CN104759636B - Method for preparing nano-gold with hawthorn seed extracting solution - Google Patents
Method for preparing nano-gold with hawthorn seed extracting solution Download PDFInfo
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- CN104759636B CN104759636B CN201510207654.6A CN201510207654A CN104759636B CN 104759636 B CN104759636 B CN 104759636B CN 201510207654 A CN201510207654 A CN 201510207654A CN 104759636 B CN104759636 B CN 104759636B
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- fructus crataegi
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Abstract
The invention discloses a method for preparing nano-gold with a hawthorn seed extracting solution. According to the method, the liquid hawthorn seed extracting solution serves as a reducing agent and a stabilizing agent to synthesize nano-gold particles, the operation can be conducted under an ordinary pressure condition, the equipment is simple, the cost is low, and the operation is easy. By means of the method, the preparation cost of the nano-gold is reduced, waste hawthorn seeds can be reused, and the environmental pollution is decreased.
Description
Technical field
The invention belongs to technical field of material, specifically, the present invention relates to the use of seed of Fructus Crataegi Aqueous extracts as point
Powder and the method for biological reductant synthesis nanometer gold.
Background technology
Nanometer gold material earns widespread respect because it has the performance of uniqueness, and its preparation and application has become current nanometer
One of technical field study hotspot.Nanometer gold and its complex have skin effect, quantum size effect, optics effect because of it
Performance should be waited to make it in Industrial Catalysis, biological medicine, bioanalytical chemistry, food safety quick detection, optical probe, sensor
There is extensively potential application prospect etc. numerous aspects.At present, in laboratory, the preparation method of nanometer silver is mainly liquid-phase reduction
Method.Using sodium borohydride (nabh4), potassium borohydride (kbh4) etc. strong reductant the gold ion in solution is reduced into elemental gold.
However, it is reported that, exposed nanometer gold is easily oxidized, and agglomeration is seriously so as to activity substantially reduces.Therefore,
In order to reduce reuniting and strengthening its stability of nanometer gold, in reduction reaction, generally require to add dispersant, such as polyethylene pyrrole
Pyrrolidone (pvp), carboxymethyl cellulose (cmc), oxolane (thf) etc. are modified to nano Au particle, strengthen its dispersion
Property, prevent from reuniting.But the use of chemical reagent improves synthesis cost, and environment is harmful to.With respect to traditional chemosynthesis
Method, the biological reducing method based on plant occurring in recent years, there is low cost, environmental protection, nano material stability height etc.
Advantage, becomes the novel fabrication method that nanometer gold material has development prospect.
Fructus Crataegi, calls Fructus Pyracanthae, Rosaceae Crataegus plant.Fructus Crataegi is very wide in whole world cultivated area, its root, rattan, leaf
All can be used as medicine, but seed of Fructus Crataegi is Fructus Crataegi eats raw, squeeze the juice and Preserved produciton industry discarded part.According to statistics, there are about every year up to a million
The seed of Fructus Crataegi of ton produces.If seed of Fructus Crataegi is directly regarded garbage loading embeading or discarding, not only cause the waste of resource, and can be to ring
Border produces pollution.There are some researches show, contain flavone, oligomeric proanthocyanidin, phenolic acid, three mushroom acid and protein isoreactivity in seed of Fructus Crataegi and become
Point, there is stronger oxidation resistance, show good dispersibility and biological reducing.Based on above-mentioned, the present invention is not
Using on the premise of any chemical reducing agent and dispersant it is proposed that seed of Fructus Crataegi Aqueous extracts synthesize nanometer gold method.The present invention
Using hydro-thermal reaction system, merely with seed of Fructus Crataegi Aqueous extracts green syt nanometer gold cheap and easy to get in nature, not only open up
The recycling of seed of Fructus Crataegi, reduces the synthesis cost of nanometer gold simultaneously, is with a wide range of applications.
Content of the invention
It is an object of the invention to provide a kind of method preparing nanometer gold with seed of Fructus Crataegi extracting solution, the method is with seed of Fructus Crataegi water
Extract is that reducing agent and stabilizer synthesize nano Au particle, and the method is carried out in atmospheric conditions, and equipment is simple, low cost, easily
In operation.Using the inventive method, reduce the preparation cost of nanometer gold, seed of Fructus Crataegi waste is obtained by, decrease environment dirty
Dye.
For achieving the above object, present invention employs technical scheme below.
