CN109158614A - A kind of preparation method of gold nanoparticle - Google Patents
A kind of preparation method of gold nanoparticle Download PDFInfo
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- CN109158614A CN109158614A CN201811085484.9A CN201811085484A CN109158614A CN 109158614 A CN109158614 A CN 109158614A CN 201811085484 A CN201811085484 A CN 201811085484A CN 109158614 A CN109158614 A CN 109158614A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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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- 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
The present invention provides a kind of preparation methods of gold nanoparticle, and Polygonum polysaccharide solution and chlorauric acid solution are mixed, the reduction reaction of gold chloride is carried out, gained reduzate system is dialysed, gold nanoparticle is obtained.The present invention prepares gold nanoparticle by template of Polygonum polysaccharide, has the advantages that materials are convenient, low in cost and raw material is environmentally friendly；The stable gold nanoparticle of the Polygonum polysaccharide of preparation, which was able to maintain in aqueous solution in one week, to be stablized, no aggregation and precipitating；Preparation condition is mild, easy to operate, reaction process is easily controllable, and the partial size of the gold nanoparticle of preparation is 16~25nm, and uniform particle sizes have high catalytic efficiency to morin.
Description
Technical field
The present invention relates to nano metal material technical field more particularly to a kind of preparation methods of gold nanoparticle.
Background technique
Nowadays, environmental pollution is increasingly severe, and organic pollution is wherein in occupation of greatly.And nanoscale goldc grains
Son has efficient catalytic degradation effect to some organic pollutants, but gold nanoparticle has easy aggregation, to lead
The shortcomings that causing catalytic activity to reduce.This disadvantage for how solving gold nanoparticle becomes people and tries to be the first the hot spot of research.Nowadays
The most commonly used is physical methods and chemical method, although more to the research of both methods both at home and abroad, technology is also more mature,
The disadvantages of being their there is production costs higher, severe reaction conditions and environment easy to pollute.Such as utilize different electronations
Agent NaBH4, polyethylene glycol, dimethyamine borane etc. also prepare palladium nano-particles originally.
It is the green synthesis techniques newly risen in recent years that biological reducing method, which prepares metal nanoparticle, this method has many excellent
Point, such as reducing condition is mild, pollution-free, biological source is wide.Wang Wenta etc. plants plant using Xiamen area more than more typical 40
Object and microorganism are prepared for the gold nanoparticle of 10~135nm as reducing agent, and find flavonoids and phenols may be biology
Reduction method prepares the main reducing substances of gold nano grain.However, the gold nanoparticle of such reducing agent preparation is in aqueous solution
Stability it is poor.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of gold nanoparticle, Jenner's grain of rice that this method is prepared
Stability is good in aqueous solution for son.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of gold nanoparticle, comprising the following steps:
Polygonum polysaccharide solution and chlorauric acid solution are mixed, the reduction reaction of gold chloride is carried out, by gained reduzate
System is dialysed, and gold nanoparticle is obtained.
Preferably, the mass concentration of the Polygonum polysaccharide solution is 0.1~30mg/mL.
Preferably, the mass concentration of the chlorauric acid solution is 0.1~20mmol/mL.
Preferably, the molar ratio of the gold chloride in the Polygonum polysaccharide and chlorauric acid solution in the Polygonum polysaccharide solution
For 1:10~40.
Preferably, the reduction reaction carries out under agitation, and the revolving speed of the stirring is 400~1000rpm.
Preferably, the temperature of the reduction reaction is 50~70 DEG C.
Preferably, the time of the reduction reaction is 4~8h.
Preferably, the molecular cut off of bag filter used by the dialysis is 8000~14000.
The present invention provides a kind of preparation method of gold nanoparticle, the present invention prepares Jenner by template of Polygonum polysaccharide
Rice corpuscles has the advantages that materials are convenient, low in cost and raw material is environmentally friendly；
The stable gold nanoparticle of Polygonum polysaccharide prepared by the present invention, which was able to maintain in aqueous solution in one week, to be stablized, nothing
Aggregation and precipitating；
Method preparation condition of the invention is mild, easy to operate, reaction process is easily controllable；
The partial size of gold nanoparticle prepared by the present invention is 16~25nm, and uniform particle sizes have high catalysis to morin
Efficiency.
