CN104759636A - 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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- CN104759636A CN104759636A CN201510207654.6A CN201510207654A CN104759636A CN 104759636 A CN104759636 A CN 104759636A CN 201510207654 A CN201510207654 A CN 201510207654A CN 104759636 A CN104759636 A CN 104759636A
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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 method utilizing hawthorn seeds Aqueous extracts as dispersant and biological reductant synthesis of nano gold.
Background technology
Nm of gold material earns widespread respect because it has unique performance, and its preparation and application have become a study hotspot in current field of nanometer technology.Nm of gold and compound thereof have because of it that performances such as skin effect, quantum size effect, optical effect make that it detects fast in Industrial Catalysis, biological medicine, bioanalytical chemistry, food security, optical probe, sensor numerous in have extensively potential application prospect.At present, the preparation method of Nano Silver mainly liquid phase reduction in laboratory.Utilize sodium borohydride (NaBH
4), potassium borohydride (KBH
4) etc. strong reductant the gold ion in solution is reduced into elemental gold.But have report to point out, exposed nm of gold is easily oxidized, and agglomeration is serious, and its activity is reduced greatly.Therefore, in order to reduce the reunion of nm of gold and strengthen its stability, in reduction reaction, often need to add dispersant, as polyvinylpyrrolidone (PVP), carboxymethyl cellulose (CMC), oxolane (THF) etc. carry out modification to nano Au particle, strengthen it dispersed, prevent from reuniting.But the use of chemical reagent improves synthesis cost, and to bad environmental.Relative to traditional chemical synthesis process, the biological reducing method based on plant occurred in recent years, have that cost is low, environmental protection, nano material stability advantages of higher, become the novel fabrication method that nm of gold material has development prospect.
Hawthorn, another name haw, rose family may.Hawthorn is very wide in whole world cultivated area, and its root, rattan, Ye Jieke are used as medicine, but hawthorn seeds is hawthorn eats raw, squeeze the juice and the discarded part of Preserved produciton industry.According to statistics, the hawthorn seeds of up to a million tons is about had to produce every year.If hawthorn seeds directly regarded garbage loading embeading or abandon, not only cause the waste of resource, and pollution can be produced to environment.There are some researches show, containing flavones, PCA, phenolic acid, three mushroom acid and protein isoreactivity compositions in hawthorn seeds, to there is stronger oxidation resistance, show good dispersiveness and biological reducing voltinism.Based on above-mentioned, the present invention, under the prerequisite not using any chemical reducing agent and dispersant, proposes the method for hawthorn seeds Aqueous extracts synthesis of nano gold.The present invention utilizes hydro-thermal reaction system, and the hawthorn seeds Aqueous extracts green syt nm of gold only utilizing occurring in nature cheap and easy to get, has not only opened up the recycling of hawthorn seeds, reduced the synthesis cost of nm of gold simultaneously, be with a wide range of applications.
Summary of the invention
The object of this invention is to provide a kind of method that nm of gold prepared by hawthorn seeds extract, the method is with hawthorn seeds Aqueous extracts for reducing agent and stabilizing agent synthesis of nano gold particle, and the method is carried out in atmospheric conditions, and equipment is simple, cost is low, be easy to operation.Adopt the inventive method, reduce the preparation cost of nm of gold, hawthorn seeds refuse is utilized, and decreases environmental pollution.
For achieving the above object, present invention employs following technical scheme.
Prepare the method for nm of gold with hawthorn seeds extract, comprise the steps:
(1), after being cleaned by hawthorn seeds, under 100 ~ 105 DEG C of conditions, then dry 12 ~ 13h pulverizes, and is sized to 200 ~ 500 μm, obtains hawthorn seeds powder;
(2) be mixed into hawthorn seeds powder solution, ultrasonic extraction 30min, vacuum filtration 15min at 40 DEG C according to the ratio of mass volume ratio 1 ︰ 30 of hawthorn seeds powder and distilled water, then through 0.45 μm of membrane filtration, obtain hawthorn seeds extract;
(3) get gold chloride powder and distilled water, the chlorauric acid solution of preparation 1 ~ 10mmol, is adjusted to 4.0 ~ 9.0 with NaOH/potassium hydroxide aqueous solution by chlorauric acid solution pH value;
(4) chlorauric acid solution prepared by the hawthorn seeds extract (2) prepared by volume and (3) mixes in the ratio of 1 ︰ 10, and at 25 ~ 60 DEG C, stirring reaction 0.5 ~ 2 h, obtains the nano-Au solution of claret.
