CN104001931A - Method for preparing precious metal palladium nanorod by means of cotton bollworm baculovirus nucleocapsid - Google Patents
Method for preparing precious metal palladium nanorod by means of cotton bollworm baculovirus nucleocapsid Download PDFInfo
- Publication number
- CN104001931A CN104001931A CN201410197014.7A CN201410197014A CN104001931A CN 104001931 A CN104001931 A CN 104001931A CN 201410197014 A CN201410197014 A CN 201410197014A CN 104001931 A CN104001931 A CN 104001931A
- Authority
- CN
- China
- Prior art keywords
- nucleocapsid
- solution
- bollworm
- baculoviral
- precious metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
A method for preparing a precious metal palladium nanorod by means of cotton bollworm baculovirus nucleocapsid mainly includes the steps that cotton bollworm karyotype polyhedron virus raw powder is dispersed through ultra-pure water to obtain grey polyhedrin suspension, alkaline hydrolysis liquid is added into the grey polyhedrin suspension, the mixture stands still for 15-25 min, then the pH value is adjusted to be 7 through acetic acid, chloroform is added, centrifugalization is carried out for 5-10 min at the speed of 5000-6000 r/min, supernatant fluid is sucked, centrifugalization is carried out for 1-2 h at the temperature of 4-10 DEG C and at the speed of 25000-30000 r/min, pigmentation is re-suspeneded through a PBS solution, and a cotton bollworm baculovirus nucleocapsid solution is obtained; a PdCl2 solution is added into the cotton bollworm baculovirus nucleocapsid solution and fully and evenly mixed, incubation is carried out in a shaking mode for 15-25 h at the temperature of 20-30 DEG C and at the speed of 130-170 r/min, and the precious metal palladium nanorod loaded by the cotton bollworm baculovirus nucleocapsid is obtained. The method is simple in process, environmentally friendly and efficient, industrial production is easy to achieve, and the prepared palladium nanorod is stable in appearance and uniform in size.
Description
Technical field
The present invention relates to a kind of preparation method of nano material, particularly the preparation method of precious metal palladium nanometer rods.
Background technology
Because noble metal nanometer material has surface-interfacial effect, small-size effect, quantum size effect, macroscopic quantum tunneling, so noble metal nanometer material shows the characteristics such as unique mechanics, electricity, optics, calorifics, magnetics, catalysis and superconduction.These unique performances make it in fields such as optics, sensor, catalysis and biological detection analyses, have important using value, thereby more and more get more and more people's extensive concerning.Another large feature of nano material is exactly that its character can change along with the change of size, pattern and composite construction thereof, so people's expectation can obtain structure, form, size adjustable by the method for simple green, be evenly distributed, the good noble metal nanometer material of stability.
In recent years, people attempt controlling by diverse ways and template the nanometer Pd material of synthetic different shape.For example, electrochemical deposition method, hydro-thermal method, template, sol-gal process etc.Wherein utilize biological template legal system to become a new trend for nanometer Pd material, as people (Journal of Colloid and Interface Science such as Alexander S.Freer, 2013,392,213 – 218) utilized the synthetic palladium nanometer rods of having prepared of tobacco mosaic virus (TMV) biological template, first they carry out genetic modification by tobacco mosaic virus (TMV), the amino acid of its capsid protein is changed to some extent, object is to adsorb better Pd nano particle, but has also increased the complexity of experimentation simultaneously.Preparation process is complicated, and manufacturing cycle extends.People (the Journal of Colloid and Interface Science such as Elizabeth S.Royston, 2009,332,402 – 407) be also that to utilize tobacco mosaic virus (TMV) be initial template, adhere to silicon thereon, then silicon/viral composite construction is prepared palladium nanometer rods as template, and experimentation is complicated, has improved production cost.People (J.Am.Chem.Soc, 2009,131 such as Yi Hsiu Chen, 9114 – 9121.) by the method for seed mediation, synthesize palladium nanometer rods, although synthesis technique has obtained simplification to a certain degree, the palladium nanometer rods knot pattern synthesizing differs, and structure is stable not.Also have some scholars to prepare palladium nanometer rods by electrochemical method, but the stability of pattern and size is all not ideal.
