CN102211204B - Method for preparing nano-gold - Google Patents
Method for preparing nano-gold Download PDFInfo
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- CN102211204B CN102211204B CN 201110116420 CN201110116420A CN102211204B CN 102211204 B CN102211204 B CN 102211204B CN 201110116420 CN201110116420 CN 201110116420 CN 201110116420 A CN201110116420 A CN 201110116420A CN 102211204 B CN102211204 B CN 102211204B
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Abstract
The invention provides a method for preparing nano-gold, which comprises the following step of: reacting chloroauric acid with a primary-amine-containing compound and an aldehyde-containing compound to obtain the nano-gold. The invention provides a method for preparing the nano-gold through reductive amination reaction. The aldehyde-containing compound and the primary-amine-containing compound which participate in the reductive amination reaction cannot reduce the chloroauric acid into the nano-gold under the reaction conditions, the reductive amination reaction makes a reaction system have the capability of reducing the chloroauric acid, and is accompanied with the generation of the nano-gold, other reducing agents and a stabilizer for the nano-gold are not required to be added, and the reduction speed and the generation speed of the nano-gold can be regulated by controlling the conditions of the reductive amination reaction. The method for preparing the nano-gold is simple, the speed is controllable, and a new way is provided for preparing the nano-gold.
Description
Technical field
The present invention relates to a kind of preparation method of nm of gold, belong to the metal nanoparticle preparation field.
Background technology
Nm of gold receives very big concern in recent years owing to have unique physics and chemistry character, is widely used in the fields such as optics, catalysis, biological medicine.With regard to the preparation of nm of gold, adopt the aqueous phase chemical reduction method more, namely under the condition that stabilizing agent exists, by reducing agent gold chloride is reduced to nm of gold.The reducing agent that utilizes comprises inorganic reducing agent and organic reducing agent, and inorganic reducing agent commonly used is the strong sodium borohydride of reproducibility, need to add in addition stabilizing agent, and reduction rate is fast but uncontrollable; Organic reducing agent commonly used is citric acid, and it plays stabilizing agent simultaneously, but at high temperature could reduce, and reduction rate also is difficult to control.Although based on multiple reducing agent, developed nm of gold preparation method miscellaneous at present, aspect the speed of growth of reduction and nm of gold, also lacked Modulatory character.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nm of gold, the reaction system of impelling of reductive amination process possesses the ability of reduction gold chloride, the generation of nm of gold is followed in reductive amination process, by control reductive amination process condition, can realize the regulation and control to reduction and nm of gold formation speed.
The preparation method of nm of gold provided by the invention comprises the steps: that gold chloride reacts and namely gets described nm of gold with containing the primary amine groups compound and contain aldehyde compound.
Among the above-mentioned preparation method, the temperature of described reaction can be 0 ℃-45 ℃, specifically can be 10 ℃, 25 ℃, 40 ℃ or 45 ℃; The time of described reaction can be 0.5 hour-24 hours, specifically can be 0.5 hour, 1 hour, 3 hours or 4 hours.
Among the above-mentioned preparation method, the described primary amine groups compound that contains can be many primary amine groups biomolecule and/or many primary amine groups polymer, and described many primary amine groups biomolecule specifically can be in chitosan oligosaccharide, shitosan, the peptide and protein at least a; Described many primary amine groups polymer specifically can be in polyethylene imine based (PEI) and the daiamid (PAMAM) at least a.
Among the above-mentioned preparation method, the described molecular weight that contains the primary amine groups compound can be 1kDa-300kDa, specifically can be 5kDa-66kDa, 5kDa, 45kDa or 66kDa.
Among the above-mentioned preparation method, the described aldehyde compound that contains can be water-soluble aldehyde, specifically can be in formaldehyde, acetaldehyde, propionic aldehyde, glyoxal, MDA, butanedial and the glutaraldehyde at least a.
Among the above-mentioned preparation method, described gold chloride, the ratio of quality and the number of copies that contains the primary amine groups compound and contain aldehyde compound can be 1: (10-30): (1-10), specifically can be 1: 20: (4-8), 1: 20: 4 or 1: 20: 8.