The present invention utilizes finite concentration gold chloride as reacting precursor, in atmospheric conditions, with hawthorn seeds Aqueous extracts Reactive Synthesis claret nm of gold.Do not need in building-up process that large-scale consersion unit, device are simple, raw material dosage is few, reaction condition is gentle, cost is lower.This preparation method also can be extended to the Green synthesis of other noble metal nanometer material.
Accompanying drawing explanation
Fig. 1 prepares the picture of gained nm of gold.
Fig. 2 prepares the ultraviolet-visible absorbance phenogram of gained nm of gold by embodiment 1.
Fig. 3 prepares the X-ray diffractogram of gained nm of gold by embodiment 1.
Fig. 4 prepares the TEM figure of gained nm of gold by embodiment 1.
Fig. 5 prepares the ultraviolet-visible absorbance phenogram of gained nm of gold by embodiment 2.
Fig. 6 prepares the TEM figure of gained nm of gold by embodiment 2.
Fig. 7 prepares the ultraviolet-visible absorbance phenogram of gained nm of gold by embodiment 3.
Fig. 8 prepares the TEM figure of gained nm of gold by embodiment 3.
embodiment 1
The inventive method is adopted to prepare nm of gold.(1), after being cleaned by hawthorn seeds, under 105 DEG C of conditions, then dry 12h pulverizes, and is sized to 200 ~ 300 μm, obtains hawthorn seeds powder; (2) be mixed into hawthorn seeds powder solution, ultrasonic extraction 30min, vacuum filtration 15min at 40 DEG C according to the ratio of mass volume ratio 1 ︰ 30 of hawthorn seeds powder and distilled water, then through 0.45 μm of membrane filtration, obtain hawthorn seeds extract; (3) get gold chloride powder and distilled water, the chlorauric acid solution of preparation 1mmol, and with NaOH/potassium hydroxide aqueous solution, chlorauric acid solution pH value is adjusted to 9.0; (4) mixed with the ratio of chlorauric acid solution in 1 ︰ 10 by hawthorn seeds extract by volume, at 60 DEG C, stirring reaction 1 h, obtains the nano-Au solution of claret.Ultraviolet-visible absorption spectra (UV-vis) characterization result of synthesized nano-Au solution is as shown in Fig. 2, and as shown in Figure 3, transmission electron microscope (TEM) characterization result is as shown in Fig. 4 for X-ray diffraction (XRD) characterization result.Transmission electron microscope observing, result shows, the nanogold particle of synthesis mostly is almost spherical, size uniformity, good dispersion, not easily reunites, and nanogold particle domain size distribution is in 3.2 ~ 8.8nm.
embodiment 2
The inventive method is adopted to prepare nm of gold.(1), after being cleaned by hawthorn seeds, under 100 DEG C of conditions, then dry 13h pulverizes, and is sized to 300 ~ 500 μm, obtains hawthorn seeds powder; (2) be mixed into hawthorn seeds powder solution, ultrasonic extraction 30min, vacuum filtration 15min at 40 DEG C according to the ratio of mass volume ratio 1 ︰ 30 of hawthorn seeds powder and distilled water, then through 0.45 μm of membrane filtration, obtain hawthorn seeds extract; (3) get gold chloride powder and distilled water, the chlorauric acid solution of preparation 5mmol, and with NaOH/potassium hydroxide aqueous solution, chlorauric acid solution pH value is adjusted to 9.0; (4) mixed with the ratio of chlorauric acid solution in 1 ︰ 10 by hawthorn seeds extract by volume, at 25 DEG C, stirring reaction 2 h, obtains the nano-Au solution of claret.Synthesized nm of gold be obtained by reacting spherical, grain size distribution is similar to example 1; Ultraviolet-visible absorption spectra (UV-vis) characterization result of synthesized nano-Au solution is as shown in Fig. 5; Transmission electron microscope (TEM) characterization result as shown in Figure 6; Transmission electron microscope observing, result shows, the nanogold particle domain size distribution of synthesis is in 10.7 ~ 17.2nm.
