CN104001931B - Bollworm baculoviral nucleocapsid is utilized to prepare the method for precious metal palladium nanometer rods - Google Patents
Bollworm baculoviral nucleocapsid is utilized to prepare the method for precious metal palladium nanometer rods Download PDFInfo
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Abstract
A kind of method utilizing bollworm baculoviral nucleocapsid to prepare precious metal palladium nanometer rods, heliothis armigera nuclear polyhedrosis virus powder ultra-pure water is mainly carried out dispersion and obtains linen polyhedral body suspension by the method, 15 ~ 25min is left standstill add alkali solution liquid in polyhedral body suspension after, chloroform is added again with after glacial acetic acid adjust ph to 7, after the centrifugal 5 ~ 10min of 5000 ~ 6000r/min, by supernatant sucking-off, at 4 ~ 10 DEG C, centrifugal 1 ~ 2h under 25000 ~ 30000r/min, gained is precipitated spot PBS solution resuspended, obtain bollworm baculoviral nucleocapsid solution, PdCl is added in this solution
2solution, fully mixes, and in 20 ~ 30 DEG C, under 130 ~ 170r/min, shaking table hatching 15 ~ 25h, namely obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.Present invention process is simple, and environment-friendly high-efficiency, is easy to realize suitability for industrialized production; The palladium nanometer rods stable appearance of preparation, size uniformity.
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-interface 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.The performance of these uniquenesses makes it have important using value in fields such as optics, sensor, catalysis and biological detection analyses, thus more and more gets 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 expect can obtain structure, form, size adjustable by simple green method, be evenly distributed, the good noble metal nanometer material of stability.
In recent years, people's trial diverse ways and template control the nanometer Pd material synthesizing different shape.Such as, electrochemical deposition method, hydro-thermal method, template, sol-gal process etc.Biological template legal system is wherein utilized to become a new trend for nanometer Pd material, as the people such as AlexanderS.Freer (JournalofColloidandInterfaceScience, 2013,392,213 – 218) make use of tobacco mosaic virus (TMV) biological template synthesis prepared palladium nanometer rods, first tobacco mosaic virus (TMV) is carried out genetic modification by them, the amino acid of its capsid protein is changed to some extent, object adsorbs Pd nano particle better, but too increase the complexity of experimentation simultaneously.Preparation process is complicated, and manufacturing cycle extends.The people such as ElizabethS.Royston (JournalofColloidandInterfaceScience, 2009,332,402 – 407) be also utilize tobacco mosaic virus (TMV) to be initial template, adhere to silicon thereon, then silicon/viral composite construction is as Template preparation palladium nanometer rods, and experimentation is complicated, improves production cost.The people such as YiHsiuChen (J.Am.Chem.Soc, 2009,131,9114 – 9121.) synthesize palladium nanometer rods by the method for seed mediation, although synthesis technique obtains simplification to a certain degree, the palladium nanometer rods knot pattern synthesized 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 consistent appearance of preparation, the bollworm baculoviral nucleocapsid that utilizes of size uniform prepare the method for precious metal palladium nanometer rods.The present invention mainly utilizes the intrinsic pattern of bollworm baculoviral nucleocapsid, by PdCl
2solution directly joins in the bollworm baculoviral nucleocapsid solution of purification, through the hatching process of special time, obtains having 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 disperse with the ultra-pure water of 100 μ L, obtain linen polyhedral body suspension, in polyhedral body suspension: the volume ratio of alkali solution liquid is the ratio of 4 ~ 6:1,15 ~ 25min is left standstill add alkali solution liquid in polyhedral body suspension after, above-mentioned alkali solution liquid is the mixed solution of 0.3mol/L sodium carbonate, 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.Be the glacial acetic acid adjust ph to 7 of 0.5mol/L again by concentration, in aforesaid liquid total amount: the volume ratio of chloroform is that the ratio of 4 ~ 6:1 adds chloroform, concussion 5 ~ 10min, after the centrifugal 5 ~ 10min of 5000 ~ 6000r/min, by supernatant liquid and supernatant sucking-off, every 4 ~ 6mL supernatant loads one and surpasses from pipe, at 4 ~ 10 DEG C, ultracentrifugation 1 ~ 2h under 25000 ~ 30000r/min, gained is precipitated spot PBS solution resuspended, PBS solution: the volume ratio of supernatant is 1:3 ~ 5, obtains bollworm baculoviral nucleocapsid solution;
(2) preparation of precious metal palladium nanometer rods:
By bollworm baculoviral nucleocapsid solution: concentration is the PdCl of 5 ~ 10mM
2the volume ratio of solution is that the ratio of 2 ~ 4:1 adds PdCl in the obtained bollworm baculoviral nucleocapsid solution of step (1)
2solution, fully mixes, and in 20 ~ 30 DEG C, under 130 ~ 170r/min, shaking table hatching 15 ~ 25h, namely obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.