Detailed description of the invention
Fig. 1 is the TEM figure for 10 nanoparticle of Polygonum polysaccharide-gold that the embodiment of the present invention 1 obtains；
Fig. 2 is the transmission electron microscope particle diameter distribution histogram for 10 nanoparticle of Polygonum polysaccharide-gold that the embodiment of the present invention 1 obtains
Figure；
Fig. 3 is the 10 nano particle catalysis morin of Polygonum polysaccharide-gold of the acquisition of the embodiment of the present invention 1 at λ=403nm
Ln (Ct/C0) and the reaction time (t) between graph of relation；
Fig. 4 is the TEM figure for 20 nanoparticle of Polygonum polysaccharide-gold that the embodiment of the present invention 2 obtains；
Fig. 5 is the transmission electron microscope particle diameter distribution histogram for 20 nanoparticle of Polygonum polysaccharide-gold that the embodiment of the present invention 2 obtains
Figure；
Fig. 6 is the 20 nano particle catalysis morin of Polygonum polysaccharide-gold of the acquisition of the embodiment of the present invention 2 at λ=403nm
Ln (Ct/C0) and the reaction time (t) between graph of relation；
Fig. 7 is the TEM figure for 30 nanoparticle of Polygonum polysaccharide-gold that the embodiment of the present invention 3 obtains；
Fig. 8 is the transmission electron microscope particle diameter distribution histogram for 30 nanoparticle of Polygonum polysaccharide-gold that the embodiment of the present invention 3 obtains
Figure；
Fig. 9 is the 30 nano particle catalysis morin of Polygonum polysaccharide-gold of the acquisition of the embodiment of the present invention 3 at λ=403nm
Ln (Ct/C0) and the reaction time (t) between graph of relation；
Figure 10 is the TEM figure for 40 nanoparticle of Polygonum polysaccharide-gold that the embodiment of the present invention 4 obtains；
Figure 11 is that the transmission electron microscope particle diameter distribution for 40 nanoparticle of Polygonum polysaccharide-gold that the embodiment of the present invention 4 obtains is straight
Fang Tu；
Figure 12 is the 40 nano particle catalysis morin of Polygonum polysaccharide-gold of the acquisition of the embodiment of the present invention 4 in λ=403nm
Ln (the C at placet/C0) and the reaction time (t) between graph of relation.
Specific embodiment
The present invention provides a kind of preparation methods of gold nanoparticle, comprising the following steps:
Polygonum polysaccharide solution and chlorauric acid solution are mixed, the reduction reaction of gold chloride is carried out, by gained reduzate
System is dialysed, and gold nanoparticle is obtained.
In the present invention, the mass concentration of the Polygonum polysaccharide solution is preferably 0.1~30mg/mL, more preferably 1~
25mg/mL, most preferably 5~20mg/mL.Polygonum polysaccharide is preferably dissolved in deionized water by the present invention obtains Polygonum polysaccharide
Solution.
In the present invention, the Polygonum polysaccharide preparation method the following steps are included:
20g fleece-flower root powder is weighed, is fitted into 250mL flask, (volume fraction is by fleece-flower root powder and ethanol solution
80%) solid-liquid ratio is 1:10, and 200mL ethanol solution is added in flask, and 90min is stirred in 70 DEG C of waters bath with thermostatic control, is centrifuged, filter
Solvent out, dry residue, the fleece-flower root powder after obtaining degreasing；
The fleece-flower root powder after 2g degreasing accurately is weighed, is added in 50mL flask, it will in the ratio that solid-liquid ratio is 1:15
30mL distilled water is added in flask, stirs 90min in 90 DEG C of waters bath with thermostatic control, centrifugation, and obtained residue is repeated above-mentioned side
Method is extracted 1 time again, and centrifugation collects the supernatant extracted twice and mixing, obtains fleece-flower root Thick many candies aqueous solution；It is thick to the fleece-flower root
The hydrogen peroxide that 10mL volume fraction is 30% is added in polysaccharide solution, decolourize 2h in 50 DEG C of thermostat water baths, is decolourized
Polygonum polysaccharide solution afterwards.
By n-butanol, 5:1 is mixed to get sevaga reagent by volume with chloroform, by volume by gained sevaga reagent
1:5 is added in the Polygonum polysaccharide solution after decoloration, is acutely shaken after mixing, is centrifuged, solvent layer and water layer intersection are gone out
Existing cotton-shaped protein precipitation separation, is repeated several times centrifugation and the operation of protein isolate matter, until water layer and solvent layer intersection
Until without cotton-shaped protein, then acquired solution is dialysed through bag filter, is freeze-dried, obtains Polygonum polysaccharide.