The method preparing nanometer gold with seed of Fructus Crataegi extracting solution, comprises the steps:
(1), after seed of Fructus Crataegi being cleaned, 12～13h is dried under the conditions of 100～105 DEG C, then pulverizes, it is sized to 200～
500 m, obtain seed of Fructus Crataegi powder；
(2) it is mixed into seed of Fructus Crataegi powder solution according to the ratio of 1 gram of seed of Fructus Crataegi powder and 30 milliliters of distilled water, ultrasonic at 40 DEG C
Extract 30min, vacuum filtration 15min, then through 0.45 m membrane filtration, obtain seed of Fructus Crataegi extracting solution；
(3) gold chloride powder and distilled water are taken, the chlorauric acid solution of preparation 1～10mmol, with sodium hydroxide/hydroxide
Aqueous solutions of potassium adjusts chlorauric acid solution ph value to 4.0～9.0；
(4) chlorauric acid solution prepared by the seed of Fructus Crataegi extracting solution prepared (2) by volume and (3) in 1 10 ratio
Mixing, stirring reaction 0.5～2 h at 25～60 DEG C, obtain the nano-Au solution of claret.
The present invention, by the use of finite concentration gold chloride as reacting precursor, in atmospheric conditions, is reacted with seed of Fructus Crataegi Aqueous extracts
Synthesis claret nanometer gold.Do not need in building-up process that large-scale consersion unit, device are simple, raw material dosage is few, reaction condition temperature
Relatively low with, cost.This preparation method also can be extended to the green preparation of other noble metal nanometer materials.
Brief description
Fig. 1 prepares the ultravioletvisible absorption phenogram of gained nanometer gold by embodiment 1.
Fig. 2 prepares the X-ray diffraction pattern of gained nanometer gold by embodiment 1.
Fig. 3 prepares the tem figure of gained nanometer gold by embodiment 1.
Fig. 4 prepares the ultravioletvisible absorption phenogram of gained nanometer gold by embodiment 2.
Fig. 5 prepares the tem figure of gained nanometer gold by embodiment 2.
Fig. 6 prepares the ultravioletvisible absorption phenogram of gained nanometer gold by embodiment 3.
Fig. 7 prepares the tem figure of gained nanometer gold by embodiment 3.
Specific embodiment
Embodiment 1
Nanometer gold is prepared using the inventive method.(1), after seed of Fructus Crataegi being cleaned, 12h is dried under the conditions of 105 DEG C, then
Pulverize, be sized to 200～300 m, obtain seed of Fructus Crataegi powder；(2) mix according to the ratio of 1 part of seed of Fructus Crataegi powder and 30 parts of distilled water
Synthesis seed of Fructus Crataegi powder solution, supersound extraction 30min at 40 DEG C, vacuum filtration 15min, then through 0.45 m membrane filtration, obtain Fructus Crataegi
Seed extracting solution；(3) take gold chloride powder and distilled water, prepare the chlorauric acid solution of 1mmol, and with sodium hydroxide/potassium hydroxide
Aqueous solution adjusts chlorauric acid solution ph value to 9.0；(4) by volume seed of Fructus Crataegi extracting solution is pressed 1 10 with chlorauric acid solution
Ratio mixing, stirring reaction 1 h at 60 DEG C, obtain the nano-Au solution of claret.The purple of synthesized nano-Au solution
, as shown in Fig. 1, x-ray diffraction (xrd) characterization result is as shown in Fig. 2 thoroughly for outward-visible absorption spectra (uv-vis) characterization result
Penetrate ultramicroscope (tem) characterization result as shown in Fig. 3.Transmission electron microscope observing, result shows, the nanogold particle of synthesis is many
For almost spherical, size uniformity, good dispersion, it is difficult to reunite, nanogold particle particle diameter distribution is in 3.2～8.8nm.