Summary of the invention
The object of the present invention is to provide that a kind of technique is simple, safe and harmless, productive rate is high, the palladium nanometer rods pattern bollworm baculoviral nucleocapsid that utilizes consistent, size uniform of preparation is prepared the method for precious metal palladium nanometer rods.The present invention is mainly the intrinsic pattern that utilizes bollworm baculoviral nucleocapsid, PdCl2 solution is directly joined in the bollworm baculoviral nucleocapsid solution of purification, through the hatching of special time, process, obtain thering is specific morphology, finely dispersed palladium nanometer rods.
Technical scheme of the present invention is as follows:
(1) preparation of bollworm baculoviral nucleocapsid:
The heliothis armigera nuclear polyhedrosis virus powder of every 1mg carries out ultrasonic dispersion with the ultra-pure water of 100 μ L, obtain linen polyhedral body suspension, in polyhedral body suspension: the ratio of the volume ratio=4～6:1 of alkali solution liquid, standing 15～25min add alkali solution liquid in polyhedral body suspension after, above-mentioned alkali solution liquid is 0.3mol/L sodium carbonate, the mixed solution of 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.The glacial acetic acid that is 0.5mol/L by concentration again regulates pH value to 7, by aforesaid liquid total amount: the mode of chloroform volume=4～6:1 adds chloroform, shakes 5～10min.After the centrifugal 5～10min of 5000～6000r/min, by supernatant liquid, it is supernatant sucking-off, every 4～6mL supernatant packs one into and surpasses from pipe, at 4～10 ℃, ultracentrifugation 1～2h under 25000～30000r/min, gained is precipitated to spot resuspended with PBS solution, PBS liquor capacity: volume=1:3～5 of former supernatant, obtain bollworm baculoviral nucleocapsid solution.
(2) preparation of precious metal palladium nanometer rods:
By bollworm baculoviral nucleocapsid solution: concentration is 5～10mMPdCl
2in the bollworm baculoviral nucleocapsid solution that the ratio of the volume=2～4:1 of solution makes to step (1), add PdCl
2solution, fully mixes, and in 20～30 ℃, under 130～170r/min, shaking table is hatched 15～25h, obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.
The present invention compares and has the following advantages with modern technologies:
1, directly adopt natural bollworm baculoviral nucleocapsid as template, raw material is simple and easy to get, safe and harmless, and production cost is low.
2, preparation method's technique is simple, mild condition, and environment-friendly high-efficiency, is easy to realize suitability for industrialized production.
3, the palladium nanometer rods pattern of preparation is stable, size homogeneous, and scattered, being expected to has important application at aspects such as catalytic fuel battery, catalytic car tail-gas and bio-sensings.
Accompanying drawing explanation
Fig. 1 is the purify TEM figure of low multiple of the bollworm baculoviral nucleocapsid that obtains of the embodiment of the present invention 1;
Fig. 2 is the low multiple palladium nanometer rods TEM figure that the embodiment of the present invention 1 prepares;
Fig. 3 is the purify TEM figure of high multiple of the bollworm baculoviral nucleocapsid that obtains of the embodiment of the present invention 2;
Fig. 4 is the high multiple palladium nanometer rods TEM figure that the embodiment of the present invention 2 prepares.
The specific embodiment
Embodiment 1
The heliothis armigera nuclear polyhedrosis virus powder of 50mg is disperseed with the cold ultra-pure water of 5mL, prepared by the PL5124-PALL model ultra-pure water instrument that ultra-pure water used is produced by pure water system Co., Ltd of Britain's High Wycombe city Vivendi, obtain linen polyhedral body suspension, to adding standing 15min after alkali solution liquid 1.25mL in polyhedral body suspension, described alkali solution liquid is 0.3mol/L sodium carbonate, the mixed solution of 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.The glacial acetic acid that is 0.5mol/L by concentration regulates pH value to 7, adds chloroform 1.25mL, concussion 5min.After the centrifugal 10min of 5000r/min, by supernatant liquid, be supernatant sucking-off, every 4mL supernatant packs one into and surpasses from pipe, at 4 ℃, centrifugal 1h under 28000r/min, precipitates spot by gained resuspended with 1.33mL PBS solution, obtains bollworm baculoviral nucleocapsid solution.