embodiment 3
The inventive method is adopted to prepare nm of gold.(1), after being cleaned by hawthorn seeds, under 105 DEG C of conditions, then dry 12h pulverizes, and is sized to 300 ~ 500 μm, obtains hawthorn seeds powder; (2) be mixed into hawthorn seeds powder solution, ultrasonic extraction 30min, vacuum filtration 15min at 40 DEG C according to the ratio of mass volume ratio 1 ︰ 30 of hawthorn seeds powder and distilled water, then through 0.45 μm of membrane filtration, obtain hawthorn seeds extract; (3) get gold chloride powder and distilled water, the chlorauric acid solution of preparation 2mmol, and with NaOH/potassium hydroxide aqueous solution, chlorauric acid solution pH value is adjusted to 4.0; (4) mixed with the ratio of chlorauric acid solution in 1 ︰ 10 by hawthorn seeds extract by volume, at 25 DEG C, stirring reaction 2 h, obtains the nano-Au solution of claret.Ultraviolet-visible absorption spectra (UV-vis) characterization result of synthesized nano-Au solution is as shown in Fig. 7; Transmission electron microscope (TEM) characterization result as shown in Figure 8; Transmission electron microscope observing, result shows, the nanogold particle domain size distribution of synthesis is in 15.4 ~ 21.6nm.
Claims (1)
1. prepare the method for nm of gold with hawthorn seeds extract, comprise the steps:
(1), after being cleaned by hawthorn seeds, under 100 ~ 105 DEG C of conditions, then dry 12 ~ 13h pulverizes, and is sized to 200 ~ 500 μm, obtains hawthorn seeds powder;
(2) be mixed into hawthorn seeds powder solution, ultrasonic extraction 30min, vacuum filtration 15min at 40 DEG C according to the ratio of mass volume ratio 1 ︰ 30 of hawthorn seeds powder and distilled water, then through 0.45 μm of membrane filtration, obtain hawthorn seeds extract;
(3) get gold chloride powder and distilled water, the chlorauric acid solution of preparation 1 ~ 10mmol, is adjusted to 4.0 ~ 9.0 with NaOH/potassium hydroxide aqueous solution by chlorauric acid solution pH value;
(4) chlorauric acid solution prepared by the hawthorn seeds extract (2) prepared by volume and (3) mixes in the ratio of 1 ︰ 10, and at 25 ~ 60 DEG C, stirring reaction 0.5 ~ 2 h, obtains the nano-Au solution of claret.
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Cited By (4)
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| CN106623970A (en) * | 2016-11-28 | 2017-05-10 | 西安石油大学 | Method for preparing nanogold with size smaller than 5 nm through banana pulp extract |
| CN107282940A (en) * | 2017-06-13 | 2017-10-24 | 上海理工大学 | A kind of method that utilization pseudo-ginseng extract solution prepares gold nano grain |
| 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 |
| CN113506648A (en) * | 2021-09-10 | 2021-10-15 | 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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| CN104174870A (en) * | 2014-08-29 | 2014-12-03 | 北京工业大学 | Green synthesis method for nanometer zero-valent iron by utilizing grape seeds and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106623970A (en) * | 2016-11-28 | 2017-05-10 | 西安石油大学 | Method for preparing nanogold with size smaller than 5 nm through banana pulp extract |
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| CN107282940A (en) * | 2017-06-13 | 2017-10-24 | 上海理工大学 | A kind of method that utilization pseudo-ginseng extract solution prepares gold nano grain |
| 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 |
| CN113506648A (en) * | 2021-09-10 | 2021-10-15 | 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 |
| 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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