CN104874812A - Preparation method of gold nanoparticles - Google Patents
Preparation method of gold nanoparticles Download PDFInfo
- Publication number
- CN104874812A CN104874812A CN201510273386.8A CN201510273386A CN104874812A CN 104874812 A CN104874812 A CN 104874812A CN 201510273386 A CN201510273386 A CN 201510273386A CN 104874812 A CN104874812 A CN 104874812A
- Authority
- CN
- China
- Prior art keywords
- solution
- specifically refers
- described step
- hepes buffer
- surfactant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a preparation method of gold nanoparticles. The preparation method comprises the following steps that a chloroauric acid solution with the concentration of 0.05-10 mmol/L and a HEPES buffer solution with the concentration of 5-50 mmol/L are prepared respectively, and the PH value of the HEPES buffer solution is adjusted to be 7.0-8.0 through sodium hydroxide; surfactants are added into the HEPES buffer solution, and a surfactant solution with the concentration of 1-2 mmol/L is prepared; the prepared chloroauric acid solution is slowly added into a reaction tank according to the mole ratio of 1:1-1: 10 of the chloroauric acid solution and the surfactant solution, and is stirred for 5-30 min at a constant speed of 200-300 r/min, and a mixed solution containing nano gold colloid is obtained; dry purification of the nano gold colloid is carried out on the mixed solution obtained in the step S400, and the gold nanoparticles are obtained. The gold nanoparticles can be prepared at normal temperature, and are good in dispersity and homogeneous degree.
Description
Technical field
The present invention relates to optical, electrical, the technical field such as biomaterial and nano material, specifically refer to a kind of preparation method of nanogold particle.
Background technology
Nm of gold has excellent electric conductivity, good stability and small-size effect, skin effect, optical effect and catalysis characteristics etc.; make it detect in glucose sensor, plant protection, drug delivery and SERS etc. obtain application at optical probe, electrochemical probe, sensor, DNA, its preparation is one of focus of current people research.
The preparation method of nm of gold mainly contains: Physical and chemical method.Wherein, Physical mainly contains vacuum vapour deposition, electrical dispersion and laser ablation etc.Physical method principle is simple, and products obtained therefrom impurity is few, quality is high, its shortcoming be higher to instrument and equipment requirement, producing cost is expensive, be mainly applicable to require not high industrialization preparation to the size and dimension of nano Au particle.Chemical method mainly contains oxidation-reduction method, electrochemical process, microemulsion method, phase transfer method, template, microwave method and photochemical method etc.The most I of particle diameter of the nanogold particle of chemical preparation reaches a few nanometer, and simple to operate, easily control, shortcoming is that the nanogold particle obtained easily is assembled, and is mainly applicable to fields such as higher optics, electricity and the biomedicines of nanogold particle performance requirement.Above chemical preparation method often needs to add multiple dispersant or stabilizing agent or flocculant in preparation, and cost is higher, length consuming time.
HEPES, 4-HEPES is a kind of hydrogen ion buffer to cytotoxic effect, the long period can control constant PH scope.
PVP, polyvinyl pyrrolidone, the abbreviation of polyvinylpyrrolidone, is a kind of non-ionic macromolecule compound, belongs to N vinylamide polymer.The relative molecular mass of polyvinylpyrrolidone from thousands of to more than 1,000,000 homopolymers, copolymer, crosslinking series of polymers product, and obtain extensive use with its excellent unique performance.
PEG, polyethylene glycol, the abbreviation of polyethylene glycol, nontoxic, nonirritant, has good water-soluble, and has good intermiscibility with many organic matter components.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nanogold particle, normal temperature can carry out the preparation of nanogold particle, and effectively suppress the reunion between nanogold particle, particle dispersion is good, uniformity is high.。
The present invention is achieved through the following technical solutions: a kind of preparation method of nanogold particle, comprises the following steps:
Step S100: compound concentration is the chlorauric acid solution of 0.05-10mmol/L;
Step S200: compound concentration is the HEPES buffer solution of 5-50mmol/L, and regulate the pH value of HEPES buffer solution to 7.0-8.0 with NaOH;
Step S300: add surfactant in the HEPES buffer solution that step S200 prepares, compound concentration is the surfactant solution of 1-2mmol/L;
Step S400: the surfactant solution prepared by step S300 introduces reaction tank, be the chlorauric acid solution that 1:1-1:10 slowly adds step S100 and prepares in reaction tank by the mol ratio of chlorauric acid solution and surfactant solution, and at the uniform velocity stir with the speed of 200-300r/min, reaction 5-30min, obtains the mixed liquor containing nm of gold colloid;
Step S500: the drying that the mixed liquor prepared by step S400 carries out nm of gold colloid is purified, and obtains nanogold particle.
In the present invention, gold chloride and HEPES can react under normal temperature condition, HEPES as reducing agent not only can with gold chloride generation redox reaction, also there is certain stabilization.First AuCl is made
4 -be reduced into gold atom and form nucleus.Time initial nucleus granularity minimum, there is very high surface energy, after a period of time, gold atom forms stable nucleus, owing to can produce N free radical containing piperazine ring in HEPES, is combined rapidly by suction-operated with the nucleus of surrounding, the growth of suppression crystal grain.On the other hand, under the acting in conjunction of HEPES and surfactant, make nanogold particle surface band positive charge, to avoid between nanogold particle collision to be mutually polymerized.Whole process suppresses the formation of second particle, therefore can obtain stable nano gold sol.For making to react completely, add excessive HEPES, one be augmenting response thing degree of supersaturation to accelerate nucleation rate, two is effects that excessive HEPES can play stabilizing agent.Surfactant, as dispersant, effectively can suppress the reunion between nanogold particle, particle dispersion is good, uniformity is high.。
Further, the surfactant solution in described step S300 refers to PVP solution.
Select PVP as surfactant, the hydrophobic chain parcel nanogold particle of PVP, makes nanogold particle well suspend in the solution, avoids the contact between nanogold particle, can obtain the ball shaped nano gold grain of the narrower dispersion of domain size distribution.Under the same terms, less and homogeneous using the nanogold particle particle diameter that PVP obtains when surfactant adds.
Further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:5-1:10 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: ultrafilter introduced by the mixed liquor prepared by step S400, adopts filtering with microporous membrane 3-5h, obtains nm of gold colloid in the below of miillpore filter; Then nm of gold colloid is placed in the drying oven of 50-60 DEG C, heat drying 3h, naturally cools to room temperature in a nitrogen environment, obtains the nanogold particle that particle diameter is less than 10nm.
When the concentration of gold chloride is 1mmol/L, product is nanogold particle mainly; When the concentration of gold chloride is 10mmol/L, start cash dendrite; When the concentration of gold chloride is 30mmol/L, product is all golden dendrite; When the concentration of gold chloride is at below 1mmol/L, the product overwhelming majority is nanogold particle, and pattern is more or less the same.
Further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:2-1:3 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: ultrafilter introduced by the mixed liquor prepared by step S400, adopts filtering with microporous membrane 3-5h, obtains nm of gold colloid in the below of miillpore filter; Then nm of gold colloid is placed in the drying oven of 50-60 DEG C, heat drying 3h, naturally cools to room temperature in a nitrogen environment, and obtaining particle diameter is the nanogold particle of 15-25nm.
Further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:1-1:2 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: ultrafilter introduced by the mixed liquor prepared by step S400, adopts filtering with microporous membrane 3-5h, obtains nm of gold colloid in the below of miillpore filter; Then nm of gold colloid is placed in the drying oven of 50-60 DEG C, heat drying 3h, naturally cools to room temperature in a nitrogen environment, and obtaining particle diameter is the nanogold particle of 25-40nm.
Further, the described preferred aperture of micro-control filter membrane is the GHP filter membrane of 0.2um or 0.45um.
Described GHP filter membrane can be used for aqueous phase and also can be used for organic phase.
Further, the surfactant solution in described step S300 refers to PEG solution.
PEG has the effect of modification to nm of gold colloid, can make the dispersiveness that nm of gold colloid keeps good in complex dielectrics, and the solution not free settling after dispersion, several weeks can be there are with collaurum form stable at normal temperatures.
Further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:5-1:10 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: the mixed liquor prepared by step S400 leaves standstill after 2-10h in standing groove, the claret liquid extracting below to supercentrifuge, with the rotating speed High Rotation Speed 2-5h of 10000r/min-16000r/min; Extract sediment and after fully washing by deionized water, be placed in the drying oven of 60-80 DEG C, heat drying 1-2h obtains dry solid particle in a nitrogen environment; Then the solid particle of drying is put into mortar and grind 0.5-1h, naturally cool to room temperature, obtaining particle diameter is the nanogold particle of 10-40nm.
Further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 2mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:5-1:10 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: the mixed liquor prepared by step S400 leaves standstill after 3h in standing groove, the claret liquid extracting below to supercentrifuge, with the rotating speed High Rotation Speed 2h of 11000r/min; Extract sediment and after fully washing by deionized water, be placed in the drying oven of 60-80 DEG C, heat drying 1h obtains dry solid particle in a nitrogen environment; Then the solid particle of drying is put into mortar and grind 0.5h, naturally cool to room temperature, obtaining particle diameter is the nanogold particle of 10-20nm.
The present invention compared with prior art, has the following advantages and beneficial effect:
(1) can prepare nm of gold colloid under normal temperature condition of the present invention, nm of gold colloid can obtain nanogold particle through filtration drying, simple to operate.
(2) size tunable of nanogold particle prepared of the present invention, and particle dispersion is good, uniformity is high.
Accompanying drawing explanation
Fig. 1 is configuration diagram of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1:
The preparation method of a kind of nanogold particle of the present embodiment, as shown in Figure 1, is mainly achieved through the following technical solutions: comprise the following steps:
Step S100: compound concentration is the chlorauric acid solution of 0.05-10mmol/L;
Step S200: compound concentration is the HEPES buffer solution of 5-50mmol/L, and regulate the pH value of HEPES buffer solution to 7.0-8.0 with NaOH;
Step S300: add surfactant in the HEPES buffer solution that step S200 prepares, compound concentration is the surfactant solution of 1-2mmol/L;
Step S400: the surfactant solution prepared by step S300 introduces reaction tank, be the chlorauric acid solution that 1:1-1:10 slowly adds step S100 and prepares in reaction tank by the mol ratio of chlorauric acid solution and surfactant solution, and at the uniform velocity stir with the speed of 200-300r/min, reaction 5-30min, obtains the mixed liquor containing nm of gold colloid;
Step S500: the drying that the mixed liquor prepared by step S400 carries out nm of gold colloid is purified, and obtains nanogold particle.
To prepare the HEPES buffer solution that the concentration of 200L is 50mmol/L, its collocation method is: the HEPES first taking 2.38kg is dissolved in the deionized water of 180L, ultrasonic, vibration until dissolve completely; Then use PH to measure the pH value of now solution is about 5.4, so slowly add the sodium hydroxide solution of 0.1mol/L and constantly stir until PH is adjusted to 7.4; Finally continue to add deionization to 200L.
Embodiment 2:
The present embodiment does further optimization on the basis of above-described embodiment, and further, the surfactant solution in described step S300 refers to PVP solution.Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
Embodiment 3: the present embodiment does further optimization on the basis of embodiment 2, further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:5-1:10 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: ultrafilter introduced by the mixed liquor prepared by step S400, adopts filtering with microporous membrane 3-5h, obtains nm of gold colloid in the below of miillpore filter; Then nm of gold colloid is placed in the drying oven of 50-60 DEG C, heat drying 3h, naturally cools to room temperature in a nitrogen environment, obtains the nanogold particle that particle diameter is less than 10nm.Other parts of the present embodiment are identical with embodiment 2, therefore repeat no more.
Embodiment 4: the present embodiment does further optimization on the basis of embodiment 2, further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:2-1:3 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: ultrafilter introduced by the mixed liquor prepared by step S400, adopts filtering with microporous membrane 3-5h, obtains nm of gold colloid in the below of miillpore filter; Then nm of gold colloid is placed in the drying oven of 50-60 DEG C, heat drying 3h, naturally cools to room temperature in a nitrogen environment, and obtaining particle diameter is the nanogold particle of 15-25nm.Other parts of the present embodiment are identical with embodiment 2, therefore repeat no more.
Embodiment 5: the present embodiment does further optimization on the basis of embodiment 2, further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:1-1:2 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: ultrafilter introduced by the mixed liquor prepared by step S400, adopts filtering with microporous membrane 3-5h, obtains nm of gold colloid in the below of miillpore filter; Then nm of gold colloid is placed in the drying oven of 50-60 DEG C, heat drying 3h, naturally cools to room temperature in a nitrogen environment, and obtaining particle diameter is the nanogold particle of 25-40nm.Other parts of the present embodiment are identical with embodiment 2, therefore repeat no more.
Embodiment 6: the present embodiment does further optimization on the basis of above-described embodiment, further, the described preferred aperture of micro-control filter membrane is the GHP filter membrane of 0.2um or 0.45um.Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
Embodiment 7: the present embodiment does further optimization on the basis of embodiment 1, further, the surfactant solution in described step S300 refers to PEG solution.Other parts of the present embodiment are identical with embodiment 1, therefore repeat no more.
Embodiment 8: the present embodiment does further optimization on the basis of embodiment 2, further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:5-1:10 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: the mixed liquor prepared by step S400 leaves standstill after 2-10h in standing groove, the claret liquid extracting below to supercentrifuge, with the rotating speed High Rotation Speed 2-5h of 10000r/min-16000r/min; Extract sediment and after fully washing by deionized water, be placed in the drying oven of 60-80 DEG C, heat drying 1-2h obtains dry solid particle in a nitrogen environment; Then the solid particle of drying is put into mortar and grind 0.5-1h, naturally cool to room temperature, obtaining particle diameter is the nanogold particle of 10-40nm.Other parts of the present embodiment are identical with embodiment 2, therefore repeat no more.
Embodiment 9: the present embodiment does further optimization on the basis of embodiment 8, further, described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 2mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:5-1:10 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: the mixed liquor prepared by step S400 leaves standstill after 3h in standing groove, the claret liquid extracting below to supercentrifuge, with the rotating speed High Rotation Speed 2h of 11000r/min; Extract sediment and after fully washing by deionized water, be placed in the drying oven of 60-80 DEG C, heat drying 1h obtains dry solid particle in a nitrogen environment; Then the solid particle of drying is put into mortar and grind 0.5h, naturally cool to room temperature, obtaining particle diameter is the nanogold particle of 10-20nm.Other parts of the present embodiment are identical with embodiment 8, therefore repeat no more.
The above is only preferred embodiment of the present invention, and not do any pro forma restriction to the present invention, every any simple modification, equivalent variations done above embodiment according to technical spirit of the present invention, all falls within protection scope of the present invention.
Claims (9)
1. a preparation method for nanogold particle, is characterized in that comprising the following steps:
Step S100: compound concentration is the chlorauric acid solution of 0.05-10mmol/L;
Step S200: compound concentration is the HEPES buffer solution of 5-50mmol/L, and regulate the pH value of HEPES buffer solution to 7.0-8.0 with NaOH;
Step S300: add surfactant in the HEPES buffer solution that step S200 prepares, compound concentration is the surfactant solution of 1-2mmol/L;
Step S400: the surfactant solution prepared by step S300 introduces reaction tank, be the chlorauric acid solution that 1:1-1:10 slowly adds step S100 and prepares in reaction tank by the mol ratio of chlorauric acid solution and surfactant solution, and at the uniform velocity stir with the speed of 200-300r/min, reaction 5-30min, obtains the mixed liquor containing nm of gold colloid;
Step S500: the drying that the mixed liquor prepared by step S400 carries out nm of gold colloid is purified, and obtains nanogold particle.
2. the preparation method of a kind of nanogold particle according to claim 1, is characterized in that: the surfactant solution in described step S300 refers to PVP solution.
3. the preparation method of a kind of nanogold particle according to claim 2, is characterized in that:
Described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:5-1:10 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: ultrafilter introduced by the mixed liquor prepared by step S400, adopts filtering with microporous membrane 3-5h, obtains nm of gold colloid in the below of miillpore filter; Then nm of gold colloid is placed in the drying oven of 50-60 DEG C, heat drying 3h, naturally cools to room temperature in a nitrogen environment, obtains the nanogold particle that particle diameter is less than 10nm.
4. the preparation method of a kind of nanogold particle according to claim 2, is characterized in that:
Described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:2-1:3 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: ultrafilter introduced by the mixed liquor prepared by step S400, adopts filtering with microporous membrane 3-5h, obtains nm of gold colloid in the below of miillpore filter; Then nm of gold colloid is placed in the drying oven of 50-60 DEG C, heat drying 3h, naturally cools to room temperature in a nitrogen environment, and obtaining particle diameter is the nanogold particle of 15-25nm.
5. the preparation method of a kind of nanogold particle according to claim 2, is characterized in that:
Described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:1-1:2 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: ultrafilter introduced by the mixed liquor prepared by step S400, adopts filtering with microporous membrane 3-5h, obtains nm of gold colloid in the below of miillpore filter; Then nm of gold colloid is placed in the drying oven of 50-60 DEG C, heat drying 3h, naturally cools to room temperature in a nitrogen environment, and obtaining particle diameter is the nanogold particle of 25-40nm.
6. the preparation method of a kind of nanogold particle according to claim 2-5 any one, is characterized in that: the described preferred aperture of micro-control filter membrane is the GHP filter membrane of 0.2um or 0.45um.
7. the preparation method of a kind of nanogold particle according to claim 1, is characterized in that: the surfactant solution in described step S300 refers to PEG solution.
8. the preparation method of a kind of nanogold particle according to claim 7, is characterized in that:
Described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 1mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:5-1:10 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: the mixed liquor prepared by step S400 leaves standstill after 2-10h in standing groove, the claret liquid extracting below to supercentrifuge, with the rotating speed High Rotation Speed 2-5h of 10000r/min-16000r/min; Extract sediment and after fully washing by deionized water, be placed in the drying oven of 60-80 DEG C, heat drying 1-2h obtains dry solid particle in a nitrogen environment; Then the solid particle of drying is put into mortar and grind 0.5-1h, naturally cool to room temperature, obtaining particle diameter is the nanogold particle of 10-40nm.
9. the preparation method of a kind of nanogold particle according to claim 8, is characterized in that:
Described step S100 specifically refers to: compound concentration is the chlorauric acid solution of 1mmol/L;
Described step S200 specifically refers to: compound concentration is the HEPES buffer solution of 20mmol/L, and regulates the pH value to 7.4 of HEPES buffer solution with NaOH;
Described step S300 specifically refers to: in the HEPES buffer solution that step S200 prepares, add surfactant, compound concentration is the surfactant solution of 2mmol/L;
Described step S400 specifically refers to: under normal temperature state, the surfactant solution prepared by step S300 introduces reaction tank, in reaction tank, the chlorauric acid solution that step S100 prepares slowly is added by the mol ratio 1:5-1:10 of chlorauric acid solution and surfactant solution, and stir 10min with the speed of 250r/min, obtain the mixed liquor containing nm of gold colloid;
Described step S500 specifically refers to: the mixed liquor prepared by step S400 leaves standstill after 3h in standing groove, the claret liquid extracting below to supercentrifuge, with the rotating speed High Rotation Speed 2h of 11000r/min; Extract sediment and after fully washing by deionized water, be placed in the drying oven of 60-80 DEG C, heat drying 1h obtains dry solid particle in a nitrogen environment; Then the solid particle of drying is put into mortar and grind 0.5h, naturally cool to room temperature, obtaining particle diameter is the nanogold particle of 10-20nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510273386.8A CN104874812A (en) | 2015-05-26 | 2015-05-26 | Preparation method of gold nanoparticles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510273386.8A CN104874812A (en) | 2015-05-26 | 2015-05-26 | Preparation method of gold nanoparticles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104874812A true CN104874812A (en) | 2015-09-02 |
Family
ID=53942633
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510273386.8A Pending CN104874812A (en) | 2015-05-26 | 2015-05-26 | Preparation method of gold nanoparticles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104874812A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107356655A (en) * | 2017-06-28 | 2017-11-17 | 东南大学 | A kind of preparation method and application of nanofiber modified electrode |
| CN108132239A (en) * | 2018-02-22 | 2018-06-08 | 合肥工业大学 | Multilayered structure surface enhanced Raman substrate construct and its control accurate of performance |
| CN109986072A (en) * | 2017-12-29 | 2019-07-09 | 吉林大学 | Four wooden fork gold nanoparticles, preparation method and applications |
| CN116140635A (en) * | 2022-12-29 | 2023-05-23 | 宁波大学 | Preparation method of nail-shaped gold nanostar |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1663715A (en) * | 2004-12-02 | 2005-09-07 | 黄德欢 | Method for preparing supported nano gold powder |
| JP2006299354A (en) * | 2005-04-21 | 2006-11-02 | Osaka Prefecture Univ | Method for producing metal nanoparticulate by high energy electron beam |
| CN101367129A (en) * | 2008-03-07 | 2009-02-18 | 浙江师范大学 | Manufacture of nano-golden particle with biological reductant Vc in reversed micellar |
| CN102990082A (en) * | 2012-12-17 | 2013-03-27 | 桂林理工大学 | Method for preparing fluorescence nano gold sol by using PVP (Poly Vinyl Pyrrolidone) through reduction modification under hydrothermal condition |
| CN103143722A (en) * | 2013-03-21 | 2013-06-12 | 江西农业大学 | Method for preparing multipod-like gold nanoparticles by chemical method |
| CN104070177A (en) * | 2014-06-28 | 2014-10-01 | 内蒙古工业大学 | Simple and novel preparation method for silver and gold nano-particles |
-
2015
- 2015-05-26 CN CN201510273386.8A patent/CN104874812A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1663715A (en) * | 2004-12-02 | 2005-09-07 | 黄德欢 | Method for preparing supported nano gold powder |
| JP2006299354A (en) * | 2005-04-21 | 2006-11-02 | Osaka Prefecture Univ | Method for producing metal nanoparticulate by high energy electron beam |
| CN101367129A (en) * | 2008-03-07 | 2009-02-18 | 浙江师范大学 | Manufacture of nano-golden particle with biological reductant Vc in reversed micellar |
| CN102990082A (en) * | 2012-12-17 | 2013-03-27 | 桂林理工大学 | Method for preparing fluorescence nano gold sol by using PVP (Poly Vinyl Pyrrolidone) through reduction modification under hydrothermal condition |
| CN103143722A (en) * | 2013-03-21 | 2013-06-12 | 江西农业大学 | Method for preparing multipod-like gold nanoparticles by chemical method |
| CN104070177A (en) * | 2014-06-28 | 2014-10-01 | 内蒙古工业大学 | Simple and novel preparation method for silver and gold nano-particles |
Non-Patent Citations (1)
| Title |
|---|
| 曾琦斐: "表面活性剂存在下HEPES缓冲溶液中制备纳米金颗粒", 《武汉工程大学学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107356655A (en) * | 2017-06-28 | 2017-11-17 | 东南大学 | A kind of preparation method and application of nanofiber modified electrode |
| CN107356655B (en) * | 2017-06-28 | 2019-06-14 | 东南大学 | A kind of preparation method and application of nanofiber modified electrode |
| CN109986072A (en) * | 2017-12-29 | 2019-07-09 | 吉林大学 | Four wooden fork gold nanoparticles, preparation method and applications |
| CN109986072B (en) * | 2017-12-29 | 2021-06-25 | 吉林大学 | Four-fork gold nano-particle, preparation method and application thereof |
| CN108132239A (en) * | 2018-02-22 | 2018-06-08 | 合肥工业大学 | Multilayered structure surface enhanced Raman substrate construct and its control accurate of performance |
| CN116140635A (en) * | 2022-12-29 | 2023-05-23 | 宁波大学 | Preparation method of nail-shaped gold nanostar |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103170645B (en) | The preparation method of nano silver wire | |
| CN103100724B (en) | Preparation method of silver nanowires | |
| CN110026569B (en) | Preparation method of nano-silver | |
| CN104874812A (en) | Preparation method of gold nanoparticles | |
| CN103361885B (en) | A kind of preparation method of antibacterial fibroin fiber film | |
| CN104289722B (en) | A kind of preparation method of nanometer silver | |
| CN110355380B (en) | Preparation method of hexagonal flaky micron-crystal silver powder | |
| CN104174864B (en) | The preparation method of a kind of nanometer or submicron order Argent grain powder | |
| CN106216710A (en) | A kind of preparation method of high-tap density high-crystallinity silver powder | |
| CN102248177B (en) | Laser-induced method for preparing spherical silver powder | |
| CN104551007A (en) | Large-scale preparation method of silver nano-sheets | |
| CN102873337A (en) | Poly-allylamine oriented platinum nano cube preparation method | |
| WO2014183243A1 (en) | Method for preparing graphene material and use thereof in chemical energy storage and/or conversion | |
| CN105345023A (en) | Preparing method for superfine silver powder good in dispersity | |
| CN108411401B (en) | Nano-selenium composite fiber and preparation method thereof | |
| CN105462365A (en) | Electric conduction nanometer copper ink preparation method | |
| CN104907557A (en) | Flower-like gold palladium heterogeneous nano particle with good electro-catalytic property and preparing method thereof | |
| CN108372310A (en) | A kind of preparation method of small-size nano-silver for water-base conductive ink | |
| CN108971513B (en) | Nano copper particle and low-cost green and environment-friendly preparation method thereof | |
| CN105921765B (en) | A kind of preparation method of the bar-shaped silver powder of size tunable | |
| CN104841946A (en) | Silver nanorod and preparing method thereof | |
| CN110181074A (en) | A kind of method that compound soft template method green prepares high length-diameter ratio silver nanowires | |
| CN111992738B (en) | Method for synthesizing nano silver particles with wide range of particle size distribution by one-pot method | |
| CN106825553B (en) | A kind of preparation method of cobalt-nitrogen-carbon nucleocapsid hybrid hollow porous carbon ball | |
| CN103978226A (en) | Micro nano silver-based material preparation method and micro nano silver-based material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20150902 Assignee: SICHAUN DICHEN AGRICULTURAL LIMITED LIABILITY COMPANY Assignor: Yi Chuansi bio tech ltd, Chengdu Contract record no.: 2016510000008 Denomination of invention: Method for preparing nano-golden particle License type: Common License Record date: 20160506 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150902 |
|
| RJ01 | Rejection of invention patent application after publication |