CN109295107A - A kind of green synthesis method of metal nanoparticle - Google Patents
A kind of green synthesis method of metal nanoparticle Download PDFInfo
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- CN109295107A CN109295107A CN201810773405.7A CN201810773405A CN109295107A CN 109295107 A CN109295107 A CN 109295107A CN 201810773405 A CN201810773405 A CN 201810773405A CN 109295107 A CN109295107 A CN 109295107A
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Abstract
A kind of green synthesis method of metal nanoparticle, its main feature is that, it include: that pale purple mould fungi is inoculated into fluid nutrient medium, it is placed in constant-temperature table, it is continuously cultivated 3-5 days under the conditions of being protected from light, makes the fluid nutrient medium pH value 6.5-7.0 of fungi, 19-30 DEG C of cultivation temperature, shaking table revolution 150rpm obtains mixed culture solution；Obtained mixed culture solution is centrifuged 15 minutes through centrifuge, the biomass of deposition discards, collect supernatant 150ml, it is transferred in reactor at room temperature, metal salt concentrate is added into reactor, makes metal salt in the ultimate density 0.5mM of solution, continues to be placed in shaking table reaction 5-15min, shaking table temperature is 25 DEG C, obtains mixed liquor；At room temperature, mixed liquor is washed 5 times through the product of high speed centrifugation after ten minutes with dehydrated alcohol, is subsequently placed in drying in vacuum freeze drier and obtains metal nanoparticle product for 24 hours.
Description
Technical field
The present invention relates to biological and chemical synthesis technical fields, are a kind of green synthesis methods of metal nanoparticle.
Background technique
Metal nanoparticle have high specific surface area and different particle sizes and shape thus compare metal material sheet
Body makes it have significant advantage in industrial circle.Metal nanoparticle can be applied to various fields include the energy, chemistry manufacture,
Biologic applications, molecular diagnosis, catalysis technique, electronics, drug, semiconductor, sensing and field of environmental technology etc..Research is wider at present
General is still preparation such as gold nanoparticle, Nano silver grain of precious metal nanoparticle etc., has been had more about valuable
The materialization synthesis of metal and the report of biological synthesis method.However, non-precious metal, such as copper nano-particle is since its is unique
Property, natural resources abundant, low cost, high yield are causing the concern of this field nanotechnology research person, and will gradually
Substitute as precious metal nanoparticle in traditional industry (such as catalytic field etc.) is shown up prominently.In recent years, related
In the report of the various physical chemistry methods of the synthesis non-precious metals nanoparticle such as copper, but the various physical chemistry methods of the prior art
Complex process, is also easy to produce secondary pollution at high cost, is restricted it in terms of business application.Thus researcher and industry
It is try to produce non-precious metal nanoparticle using various nontoxic environmental-friendly green bio synthetic methods.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide a kind of scientific and reasonable, can operate
Property strong, at low cost, short, high yield the time required to synthesis, metal nanoparticle obtained is stablized, and the metal of no pollution to the environment
The green synthesis method of nanoparticle.
Solve its technical problem the technical solution adopted is that, a kind of green synthesis method of metal nanoparticle, feature
Be, it the following steps are included:
1) use depositary institution: China General Microbiological culture presevation administrative center, the preservation time: on December 1st, 2013, strain are compiled
Number pale purple mould (Penicillium lilacinum) for being CGMMC NO:3.5376, strain names people (Thom), belongs to
The fungi that Penicillium mould belongs to, is inoculated into 200ml fluid nutrient medium, the fluid nutrient medium for being vaccinated with fungi is placed in
It in constant-temperature table, is continuously cultivated 3-5 days under the conditions of being protected from light, the fluid nutrient medium pH value for being vaccinated with fungi is 6.5-7.0, culture
Temperature is 19-30 DEG C, and shaking table revolution is 150rpm, obtains mixed culture solution；The fluid nutrient medium includes glucose
10g/L, yeast extract 1g/L, peptone 5g/L；
2) the mixed culture solution for obtaining step 1) is centrifuged 15min through centrifuge with the revolving speed of 4500-5000rpm, deposition
Biomass discards, and collects supernatant；
3) the supernatant 150ml for collecting step 2, being transferred to volume at room temperature is in 500ml reactor, to reaction
Metal salt concentrate is added in device, makes metal salt in the ultimate density 0.5mM of solution, is continued to be placed in shaking table reaction 5-15min, be shaken
Bed tempertaure is 25 DEG C, obtains mixed liquor；
4) product of the mixed liquor that at room temperature, step 3) is obtained after 10000rpm high speed centrifugation 10min, after centrifugation
It is washed 5 times with dehydrated alcohol, is placed on drying in vacuum freeze drier and obtains metal nanoparticle product for 24 hours.
