy to operate, pattern and feature the becomes main method that low cost prepares nm of gold such as size is controlled.But most chemical method needs to introduce more chemical reagent, there is production cost higher, and may bring the problems such as certain environmental pollution.
Sodium alginate (sodiumalginate, be called for short SA) be the class natural polysaccharide be 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, have excellent biocompatibility, being thus recognized is one of the most rising biodegradable macromolecular material.In addition, spin in industry in print, sodium alginate can be used as the dyeing auxiliaries of reactive dye, is sizing agent and the printing paste of the best of modern dyeing industry, has been widely used in the stamp of the various fabrics such as cotton, hair, silk, nylon.In the 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 method preparing nano particle emerging in recent years.Hydro-thermal method, is also called hydrothermal method, refers in sealed pressure vessel, take water as solvent, under the condition of high temperature (> 100 DEG C), high pressure (> 9.81MPa), and 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 patent discloses polyacrylic acid Synthesized by Hydrothermal Method gold of CN10056388C, chlorauric acid solution is added after polyacrylic acid being dissolved in water, obtain reaction precursor liquid solution, gained precursor solution is poured in autoclave, 40min ~ 4h is reacted at 100 ~ 200 DEG C, centrifugal after cooling, washing, obtains nm of gold.But this patent is reacted at high temperature under high pressure, and what utilize be technical grade polyacrylic acid is reducing agent, adds industrialization cost, in addition, nano Au particle particle diameter prepared by this invention is comparatively large, is 100 ~ 200nm, limits the scope of nm of gold Follow-up Industryization application.
The present invention utilizes hydro-thermal reaction system, only utilize occurring in nature renewable and the sodium alginate of easily degraded reduces gold ion under normal temperature or low temperature, do not adopt other any reducing agents, pattern and the controlled nm of gold of size are prepared, the method energy-saving and environment friendly, at present also not about the relevant report of this respect.
Summary of the invention
For overcoming the deficiency that prior art exists, for new way is opened up in the preparation of nm of gold, the object of the present invention is to provide a kind of nm of gold green syt method, using reproducible biomass resource sodium alginate as reducing agent and stabilizing agent, without the need to introducing other chemical reagent, and technique is simple, easy to operate, energy consumption is low, the nano Au particle obtained varies in color, size is controlled, be uniformly dispersed, soilless sticking, productive rate are high.
For achieving the above object, the technical solution used in the present invention is as follows: a kind of method utilizing sodium alginate green syt nm of gold, comprises the steps:
1) gold chloride (HAuCl of variable concentrations is prepared
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, mix, obtain 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 synthesis 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 described in step 3) is 20 ~ 80 DEG C, 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 served the effect of reducing agent in synthetic reaction, also serve the effect of stabilizing agent and dispersant, without the need to re-using other any reduction, stable, dispersing agent, 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 advocated; (3) the inventive method is without the need to high-temperature high-pressure reaction kettle, can react at ambient temperature, low-energy environment-friendly, can also carry out Reaction time shorten by regulating reaction temperature; (4) the inventive method technique is simple, easy to operate, the size tunable of nm of gold, and the GRR of product is high, is conducive to expanding production; (5) the inventive method controls the color of nm of gold by the particle diameter of nm of gold controlling synthesis, and the nanogold particle particle diameter of preparation is little, 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 the obtained nm of gold of embodiment 1 and uv-visible absorption spectroscopy figure thereof.In FIG, abscissa is wavelength (nm), and ordinate is absorbance, and maximum absorption band is 521nm.
Fig. 2 is the obtained nm of gold of embodiment 3 and uv-visible absorption spectroscopy figure thereof.In fig. 2, abscissa is wavelength (nm), and ordinate is absorbance, and maximum absorption band is 532nm.
Fig. 3 is the obtained nm of gold of embodiment 5 and uv-visible absorption spectroscopy figure thereof.In figure 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 obtains.In the diagram, scale is 20nm.
Detailed description of the invention
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 thereto:
Embodiment 1
A kind of method utilizing sodium alginate green syt nm of gold of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of variable concentrations is prepared;
2) mixed with sodium alginate soln by chlorauric acid solution, the gold chloride concentration in mixed liquor is 10
-4mol/L, the mass percent concentration of sodium alginate is 0.5%, and magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 20 DEG C of thermostat water baths and react 30min, collect products therefrom, the nm of gold obtained for pink, particle size range is distributed between 5 ~ 20nm.
Embodiment 2
A kind of method utilizing sodium alginate green syt nm of gold of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of variable concentrations is prepared;
2) mixed with sodium alginate soln by chlorauric acid solution, the gold chloride concentration in mixed liquor is 10
-3mol/L, the mass percent concentration of sodium alginate is 5%, and magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 60 DEG C of thermostat water baths and react 20min, collect products therefrom, the nm of gold obtained for pink, particle size range is distributed between 5 ~ 20nm.
