CN109894627A - The synthetic method of noble metal nano particles - Google Patents

The synthetic method of noble metal nano particles Download PDF

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Publication number
CN109894627A
CN109894627A CN201910122391.7A CN201910122391A CN109894627A CN 109894627 A CN109894627 A CN 109894627A CN 201910122391 A CN201910122391 A CN 201910122391A CN 109894627 A CN109894627 A CN 109894627A
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China
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noble metal
nano particles
metal nano
birch
solution
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CN201910122391.7A
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李程程
陈东
丁健
王利斌
史仲平
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Jiangnan University
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Jiangnan University
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Abstract

The invention discloses a kind of synthetic methods of noble metal nano particles, comprising: disperses birch-leaf pear bar water extract in precious metal solution, reacts, obtain noble metal nano particles, noble metal is selected from gold or/and silver.The present invention is using birch-leaf pear bar water extract as reducing agent and stabilizer, and using gold chloride or silver nitrate solution as raw material, the noble metal nano particles being evenly distributed have been made in short time reaction.Transmission electron microscope shows synthesized noble metal nano particles even size distribution, and for the average-size of gold nano grain in 52.2nm or so, the average-size of silver nano-grain has good dispersibility in 19.9nm or so.Since the raw material sources of this method are safe and harmless, the reaction time is short, and reaction temperature only room temperature, therefore, this method is expected to be used widely in terms of green syt noble metal nano particles.