As shown in Figure 1, can find out that template used is rod shaped structure, bollworm baculoviral nucleocapsid in figure is evenly distributed, length is 280～400nm, diameter is 30～45nm, and pattern is intact, and concentration is moderate, only have small part virus nucleocapsid that flexural deformation or fracture have occurred, be suitable as the template of preparing palladium nanometer rods.
Get 300 μ L bollworm baculoviral nucleocapsid solution and add the PdCl that 100 μ L concentration are 5mM
2solution, fully mixes, and in 25 ℃, under 150r/min, shaking table is hatched 20h, obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.
As shown in Figure 3, can see that resulting palladium nanometer rods is uniformly distributed, not reunite, size and shape is consistent with template.
Embodiment 2
The heliothis armigera nuclear polyhedrosis virus powder of 50mg is disperseed with the cold ultra-pure water of 5mL, prepared by the PL5124-PALL model ultra-pure water instrument that ultra-pure water used is produced by pure water system Co., Ltd of Britain's High Wycombe city Vivendi, obtain linen polyhedral body suspension; To polyhedral body suspension, add standing 25min after alkali solution liquid 0.83mL, described alkali solution liquid is 0.3mol/L sodium carbonate, the mixed solution of 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.The glacial acetic acid that is 0.5mol/L by concentration regulates pH value to 7, adds chloroform 1.46mL, concussion 8min.After the centrifugal 5min of 6000r/min, by supernatant liquid, be supernatant sucking-off, every 6mL supernatant packs one into and surpasses from pipe, at 10 ℃, centrifugal 2h under 30000r/min, every gained precipitation spot is resuspended with 1.2mL PBS solution, obtain bollworm baculoviral nucleocapsid solution.
As shown in Figure 2, can see that baculoviral nucleocapsid is by a plurality of capsomere spirals stacking composition, the essence of capsomere is protein, so at the surface uniform of capsomere many active function groups that distributing, as hydroxyl, carboxyl, the forming core that these active function groups are noble metal provides site.And a lot of protein all has reproducibility, these protein with reproducibility are reduced to palladium atom being adsorbed on surperficial Pd ion, and palladium atom is assembled and become palladium nanometer rods on baculoviral nucleocapsid.
Get 500 μ L bollworm baculoviral nucleocapsid solution, add the PdCl that 250 μ L concentration are 5mM
2solution, fully mixes, and in 20 ℃, under 130r/min, shaking table is hatched 25h, obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.
As shown in Figure 4, the palladium nanorod surfaces in figure is smooth evenly, illustrates that palladium disperses uniformly in its template, and this nanometer rods is about as 300nm, and diameter is about 30nm.
Embodiment 3
The heliothis armigera nuclear polyhedrosis virus powder of 50mg is disperseed with the cold ultra-pure water of 5mL, prepared by the PL5124-PALL model ultra-pure water instrument that ultra-pure water used is produced by pure water system Co., Ltd of Britain's High Wycombe city Vivendi, obtain linen polyhedral body suspension, to adding standing 20min after 1mL alkali solution liquid in polyhedral body suspension, described alkali solution liquid is 0.3mol/L sodium carbonate, the mixed solution of 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.The glacial acetic acid that is 0.5mol/L by concentration regulates pH value to 7, adds chloroform 1mL, concussion 10min.After the centrifugal 10min of 5500r/min, by supernatant liquid, be supernatant sucking-off, every 5mL supernatant packs one into and surpasses from pipe, at 6 ℃, centrifugal 1.5h under 25000r/min, every gained precipitation spot is resuspended with 1.25mL PBS solution, obtain bollworm baculoviral nucleocapsid solution.
Get 300 μ L bollworm baculoviral nucleocapsid solution, add the PdCl that 75 μ L concentration are 10mM
2solution, fully mixes, and in 30 ℃, under 170r/min, shaking table is hatched 15h, obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.