Among the above-mentioned preparation method, the solvent of described reaction can be water.
Among the above-mentioned preparation method, described reaction can be carried out under static condition or stirring.
The invention provides the nm of gold of said method preparation, the particle diameter of described nm of gold is 6nm-35nm, specifically can be 7nm-20nm, 6nm-25nm, 11nm-33nm or 12nm-35nm.
The invention provides a kind of method of utilizing reductive amination process to prepare nm of gold.Under described reaction condition, what participate in reductive amination process contains aldehyde compound and contains the primary amine groups compound that all can not to reduce gold chloride be nm of gold, the reaction system of impelling of reductive amination process possesses the ability of reduction gold chloride, the generation of nm of gold is followed in reductive amination process, need not to add the stabilizing agent of other reducing agent and nm of gold, by control reductive amination process condition, can realize the regulation and control to reduction and nm of gold formation speed.The preparation method of the nm of gold that the present invention proposes is simple, speed is controlled, for the preparation of nm of gold provides new approach.
Description of drawings
Fig. 1 is the ultraviolet-visible extinction spectrum figure of the nm of gold of embodiment 1 preparation.
Fig. 2 is the transmission electron microscope photo of the nm of gold of embodiment 1 preparation.
Fig. 3 is the ultraviolet-visible extinction spectrum figure of the nm of gold of embodiment 2 preparations.
Fig. 4 is the transmission electron microscope photo of the nm of gold of embodiment 2 preparations.
The specific embodiment
Employed experimental technique is conventional method if no special instructions among the following embodiment.
Used material, reagent etc. if no special instructions, all can obtain from commercial channels among the following embodiment.
The model of used ultraviolet-visible spectrophotometer is TU-1900 type dual-beam ultraviolet-uisible spectrophotometer among the following embodiment.
The model of used transmission electron microscope is JEM-1011 type transmission electricity electron microscope among the following embodiment.
The preparation of embodiment 1, nm of gold
Under 10 ℃, 1mL glutaraldehyde water solution (containing the 20mg glutaraldehyde) is joined in the acetic acid solution (contain the 100mg shitosan, the mean molecule quantity of shitosan is 45kDa) of 10mL shitosan, behind the reaction 1h, add 0.5mLHAuCl
4The aqueous solution (contains 5mg HAuCl
4), then the ratio of quality and the number of copies of gold chloride, shitosan and glutaraldehyde is 1: 20: 4, stirs 4h, obtains red nano-Au solution, records absorption maximum at the 526nm place, as shown in Figure 1 at ultraviolet-visible spectrophotometer; The treated nm of gold that namely gets, its transmission electron microscope photo as shown in Figure 2, its particle diameter is 7nm-20nm.
The preparation of embodiment 2, nm of gold
Under 45 ℃, with 0.5mL HAuCl
4The aqueous solution (contains 5mg HAuCl
4) acetic acid solution that joins the 10mL shitosan (contains the 100mg shitosan, the molecular weight of shitosan is 45kDa) in, then add 1mL glutaraldehyde water solution (containing the 20mg glutaraldehyde), then the ratio of quality and the number of copies of gold chloride, shitosan and glutaraldehyde is 1: 20: 4, stir 0.5h, obtain red nano-Au solution, record absorption maximum at the 532nm place, as shown in Figure 3 at ultraviolet-visible spectrophotometer; The treated nm of gold that namely gets, its transmission electron microscope photo as shown in Figure 4, its particle diameter is 6nm-25nm.
The preparation of embodiment 3, nm of gold
Under 25 ℃, with 0.5mL HAuCl
4The aqueous solution (contains 5mg HAuCl
4) join the 10mL Bovine Serum Albumin in Aqueous Solution and (contain the 100mg bovine serum albumin(BSA), the molecular weight of bovine serum albumin(BSA) is 66kDa) in, then add 1mL glutaraldehyde water solution (containing the 20mg glutaraldehyde), then the ratio of quality and the number of copies of gold chloride, bovine serum albumin(BSA) and glutaraldehyde is 1: 20: 4, stir 3h, obtain red nano-Au solution, record absorption maximum at the 536nm place at ultraviolet-visible spectrophotometer, the nm of gold particle diameter is 11nm-33nm.