In the present invention, the mass concentration of the chlorauric acid solution is preferably 0.1~20mmol/mL, more preferably 5~
15mmol/mL, most preferably 8~12mmol/mL.Gold chloride is preferably dissolved in deionized water and obtains chlorauric acid solution by the present invention.
In the present invention, gold chloride in the Polygonum polysaccharide and chlorauric acid solution in the Polygonum polysaccharide solution rubs
You are than being preferably 1:10~40, more preferably 1:20~30.
In the present invention, the reduction reaction preferably carries out under agitation, and the revolving speed of the stirring is preferably 400~
1000rpm, more preferably 600~800rpm.
In the present invention, the temperature of the reduction reaction is preferably 50~70 DEG C, and more preferably 55~65 DEG C.
In the present invention, the time of the reduction reaction is preferably 4~8h, more preferably 5~6h.The present invention is preferably in perseverance
The reduction reaction is carried out in warm metal blending instrument.
In the present invention, the molecular cut off of bag filter used by the dialysis is preferably 8000~14000.The present invention
It is preferred that dialysing when aubergine is presented in reaction solution.The present invention does not have special limitation to the mode of the dialysis, selects
Mode well known to those skilled in the art is dialysed.The present invention removes the impurity such as chloride ion by dialysis.
After completing the dialysis, the present invention preferably collects dialysis acquired solution, obtains the aqueous solution of gold nanoparticle, so
It is afterwards that the aqueous solution of gold nanoparticle is dry, obtain gold nanoparticle.
It is described in detail below with reference to preparation method of the embodiment to gold nanoparticle provided by the invention, but not
They can be interpreted as limiting the scope of the present invention.
Embodiment 1
Polygonum polysaccharide is dissolved in deionized water, the Polygonum polysaccharide solution of 0.1mg/mL is configured to, by 0.1mg/mL
Polygonum polysaccharide solution and chlorauric acid solution are mixed in centrifugation in the ratio that the molar ratio of Polygonum polysaccharide and gold chloride is 1:10
Centrifuge tube is put into thermostat metal blending instrument by Guan Zhong, and the revolving speed of setting thermostat metal blending instrument is 400rpm, and thermostat metal is mixed
The temperature of even instrument is 50 DEG C, carries out reduction reaction 4h, becomes aubergine to reaction solution, be 8000-14000 with molecular cut off
Bag filter dialysis solution, obtain 10 nanoparticle of Polygonum polysaccharide-gold solution.
Through experiments, it was found that 10 nano-particle solution of Polygonum polysaccharide-gold without aggregation or precipitates in one week, divide well
It dissipates in aqueous solution.
Fig. 1 is the transmission electron microscope picture of 10 nanoparticle of Polygonum polysaccharide-gold, shows that its pattern is spherical.Fig. 2 is in Fig. 1
Polygonum polysaccharide-gold nanoparticle particle diameter distribution histogram, it shows Polygonum polysaccharide-gold 10 nanoparticle of preparation
Partial size is 16.45 ± 4.27nm, and 10 nanoparticle of Polygonum polysaccharide-gold has the characteristics that compared with small particle.
It takes the morin solution of 30 μ L 5mM in cuvette, 1910 μ L deionized waters is added, it is 2 μM that 30 μ L concentration, which are added,
10 nano-particle solution of Polygonum polysaccharide-gold (10 nano-particle solution of Polygonum polysaccharide-gold prepared by embodiment 1 is prepared
Into), then to the hydrogenperoxide steam generator of 30 μ L 0.4mg/mL of cuvette addition, extinction under 403nm is surveyed with ultraviolet specrophotometer
Degree changes over time curve.As shown in figure 3, show 10 nanoparticle of Polygonum polysaccharide-gold can catalysis oxidation morin, this is anti-
It should be pseudo-first-order reaction；The ratio of the amount of substance of 10 nanoparticle of Polygonum polysaccharide-gold and morin is 1:2500, this reaction is urged
Changing rate constant is 5.97 × 10-3s-1, this reacts catalytic efficiency with higher.