Claims (2)
1. utilize bollworm baculoviral nucleocapsid to prepare a method for precious metal palladium nanometer rods, it is characterized in that, described method comprises the steps:
(1) preparation of bollworm baculoviral nucleocapsid:
The heliothis armigera nuclear polyhedrosis virus powder of every 1mg carries out ultrasonic dispersion with the ultra-pure water of 100 μ L, obtain linen polyhedral body suspension, in polyhedral body suspension: the ratio of the volume ratio=4～6:1 of alkali solution liquid, standing 15～25min add alkali solution liquid in polyhedral body suspension after, the glacial acetic acid that is 0.5mol/L by concentration again regulates pH value to 7, by aforesaid liquid total amount: the mode of chloroform volume=4～6:1 adds chloroform, concussion 5～10min, after the centrifugal 5～10min of 5000～6000r/min, by supernatant liquid, it is supernatant sucking-off, every 4～6mL supernatant packs one into and surpasses from pipe, at 4～10 ℃, ultracentrifugation 1～2h under 25000～30000r/min, gained is precipitated to spot resuspended with PBS solution, PBS liquor capacity: volume=1:3～5 of former supernatant, obtain bollworm baculoviral nucleocapsid solution,
(2) preparation of precious metal palladium nanometer rods:
By bollworm baculoviral nucleocapsid solution: concentration is 5～10mMPdCl
2in the bollworm baculoviral nucleocapsid solution that the ratio of the volume=2～4:1 of solution makes to step (1), add PdCl
2solution, fully mixes, and in 20～30 ℃, under 130～170r/min, shaking table is hatched 15～25h, obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.
2. the preparation method of the noble metal nano particles of caryogram polyhedrin according to claim 1 load, it is characterized in that: described alkali solution liquid is 0.3mol/L sodium carbonate the mixed solution of 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410197014.7A CN104001931B (en) | 2014-05-12 | 2014-05-12 | Bollworm baculoviral nucleocapsid is utilized to prepare the method for precious metal palladium nanometer rods |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410197014.7A CN104001931B (en) | 2014-05-12 | 2014-05-12 | Bollworm baculoviral nucleocapsid is utilized to prepare the method for precious metal palladium nanometer rods |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104001931A true CN104001931A (en) | 2014-08-27 |
| CN104001931B CN104001931B (en) | 2016-01-06 |
Family
ID=51362997
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410197014.7A Active CN104001931B (en) | 2014-05-12 | 2014-05-12 | Bollworm baculoviral nucleocapsid is utilized to prepare the method for precious metal palladium nanometer rods |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104001931B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104668579A (en) * | 2015-02-11 | 2015-06-03 | 燕山大学 | Method for preparing palladium nano wires by use of heliothis armigera nuclear polyhedrin |
| CN104741618A (en) * | 2015-02-13 | 2015-07-01 | 燕山大学 | Method for preparing platinum nanowires through helicoverpa armigera nuclear polyhedron extractives |
| CN114769610A (en) * | 2022-04-02 | 2022-07-22 | 西北工业大学 | Method for preparing gold-palladium nano alloy by using protein assembly |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6783569B2 (en) * | 2001-08-16 | 2004-08-31 | Korea Advanced Institute Of Science And Technology | Method for synthesis of core-shell type and solid solution alloy type metallic nanoparticles via transmetalation reactions and applications of same |
| CN1795141A (en) * | 2003-05-13 | 2006-06-28 | 新留康郎 | Method for preparation of metal nano-rod and use thereof |
| CN101130883A (en) * | 2006-08-22 | 2008-02-27 | 国家纳米科学中心 | Rectangular bimetallic nano rod with gold nucleus and palladium shell and method for making the same |
| CN101229920A (en) * | 2007-12-07 | 2008-07-30 | 燕山大学 | Method for preparing beta-BC2N nano-rod under temperate condition |
| CN101530923A (en) * | 2009-02-25 | 2009-09-16 | 同济大学 | Method for preparing Fe-Ni-Pt alloy nanorod |
| CN103170641A (en) * | 2013-03-19 | 2013-06-26 | 燕山大学 | Method of preparing platinum nano particles by using cotton bollworm karyotype polyhedrin |
-
2014
- 2014-05-12 CN CN201410197014.7A patent/CN104001931B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6783569B2 (en) * | 2001-08-16 | 2004-08-31 | Korea Advanced Institute Of Science And Technology | Method for synthesis of core-shell type and solid solution alloy type metallic nanoparticles via transmetalation reactions and applications of same |