The present invention has the following advantages compared 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, and mild condition, environment-friendly high-efficiency, is easy to realize suitability for industrialized production.
3, the palladium nanometer rods stable appearance of preparation, size uniformity, scattered, be expected to there is important application in catalytic fuel cell, catalytic car tail-gas and bio-sensing etc.
Accompanying drawing explanation
Fig. 1 be the embodiment of the present invention 1 purify the bollworm baculoviral nucleocapsid obtained low multiple TEM figure;
Fig. 2 is that the low multiple palladium nanometer rods TEM that the embodiment of the present invention 1 prepares schemes;
Fig. 3 be the embodiment of the present invention 2 purify the bollworm baculoviral nucleocapsid obtained high multiple TEM figure;
Fig. 4 is that the high multiple palladium nanometer rods TEM that the embodiment of the present invention 2 prepares schemes.
Detailed description of the invention
Embodiment 1
Ultra-pure water cold for the heliothis armigera nuclear polyhedrosis virus powder 5mL of 50mg is disperseed, prepared by the PL5124-PALL model ultra-pure water instrument that ultra-pure water used is produced by pure water system Co., Ltd of Vivendi of High Wycombe city of Britain, obtain linen polyhedral body suspension, 15min is left standstill add alkali solution liquid 1.25mL in polyhedral body suspension after, described alkali solution liquid is the mixed solution of 0.3mol/L sodium carbonate, 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.By the glacial acetic acid adjust ph to 7 that concentration is 0.5mol/L, add chloroform 1.25mL, concussion 5min.After the centrifugal 10min of 5000r/min, by supernatant liquid and supernatant sucking-off, every 4mL supernatant loads one and surpasses from pipe, and at 4 DEG C, centrifugal 1h under 28000r/min, precipitates spot 1.33mLPBS solution resuspended by gained, obtains bollworm baculoviral nucleocapsid solution.
As shown in Figure 1, can find out that template used is rod-like structure, bollworm baculoviral nucleocapsid in figure is evenly distributed, length is 280 ~ 400nm, diameter is 30 ~ 45nm, and pattern is intact, moderate concentration, only have small part virus nucleocapsid to there occurs flexural deformation or fracture, be suitable as the template preparing palladium nanometer rods.
Getting 300 μ L bollworm baculoviral nucleocapsid solution, to add 100 μ L concentration be the PdCl of 5mM
2solution, fully mixes, and in 25 DEG C, under 150r/min, shaking table hatching 20h, namely obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.
As shown in Figure 3, can see that obtained palladium nanometer rods is uniformly distributed, do not reunite, size and shape is consistent with template.
Embodiment 2
Ultra-pure water cold for the heliothis armigera nuclear polyhedrosis virus powder 5mL of 50mg is disperseed, prepared by the PL5124-PALL model ultra-pure water instrument that ultra-pure water used is produced by pure water system Co., Ltd of Vivendi of High Wycombe city of Britain, obtain linen polyhedral body suspension; Leave standstill 25min after adding alkali solution liquid 0.83mL to polyhedral body suspension, described alkali solution liquid is the mixed solution of 0.3mol/L sodium carbonate, 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.By the glacial acetic acid adjust ph to 7 that concentration is 0.5mol/L, add chloroform 1.46mL, concussion 8min.After the centrifugal 5min of 6000r/min, by supernatant liquid and supernatant sucking-off, every 6mL supernatant loads one and surpasses from pipe, at 10 DEG C, centrifugal 2h under 30000r/min, often will prop up gained precipitation spot 1.2mLPBS solution resuspended, obtain bollworm baculoviral nucleocapsid solution.
