CN105750561B - A kind of method for purifying copper nano-cluster - Google Patents
A kind of method for purifying copper nano-cluster Download PDFInfo
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- CN105750561B CN105750561B CN201610152252.5A CN201610152252A CN105750561B CN 105750561 B CN105750561 B CN 105750561B CN 201610152252 A CN201610152252 A CN 201610152252A CN 105750561 B CN105750561 B CN 105750561B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
A kind of method for purifying copper nano-cluster, comprises the following steps：1), BSA dissolvings are formed to the solution of clear in aqueous；2), by copper ion according to BSA：Cu2+Weight ratio is 10~40:1~10 adds in the solution that step 1) obtains, and is well mixed；3), under stirring, add in the solution that sodium hydroxide obtains to step 2), while adjust the pH value of solution, stirred at 37~60 DEG C and copper nano-cluster stoste is made；4), HNO is added in copper nano-cluster stoste prepared by step 3)3, the pH to 3~6 of copper nano-cluster stoste is adjusted, generates copper nano-cluster precipitation；5), by the copper nano-cluster pelleting centrifugation of step 4) generation, separation, cleaning；6) the copper nano-cluster precipitation after, step 5) is cleaned is dispersed in the solution that clear is formed in sodium hydroxide solution again, that is, obtains copper nano-cluster.Its advantage is：The material of copper ions is used as major ingredient, copper nano-cluster is prepared as auxiliary material using BSA or DNA, glutathione, it is simple to operate, environmentally friendly, and cost is cheap.
Description
Technical field
The present invention relates to chemistry and bioscience technology field, specifically a kind of method for purifying copper nano-cluster.
Background technology
With the reduction of metal nanoparticle yardstick, its level structure can occur drastically to change, the electricity near fermi level
Sub- energy level is transitioned into discrete energy levels from quasicontinuum state.The change of level structure causes metal nanometer cluster has to be different from body gold
The special performance of category；
In the last few years, it is that Material synthesis is water-soluble with reagents such as various template molecules and stabilizer such as protein, DNA, mercaptan
The fluorescence metal nano-cluster of property becomes the focus of research.During synthesis, it is necessary to using substantial amounts of template molecule and surely
Determine agent, and these molecules are possible to that substance reactions can be analyzed with a lot, so as to cause very big puzzlement to follow-up detection.And
The inner filtering effect of synthetic raw material can also reduce the fluorescence of synthesized cluster.So water-soluble nano cluster is purified to for current work
The emphasis of work.As far as we know, at present mainly using 3 kinds of methods come purifying nano cluster：Dialysis, ultrafiltration and chromatographic separation technology.
And comparatively these methods purify more complicated, time-consuming, refining effect is unsatisfactory.Therefore, how using simple method
It is current urgent problem to be solved to purify copper nano-cluster.
The content of the invention
In order to overcome the shortcomings of above-mentioned technological deficiency, the present invention devises cost cheap, simple to operate, energy-conserving and environment-protective one
The method of kind purification copper nano-cluster.
A kind of method for purifying copper nano-cluster of the present invention, comprises the following steps：
1), BSA dissolvings are formed to the solution of clear in aqueous, wherein, BSA is bovine serum albumin(BSA)；
2), by copper ion according to BSA：Cu2+Weight ratio is 10~40:1~10 adds in the solution that step 1) obtains, mixing
Uniformly；
3), under stirring, add in the solution that is obtained to step 2) of sodium hydroxide, at the same adjust the pH value of solution to
9~13, stirred at 37~60 DEG C and copper nano-cluster stoste is made；
4) 0.1~1M HNO, are added in copper nano-cluster stoste prepared by step 3)3, the pH of regulation copper nano-cluster stoste
To 3~6, generation copper nano-cluster precipitates；
5), by the copper nano-cluster pelleting centrifugation of step 4) generation, separation, cleaning；
6) the copper nano-cluster precipitation after, step 5) is cleaned is dispersed in sodium hydroxide solution again forms clear
Solution, the pH value of solution is treated between 9~12, that is, obtain copper nano-cluster.
Preferably, BSA is substituted from glutathione in step 1)；
Preferably, step 2) BSA：Cu2+Weight ratio preferably 25:5；
Preferably, the HNO of stoste is added in step 4)3Amount be preferably 0.5M；
Preferably, HNO is substituted from HAc in step 4)3；
Preferably, it is to centrifuge, separate under 10000~12000 turns of rotating speed in step 5)；
Preferably, in step 5), copper nano-cluster is precipitated and cleaned 3~5 times with 5~10mL deionized water；
A kind of method for purifying copper nano-cluster of the present invention, its advantage are：The material of copper ions is used as major ingredient, with BSA
It is simple to operate, environmentally friendly or DNA, glutathione are that auxiliary material prepares copper nano-cluster, and cost is cheap.
