CN101934379A - Method for preparing gold nanoparticles - Google Patents
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- CN101934379A CN101934379A CN 201010505779 CN201010505779A CN101934379A CN 101934379 A CN101934379 A CN 101934379A CN 201010505779 CN201010505779 CN 201010505779 CN 201010505779 A CN201010505779 A CN 201010505779A CN 101934379 A CN101934379 A CN 101934379A
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Abstract
The invention discloses a method for preparing gold nanoparticles by using compound high-molecular protective agents under the action of microwaves, comprising the following steps of: mixing polyvinylpyrrolidone and a polyethylene glycol compound protective agent with a chloroauric acid solution; fast reducing the chloroauric acid solution into the gold nanoparticles by taking sodium citrate as a reductant in a microwave reactor; after microwave reaction is finished, adding hexadecyl trimethyl ammonium bromide to prevent the growth of the gold nanoparticles; separating finial products, and then washing by using water so as to obtain spherical gold nanoparticles with grain diameters between 15 nanometers and 60 nanometers and intensively distributed. The gold nanoparticles obtained by taking the polyvinylpyrrolidone and the polyethylene glycol as the compound high-molecular protective agents have uniform grain diameter and good product stability; in the invention, the whole preparation process of the gold nanoparticles through a microwave method only needs less than 20 minutes, thereby enhancing the reaction rate and providing a new way for the preparation of the gold nanoparticles; and in addition, the prepared gold nanoparticles can be used for biomedical detection and biochemical products.
Description
Technical field
The invention belongs to the nano metal material preparing technical field, relating to a kind of is protective agent with the composite high-molecular compound, and is the preparation method of the nano Au particle of heater means with the microwave.
Background technology
The develop rapidly of nanometer technology is that new direction has been opened up in the application of nano particle in life science and bioanalysis.Because its unique physics, chemical property, nano particle has caused scientific worker's very big concern, and its application aspect chemistry and bio-sensing is also more and more.
Nano Au particle has all demonstrated great using value in a lot of fields with its good stable, small-size effect, skin effect, optical effect and unique biological compatibility.Prepare by easy method that monodispersity is good, particle diameter is controlled and all once high nano Au particle is important research focus always.
Nano particle is because size is little, and its less stable very easily is subjected to the influence of various factors in preparation and the storage process, make final product cut size all once descend.Water-soluble high-molecular compound has the colloid protective effect, so add macromolecule dispersant in preparation process, can improve the stability of nano Au particle in the aqueous solution.Prior preparation method is many, and heat time heating time is all longer with conventional thermal source heating, and the reaction time is long more, and is unfavorable more for the preparation of nano Au particle, its gold particle for preparing all once went up not ideal enough.Heating using microwave is even rapidly, does not need heat transfer process, has automatic hot stationary performance, and it is overheated to avoid; And generate heat owing to the material that contains moisture very easily directly absorbs microwave,, therefore except that a spot of loss, almost do not have other losses not through other intermediate conversion links, can be than the about 30%-50% of general conventional heating power saving.
Summary of the invention:
The objective of the invention is to: the problem long based on the existing nm of gold technology of preparing time, that product stability has much room for improvement; the invention provides a kind of is protectant nm of gold microwave assistant preparation method with the composite high-molecular compound; utilize the quick and uniform characteristics shortening preparation of product cycle of heating using microwave; utilize the coordinating protection effect that shows under organic polymer protective agent polyvinylpyrrolidone and the polyethylene glycol acting in conjunction simultaneously; and the particle diameter control action of softex kw, realize the nano Au particle of preparation particle diameter homogeneous and controllable fast.
The preparation method of nano Au particle of the present invention may further comprise the steps:
1, polyvinylpyrrolidonesolution solution, polyglycol solution and aqueous solution of chloraurate are mixed;
2, adopt the microwave reactor heating, stir, add sodium citrate solution, obtain nano-Au solution after the reaction;
3, add the growth that softex kw solution stops nm of gold;
4, obtain nano Au particle by low speed and high speed centrifugation separation.
The concentration of described chlorauric acid solution is 50-200 μ g/mL, and consumption is 100-200mL.
Described sodium citrate solution concentration is 0.01-0.04g/mL, and consumption is 1-20mL.
The concentration of described polyvinylpyrrolidonesolution solution is 0.01-0.02g/mL, and consumption is 5-20mL.