Description

The synthetic method of noble metal nano particles
Technical field
The invention belongs to biotechnology and field of nanometer material technology, be related to nano particle synthesis more particularly to your a kind of gold The synthetic method of metal nano-particle.
Background technique
Currently, nanotechnology is widely used for all trades and professions, vigorous growth has been obtained, has been had received widespread attention. Nano particle has good antibacterial, anti-inflammatory, anti-oxidant and blood vessel formation against function, embodies good therapeutic effect, Biological medicine, electronics industry, agricultural and light industry field have a wide range of applications, due to its spy compared with other large materials Different size, shape, specific surface area and composition characteristic imparts their superior physicochemical characteristics, mechanical performance, heat Stability and biological characteristics.
The synthetic method of metal nanoparticle includes chemical method, physical method and bioanalysis.Traditional noble metal nano Grain synthetic method mostly uses chemical reagent reduction method, is related to the chemical reducing agents such as ethylenediamine, sodium borohydride among these, they Use the problems such as bringing potential environmental pollution and bio-toxicity.Therefore, people begin look for synthesis noble metal nano The alternative of particle, to realize green, sustainable development.A variety of natural origin substances are used to " green conjunction extensively At " metal nanoparticle, if plant, bacterium, fungi are even viral, this synthesis both can occur in vivo or send out Life in vitro, not only ensure that environmental-friendly but also save resource, simultaneously because the constituent difference of natural materials is imparted and received The different biological characteristics of rice grain.
Plant extracts be used to synthesize metal nanoparticle report also have very much, synthesized nano particle antibacterial, Anti-inflammatory, anti-oxidant and anticancer aspect all shows certain superiority.Different plant extracts are due to its constituent Difference, the size and character of synthesized noble metal nano particles are also different greatly.But most bioanalysis synthesizes metal nano Often the period is longer for grain, while developing more plant extracts not is only that synthesizing for nano particle provides new thinking, is also opened The application category of plant extracts is opened up.
Summary of the invention
Goal of the invention: the technical problem to be solved in the present invention is to provide a kind of using birch-leaf pear bar extract (PSE) as also Former agent and stabilizer, the method for synthesizing noble metal nano particles, to solve existing noble metal nano particles synthesis energy consumption, time-consuming And the problems such as pollution environment, while also developing synthesis of the novel reducer for metal nanoparticle.
Technical solution: the synthetic method of noble metal nano particles of the present invention, comprising: by birch-leaf pear bar water extract It is scattered in precious metal solution, reacts, obtain noble metal nano particles.
Further, it will be then added in precious metal solution after the dissolution of birch-leaf pear bar water extract.
The noble metal is selected from gold or/and silver.
The precious metal solution is 10~200mg/L AgNO3Solution or/and 10~200mg/L HAuCl4Solution.It is preferred that , AgNO3The concentration of solution is 40~60mg/L, HAuCl4The concentration of solution is 40~60mg/L, it is furthermore preferred that AgNO3It is molten The concentration of liquid is 50mg/L, HAuCl4The concentration of solution is 50mg/L.
Concentration of the birch-leaf pear bar water extract in precious metal solution is 0.1~10mg/mL, it is preferred that birch-leaf pear bar water Concentration of the extract in precious metal solution is 0.2~1mg/mL.Experiment shows birch-leaf pear bar water extract in precious metal solution In concentration be 0.45~0.6mg/mL when, the yield for synthesizing nano particle is higher.
The reaction time is 1~60min, and reaction temperature is 15~100 DEG C;Preferably, the reaction time be 30~ 60min;The preferred reaction time for synthesizing gold nano grain is 40~45min, and the preferred reaction time for synthesizing silver nano-grain is 50~60min.
The preparation method of the birch-leaf pear bar water extract includes: to be added to the water birch-leaf pear bar, after boiling 10~60min, mistake Filter takes supernatant, obtains birch-leaf pear bar water extract after dry after filtrate centrifugation.
The utility model has the advantages that
1, the method for present invention synthesis noble metal nano particles is not required to adjust pH and heat treatment, only needs room temperature, Reaction time is short, without heating, greatly reduces energy consumption.
2, without adding any chemical reducing agent and stabilizer, eliminating when present invention synthesis noble metal nano particles Reagent contamination is learned, green syt is realized.
3, the present invention is short using gold chloride or silver nitrate solution as raw material using birch-leaf pear bar water extract as reducing agent and stabilizer The noble metal nano particles being evenly distributed have been made in time response.Transmission electron microscope shows synthesized noble metal nano particles ruler Very little to be evenly distributed, the average-size of gold nano grain is in 52.2nm or so, and the average-size of silver nano-grain is on the left side 19.9nm The right side has good dispersibility.Since the raw material sources of this method are safe and harmless, the reaction time is short, and only room temperature is reaction temperature Can, therefore, this method is expected to be used widely in terms of green syt noble metal nano particles.
Detailed description of the invention
Fig. 1 is birch-leaf pear bar extracting solution preparation flow figure in embodiment 1;
Fig. 2 be embodiment 2 in PSE synthesize gold nano grain when the differential responses time color change schematic diagram, from a left side to The right side is followed successively by the result of 5,15,30 and 60min;
Fig. 3 be embodiment 2 in PSE synthesize silver nano-grain when the differential responses time color change schematic diagram, from a left side to The right side is followed successively by the result of 5,15,30 and 60min;
The ultraviolet spectra of gold (A), silver-colored (B) nano particle that Fig. 4 synthesizes for different time in embodiment 2 and embodiment 3 shows It is intended to;
Fig. 5 is the color signal of the gold (A) of Best Times synthesis in embodiment 2 and embodiment 3, silver-colored (B) nano particle Figure;
Fig. 6 is the UV scanning light of the gold (A) of Best Times synthesis in embodiment 2 and embodiment 3, silver-colored (B) nano particle Compose schematic diagram;
The transmission electron microscope of gold (A), silver-colored (B) nano particle that Fig. 7 synthesizes for Best Times in embodiment 2 and embodiment 3 shows It is intended to;
Fig. 8 is the particle diameter distribution of the gold (A) of Best Times synthesis, silver-colored (B) nano particle in embodiment 2 and embodiment 3 Figure;
Fig. 9 is the zeta current potential result signal of the gold, silver nano particle of Best Times synthesis in embodiment 2 and embodiment 3 Figure.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention Rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalences of the invention The modification of form falls within the application range as defined in the appended claims.
1 birch-leaf pear bar of embodiment extracts liquid and preparation method thereof
The water that 200mL is added after 50g birch-leaf pear bar is cut short is weighed, 30min is boiled, obtains filtrate with one layer of filter paper filtering, it will Filtrate is centrifuged 20min with 7000rpm, takes supernatant to be lyophilized into powder and obtains birch-leaf pear bar water extract (PSE) powder, spare, preparation flow is shown in Fig. 1.
2 PSE of embodiment synthesizes gold nano grain
PSE powder is made into the aqueous solution of 10mg/mL, the gold chloride for taking 0.625mL to be added to 10mL 50mg/L is water-soluble It in liquid, is stirred to react, reaction temperature is room temperature.It samples and takes pictures in 5,15,30 and 60min respectively.As a result see Fig. 2, Occurs claret when 5min in reaction solution, which is the characteristic color of gold nano grain, illustrates to synthesize after reacting 5min Gold nano grain.
3 PSE of embodiment synthesizes silver nano-grain
PSE is made into the solution of 10mg/mL, 0.625mL is taken to be added in the silver nitrate solution of 10mL 50mg/L, is stirred Reaction.It samples and takes pictures in 5,15,30 and 60min respectively.As a result see Fig. 3, occur in reaction solution in 15min pale brown Color, the color are the characteristic color of silver nano-grain, illustrate to have synthesized silver nano-grain after reacting 15min.
The UV absorption of 4 gold, silver nano particle different time of embodiment
Select 350~700nm scanning range in embodiment 2-3 different time synthesize noble metal nano particles with And PSE sample carries out ultra-violet absorption spectrum detection, as a result sees Fig. 4, the gold, silver nano particle of PSE synthesis is respectively in 547nm (A), there is maximum absorption band at 427nm (B).
The UV absorption of the 5 best generated time of gold, silver nano particle of embodiment
According to UV absorption data, it is best generated time that it is highest, which to choose peak value, when the best synthesis of gold nano grain Between be determined as 45min, the best generated time of silver nano-grain is 60min, the gold, silver nanometer that best generated time synthesizes Particle such as Fig. 5 selects the scanning range of 350~700nm to the embodiment 2-3 noble metal nano particles synthesized and PSE sample Ultra-violet absorption spectrum detection is carried out, as a result sees Fig. 6, the gold, silver nano particle of PSE synthesis is respectively in 547nm (A), 427nm (B) there is maximum absorption band at.
Embodiment 6 is using transmission electron microscope to the morphology observation to gold, silver nano particle
Gold nano grain has preferable load drug effect fruit within the scope of 20~100nm, and compared with the silver nano-grain of small particle It is more advantageous to performance antibacterial action.Above-described embodiment 2 and 3 Best Times of embodiment is taken to synthesize the gold, silver nano particle obtained molten Liquid 10uL, which is dripped to, carries out transmission electron microscope observing on the copper mesh of 400 mesh, as a result see that Fig. 7, the gold nano grain of formation are spherical junctions Structure, silver nano-grain are spherical structure.Particle diameter distribution statistics is carried out simultaneously, as a result sees Fig. 8, the results showed that the gold nano grain Partial size is evenly distributed in 52.2nm or so, morphological rules, according to statistics, has 70.3% gold nano grain at 48-59 nanometers Range, the gold nano grain of the partial size are conducive to carry medicine by cell endocytic, play good therapeutic effect;The silver nano-grain Partial size has 86% silver nano-grain in 15-25 nanometer range, size is smaller to be conducive to antibacterial in 19.9nm or so according to statistics Deng application.
Embodiment 7 charges situation using DLS analyzer analysis gold, silver nano particle
The Zeta potential of the gold, silver nano particle and PSE of embodiment 2 and the synthesis of 3 Best Times of embodiment uses Zetasizer 3000 (Malvern Instruments, Nano ZS, United Kingdom) is analyzed.Current potential is lower, Illustrate that the stability of particle is better, such as Fig. 9, PSE and synthesized gold, silver nano particle current potential respectively are -13, -15 With -18, illustrate that synthesized particle stability is enhanced, the stability enhancing of especially Nano silver grain becomes apparent from.

