CN113210622A - Preparation method for synthesizing gold nanoparticles with different particle sizes by one-step method of direct reduction of carbon black - Google Patents

Preparation method for synthesizing gold nanoparticles with different particle sizes by one-step method of direct reduction of carbon black Download PDF

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CN113210622A
CN113210622A CN202110388157.6A CN202110388157A CN113210622A CN 113210622 A CN113210622 A CN 113210622A CN 202110388157 A CN202110388157 A CN 202110388157A CN 113210622 A CN113210622 A CN 113210622A
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carbon black
aunps
gold nanoparticles
particle sizes
different particle
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CN113210622B (en
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崔大祥
彭家伟
周诚
梁辉
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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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
    • 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 invention provides a preparation method for synthesizing gold nanoparticles with different particle sizes by a carbon black direct reduction one-step method, which relates to the technical field of nano materials and comprises the following steps: first 10 mL of 2 mg mL‑1XC-72 carbon black is added into a polytetrafluoroethylene reaction kettle after being subjected to ultrasonic dispersion for 30 min, and then 20 mL of 2wt% HAuCl is added4After being mixed uniformly, the mixture is subjected to hydrothermal reaction for 2 hours at 180 ℃. And filtering the product by a 0.22-micron syringe filter, centrifuging by 1, alternately washing by deionized water and absolute ethyl alcohol, and dispersing in water again to obtain the AuNPs solution with good dispersibility. The method has the advantages of simple operation, low cost, controllable size, large-scale preparation of AuNPs and the like, and the prepared AuNPs show good biocompatibility, thereby providing wide application prospect in the fields of colloidal gold immunochromatography, immunolabeling and the like.

Description

Preparation method for synthesizing gold nanoparticles with different particle sizes by one-step method of direct reduction of carbon black
Technical Field
The invention relates to the technical field of nano materials, relates to a preparation method for synthesizing gold nanoparticles by a one-step method through direct reduction of carbon black, and particularly relates to a novel preparation method of gold nanoparticles with good dispersibility, controllable size and good biocompatibility.
Technical Field
Gold nanoparticles (AuNPs) are one of the most studied precious metal nanoparticles, and have the advantages of stable property, uniform particle size, good biocompatibility, easy modification and the like, so that the gold nanoparticles are widely applied to the fields of nano biosensors, biological imaging and the like. The current AuNPs synthesis method can be mainly divided into a physical method and a chemical method. The physical method is to disperse the massive solid gold materials into small gold nanoparticles, the operation method needs complicated instruments and equipment, the reaction conditions are harsh, and the obtained gold nanoparticles are not uniform in particle size distribution. The chemical method mainly uses a gold compound as a precursor, firstly reduces the gold compound to form gold atoms through adding a reducing agent, and then further aggregates the gold atoms to form AuNPs with different particle sizes. The chemical method is widely applied because of simple operation and strong controllability, and the prepared gold nanoparticles have uniform particle size. The most common chemical reduction method at present is that of Turkevitch-Frens uses sodium citrate as a reducing agent to reduce chloroauric acid (HAuCl) by a multi-step growth method under boiling conditions4) The method can control the size to be 10-150 nm, the size with good dispersity and uniform grain diameter is only about 13nm, the number of required growth steps is increased along with the increase of the synthetic size, excessive operation not only causes difficulty in grain diameter control and high cost and difficulty in large-scale preparation, but also further influences the combinability and modification of AuNPs due to the accumulation of reducing ions on the surfaces of the AuNPs in the preparation process, so that the biocompatibility of the AuNPs is reduced.
Therefore, a synthesis method for preparing gold nanoparticles with different sizes and good size monodispersity and biocompatibility in one step on a large scale is urgently needed.
Disclosure of Invention
In order to solve the problems of complicated operation steps, difficult control of particle size and the like in the process of synthesizing AuNPs with different sizes by the existing multi-step growth method, the invention aims to provide a preparation method for synthesizing gold nanoparticles with different sizes by a carbon black direct reduction one-step method.
The invention aims to provide the following scheme for realizing: preparation for synthesizing gold nanoparticles with different particle sizes by one-step method of direct reduction of carbon blackThe method utilizes XC-72 carbon black as a reducing agent and adjusts XC-72 carbon black and HAuCl4The method for preparing the AuNPs with controllable size, good dispersibility and good biocompatibility by a one-step hydrothermal method under neutral, acidic or alkaline conditions comprises the following steps:
first 10 mL of 2 mg mL-1XC-72 carbon black is added into a polytetrafluoroethylene reaction kettle after being subjected to ultrasonic dispersion for 30 min, and then 20 mL of 0.5-2.5wt% HAuCl is added4After being uniformly mixed, the mixture is subjected to hydrothermal reaction for 2 hours at the temperature of 120-200 ℃ to obtain a product;
and filtering the product by a 0.22-micron syringe filter, centrifuging, alternately washing by water and absolute ethyl alcohol, and then re-dispersing in water to obtain the AuNPs solution.
Preferably, the AuNPs solution is obtained by filtering 3 times by using a syringe filter, centrifuging for 10 min at 1000 rpm, washing for three times by using water and absolute ethyl alcohol, and then re-dispersing in water.
Preferably, the hydrothermal reaction temperature is 180 ℃.
The reducing agent adopted by the invention is XC-72 carbon black (VULCAN XC72 carbon black), and HAuCl is reduced under neutral, acidic and alkaline conditions4The preparation of AuNPs is within the scope of the present invention.
Preferably, the reaction conditions are such that the hydrothermal temperature is 180 ℃.
The method can regulate the synthetic particle size of AuNPs and improve the biocompatibility of the AuNPs.
The good biocompatibility of the product provides wide application prospect for the product in the fields of colloidal gold immunochromatography, immune marking and the like. The method solves the harsh requirement on a reducing agent when AuNPs are prepared by the traditional chemical reduction method, and the method can reduce a gold compound to generate the AuNPs only by using XC-72 carbon black with wide material sources and low cost, and is suitable for large-scale production of the AuNPs.
The invention utilizes XC-72 carbon black as a reducing agent and adjusts XC-72 carbon black and HAuCl4The AuNPs with different sizes and better dispersibility can be obtained by simple one-step hydrothermal method. Compared with the traditional multi-step growth reduction method, the used XC-72 carbon black has wide material source, is green and has no pollutionPollution, low cost and the like; and the prepared AuNPs show better biocompatibility, and provide wide application prospects in the fields of colloidal gold immunochromatography, immunolabeling and the like. In conclusion, the method is efficient, rapid, simple and cheap, and has remarkable economic and social benefits.
Drawings
FIG. 1 is a diagram of the mechanism of AuNPs synthesis according to the present invention;
FIG. 2 is a diagram showing the influence of reaction temperature on ultraviolet absorption spectrum in an AuNPs synthesis system;
FIG. 3 shows XC-72 carbon black and HAuCl in AuNPs synthesis system4The mass ratio affects the TEM image of the particle size results, where FIG. 3A and FIG. 3B are XC-72 carbon black and HAuCl, respectively4The mass ratio is 1:5 and 1: 25;
FIG. 4 is a graph showing UV absorption spectra of AuNPs prepared by different methods after incubation with Bovine Serum Albumin (BSA).
Detailed Description
Example 1
Gold nanoparticles with different particle sizes are synthesized by a carbon black direct reduction one-step method, XC-72 carbon black is used as a reducing agent, and XC-72 carbon black and HAuCl are adjusted4The mass ratio of AuNPs is controlled by a one-step hydrothermal method under neutral, acidic or alkaline conditions, and the AuNPs with controllable size, good dispersibility and good biocompatibility are prepared according to the following steps:
first 10 mL of 2 mg mL-1XC-72 carbon black is added into a polytetrafluoroethylene reaction kettle after being subjected to ultrasonic dispersion for 30 min, and then 20 mL of 2wt% HAuCl is added4After being uniformly mixed, the mixture is subjected to hydrothermal reaction for 2 hours at 120 ℃, 140 ℃, 160 ℃, 180 ℃ and 200 ℃ respectively to obtain a product;
and filtering the product by a 0.22-micron syringe filter for 3 times, centrifuging at 1000 rpm for 10 min, alternately washing the product with water and absolute ethyl alcohol for three times, and dispersing the product in water again to obtain the AuNPs solution with good dispersibility.
As can be seen from FIG. 1, XC-72 carbon black is cracked into small molecular substances at high temperature, and the reduction of HAuCl is increased4Thereby producing AuNPs.
As shown in fig. 2, the maximum ultraviolet absorption peak of AuNPs is at 525 nm, and the intensity of the absorption peak of AuNPs increases with the increase of the reaction temperature, which indicates that the concentration of the generated AuNPs increases, and the intensity of the absorption peak decreases when the temperature is higher than 180 ℃, which may affect XC-72 carbon black or the generated AuNPs structure due to the excessive temperature, and in conclusion, 180 ℃ is selected as the optimal reaction temperature.
Example 2
Gold nanoparticles with different particle sizes are synthesized by a carbon black direct reduction one-step method, similar to the example 1, and are prepared by the following steps:
first 10 mL of 2 mg mL-1XC-72 carbon black is added into a polytetrafluoroethylene reaction kettle after being subjected to ultrasonic dispersion for 30 min, and then 20 mL of HAuCl with the weight percentages of 0.5 wt%, 1 wt%, 1.5 wt%, 2wt% and 2.5wt% are respectively added4After being uniformly mixed, carrying out hydrothermal reaction for 2 h at 180 ℃ to obtain a product;
and filtering the product by a 0.22-micron syringe filter for 3 times, centrifuging the product for 10 min at 1000 rpm, washing the product by water and absolute ethyl alcohol for three times, and dispersing the product in water again to obtain the AuNPs solution with good dispersibility.
As shown in FIG. 3, when XC-72 carbon black is used with HAuCl4When the mass ratio is 1:5, the grain size of the prepared AuNPs is about 10 nm (figure 3A); when XC-72 carbon black is mixed with HAuCl4When the mass ratio is 1:25, the prepared AuNPs have the particle size of about 50 nm (figure 3B) and have good size monodispersity.
Shows that the particle size of the generated AuNPs is along with XC-72 carbon black and HAuCl4The mass ratio is increased, so that the mass ratio can be increased by adjusting XC-72 carbon black and HAuCl in the reaction system4Mass ratio to prepare AuNPs of different particle sizes.
Example 3
Gold nanoparticles with different particle sizes are synthesized by a carbon black direct reduction one-step method, similar to the example 1, and are prepared by the following steps:
first, 10 mL of 2 mg mL was taken-1XC-72 carbon black is added into a polytetrafluoroethylene reaction kettle after being subjected to ultrasonic dispersion for 30 min, and then 20 mL of 2wt% HAuCl are added4After being uniformly mixed, the mixture is subjected to hydrothermal reaction for 1 hour, 2 hours, 3 hours, 4 hours and 5 hours at the set temperature of 180 ℃ respectively to obtain products;
and filtering the product by a 0.22-micron syringe filter for 3 times, centrifuging the product for 10 min at 1000 rpm, washing the product by water and absolute ethyl alcohol for three times, and dispersing the product in water again to obtain the AuNPs solution with good dispersibility.
In order to verify the good biocompatibility of AuNPs prepared by the method, XC-72 carbon black and classical citric acid are respectively used as reducing agents and equal amount of HAuCl in experiments4AuNPs (designated AuNPs (XC-72) and AuNPs (lemon), respectively) were prepared by reaction, the prepared AuNPs were incubated with colloidal gold immunologically active site blocker Bovine Serum Albumin (BSA) commonly used in immunodiagnosis for 1 hour, then unbound BAS was removed by centrifugation, and the incubated conjugate was resuspended in 0.01mol/L PBS buffer and the UV absorbance intensity of BAS at 270 nm was recorded.
FIG. 4 is a graph showing UV absorption spectra of AuNPs prepared by different methods after incubation with Bovine Serum Albumin (BSA), as shown in FIG. 4, the UV absorption value of AuNPs (XC-72) at 270 nm is significantly stronger than that of AuNPs (lemon), which indicates that more BSA is bound to the surface of AuNPs (XC-72) than to the surface of AuNPs (XC-72), and thus the AuNPs prepared by the present invention have better biocompatibility.

Claims (4)

1. A preparation method for synthesizing gold nanoparticles with different particle sizes by a one-step method of direct reduction of carbon black is characterized in that XC-72 carbon black is used as a reducing agent, and XC-72 carbon black and HAuCl are adjusted4The method for preparing the AuNPs with controllable size, good dispersibility and good biocompatibility by a one-step hydrothermal method under neutral, acidic or alkaline conditions comprises the following steps:
first 10 mL of 2 mg mL-1XC-72 carbon black is added into a polytetrafluoroethylene reaction kettle after being subjected to ultrasonic dispersion for 30 min, and then 20 mL of 0.5-2.5wt% HAuCl is added4After being uniformly mixed, the mixture is subjected to hydrothermal reaction for 2 hours at the temperature of 120-200 ℃ to obtain a product;
and filtering and centrifuging the product by a 0.22-micron syringe filter in sequence, alternately washing the product by water and absolute ethyl alcohol, and then re-dispersing the product in water to obtain the AuNPs solution.
2. The preparation method for synthesizing gold nanoparticles with different particle sizes by the one-step direct reduction of carbon black as claimed in claim 1, wherein the AuNPs solution is obtained by a one-step hydrothermal method under neutral conditions.
3. The method for preparing gold nanoparticles with different particle sizes by the one-step direct reduction of carbon black as claimed in claim 1, wherein the AuNPs solution is obtained by filtering with a syringe filter for 3 times, centrifuging at 1000 rpm for 10 min, washing with water and absolute ethyl alcohol for three times, and then re-dispersing in water.
4. The method for preparing gold nanoparticles with different particle sizes by using the one-step direct reduction method of carbon black according to claim 1, wherein the hydrothermal reaction temperature is 180 ℃.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100154591A1 (en) * 2008-12-23 2010-06-24 Islam M Rafiq Household microwave-mediated carbohydrate-based production of silver nanomaterials
US20160141630A1 (en) * 2013-08-01 2016-05-19 Nanyang Technological University Method for forming noble metal nanoparticles on a support
US20160303544A1 (en) * 2013-11-04 2016-10-20 Portland State University Method of making a metallic composite and use thereof
US20190367368A1 (en) * 2016-11-17 2019-12-05 Research Institute Of Petroleum Industry Formulation for the synthesis of thermal nanofluid based on carbon nanodots
CN110947381A (en) * 2018-09-27 2020-04-03 湖南大学 Carbon black limited nano gold catalyst and preparation method thereof
CN111975010A (en) * 2019-05-21 2020-11-24 中国药科大学 Preparation of gold nanoparticles based on D-arabinose reduction

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100154591A1 (en) * 2008-12-23 2010-06-24 Islam M Rafiq Household microwave-mediated carbohydrate-based production of silver nanomaterials
US20160141630A1 (en) * 2013-08-01 2016-05-19 Nanyang Technological University Method for forming noble metal nanoparticles on a support
US20160303544A1 (en) * 2013-11-04 2016-10-20 Portland State University Method of making a metallic composite and use thereof
US20190367368A1 (en) * 2016-11-17 2019-12-05 Research Institute Of Petroleum Industry Formulation for the synthesis of thermal nanofluid based on carbon nanodots
CN110947381A (en) * 2018-09-27 2020-04-03 湖南大学 Carbon black limited nano gold catalyst and preparation method thereof
CN111975010A (en) * 2019-05-21 2020-11-24 中国药科大学 Preparation of gold nanoparticles based on D-arabinose reduction

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