The concentration of described polyglycol solution is 0.01-0.03g/mL, and consumption is 5-20mL.
The concentration of described softex kw solution is 0.01-0.02g/mL, and consumption is 5-40mL.
The power of described microwave reactor is 300-650W.
Described mixing speed is 100-300r/min.
The concrete operations of above-mentioned steps 2 are as follows: polyvinylpyrrolidonesolution solution, polyglycol solution and aqueous solution of chloraurate are mixed, the heating of employing microwave reactor, stir, 1.5 solution boiling after minute, add sodium citrate solution fast, under stirring condition, continue microwave reaction, stop reaction after 5-10 minute, obtain nano-Au solution.
The present invention obtains particle diameter at 15-60nm, and the ball shaped nano gold particle of centralized particle diameter.
The invention has the advantages that: the invention provides a kind of method for preparing nano Au particle,, can obtain the nano Au particle of different-grain diameter by changing the ratio of natrium citricum and chlorauric acid solution; Under two kinds of protectant synergies, nano Au particle all is protected in preparation and storage process, and its stability improves greatly; Softex kw can make nano Au particle no longer increase later at reaction terminating, thereby reaches the effect that accurate control nano Au particle particle diameter distributes.
The invention provides the method for utilizing microwave reaction to prepare nano Au particle, compare with conventional heating means, microwave can be directly produces fuel factor to the molecule of reaction solution, heating process from the inside to the outside, reaction solution is heated evenly fast.Therefore, microwave reaction has saved the time of preheating, heating, and the preparation process required time can be shortened in 20 minutes from 45 minutes of routine, greatly reduces the suffered harmful effect of nano Au particle in the preparation process.
Description of drawings:
Fig. 1 is the transmission electron microscope picture with the nano Au particle of several different-grain diameters of method preparation of the present invention.Wherein, A is 15nm; B is 40nm; C is 60nm.
Fig. 2 is the ultraviolet-visible absorption spectroscopy figure of A, B among Fig. 1, C nano Au particle correspondence.
The specific embodiment:
Embodiment 1:
Adding concentration in there-necked flask is the chlorauric acid solution 100mL of 100 μ g/mL, adds polyvinylpyrrolidonesolution solution 10mL, polyglycol solution 10mL.There-necked flask is put into the microwave reactor reaction, and the setting microwave power is 650W, solution boiling after 1.5 minutes.Adding concentration fast is the sodium citrate solution 2mL of 0.02g/mL, continues microwave reaction under the stirring of 300r/min, and microwave power is 325W, stops reaction after 5 minutes.After reaction finishes, add the softex kw solution cessation reaction of 10mL.At last reaction solution is carried out the low-speed centrifugal of 1000r/min by supercentrifuge, get the high speed centrifugation that supernatant liquor carries out 11000r/min again, its lower sediment obtains product with the second distillation water washing, and its particle diameter is 15nm.
Embodiment 2:
Adding concentration in there-necked flask is the chlorauric acid solution 100mL of 100 μ g/mL, adds polyvinylpyrrolidonesolution solution 10mL, polyglycol solution 10mL.There-necked flask is put into the microwave reactor reaction, and the setting microwave power is 650W, solution boiling after 1.5 minutes.Adding concentration fast is the sodium citrate solution 4mL of 0.02g/mL, continues microwave reaction under the stirring of 200r/min, and microwave power is 390W, stops reaction after 6 minutes.After reaction finishes, add the softex kw solution cessation reaction of 10mL.At last reaction solution is carried out the low-speed centrifugal of 1000r/min by supercentrifuge, get the high speed centrifugation that supernatant liquor carries out 11000r/min again, its lower sediment obtains product with the second distillation water washing, and its particle diameter is 40nm.
Embodiment 3:
Adding concentration in there-necked flask is the chlorauric acid solution 100mL of 100 μ g/mL, adds polyvinylpyrrolidonesolution solution 10mL, polyglycol solution 10mL.There-necked flask is put into the microwave reactor reaction, and the setting microwave power is 650W, solution boiling after 1.5 minutes.Adding concentration fast is the sodium citrate solution 1mL of 0.02g/mL, continues microwave reaction under the stirring of 100r/min, and microwave power is 325W, stops reaction after 8 minutes.After reaction finishes, add the softex kw solution cessation reaction of 20mL.At last reaction solution is carried out the low-speed centrifugal of 1000r/min by supercentrifuge, get the high speed centrifugation that supernatant liquor carries out 11000r/min again, its lower sediment obtains product with the second distillation water washing, and its particle diameter is 60nm.