The preparation of embodiment 4, nm of gold
Under 40 ℃, the positive propionic aldehyde aqueous solution of 1mL (containing the positive propionic aldehyde of 40mg) is joined in the 10mL chitosan oligosaccharide aqueous solution (contain the 100mg chitosan oligosaccharide, the mean molecule quantity of chitosan oligosaccharide is 5kDa), then add 0.5mL HAuCl
4The aqueous solution (contains 5mg HAuCl
4), then the ratio of quality and the number of copies of gold chloride, chitosan oligosaccharide and positive propionic aldehyde is 1: 20: 8, stirs 3h, obtains red nano-Au solution, records absorption maximum at the 534nm place at ultraviolet-visible spectrophotometer, the nm of gold particle diameter is 12nm-35nm.
In the situation that does not deviate from spirit of the present invention and essence thereof, those of ordinary skill in the art may make according to the present invention various corresponding changes and distortion, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (6)
1. the preparation method of a nm of gold, may further comprise the steps: gold chloride and many primary amine groups biomolecule and/or many primary amine groups polymer and water-soluble aldehyde react and namely get described nm of gold;
The ratio of quality and the number of copies of described gold chloride, many primary amine groups biomolecule and/or many primary amine groups polymer and water-soluble aldehyde is 1:(10-30): (1-10).
2. method according to claim 1, it is characterized in that: the temperature of described reaction is 0 ℃-45 ℃; The time of described reaction is 0.5 hour-24 hours.
3. method according to claim 1 and 2 is characterized in that: described many primary amine groups biomolecule and/or many primary amine groups polymer are at least a in chitosan oligosaccharide, shitosan, polypeptide, protein, the polyethylene imine based and daiamid.
4. method according to claim 3, it is characterized in that: the molecular weight of described many primary amine groups biomolecule and/or many primary amine groups polymer is 1kDa-300kDa.
5. method according to claim 1 and 2, it is characterized in that: described water-soluble aldehyde is at least a in formaldehyde, acetaldehyde, propionic aldehyde, glyoxal, MDA, butanedial and the glutaraldehyde.
6. method according to claim 1, it is characterized in that: the solvent of described reaction is water.
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| CN 201110116420 CN102211204B (en) | 2011-05-06 | 2011-05-06 | Method for preparing nano-gold |
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| CN 201110116420 CN102211204B (en) | 2011-05-06 | 2011-05-06 | Method for preparing nano-gold |
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| CN102211204B true CN102211204B (en) | 2013-03-27 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102581300A (en) * | 2012-03-23 | 2012-07-18 | 武汉大学 | Gold nano particle preparation method |
| CN103143722B (en) * | 2013-03-21 | 2014-12-17 | 江西农业大学 | Method for preparing multipod-like gold nanoparticles by chemical method |
| CN104353845B (en) * | 2014-11-20 | 2016-08-24 | 首都师范大学 | The method of different-shape nano gold grain prepared by the tryptophan of pentanedial decoration |
| CN115592124B (en) * | 2022-09-14 | 2023-12-15 | 苏州大学 | Nanometer colloidal gold and preparation method thereof |
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| US5248772A (en) * | 1992-01-29 | 1993-09-28 | Coulter Corporation | Formation of colloidal metal dispersions using aminodextrans as reductants and protective agents |
| CN100484631C (en) * | 2005-05-24 | 2009-05-06 | 南京大学 | Preparation method of catalyst with metal nanoparticles loaded on carbon nano hollow balls |
| US7291292B2 (en) * | 2005-08-26 | 2007-11-06 | E.I. Du Pont De Nemours And Company | Preparation of silver particles using thermomorphic polymers |
| DE102006055763B4 (en) * | 2006-11-21 | 2011-06-22 | Militz, Detlef, 15366 | Process for metallizing polyester, metallized polyester and its use |
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| CN101934379B (en) * | 2010-10-13 | 2012-02-22 | 中南大学 | Method for preparing gold nanoparticles |
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