Embodiment 3
A kind of method utilizing sodium alginate green syt nm of gold of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of variable concentrations is prepared;
2) mixed with sodium alginate soln by chlorauric acid solution, the gold chloride concentration in mixed liquor is 10
-3mol/L, the mass percent concentration of sodium alginate is 1%, and magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 60 DEG C of thermostat water baths and react 20min, collect products therefrom, the nm of gold obtained is aubergine, and particle size range is distributed between 20 ~ 60nm.
Embodiment 4
A kind of method utilizing sodium alginate green syt nm of gold of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of variable concentrations is prepared;
2) mixed with sodium alginate soln by chlorauric acid solution, the gold chloride concentration in mixed liquor is 10
-2mol/L, the mass percent concentration of sodium alginate is 5%, and magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 80 DEG C of thermostat water baths and react 10min, collect products therefrom, the nm of gold obtained is aubergine, and particle size range is distributed between 20 ~ 60nm.
Embodiment 5
A kind of method utilizing sodium alginate green syt nm of gold of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of variable concentrations is prepared;
2) mixed with sodium alginate soln by chlorauric acid solution, the gold chloride concentration in mixed liquor is 10
-2mol/L, the mass percent concentration of sodium alginate is 2.5%, and magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 40 DEG C of thermostat water baths and react 10min, collect products therefrom, the nm of gold obtained is purple, and particle size range is distributed between 60 ~ 100nm.
Embodiment 6
A kind of method utilizing sodium alginate green syt nm of gold of the present embodiment, its concrete steps are as follows:
1) chlorauric acid solution and the sodium alginate soln of variable concentrations is prepared;
2) mixed with sodium alginate soln by chlorauric acid solution, the gold chloride concentration in mixed liquor is 10
-3mol/L, the mass percent concentration of sodium alginate is 0.5%, and magnetic agitation, mixes, and obtains reaction precursor liquid solution;
3) by step 2) described in reaction precursor liquid solution, be placed in 80 DEG C of thermostat water baths and react 5min, collect products therefrom, the nm of gold obtained is purple, and particle size range is distributed between 60 ~ 100nm.
Claims (3)
1. utilize a method for sodium alginate green syt nm of gold, comprise the steps:
1) chlorauric acid solution and the sodium alginate soln of variable concentrations is prepared;
2) mixed by a certain percentage with sodium alginate soln by the chlorauric acid solution described in step 1), magnetic agitation, mix, obtain reaction precursor liquid solution, in wherein said reaction precursor liquid solution, the mass percent concentration of sodium alginate is 0.5%-5%;
3) by step 2) described in reaction precursor liquid solution, be placed in thermostat water bath, under the temperature conditions of 20-80 DEG C after isothermal reaction 5-30min, collect products therefrom, preparation nm of gold particle diameter be 5-100nm.
2. a kind of method utilizing sodium alginate green syt nm of gold according to claim 1, is characterized in that: described step 2) concentration of gold chloride is 10 in mixed liquor
-2-10
-4mol/L.
3., according to a kind of method utilizing sodium alginate green syt nm of gold described in claim 1, it is characterized in that:
Described step 2) in the sodium alginate that adds preferably extract from marine alga or sea-tangle.
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| CN104858448B (en) * | 2015-05-11 | 2017-10-20 | 华南理工大学 | The green synthesis method of nanogold in lignin liquor |
| CN105618786B (en) * | 2016-01-22 | 2017-12-05 | 青岛大学 | A kind of preparation method for the cage-shaped nano electrum for being suitable for use as organic dyestuff 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 |
| 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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| JP2005060815A (en) * | 2003-08-12 | 2005-03-10 | Otsuka Yakuhin Kogyo Kk | Production method of gold colloid |
| CN100553834C (en) * | 2007-03-17 | 2009-10-28 | 广西师范大学 | The easy quick method for preparing green silver nano-particle |
| CN100563881C (en) * | 2008-01-23 | 2009-12-02 | 厦门大学 | A kind of method of polyacrylic acid hydro-thermal synthesis of nano gold |
| CN101368194B (en) * | 2008-10-10 | 2010-09-15 | 厦门大学 | Microorganism reduction preparation method for triangular gold nano-slice |
| CN101433959A (en) * | 2008-12-22 | 2009-05-20 | 中国科学院长春应用化学研究所 | Method for preparing hollow nano gold powder material |
| CN101776608B (en) * | 2009-10-29 | 2011-07-20 | 广西师范大学 | Method for measuring trace Hg2+ by using aptamer modified nano gold rhenium catalysis-tellurium particle resonance scattering spectrum |
| TWI436950B (en) * | 2010-09-09 | 2014-05-11 | Taiwan Hopax Chems Mfg Co Ltd | Chitosan modified nano-gold particle and method for preparing the same |
| CN103157413B (en) * | 2013-03-28 | 2014-05-07 | 湖南农业大学 | Method for preparing sodium alginate microcapsule-supported nanoscale zero-valent iron particles |
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