Claims (9)
1. the preparation method of a nano Au particle is characterized in that, may further comprise the steps:
1) polyvinylpyrrolidonesolution solution, polyglycol solution and aqueous solution of chloraurate are mixed;
2) adopt the microwave reactor heating, stir, add sodium citrate solution, obtain nano-Au solution after the reaction;
3) add the growth that softex kw solution stops nm of gold;
4) obtain nano Au particle by low speed and high speed centrifugation separation.
2. the preparation method of nano Au particle according to claim 1 is characterized in that, the concentration of described chlorauric acid solution is 50-200 μ g/mL, and consumption is 100-200mL.
3. the preparation method of nano Au particle according to claim 1 is characterized in that, described sodium citrate solution concentration is 0.01-0.04g/mL, and consumption is 1-20mL.
4. the preparation method of nano Au particle according to claim 1 is characterized in that, the concentration of described polyvinylpyrrolidonesolution solution is 0.01-0.02g/mL, and consumption is 5-20mL.
5. the preparation method of nano Au particle according to claim 1 is characterized in that, the concentration of described polyglycol solution is 0.01-0.03g/mL, and consumption is 5-20mL.
6. the preparation method of nano Au particle according to claim 1 is characterized in that, the concentration of described softex kw solution is 0.01-0.02g/mL, and consumption is 5-40mL.
7. the preparation method of nano Au particle according to claim 1 is characterized in that, the power of described microwave reactor is 300-650W.
8. the preparation method of nano Au particle according to claim 1 is characterized in that, described mixing speed is 100-300r/min.
9. the preparation method of nano Au particle according to claim 1, it is characterized in that, polyvinylpyrrolidonesolution solution, polyglycol solution and aqueous solution of chloraurate are mixed, the heating of employing microwave reactor is stirred, solution boiling after 1.5 minutes, add sodium citrate solution fast, under stirring condition, continue microwave reaction, stop reaction after 5-10 minute, obtain nano-Au solution.
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| CN2010105057794A CN101934379B (en) | 2010-10-13 | 2010-10-13 | Method for preparing gold nanoparticles |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211204A (en) * | 2011-05-06 | 2011-10-12 | 中国科学院化学研究所 | Method for preparing nano-gold |
| CN102218542A (en) * | 2011-05-12 | 2011-10-19 | 陕西科技大学 | Nanogold preparation method |
| CN102895987A (en) * | 2012-10-12 | 2013-01-30 | 中南大学 | Method for preparing Au/g-C3N4 composite-type micro-nano material |
| CN102962474A (en) * | 2012-12-13 | 2013-03-13 | 北京航空航天大学 | Controllable synthetic method for preparing gold-nickel core-shell nanostructure with ethylene glycol system |
| CN103768080A (en) * | 2013-12-30 | 2014-05-07 | 浙江工业大学 | Targeting preparation for resisting drug-resistant tumor, as well as preparation method and application thereof |
| CN103878382A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for special-shaped gold nanocrystals and application on detection of tripolycyanamide by using surface enhanced Raman scattering |
| CN104209534A (en) * | 2014-07-30 | 2014-12-17 | 苏州铉动三维空间科技有限公司 | Preparation method for hybrid structure of iron hydroxide nanorods-gold nanoparticles |
| CN105288620A (en) * | 2015-10-16 | 2016-02-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of gold nanoflowers for targeting therapy of tumors |
| CN105478790A (en) * | 2014-09-17 | 2016-04-13 | 济南大学 | Monocrystal gold nano balls and preparation method thereof |
| CN106855571A (en) * | 2016-12-29 | 2017-06-16 | 广州华弘生物科技有限公司 | A kind of antistreptolysin O (ASO) quick diagnosis reagent kit and its application method |
| CN107252897A (en) * | 2017-06-29 | 2017-10-17 | 牡丹江师范学院 | A kind of preparation method of the golden nanometer particle composite of polyoxometallate modification |