Fungi amount in the step 1) is 1.5-2g/L.
It is described 1) in fluid nutrient medium can also be Potato-dextrose solution.
Metal salt concentrate in the step 3) is CuSO4, AgCl or AuCl4。
It beneficial effects of the present invention and is advantageous in that relative to other methods:
1) represent fungi strain: the Penicillium lilacinum strain extracted in natural environment to represent strain,
The fungi of Penicillium Pseudomonas, particular for tolerance relatively high-concentration metallic ions (more than 50mg/L)
Penicillium bacterial strain；
2) present invention is mainly used for synthesis copper or copper oxide nano particles, but are not limited to synthesis copper or copper oxide nano particle,
Synthesis belongs to gold, silver or ferric oxide nano particles of metal nanoparticle etc.；
3) nanoparticle synthesis technology of the present invention is stablized, within the scope of defined operating condition by technological parameter (temperature,
PH, reaction time etc.) influence it is small；
4) present invention uses extracellular synthetic technology, without the additional additional process steps from separation nanoparticle intracellular, normal
Normal temperature and pressure carries out, the redox and catalysis of main protein, enzyme and other biological molecule using fungal organism exocytosis
Performance, simple process save the energy, and yield is high, at low cost；
5) scientific and reasonable, strong operability of the invention, no pollution to the environment.
Detailed description of the invention
Fig. 1 is a kind of sweeping for the nanoparticle of the green synthesis method synthesis of metal nanoparticle of the embodiment of the present invention 1
Retouch electron microscope；
Fig. 2 is a kind of XPS spectrum of the nanoparticle of the green synthesis method synthesis of metal nanoparticle of the embodiment of the present invention 1
Cu2P spectrogram；
Fig. 3 is a kind of XPS spectrum of the nanoparticle of the green synthesis method synthesis of metal nanoparticle of the embodiment of the present invention 1
O1S spectrogram.
Specific embodiment
Of the invention is described further below with drawings and examples.
A kind of green synthesis method of metal nanoparticle of the invention, comprises the step of:
1) depositary institution: China General Microbiological culture presevation administrative center, address: Chaoyang District Beijing North Star West Road 1 is used
Institute 3, preservation time: on December 1st, 2013, the Penicillium lilacinum that strain number is CGMMC NO:3.5376
(pale purple mould) belongs to the fungi of Penicillium mould category, is distributed widely in nature, in synthesis metal nanoparticle
In, which can secrete a large amount of ectoenzyme and biomolecule, its mechanism for being used for nanoparticle may relate at present
The oxidoreducing enzyme such as including sulfite reductase, and using reduced form cigarette nicotinamide-adenine dinucleotide phosphate as coenzyme, lead to
It crosses to form redox center, realizes the biological reducing of the metal ions such as copper at metal simple-substance or through further biochemical reaction shape
At its oxide, while the biomolecule such as protein secreted can further keep producing as nanoparticle capturing agent and stabilizer
The stability of product nanoparticle；Fungi is inoculated into 200ml fluid nutrient medium, the fluid nutrient medium for being vaccinated with fungi is placed in
It in constant-temperature table, is continuously cultivated 3-5 days under the conditions of being protected from light, the fluid nutrient medium pH value for being vaccinated with fungi is 6.5-7.0, culture
Temperature is 19-30 DEG C, and shaking table revolution is 150rpm, obtains mixed culture solution；The fluid nutrient medium includes 2 grams of grapes
Sugar, 0.2 gram of yeast extract, 1 gram of peptone, i.e. glucose 10g/L, yeast extract 1g/L, peptone 5g/L；
2) the mixed culture solution for obtaining step 1) is centrifuged 15min through centrifuge with the revolving speed of 4500-5000rpm, deposition
Biomass discards, and collects supernatant；
3) the supernatant 150ml for collecting step 2, being transferred to volume at room temperature is in 500ml reactor, to reaction
Metal salt concentrate is added in device, makes metal salt in the ultimate density 0.5mM of solution, is continued to be placed in shaking table reaction 5-5min, be shaken
Bed tempertaure is 25 DEG C, obtains mixed liquor；
4) product of the mixed liquor that at room temperature, step 3) is obtained after 10000rpm high speed centrifugation 10min, after centrifugation
It is washed 5 times with dehydrated alcohol, is placed on drying in vacuum freeze drier and obtains metal nanoparticle product for 24 hours.