Concrete mode
Using specific embodiment, the present invention will be further described below：
Embodiment one：
1), 75mg BSA are dissolved in the solution that clear is formed in the 5ml aqueous solution；
2), by 5mg CuSO4·5H2O is dissolved in 1ml water, is added in the solution of step 1) acquisition, is well mixed；
3) in the solution that, under stirring, addition 140ul, 1M sodium hydroxide obtains to step 2), solution is adjusted
PH value is to continuing to stir obtained copper nano-cluster stoste at a temperature of 12,55 DEG C；
4) 1M HAc, are added in copper nano-cluster stoste prepared by step 3), adjust the pH to 6 of copper nano-cluster stoste, are promoted
Enter the generation of copper nano-cluster precipitation；
5), the copper nano-cluster that step 4) generates is deposited under 10000 turns of rotating speed and centrifuges, separate, then by precipitation 8mL
Deionized water clean 3 times；
6) precipitation after, step 5) is cleaned is dispersed in the solution that clear is formed in sodium hydroxide solution again, treats
When the pH value of solution is 11, that is, copper nano-cluster can be obtained by seeing.
Embodiment two：
1), 20mg glutathione is dissolved in the solution that clear is formed in the 1ml aqueous solution；
2), by 5mg CuSO4·5H2O is dissolved in 1ml water, is added in the solution of step 1) acquisition, is well mixed；
3) in the solution that, under stirring, addition 40ul, 1M sodium hydroxide obtains to step 2), solution is adjusted
PH value is to continuing to stir obtained copper nano-cluster stoste at a temperature of 9,50 DEG C；
4) 0.8M HAc, are added in copper nano-cluster stoste prepared by step 3), adjust the pH to 4 of copper nano-cluster stoste,
Promote the generation of copper nano-cluster precipitation；
5), the copper nano-cluster that step 4) generates is deposited under 10800 turns of rotating speed and centrifuges, separate, then by precipitation 5mL
Deionized water clean 4 times；
6) precipitation after, step 5) is cleaned is dispersed in the solution that clear is formed in sodium hydroxide solution again, treats
When the pH value of solution is 9, that is, copper nano-cluster can be obtained by seeing.
Embodiment three：
1), 10mg BSA are dissolved in the solution that clear is formed in the 1ml aqueous solution；
2), by 1mg CuSO4·5H2O is dissolved in 0.2ml water, is added in the solution of step 1) acquisition, is well mixed；
3) in the solution that, under stirring, addition 25ul, 1M sodium hydroxide obtains to step 2), solution is adjusted
PH value is to continuing to stir obtained copper nano-cluster stoste at a temperature of 11,58 DEG C；
4), the copper nano-cluster stoste prepared in step 3) adds 0.9M HNO3, the pH to 5 of copper nano-cluster stoste is adjusted, is promoted
Enter the generation of copper nano-cluster precipitation；
5), the copper nano-cluster that step 4) generates is deposited under 11000 turns of rotating speed and centrifuges, separate, then by precipitation 7mL
Deionized water clean 5 times；
6) precipitation after, step 5) is cleaned is dispersed in the solution that clear is formed in sodium hydroxide solution again, treats
When the pH value of solution is 11, that is, copper nano-cluster can be obtained by seeing.
Example IV：
1), 25mg glutathione is dissolved in the solution that clear is formed in the 2ml aqueous solution；
2), by 5mg CuSO4·5H2O is dissolved in 1ml water, is added in the solution of step 1) acquisition, is well mixed；
3) in the solution that, under stirring, addition 60ul, 1M sodium hydroxide obtains to step 2), solution is adjusted
PH value is to continuing to stir obtained copper nano-cluster stoste at a temperature of 13,60 DEG C；
4) 1M HAc, are added in copper nano-cluster stoste prepared by step 3), adjust the pH to 6 of copper nano-cluster stoste, are promoted
Enter the generation of copper nano-cluster precipitation；
5), the copper nano-cluster that step 4) generates is deposited under 12000 turns of rotating speed and centrifuges, separate, then by precipitation 9mL
Deionized water clean 4 times；
6) precipitation after, step 5) is cleaned is dispersed in the solution that clear is formed in sodium hydroxide solution again,
When the pH value of solution is 12, that is, copper nano-cluster can be obtained by seeing.