| CN108500293A (en) * | 2018-05-21 | 2018-09-07 | 浙江理工大学 | A kind of microwave assisting method prepares the method and Au nano flowers of Au nano flowers |
| CN113125408A (en) * | 2021-03-11 | 2021-07-16 | 上海应用技术大学 | On-site rapid detection method for volatile benzaldehyde in exhaled breath of human body |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876292A (en) * | 2006-06-02 | 2006-12-13 | 中国科学院长春应用化学研究所 | Nanometer gold grain microwave synthesis method |
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2010
- 2010-10-13 CN CN2010105057794A patent/CN101934379B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876292A (en) * | 2006-06-02 | 2006-12-13 | 中国科学院长春应用化学研究所 | Nanometer gold grain microwave synthesis method |
Non-Patent Citations (1)
| Title |
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| 《化学进展》 20080131 宋香宁等 金纳米晶制备和表面修饰中的分子配体 第4节表面活性剂分子部分 1-3 , 2 * |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211204A (en) * | 2011-05-06 | 2011-10-12 | 中国科学院化学研究所 | Method for preparing nano-gold |
| CN102218542A (en) * | 2011-05-12 | 2011-10-19 | 陕西科技大学 | Nanogold preparation method |
| CN102218542B (en) * | 2011-05-12 | 2013-04-10 | 陕西科技大学 | Nanogold preparation method |
| CN102895987A (en) * | 2012-10-12 | 2013-01-30 | 中南大学 | Method for preparing Au/g-C3N4 composite-type micro-nano material |
| CN102962474A (en) * | 2012-12-13 | 2013-03-13 | 北京航空航天大学 | Controllable synthetic method for preparing gold-nickel core-shell nanostructure with ethylene glycol system |
| CN102962474B (en) * | 2012-12-13 | 2014-10-22 | 北京航空航天大学 | Controllable synthetic method for preparing gold-nickel core-shell nanostructure with ethylene glycol system |
| CN103878382B (en) * | 2012-12-20 | 2016-06-08 | 江南大学 | A kind of preparation method of the special appearance gold nano-crystal detecting tripolycyanamide for surface enhanced raman spectroscopy |
| CN103878382A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for special-shaped gold nanocrystals and application on detection of tripolycyanamide by using surface enhanced Raman scattering |
| CN103768080A (en) * | 2013-12-30 | 2014-05-07 | 浙江工业大学 | Targeting preparation for resisting drug-resistant tumor, as well as preparation method and application thereof |
| CN103768080B (en) * | 2013-12-30 | 2017-04-05 | 浙江工业大学 | A kind of targeting preparation of overriding resistance tumor, preparation method and application |
| CN104209534A (en) * | 2014-07-30 | 2014-12-17 | 苏州铉动三维空间科技有限公司 | Preparation method for hybrid structure of iron hydroxide nanorods-gold nanoparticles |
| CN105478790A (en) * | 2014-09-17 | 2016-04-13 | 济南大学 | Monocrystal gold nano balls and preparation method thereof |
| CN105478790B (en) * | 2014-09-17 | 2017-09-22 | 济南大学 | Monocrystalline gold nano ball and preparation method thereof |
| CN105288620A (en) * | 2015-10-16 | 2016-02-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of gold nanoflowers for targeting therapy of tumors |
| CN105288620B (en) * | 2015-10-16 | 2018-08-17 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of Jenner's popped rice for neoplasm targeted therapy |
| CN106855571A (en) * | 2016-12-29 | 2017-06-16 | 广州华弘生物科技有限公司 | A kind of antistreptolysin O (ASO) quick diagnosis reagent kit and its application method |
| CN107252897A (en) * | 2017-06-29 | 2017-10-17 | 牡丹江师范学院 | A kind of preparation method of the golden nanometer particle composite of polyoxometallate modification |
| CN108500293A (en) * | 2018-05-21 | 2018-09-07 | 浙江理工大学 | A kind of microwave assisting method prepares the method and Au nano flowers of Au nano flowers |
| CN108500293B (en) * | 2018-05-21 | 2021-09-07 | 浙江理工大学 | Method for preparing Au nanoflower by microwave-assisted method and Au nanoflower |
| CN113125408A (en) * | 2021-03-11 | 2021-07-16 | 上海应用技术大学 | On-site rapid detection method for volatile benzaldehyde in exhaled breath of human body |
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| CN101934379B (en) | 2012-02-22 |
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