Claims (10)

1. a kind of synthetic method of noble metal nano particles characterized by comprising your gold dispersed by birch-leaf pear bar water extract Belong in solution, reaction obtains noble metal nano particles.
2. the synthetic method of noble metal nano particles according to claim 1, which is characterized in that by birch-leaf pear bar water extract It is then added in precious metal solution after dissolution.
3. the synthetic method of noble metal nano particles according to claim 1, which is characterized in that noble metal be selected from gold or/ And silver.
4. the synthetic method of noble metal nano particles according to claim 1, which is characterized in that precious metal solution be 10~ 200mg/L AgNO3Solution or/and 10~200mg/L HAuCl4Solution.
5. the synthetic method of noble metal nano particles according to claim 4, which is characterized in that AgNO3The concentration of solution is 40~60mg/L, HAuCl4The concentration of solution is 40~60mg/L.
6. the synthetic method of noble metal nano particles according to claim 1, which is characterized in that birch-leaf pear bar water extract exists Concentration in precious metal solution is 0.1~10mg/mL.
7. the synthetic method of noble metal nano particles according to claim 6, which is characterized in that birch-leaf pear bar water extract exists Concentration in precious metal solution is 0.2~1mg/mL.
8. the synthetic method of noble metal nano particles according to claim 1, which is characterized in that the reaction time be 1~ 60min, reaction temperature are 15~100 DEG C.
9. the synthetic method of noble metal nano particles according to claim 8, which is characterized in that reaction temperature is 20~30 ℃。
10. the synthetic method of noble metal nano particles according to claim 1, which is characterized in that the birch-leaf pear bar water mentions The preparation method for taking object includes: to be added to the water birch-leaf pear bar, and after boiling 10~60min, filtering takes supernatant after filtrate centrifugation, does Birch-leaf pear bar water extract is obtained after dry.
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CN111230135A (en) * 2020-03-17 2020-06-05 江南大学 Method for preparing gold nanoparticles
CN111230135B (en) * 2020-03-17 2021-08-24 江南大学 Method for preparing gold nanoparticles

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Application publication date: 20190618