Fungi amount in the step 1) is 1.5-2.0g/L.
It is described 1) in fluid nutrient medium can also be Potato-dextrose solution.
Metal salt concentrate in the step 3) is CuSO4, AgCl or AuCl4。
Embodiment 1: a kind of green synthesis method synthesis copper oxide nano particle of metal nanoparticle of embodiment 1
Step includes:
1) fungi of fungi amount 1.5g/L is inoculated into 200ml fluid nutrient medium, the Liquid Culture of the fungi will be vaccinated with
Base is placed in constant-temperature table, is continuously cultivated under the conditions of being protected from light 5 days, and the fluid nutrient medium pH value of the fungi is 6.5, culture temperature
Degree is 30 DEG C, and shaking table revolution is 150rpm, obtains mixed culture solution；The fluid nutrient medium includes 2 grams of glucose, 0.2
Gram yeast extract, 1 gram of peptone
2) the mixed culture solution for obtaining step 1) is centrifuged 15min, the biology of deposition through centrifuge with the revolving speed of 4500rpm
Matter discards, and collects supernatant；
3) the supernatant 150ml for collecting step 2, being transferred to volume at room temperature is in 500ml reactor, to reaction
The CuSO for belonging to metal salt concentrate one kind is added in device4, make CuSO4It is 0.5mM in the ultimate density of solution, continues to be placed in shaking table
5min is reacted, shaking table temperature is 25 DEG C, obtains mixed liquor；
4) product of the mixed liquor that at room temperature, step 3) is obtained after 10000rpm high speed centrifugation 10min, after centrifugation
It is washed 5 times with dehydrated alcohol, is placed on drying in vacuum freeze drier and obtains copper oxide nano particle product for 24 hours.
A kind of embodiment 2: the step of the green synthesis method synthesis copper oxide nano particle of metal nanoparticle of embodiment 2
Suddenly include:
1) fungi of fungi amount 1.7g/L is inoculated into 200ml fluid nutrient medium, the Liquid Culture of the fungi will be vaccinated with
Base is placed in constant-temperature table, is continuously cultivated under the conditions of being protected from light 4 days, and the fluid nutrient medium pH value of the fungi is 6.5, culture temperature
Degree is 25 DEG C, and shaking table revolution is 150rpm, obtains mixed culture solution；The fluid nutrient medium includes 2 grams of glucose, 0.2
Gram yeast extract, 1 gram of peptone；
2) the mixed culture solution for obtaining step 1) is centrifuged 15min, the biology of deposition through centrifuge with the revolving speed of 4700rpm
Matter discards, and collects supernatant；
3) the supernatant 150ml for collecting step 2, being transferred to volume at room temperature is in 500ml reactor, to reaction
The CuSO for belonging to metal salt concentrate one kind is added in device4, make CuSO4It is 0.5mM in the ultimate density of solution, continues to be placed in shaking table
10min is reacted, shaking table temperature is 25 DEG C, obtains mixed liquor；
4) product of the mixed liquor that at room temperature, step 3) is obtained after 10000rpm high speed centrifugation 10min, after centrifugation
It is washed 5 times with dehydrated alcohol, is placed on drying in vacuum freeze drier and obtains copper oxide nano particle product for 24 hours.
A kind of embodiment 3: the step of the green synthesis method synthesis copper oxide nano particle of metal nanoparticle of embodiment 3
Suddenly include:
1) fungi of fungi amount 2.0g/L is inoculated into 200ml fluid nutrient medium, the Liquid Culture of the fungi will be vaccinated with
Base is placed in constant-temperature table, is continuously cultivated under the conditions of being protected from light 5 days, and the fluid nutrient medium pH value of the fungi is 7.0, culture temperature
Degree is 19 DEG C, and shaking table revolution is 150rpm, obtains mixed culture solution；The fluid nutrient medium includes 2 grams of glucose, 0.2
Gram yeast extract, 1 gram of peptone；
2) the mixed culture solution for obtaining step 1) is centrifuged 15min, the biology of deposition through centrifuge with the revolving speed of 5000rpm
Matter discards, and collects supernatant；
3) the supernatant 150ml for collecting step 2, being transferred to volume at room temperature is in 500ml reactor, to reaction
The CuSO for belonging to metal salt concentrate one kind is added in device4, make CuSO4It is 0.5mM in the ultimate density of solution, continues to be placed in shaking table
15min is reacted, shaking table temperature is 25 DEG C, obtains mixed liquor；
4) product of the mixed liquor that at room temperature, step 3) is obtained after 10000rpm high speed centrifugation 10min, after centrifugation
It is washed 5 times with dehydrated alcohol, is placed on drying in vacuum freeze drier and obtains copper oxide nano particle product for 24 hours.
A kind of embodiment 4: the step of the green synthesis method synthesis copper oxide nano particle of metal nanoparticle of embodiment 3
Suddenly include:
1) fungi of fungi amount 2.0g/L is inoculated into 200ml fluid nutrient medium, the Liquid Culture of the fungi will be vaccinated with
Base is placed in constant-temperature table, is continuously cultivated under the conditions of being protected from light 3 days, and the fluid nutrient medium pH value of the fungi is 6.5, culture temperature
Degree is 23 DEG C, and shaking table revolution is 150rpm, obtains mixed culture solution；The fluid nutrient medium includes 2 grams of glucose, 0.2
Gram yeast extract, 1 gram of peptone；
2) the mixed culture solution for obtaining step 1) is centrifuged 10min, the biology of deposition through centrifuge with the revolving speed of 4500rpm
Matter discards, and collects supernatant；
3) the supernatant 150ml for collecting step 2, being transferred to volume at room temperature is in 500ml reactor, to reaction
The CuSO for belonging to metal salt concentrate one kind is added in device4, make CuSO4It is 0.5mM in the ultimate density of solution, continues to be placed in shaking table
8min is reacted, shaking table temperature is 25 DEG C, obtains mixed liquor；
4) product of the mixed liquor that at room temperature, step 3) is obtained after 10000rpm high speed centrifugation 10min, after centrifugation
It is washed 5 times with dehydrated alcohol, is placed on drying in vacuum freeze drier and obtains copper oxide nano particle product for 24 hours.
The embodiment of the present invention is limited embodiment, is only used for that the present invention is further illustrated, not exhaustive, not
Restriction of the composition to claims, the enlightenment that those skilled in the art obtain according to embodiments of the present invention, without
Creative work would occur to other substantially equivalent substitutions, all fall in the scope of protection of the present invention.
Metal salt dosage used in the embodiment of the present invention is CuSO to add metal salt concentrate4, but and it is not exclusive specified,
It further include the AgCl of metal salt, AuCl4Deng.
The metal nanoparticle product copper oxide nano particle that the embodiment of the present invention obtains, can be according to ultra-violet absorption spectrum, X
X ray diffraction and Raman spectrum further identify corresponding product.
It includes energy that the metal nano material that the present invention synthesizes, which can be applied to all fields being related to including metal nanoparticle,
Source, chemical manufacture, biologic applications, molecular diagnosis, catalysis technique, electronics, drug, semiconductor, sensing and field of environmental technology etc..
As shown in Figure 1, the SEM of the nanoparticle synthesized by the green synthesis method of metal nanoparticle of the present invention scans electricity
The surface topography of the bright nanoparticle of mirror chart, HR-TEM measurement further confirm that nanoparticle is spherical shape, and partial size is about 20nm.
As shown in Fig. 2, the nanoparticle XPS spectrum figure synthesized by the green synthesis method of metal nanoparticle of the present invention
Cu2P, all peak positions (933.6 e V-962.1eV) shown in map are consistent with the result of pertinent literature report.Wherein
Show that apparent peak respectively represents Cu2p3/2 and Cu2p1/2 at 933.4eV and 953.7eV, as both Cu2p3/2 and Cu2p1/2
Combination can difference show the formation for having copper oxide nano particle if it is larger than or equal to 20eV.
As shown in figure 3, the nanoparticle XPS spectrum figure synthesized by the green synthesis method of metal nanoparticle of the present invention
Spectral peak in O1s spectrum positioned at 532.1eV further identifies copper and oxygen is combined into copper oxide nano particle.
Claims (4)
1. a kind of green synthesis method of metal nanoparticle, characterized in that it the following steps are included:
1) use depositary institution: China General Microbiological culture presevation administrative center, the preservation time: on December 1st, 2013, strain are compiled
Number pale purple mould (Penicillium lilacinum) for being CGMMC NO:3.5376, strain names people (Thom), belongs to
The fungi that Penicillium mould belongs to, is inoculated into 200ml fluid nutrient medium, the fluid nutrient medium for being vaccinated with fungi is placed in
It in constant-temperature table, is continuously cultivated 3-5 days under the conditions of being protected from light, the fluid nutrient medium pH value for being vaccinated with fungi is 6.5-7.0, culture
Temperature is 19-30 DEG C, and shaking table revolution is 150rpm, obtains mixed culture solution；The fluid nutrient medium includes glucose
10g/L, yeast extract 1g/L, albumen 5g/L；
2) the mixed culture solution for obtaining step 1) is centrifuged 15min through centrifuge with the revolving speed of 4500-5000rpm, deposition
Biomass discards, and collects supernatant；
3) the supernatant 150ml for collecting step 2, being transferred to volume at room temperature is in 500ml reactor, to reaction
Metal salt concentrate is added in device, makes metal salt in the ultimate density 0.5mM of solution, is continued to be placed in shaking table reaction 5-15min, be shaken
Bed tempertaure is 25 DEG C, obtains mixed liquor；
4) product of the mixed liquor that at room temperature, step 3) is obtained after 10000rpm high speed centrifugation 10min, after centrifugation
It is washed 5 times with dehydrated alcohol, is placed on drying in vacuum freeze drier and obtains metal nanoparticle product for 24 hours.
2. a kind of green synthesis method of metal nanoparticle according to claim 1, characterized in that in the step 1)
Fungi amount be 1.5-2g/L.
3. a kind of green synthesis method of metal nanoparticle according to claim 1, characterized in that in the step 1)
Fluid nutrient medium can also be Potato-dextrose solution.
4. a kind of green synthesis method of metal nanoparticle according to claim 1, characterized in that in the step 3)
Metal salt concentrate be CuSO4, AgCl or AuCl4。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050214916A1 (en) * | 2004-03-26 | 2005-09-29 | Council Of Scientific And Industrial Research | Biological process for synthesis of oxide nanoparticles |
| CN105112453A (en) * | 2015-09-19 | 2015-12-02 | 中国科学院生态环境研究中心 | Preparation method of nano-particle material |
| US20160185638A1 (en) * | 2014-12-24 | 2016-06-30 | Jianmeng Chen | Fungi-bacteria composite microecologics and methods for preparing and using the same |
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2018
- 2018-07-14 CN CN201810773405.7A patent/CN109295107A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050214916A1 (en) * | 2004-03-26 | 2005-09-29 | Council Of Scientific And Industrial Research | Biological process for synthesis of oxide nanoparticles |
| US20160185638A1 (en) * | 2014-12-24 | 2016-06-30 | Jianmeng Chen | Fungi-bacteria composite microecologics and methods for preparing and using the same |
| CN105112453A (en) * | 2015-09-19 | 2015-12-02 | 中国科学院生态环境研究中心 | Preparation method of nano-particle material |
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Application publication date: 20190201 |