Embodiment 2
Polygonum polysaccharide is dissolved in deionized water, the Polygonum polysaccharide solution of 1mg/mL is configured to, what is first by 1mg/mL
Black polysaccharide solution and chlorauric acid solution are mixed in centrifuge tube in the ratio that the molar ratio of Polygonum polysaccharide and gold chloride is 1:20,
Centrifuge tube is put into thermostat metal blending instrument, the revolving speed of setting thermostat metal blending instrument is 500rpm, thermostat metal blending instrument
Temperature is 55 DEG C, carries out reduction reaction 5h, becomes aubergine to reaction solution, the dialysis for being 8000-14000 with molecular cut off
Bag dialysis solution, that is, obtain the solution of 20 nanoparticle of Polygonum polysaccharide-gold.
Through experiments, it was found that tuber of multiflower knotweed polysaccharide -20 nano-particle solution of gold without aggregation or precipitates in one week, disperse well
In aqueous solution.
Fig. 4 is the transmission electron microscope picture of Polygonum polysaccharide-gold 70, shows that its pattern is spherical.Fig. 5 is the fleece-flower root in Fig. 4
Polysaccharide-gold nanoparticle particle diameter distribution histogram, it shows that the partial size of 20 nanoparticle of Polygonum polysaccharide-gold of preparation is
17.44 ± 11.15nm, 20 nanoparticle of Polygonum polysaccharide-gold have the characteristics that compared with small particle.
It takes the morin solution of 30 μ L 5mM in cuvette, 1910 μ L deionized waters is added, it is 2 μM that 30 μ L concentration, which are added,
20 nano-particle solution of Polygonum polysaccharide-gold (20 nano-particle solution of Polygonum polysaccharide-gold prepared by embodiment 2 is prepared
Into), then to the hydrogenperoxide steam generator of 30 μ L 0.4mg/ml of cuvette addition, extinction under 403nm is surveyed with ultraviolet specrophotometer
Degree changes over time curve.As shown in fig. 6, show 20 nanoparticle of Polygonum polysaccharide-gold can catalysis oxidation morin, this is anti-
It should be pseudo-first-order reaction；The ratio of the amount of substance of 20 nanoparticle of Polygonum polysaccharide-gold and morin is 1:2500, this reaction is urged
Changing rate constant is 3.57 × 10-3s-1, this reacts catalytic efficiency with higher.
Embodiment 3
Polygonum polysaccharide is dissolved in deionized water, the Polygonum polysaccharide solution of 10mg/mL is configured to, by 10mg/mL what
Tuber of multiflower knotweed polysaccharide solution and chlorauric acid solution are mixed in centrifuge tube in the ratio that the molar ratio of Polygonum polysaccharide and gold chloride is 1:30
In, centrifuge tube is put into thermostat metal blending instrument, the revolving speed of setting thermostat metal blending instrument is 700rpm, and thermostat metal mixes
Instrument temperature is 60 DEG C, carries out reduction reaction 6h, becomes aubergine to reaction solution, be the saturating of 8000-14000 with molecular cut off
Analysis bag is dialysed final solution, that is, obtains the solution of 30 nanoparticle of Polygonum polysaccharide-gold.
Through experiments, it was found that tuber of multiflower knotweed polysaccharide -30 nano-particle solution of gold without aggregation or precipitates in one week, disperse well
In aqueous solution.
Fig. 7 is the transmission electron microscope picture of 30 nanoparticle of Polygonum polysaccharide-gold, shows that its pattern is spherical.
Fig. 8 is Polygonum polysaccharide-gold nanoparticle particle diameter distribution histogram in Fig. 7, it shows the fleece-flower root of preparation
The partial size of 30 nanoparticle of polysaccharide-gold is 16.62 ± 7.46nm, and 30 nanoparticle of Polygonum polysaccharide-gold has compared with small particle
Feature.
It takes the morin solution of 30 μ L 5mM in cuvette, 1910 μ L deionized waters is added, it is 2 μM that 30 μ L concentration, which are added,
30 nano-particle solution of Polygonum polysaccharide-gold (30 nano-particle solution of Polygonum polysaccharide-gold prepared by embodiment 3 is prepared
Into), then to the hydrogenperoxide steam generator of 30 μ L 0.4mg/ml of cuvette addition, extinction under 403nm is surveyed with ultraviolet specrophotometer
Degree changes over time curve.As shown in figure 3, show 30 nanoparticle of Polygonum polysaccharide-gold can catalysis oxidation morin, this is anti-
It should be pseudo-first-order reaction；The ratio of the amount of substance of 30 nanoparticle of Polygonum polysaccharide-gold and morin is 1:2500, this reaction is urged
Changing rate constant is 4.89 × 10-3s-1, this reacts catalytic efficiency with higher.