As shown in Figure 2, can see that baculoviral nucleocapsid forms by multiple capsomere spiral is stacking, the essence of capsomere is protein, so be dispersed with many active function groups at the surface uniform of capsomere, 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 palladium atom being adsorbed on surperficial Pd ion reduction, and palladium atom is assembled on baculoviral nucleocapsid becomes palladium nanometer rods.
Get 500 μ L bollworm baculoviral nucleocapsid solution, adding 250 μ L concentration is the PdCl of 5mM
2solution, fully mixes, and in 20 DEG C, under 130r/min, shaking table hatching 25h, namely obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.
As shown in Figure 4, the palladium nanorod surfaces smooth even in figure, illustrate that palladium disperses uniformly in its template, this nanometer rods is about as 300nm, and diameter is about 30nm.
Embodiment 3
Ultra-pure water cold for the heliothis armigera nuclear polyhedrosis virus powder 5mL of 50mg is disperseed, prepared by the PL5124-PALL model ultra-pure water instrument that ultra-pure water used is produced by pure water system Co., Ltd of Vivendi of High Wycombe city of Britain, obtain linen polyhedral body suspension, 20min is left standstill add 1mL alkali solution liquid in polyhedral body suspension after, described alkali solution liquid is the mixed solution of 0.3mol/L sodium carbonate, 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.By the glacial acetic acid adjust ph to 7 that concentration is 0.5mol/L, add chloroform 1mL, concussion 10min.After the centrifugal 10min of 5500r/min, by supernatant liquid and supernatant sucking-off, every 5mL supernatant loads one and surpasses from pipe, at 6 DEG C, centrifugal 1.5h under 25000r/min, often will prop up gained precipitation spot 1.25mLPBS solution resuspended, obtain bollworm baculoviral nucleocapsid solution.
Get 300 μ L bollworm baculoviral nucleocapsid solution, adding 75 μ L concentration is the PdCl of 10mM
2solution, fully mixes, and in 30 DEG C, under 170r/min, shaking table hatching 15h, namely 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 disperse with the ultra-pure water of 100 μ L, obtain linen polyhedral body suspension, in polyhedral body suspension: the volume ratio of alkali solution liquid is the ratio of 4 ~ 6:1, 15 ~ 25min is left standstill add alkali solution liquid in polyhedral body suspension after, be the glacial acetic acid adjust ph to 7 of 0.5mol/L again by concentration, in aforesaid liquid total amount: the volume ratio of chloroform is that the ratio of 4 ~ 6:1 adds chloroform, concussion 5 ~ 10min, after the centrifugal 5 ~ 10min of 5000 ~ 6000r/min, by supernatant liquid and supernatant sucking-off, every 4 ~ 6mL supernatant loads one and surpasses from pipe, at 4 ~ 10 DEG C, ultracentrifugation 1 ~ 2h under 25000 ~ 30000r/min, gained is precipitated spot PBS solution resuspended, PBS solution: the volume ratio of supernatant is 1:3 ~ 5, obtain bollworm baculoviral nucleocapsid solution,
(2) preparation of precious metal palladium nanometer rods:
By bollworm baculoviral nucleocapsid solution: concentration is the PdCl of 5 ~ 10mM
2the volume ratio of solution is that the ratio of 2 ~ 4:1 adds PdCl in the obtained bollworm baculoviral nucleocapsid solution of step (1)
2solution, fully mixes, and in 20 ~ 30 DEG C, under 130 ~ 170r/min, shaking table hatching 15 ~ 25h, namely obtains the precious metal palladium nanometer rods of bollworm baculoviral nucleocapsid load.
2. the method utilizing bollworm baculoviral nucleocapsid to prepare precious metal palladium nanometer rods according to claim 1, it is characterized in that: described alkali solution liquid is the mixed solution of 0.3mol/L sodium carbonate, 0.5mol/L sodium chloride and 0.03mol/L disodium ethylene diamine tetraacetate.
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| CN104741618B (en) * | 2015-02-13 | 2016-10-05 | 燕山大学 | Utilize the method that bollworm polyhedrosis protein extract prepares Pt nanowires |
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