| CN1795141A (en) * | 2003-05-13 | 2006-06-28 | 新留康郎 | Method for preparation of metal nano-rod and use thereof |
| CN101130883A (en) * | 2006-08-22 | 2008-02-27 | 国家纳米科学中心 | Rectangular bimetallic nano rod with gold nucleus and palladium shell and method for making the same |
| CN101229920A (en) * | 2007-12-07 | 2008-07-30 | 燕山大学 | Method for preparing beta-BC2N nano-rod under temperate condition |
| CN101530923A (en) * | 2009-02-25 | 2009-09-16 | 同济大学 | Method for preparing Fe-Ni-Pt alloy nanorod |
| CN103170641A (en) * | 2013-03-19 | 2013-06-26 | 燕山大学 | Method of preparing platinum nano particles by using cotton bollworm karyotype polyhedrin |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104668579A (en) * | 2015-02-11 | 2015-06-03 | 燕山大学 | Method for preparing palladium nano wires by use of heliothis armigera nuclear polyhedrin |
| CN104741618A (en) * | 2015-02-13 | 2015-07-01 | 燕山大学 | Method for preparing platinum nanowires through helicoverpa armigera nuclear polyhedron extractives |
| CN114769610A (en) * | 2022-04-02 | 2022-07-22 | 西北工业大学 | Method for preparing gold-palladium nano alloy by using protein assembly |
| CN114769610B (en) * | 2022-04-02 | 2023-08-11 | 西北工业大学 | Method for preparing gold-palladium nano alloy by utilizing protein assembly |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104001931B (en) | 2016-01-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106987922B (en) | The cellulose nano-fibrous electrostatic spinning preparation method of hollow porous structure | |
| CN103500622B (en) | Magnetism inorganic nanoparticle/ordered mesopore silica nuclear shell composite microsphere and preparing method thereof | |
| CN107486157B (en) | Multi-walled carbon nanotube/metal organic framework composite material and preparation method | |
| CN104001931A (en) | Method for preparing precious metal palladium nanorod by means of cotton bollworm baculovirus nucleocapsid | |
| CN110075770A (en) | Magnetic order mesoporous carbon-based or polymer-based core-shell structure microballoon and preparation method thereof | |
| CN107626283B (en) | Utilize the method for antibiotic in multi-walled carbon nanotube/metal organic framework composite material adsorbed water body | |
| CN103170641B (en) | Method of preparing platinum nano particles by using cotton bollworm karyotype polyhedrin | |
| CN104403132B (en) | Preparation method for cellulose based nano silver composite material | |
| CN104324756A (en) | Preparation method and applications of mesoporous metal organic complex base composite material | |
| CN105731535B (en) | A kind of preparation method of Zinc oxide/titanium dioxide composite nano materials | |
| CN112457676B (en) | Preparation method of metal organic framework/precious metal simple substance nanocomposite | |
| CN103011182A (en) | Synthesis method of vesicular mesoporous silicon dioxide | |
| CN102225470A (en) | Method for preparing gold nanoparticles based on environmentally-friendly chemical method | |
| CN110152683A (en) | One kind can rotation magnetic nano chain supported palladium nano-particle catalyst and preparation method thereof | |
| CN105565360A (en) | Method for synthesizing and controlling cerium dioxide micro-nano structure and morphology by hydrothermal process | |
| CN102874823A (en) | Method for preparing silicon dioxide hollow microspheres with uniform shape by taking pollen grains as biological template | |
| CN103359773A (en) | Preparation method of zinc oxide nanorod | |
| CN205886517U (en) | Air filter | |
| Chen et al. | Self-catalyzed strategy to form hollow carbon nanospheres for CO2 capture | |
| CN101891208B (en) | Method for preparing submicron silicon dioxide spherical particles | |
| CN102941118A (en) | Au nanometer core-shell structure catalyst and preparation method thereof | |
| CN104741618B (en) | Utilize the method that bollworm polyhedrosis protein extract prepares Pt nanowires | |
| CN104437658B (en) | Porous silicon oxide nano material as well as preparation method and application thereof | |
| CN110842212A (en) | Superfine Pd tetrahedral nano material and preparation method and application thereof | |
| CN102718255B (en) | Preparation method of titanium dioxide hollow nano structure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |