CN111468739A - Magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle, preparation method thereof and dye degradation method - Google Patents

Magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle, preparation method thereof and dye degradation method Download PDF

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CN111468739A
CN111468739A CN202010225133.4A CN202010225133A CN111468739A CN 111468739 A CN111468739 A CN 111468739A CN 202010225133 A CN202010225133 A CN 202010225133A CN 111468739 A CN111468739 A CN 111468739A
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core
coated
shell structure
structure composite
nickel
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林红军
申利国
刘莹
黄正义
邓颖
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Zhejiang Normal University CJNU
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Zhejiang Normal University CJNU
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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
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17—Metallic particles coated with metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts

Abstract

The invention provides a magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle, a preparation method thereof and a dye degradation method, wherein the preparation method of the magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle comprises the following steps: preparing a nickel reducing solution; and adding a soluble silver salt into the nickel reducing solution, fully reacting to obtain a solid precipitate, and then sequentially separating, washing, drying and grinding the solid precipitate to obtain the Ni-coated Ag core-shell structure composite nano-particles. The method deposits the metal nickel nano particles on the surface of the silver by a one-step chemical deposition method to form the core-shell type nickel/silver nano structure catalyst, has simple operation and low cost, is easy to realize industrial application, and has important significance in the application aspect of printing and dyeing wastewater.

Description

Magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle, preparation method thereof and dye degradation method
Technical Field
The invention relates to the technical field of catalyst degradation dyes, in particular to magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticles, a preparation method thereof and a dye degradation method.
Background
Nowadays, dyes in the textile, paper, leather and cosmetic industries are very dangerous both to humans and to the environment, due to their toxic and carcinogenic nature, polluting water resources. Efforts have been made to develop effective techniques for removing organic contaminants from aqueous media. Various techniques are used in wastewater treatment, such as chemical oxidation, adsorption, photocatalysis and membrane separation, which are costly and have some limitations. Among them, "photocatalysis" is considered as a green technology with low energy consumption and cost-effectiveness to environmental issues.
Novel materials are synthesized by alloying two or more metals to create or engineer multifunctional alloy nanospheres with unique and excellent catalytic properties, magnetic, electrical, thermal, electronic, hydrogen evolution and optical properties. Nickel nanospheres are of interest due to their potential application as nanocatalysts and important low cost, electrical conductivity and magnetic properties. On the other hand, silver nanospheres have attracted great interest due to their high chemical stability, optical properties, excellent electrical conductivity and strong antibacterial properties. Therefore, it is desirable to directionally assemble metallic Ni on the surface of Ag by surface strategy.
In conclusion, the research and development of the magnetic Ni @ Ag nanosphere for degrading various different dyes has important application value and academic significance.
Disclosure of Invention
The invention mainly aims to provide magnetic recyclable Ni-coated Ag core-shell structure composite nano-particles, a preparation method thereof and a dye degradation method.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a method for preparing magnetically recoverable Ni-coated Ag core-shell structure composite nanoparticles.
The preparation method of the magnetic recyclable Ni-coated Ag core-shell structure composite nano-particles comprises the following steps:
s1, preparing a nickel reducing solution;
and S2, adding soluble silver salt into the nickel reducing solution, fully reacting to obtain solid precipitate, and then sequentially separating, washing, drying and grinding the solid precipitate to obtain the Ni-coated Ag core-shell structure composite nano-particles.
Further, in step S1, the method for preparing the nickel reducing solution includes:
s1-1, mixing nickel salt, sodium pyrophosphate, ammonia water and a borane reducing agent according to the weight part ratio of 20-30: 45-55: 40-50: 1-2, adding the mixture into deionized water to obtain a mixed solution;
s1-2, fully stirring the mixed solution obtained in the step S1-1 under ultrasound to obtain a nickel reducing solution.
Further, in step S1-1, the ratio of the nickel salt, sodium pyrophosphate, ammonia water, and borane reducing agent in parts by weight is 25: 50: 45: 1.5.
further, at step S1-1, the nickel salt includes nickel sulfate hexahydrate (NiSO)4·6H2O), nickel sulfate heptahydrate, anhydrous nickel sulfate, anhydrous nickel chloride, and nickel carbonate.
Further, in the step S1-2, the ultrasonic stirring time is 15-20 mim.
Further, in step S2, the mass ratio of the soluble silver salt to the nickel reducing solution is 1: 10 to 100.
Further, in step S2, the soluble silver salt and the nickel reducing solution fully react at 20 to 30 ℃ for 15 to 25min to obtain the solid precipitate.
Further, in step S2, the drying process is performed by standing at room temperature for 24 hours or in an oven at 30 ℃ for 6 hours.
Further, in step S2, the soluble silver salt includes silver perchlorate (AgClO)4) And silver nitrate (AgNO)3)。
In order to achieve the above object, according to a second aspect of the present invention, there is provided a Ni-coated Ag core-shell structure composite nanoparticle.
The Ni-coated Ag core-shell structure composite nano-particles are prepared according to the preparation method of the magnetic recyclable Ni-coated Ag core-shell structure composite nano-particles.
In order to achieve the above object, according to a third aspect of the present invention, there is provided a dye degradation method.
The dye degradation method takes the Ni-coated Ag core-shell structure composite nano-particles prepared by the preparation method of the magnetic recyclable Ni-coated Ag core-shell structure composite nano-particles as a catalyst, and comprises the following steps:
weighing a certain amount of the Ni-coated Ag core-shell structure composite nano-particles and a certain volume of dye solution, wherein the mass-to-volume ratio of the Ni-coated Ag core-shell structure composite nano-particles to the dye solution is 1 mg: 1M L-1 mg: 5M L, and sodium borohydride with the concentration of 0.02-0.15M is added into the dye solution;
the photocatalytic reaction is carried out under ultraviolet illumination or simulated sunlight.
Further, the dye in the dye solution is methylene blue, rhodamine B, tiger red sodium salt, orange G, congo red, methylene orange, crystal violet, indigo carmine or neutral red.
In the invention, the magnetic Ni @ Ag nanosphere is successfully developed for the first time to degrade the dye. Depositing metal nickel nano particles on the surface of silver by a one-step chemical deposition method to form the core-shell type nickel/silver nano structure catalyst.
In the photocatalysis experiment of the invention, the result shows that the Ni @ Ag nano-structure catalyst shows excellent performance of degrading dye by photocatalysis. The degradation rate of all 9 dyes was over 85% after exposure to uv light for 3 minutes. The degradation rate of the MB solution after 10 continuous kinetic cycles is still about 98 percent, which shows that the Ni @ Ag nano-structured catalyst still has excellent reusability and high stability. The recovery process of the Ni @ Ag nanostructured catalyst is easy because it requires only a magnet to suck the catalyst out of the dye solution. Due to its low cost and excellent catalytic activity, Ni @ Ag nanostructured catalysts may be a new material for photocatalytic degradation of dyes in practical applications.
The invention has the beneficial effects that:
(1) the invention deposits metal nickel nano particles on the surface of silver by a chemical deposition method to form the core-shell type silver/nickel nano structure catalyst. The method has strong applicability, can easily realize covering, has simple equipment and low cost, and is easy to realize large-scale industrial application.
(2) The method reduces nickel on the surface of silver, and has the advantages of mild reaction process conditions, no energy consumption, high reaction efficiency and obvious popularization advantage.
(3) The invention has wide application range and can be applied to various composite metal catalysts. The metal may be nickel, copper, silver, etc.
(4) The method can be suitable for preparing Fe3O4@ Ag and Co @ Ag catalysts.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a Transmission Electron Microscope (TEM) image of Ni-coated Ag core-shell structure composite nanoparticles in an example of the present invention;
FIG. 2 is a comparison graph of the catalytic degradation effect of Ni-coated Ag core-shell structure composite nanoparticles and the existing catalyst in the embodiment of the present invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
The invention discloses a preparation method of magnetic recyclable Ni-coated Ag core-shell structure composite nano-particles, which specifically comprises the following steps:
s1, adding 20-30 parts of nickel salt, 45-55 parts of sodium pyrophosphate, 40-50 parts of ammonia water (28%) and 1-2 parts of borane reducing agent into a clean beaker, pouring 1L parts of deionized water, and fully stirring for 15-25 min under ultrasonic to completely dissolve solid powder into an aqueous solution, thereby obtaining a uniform nickel (Ni) reducing solution.
S2, mixing the components in a mass ratio of 1: pouring soluble silver salt into the nickel reducing solution according to the proportion of 10-100, fully reacting for 15-25 min at 20-30 ℃ to obtain solid precipitate, separating the solid precipitate through Whatman filter paper, washing with deionized water, standing at normal temperature for 24 hours or standing in an oven at 30 ℃ for 6 hours, and finally grinding to obtain the dried magnetic Ni-coated Ag core-shell structure composite nano-particles.
The following will describe in detail the preparation method of the magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle by specific examples.
Example 1:
adding 25 parts of nickel sulfate hexahydrate, 50 parts of sodium pyrophosphate, 45 parts of ammonia water (28%) and 1.5 parts of borane reducing agent into a clean beaker, pouring 1L deionized water, and fully stirring for 20min under ultrasonic to completely dissolve solid powder into an aqueous solution, thereby obtaining a uniform Ni reducing solution.
Pouring 5m L silver nitrate solution into the Ni reducing solution, fully reacting for 20min at 25 ℃ to obtain solid precipitate, separating the solid precipitate by Whatman filter paper, washing with deionized water, standing the solid precipitate-Ni-coated Ag nano-particles for 24 h at normal temperature for drying, and fully grinding to obtain the dried magnetic Ni-coated Ag core-shell structure composite nano-particles.
Example 2:
adding 20 parts of anhydrous nickel chloride, 55 parts of sodium pyrophosphate, 40 parts of ammonia water (28%) and 1 part of borane reducing agent into a clean beaker, pouring 1L deionized water, and fully stirring for 15min under ultrasonic to completely dissolve solid powder into the aqueous solution, thereby obtaining the uniform Ni reducing solution.
Pouring 5m L silver nitrate solution into the Ni reducing solution, fully reacting for 15min at 20 ℃ to obtain solid precipitate, separating the solid precipitate by Whatman filter paper, washing with deionized water, placing the solid precipitate-Ni-coated Ag nano-particles in an oven at 30 ℃ for 6 hours for drying treatment, and fully grinding to obtain the dried magnetic Ni-coated Ag core-shell structure composite nano-particles.
Example 3:
adding 30 parts of nickel carbonate, 45 parts of sodium pyrophosphate, 50 parts of ammonia water (28%) and 2 parts of borane reducing agent into a clean beaker, pouring 1L deionized water, and fully stirring for 25min under ultrasonic to completely dissolve solid powder into the aqueous solution, thereby obtaining uniform Ni reducing solution.
And pouring 10m of L silver nitrate solution into the Ni reducing solution, fully reacting for 25min at 35 ℃ to obtain solid precipitate, separating the solid precipitate by Whatman filter paper, washing with deionized water, standing at normal temperature for 24 hours for drying, fully grinding, and finally obtaining the dried magnetic Ni-coated Ag core-shell structure composite nano-particles.
The Ni-coated Ag core-shell structure composite nano-particles are prepared according to the preparation method in the embodiment 1-3, TEM test is carried out on the magnetic Ni-coated Ag core-shell structure composite nano-particles in order to examine the appearance of the magnetic Ni-coated Ag core-shell structure composite nano-particles, and the result is shown in figure 1, wherein the Ni-coated Ag core-shell structure composite nano-particles are of a spherical structure with Ag as an inner core and Ni coated outside; meanwhile, the successful preparation of the Ni @ Ag nano catalyst is also proved, and the chemical formula of the Ni-coated Ag core-shell structure composite nano particle is Ni @ Ag, wherein @ represents coated.
The invention also discloses a dye degradation method, which takes the Ni-coated Ag core-shell structure composite nano-particles prepared by the preparation method in the embodiment 1-3 as a catalyst, and the experiment for catalyzing and degrading dye by using the catalyst is explained in detail by the specific embodiment.
Example 4:
weighing 20mg of Ni-coated Ag core-shell structure composite nano-particles, then pouring the Ni-coated Ag core-shell structure composite nano-particles into 30m L Methylene Blue (MB) solution, wherein the pH value of the MB solution is 4, the MB concentration in the MB solution is 20 mg/L, and sodium borohydride (NaBH)4) The concentration of (A) is 0.1M;
and respectively carrying out photocatalytic reaction under ultraviolet illumination and simulated sunlight, and recording degradation rate data of the Ni-coated Ag core-shell structure composite nano-particles in different illumination scenes.
Example 5:
the rhodamine b (rh b) dye solution was catalytically degraded using the method of example 4.
Example 6:
the tiger red sodium salt (RB) dye solution was catalytically degraded using the method of example 4.
Example 7:
the Orange G (OG) dye solution was subjected to catalytic degradation using the method of example 4.
Example 8:
congo Red (CR) dye solutions were catalytically degraded using the method of example 4.
Example 9:
the catalytic degradation of the Methylene Orange (MO) dye solution was carried out using the method of example 4.
Example 10:
the catalytic degradation of the Crystal Violet (CV) dye solution was carried out using the method in example 4.
Example 11:
the Indigo Carmine (IC) dye solution was subjected to catalytic degradation using the method of example 4.
Example 12:
the Neutral Red (NR) dye solution was catalytically degraded using the method of example 4.
The experimental results show that the degradation degrees of Methylene Blue (MB), rhodamine B (Rh B), tiger red sodium salt (RB), orange yellow G (OG), Congo Red (CR), Methylene Orange (MO), Crystal Violet (CV), Indigo Carmine (IC) and Neutral Red (NR) are respectively 99.61%, 99.56%, 99.68%, 99.37%, 99.98%, 99.17%, 99.66%, 88.62% and 94.23% after the ultraviolet irradiation is carried out for 3 minutes; the degradation degrees of Methylene Blue (MB), rhodamine (Rh B), tiger red sodium salt (RB), orange g (og), Congo Red (CR), Methylene Orange (MO), Crystal Violet (CV), Indigo Carmine (IC) and Neutral Red (NR) after 3 minutes of simulated solar irradiation were 99.68%, 99.16%, 92.80%, 82.17%, 98.01%, 99.81%, 99.81%, 76.23% and 83.63%, respectively.
In the present invention, to further investigate the stability of the magnetic Ni @ Ag nanocatalysts to degradation dyes, tests were performed with Methylene Blue (MB) dye solutions, repeated for 10 cycles. The results show that the magnetic Ni @ Ag nanocatalyst shows sustained stability to degradation of methylene blue dye.
To investigate NaBH4The concentration of (A) on the degradation effect of the dye, the present invention on NaBH in the dye solution4The addition concentration of (b) was tested. Specifically, the test was performed with Methylene Blue (MB) dye solution using the method of example 4, NaBH4Are 0, 0.02M, 0.05M, 0.08M, 0.1M and 0.15M, respectively. With NaBH4The degradation effect of the dye is obviously improved when the concentration is increased, and when NaBH is used4At a concentration of 0.15M, the dye was completely degraded.
To further illustrate the catalytic reduction of the magnetic Ni @ Ag nano-catalyst to the dyeTo solve the effects, the invention carries out comparative experiments. Specifically, BiVO is used separately4、C3N4、TiO2And Ni @ Ag as a catalyst, a Methylene Blue (MB) dye solution was subjected to a photocatalytic reaction according to the catalytic reaction method in example 4. As shown in FIG. 2, under the same catalytic reaction conditions, the magnetic Ni @ Ag nano-catalyst has a better catalytic degradation effect.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (10)