Embodiment 2
Nanometer gold is prepared using the inventive method.(1), after seed of Fructus Crataegi being cleaned, 13h is dried under the conditions of 100 DEG C, then
Pulverize, be sized to 300～500 m, obtain seed of Fructus Crataegi powder；(2) mix with the ratio of 30 parts of distilled water according to 1 part of seed of Fructus Crataegi powder
Become seed of Fructus Crataegi powder solution, supersound extraction 30min at 40 DEG C, vacuum filtration 15min, then through 0.45 m membrane filtration, obtain seed of Fructus Crataegi
Extracting solution；(3) take gold chloride powder and distilled water, prepare the chlorauric acid solution of 5mmol, and with sodium hydroxide/potassium hydroxide water
Solution adjusts chlorauric acid solution ph value to 9.0；(4) by volume seed of Fructus Crataegi extracting solution is pressed 1 10 with chlorauric acid solution
Ratio mixes, and stirring reaction 2 h at 25 DEG C obtains the nano-Au solution of claret.Synthesized nanometer gold reaction obtains ball
Shape, grain size distribution similar to example 1；Ultraviolet-visible absorption spectra (uv-vis) table of synthesized nano-Au solution
Levy result as shown in Fig. 4；Transmission electron microscope (tem) characterization result is as shown in Figure 5；Transmission electron microscope observing, result shows,
The nanogold particle particle diameter distribution of synthesis is in 10.7～17.2nm.
Embodiment 3
Nanometer gold is prepared using the inventive method.(1), after seed of Fructus Crataegi being cleaned, 12h is dried under the conditions of 105 DEG C, then
Pulverize, be sized to 300～500 m, obtain seed of Fructus Crataegi powder；(2) mix with the ratio of 30 parts of distilled water according to 1 part of seed of Fructus Crataegi powder
Become seed of Fructus Crataegi powder solution, supersound extraction 30min at 40 DEG C, vacuum filtration 15min, then through 0.45 m membrane filtration, obtain seed of Fructus Crataegi
Extracting solution；(3) take gold chloride powder and distilled water, prepare the chlorauric acid solution of 2mmol, and with sodium hydroxide/potassium hydroxide water
Solution adjusts chlorauric acid solution ph value to 4.0；(4) by volume seed of Fructus Crataegi extracting solution is pressed 1 10 with chlorauric acid solution
Ratio mixes, and stirring reaction 2 h at 25 DEG C obtains the nano-Au solution of claret.The ultraviolet of synthesized nano-Au solution-
Visible absorption spectra (uv-vis) characterization result is as shown in Figure 6；Transmission electron microscope (tem) characterization result is as shown in Figure 7；Thoroughly
Radio sem observation, result shows, the nanogold particle particle diameter distribution of synthesis is in 15.4～21.6nm.
Claims (1)
1. the method preparing nanometer gold with seed of Fructus Crataegi extracting solution, comprises the steps:
(1), after seed of Fructus Crataegi being cleaned, 12～13h is dried under the conditions of 100～105 DEG C, then pulverizes, be sized to 200～500
M, obtains seed of Fructus Crataegi powder；
(2) it is mixed into seed of Fructus Crataegi powder solution, supersound extraction at 40 DEG C according to the ratio of 1 gram of seed of Fructus Crataegi powder and 30 milliliters of distilled water
30min, vacuum filtration 15min, then through 0.45 m membrane filtration, obtain seed of Fructus Crataegi extracting solution；
(3) gold chloride powder and distilled water are taken, the chlorauric acid solution of preparation 1～10mmol, with sodium hydroxide/potassium hydroxide water
Solution adjusts chlorauric acid solution ph value to 4.0～9.0；
(4) chlorauric acid solution prepared seed of Fructus Crataegi extracting solution prepared by (2) with (3) by volume is mixed in 1 10 ratio,
Stirring reaction 0.5～2 h at 25～60 DEG C, obtains the nano-Au solution of claret.
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| CN106623970B (en) * | 2016-11-28 | 2018-07-03 | 西安石油大学 | It is a kind of that method of the size less than 5nm nanogold is prepared using banana pulp extract |
| CN107282940B (en) * | 2017-06-13 | 2021-02-19 | 上海理工大学 | Method for preparing gold nanoparticles by using pseudo-ginseng extracting solution |
| CN107598153A (en) * | 2017-08-30 | 2018-01-19 | 西安理工大学 | A kind of preparation method of the Silver Nanoparticles of anti-pancreatic cancer and lung cancer |
| CN113506648B (en) * | 2021-09-10 | 2021-12-21 | 西安宏星电子浆料科技股份有限公司 | Inner-layer gold conductor paste for Ca-B-Si system LTCC |
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| CN101786168B (en) * | 2010-01-08 | 2012-06-20 | 厦门大学 | Method for preparing flower-like nanometer gold |
| CN101912976A (en) * | 2010-08-24 | 2010-12-15 | 厦门大学 | Method for preparing silver nano granules by reducing plant extract |
| CN102189269A (en) * | 2011-04-29 | 2011-09-21 | 上海交通大学 | Method for preparing Au nanoparticles with chloroplast as template in water phase mode |
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