Embodiment 4
Polygonum polysaccharide is dissolved in deionized water, the Polygonum polysaccharide solution of 30mg/mL is configured to, by 30mg/mL what
Tuber of multiflower knotweed polysaccharide solution and chlorauric acid solution are mixed in centrifuge tube in the ratio that the molar ratio of Polygonum polysaccharide and gold chloride is 1:40
In, centrifuge tube is put into thermostat metal blending instrument, the revolving speed of setting thermostat metal blending instrument is 1000rpm, and thermostat metal is mixed
Even instrument temperature is 70 DEG C, carries out reduction reaction 8h, becomes aubergine to reaction solution, be 8000-14000's with molecular cut off
Bag filter is dialysed final solution, that is, obtains the solution of 40 nanoparticle of Polygonum polysaccharide-gold.
Through experiments, it was found that tuber of multiflower knotweed polysaccharide -40 nano-particle solution of gold without aggregation or precipitates in one week, disperse well
In aqueous solution.
Figure 10 is the transmission electron microscope picture of Polygonum polysaccharide-gold 40, shows that its pattern is spherical.Figure 11 is what head in Figure 10
The particle diameter distribution histogram of black polysaccharide-gold nanoparticle, it shows that the partial size of 40 nanoparticle of Polygonum polysaccharide-gold of preparation is
25.24 ± 7.84nm, 40 nanoparticle of Polygonum polysaccharide-gold have the characteristics that compared with small particle.
It takes the morin solution of 30 μ L 5mM in cuvette, 1910 μ L deionized waters is added, it is 2 μM that 30 μ L concentration, which are added,
40 nano-particle solution of Polygonum polysaccharide-gold (40 nano-particle solution of Polygonum polysaccharide-gold prepared by embodiment 4 is prepared
Into), then to the hydrogenperoxide steam generator of 30 μ L 0.4mg/ml of cuvette addition, extinction under 403nm is surveyed with ultraviolet specrophotometer
Degree changes over time curve.As shown in figure 12, show 40 nanoparticle of Polygonum polysaccharide-gold can catalysis oxidation morin, this
Reaction is pseudo-first-order reaction；The ratio of the amount of substance of 40 nanoparticle of Polygonum polysaccharide-gold and morin is 1:2500, this reaction
Catalytic rate constant is 4.96 × 10-3s-1, this reacts catalytic efficiency with higher.
As seen from the above embodiment, the present invention provides a kind of preparation method of gold nanoparticle, the fleece-flower root of preparation is more
The stable gold nanoparticle of sugar, which was able to maintain in aqueous solution in one week, to be stablized, no aggregation and precipitating；Preparation condition is mild, operates
Simply, reaction process is easily controllable, and the partial size of the gold nanoparticle of preparation is 16~25nm, and uniform particle sizes have morin
High catalytic efficiency.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of gold nanoparticle, comprising the following steps:
Polygonum polysaccharide solution and chlorauric acid solution are mixed, the reduction reaction of gold chloride is carried out, by gained reduzate system
It dialyses, obtains gold nanoparticle.
2. preparation method according to claim 1, which is characterized in that the mass concentration of the Polygonum polysaccharide solution is
0.1~30mg/mL.
3. preparation method according to claim 1, which is characterized in that the mass concentration of the chlorauric acid solution be 0.1~
20mmol/mL。
4. preparation method according to any one of claims 1 to 3, which is characterized in that in the Polygonum polysaccharide solution
Polygonum polysaccharide and chlorauric acid solution in gold chloride molar ratio be 1:10~40.
5. preparation method according to claim 1, which is characterized in that the reduction reaction carries out under agitation, institute
The revolving speed for stating stirring is 400~1000rpm.
6. preparation method according to claim 1, which is characterized in that the temperature of the reduction reaction is 50~70 DEG C.
7. preparation method according to claim 1, which is characterized in that the time of the reduction reaction is 4~8h.
8. preparation method according to claim 1, which is characterized in that the retention molecule of bag filter used by the dialysis
Amount is 8000~14000.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109894627A (en) * | 2019-02-19 | 2019-06-18 | 江南大学 | The synthetic method of noble metal nano particles |
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Application publication date: 20190108 |