1. A preparation method of magnetic recyclable Ni-coated Ag core-shell structure composite nano-particles is characterized by comprising the following steps:
s1, preparing a nickel reducing solution;
and S2, adding soluble silver salt into the nickel reducing solution, fully reacting to obtain solid precipitate, and then sequentially separating, washing, drying and grinding the solid precipitate to obtain the Ni-coated Ag core-shell structure composite nano-particles.
2. The method for preparing magnetically recoverable Ni-coated Ag core-shell structure composite nanoparticles according to claim 1, wherein in step S1, the method for preparing the nickel reducing solution comprises:
s1-1, mixing nickel salt, sodium pyrophosphate, ammonia water and a borane reducing agent according to the weight part ratio of 20-30: 45-55: 40-50: 1-2, adding the mixture into deionized water to obtain a mixed solution;
s1-2, fully stirring the mixed solution obtained in the step S1-1 under ultrasound to obtain a nickel reducing solution.
3. The preparation method of the magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle as claimed in claim 2, wherein in step S1-1, the weight ratio of the nickel salt, sodium pyrophosphate, ammonia water and borane reducer is 25: 50: 45: 1.5.
4. the preparation method of the magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle as claimed in claim 2, wherein in step S1-2, the ultrasonic stirring time is 15-20 mim.
5. The method for preparing magnetic recoverable Ni-coated Ag core-shell structure composite nanoparticles according to claim 1, wherein in step S2, the mass ratio of the soluble silver salt to the nickel reducing solution is 1: 10 to 100.
6. The method for preparing magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticles as claimed in claim 1, wherein in step S2, the soluble silver salt and the nickel reducing solution react at 20-30 ℃ for 15-25 min to obtain the solid precipitate.
7. The method for preparing magnetically recoverable Ni-coated Ag core-shell structure composite nanoparticles according to claim 1, wherein the drying process is performed at room temperature for 24 hours or at 30 ℃ in an oven for 6 hours in step S2.
8. The Ni-coated Ag core-shell structure composite nanoparticle prepared by the preparation method of the magnetic recoverable Ni-coated Ag core-shell structure composite nanoparticle according to any one of claims 1 to 7.
9. A dye degradation method is characterized in that Ni-coated Ag core-shell structure composite nanoparticles prepared by the preparation method of magnetic recoverable Ni-coated Ag core-shell structure composite nanoparticles according to any one of claims 1 to 7 are used as a catalyst, and the method comprises the following steps:
weighing a certain amount of the Ni-coated Ag core-shell structure composite nano-particles and a certain volume of dye solution, wherein the mass-to-volume ratio of the Ni-coated Ag core-shell structure composite nano-particles to the dye solution is 1 mg: 1M L-1 mg: 5M L, and sodium borohydride with the concentration of 0.02-0.15M is added into the dye solution;
the photocatalytic reaction is carried out under ultraviolet illumination or simulated sunlight.
10. The dye degradation method according to claim 9, wherein the dye in the dye solution is methylene blue, rhodamine B, tiger red sodium salt, orange G, congo red, methylene orange, crystal violet, indigo carmine, or neutral red.
CN202010225133.4A 2020-03-26 2020-03-26 Magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle, preparation method thereof and dye degradation method Pending CN111468739A (en)

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