Embodiment five：
1), 30mg BSA are dissolved in the solution that clear is formed in the 2ml aqueous solution；
2), by 2mg CuSO4·5H2O is dissolved in 0.4ml water, is added in the solution of step 1) acquisition, is well mixed；
3) in the solution that, under stirring, addition 70ul, 1M sodium hydroxide obtains to step 2), solution is adjusted
PH value is to continuing to stir obtained copper nano-cluster stoste at a temperature of 12,58 DEG C；
4) 0.9M HNO, are added in copper nano-cluster stoste prepared by step 3)3, adjust copper nano-cluster stoste pH to
5.8, promote the generation of copper nano-cluster precipitation；
5), the copper nano-cluster that step 4) generates is deposited under 10600 turns of rotating speed and centrifuges, separate, then precipitation is used
10mL deionized water is cleaned 3 times；
6) precipitation after, step 5) is cleaned is dispersed in the solution that clear is formed in sodium hydroxide solution again,
When the pH value of solution is 10, that is, copper nano-cluster can be obtained by seeing.
In above-described embodiment, CuSO4·5H2O can be substituted with the acidic materials of other copper ions.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (4)
- A kind of 1. method for purifying copper nano-cluster, it is characterised in that：Comprise the following steps：1), BSA dissolvings are formed to the solution of clear in aqueous, wherein, BSA is bovine serum albumin(BSA)；2), by copper ion according to BSA：Cu2+Weight ratio is 10~40:1~10 adds in the solution that step 1) obtains, and mixing is equal It is even；3), under stirring, add in the solution that is obtained to step 2) of sodium hydroxide, at the same adjust the pH value of solution to 9~ 13, stirred at 37~60 DEG C and copper nano-cluster stoste is made；4) 0.1~1M HNO, are added in copper nano-cluster stoste prepared by step 3)3, adjust copper nano-cluster stoste pH to 3~ 6, generation copper nano-cluster precipitation；5), by the copper nano-cluster pelleting centrifugation of step 4) generation, separation, cleaning；Copper nano-cluster is precipitated and cleaned 3~5 times with 5~10mL deionized water；6) the copper nano-cluster precipitation after, step 5) is cleaned is dispersed in sodium hydroxide solution again forms the molten of clear Liquid, the pH value of solution is treated between 9~12, that is, obtain copper nano-cluster.
- A kind of 2. method for purifying copper nano-cluster according to claim 1, it is characterised in that：Gluathione is selected in step 1) Peptide substitutes BSA.
- A kind of 3. method for purifying copper nano-cluster according to claim 1, it is characterised in that：Stoste is added in step 4) HNO3Amount be 0.5M.
- A kind of 4. method for purifying copper nano-cluster according to claim 1, it is characterised in that：It is 10000 in step 5) Centrifuge, separate under~12000 turns of rotating speed.
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| CN105963709B (en) * | 2016-06-08 | 2019-01-11 | 湖北大学 | A kind of preparation method of folic acid label copper nano-cluster |
| CN108127124B (en) * | 2016-12-01 | 2020-01-14 | 中国科学院大连化学物理研究所 | Preparation method of copper nanocluster with adjustable fluorescence color |
| CN109596580B (en) * | 2018-09-06 | 2020-12-29 | 天津师范大学 | Method for quantitatively detecting glutamic-pyruvic transaminase in solution based on copper nano-cluster fluorescent probe |
| CN109794618A (en) * | 2019-01-15 | 2019-05-24 | 南通纺织丝绸产业技术研究院 | The preparation of the copper nano-cluster of sericin package and fluorescence probe |
| CN111570820B (en) * | 2020-04-21 | 2022-01-11 | 武汉理工大学 | Preparation method and application of copper nanocluster |
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| JP2005097642A (en) * | 2003-09-22 | 2005-04-14 | Tanaka Kikinzoku Kogyo Kk | Noble metal-metal oxide composite cluster |
| CN103868899A (en) * | 2014-02-27 | 2014-06-18 | 天津大学 | Fluorescence detection method for kojic acid in food and environmental sample |
| CN104458050A (en) * | 2014-11-27 | 2015-03-25 | 江南大学 | Fluorescent copper namo clusters for living cell temperature monitoring |
| CN104807795A (en) * | 2015-05-06 | 2015-07-29 | 江南大学 | Fast preparation method of biological affinity copper nanometer cluster |
| CN104972135B (en) * | 2015-05-28 | 2017-03-01 | 天津师范大学 | The synthetic method of near infrared fluorescent probe copper nano-cluster and its application |
| CN105382269B (en) * | 2015-11-09 | 2017-05-10 | 东南大学 | Method for preparing water-soluble light-emitting gold nanoclusters based on substitution method and aggregation inducement |
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