CN106905543B - A kind of preparation method of nano silver gel fluorescent solutions - Google Patents

A kind of preparation method of nano silver gel fluorescent solutions Download PDF

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CN106905543B
CN106905543B CN201710154332.9A CN201710154332A CN106905543B CN 106905543 B CN106905543 B CN 106905543B CN 201710154332 A CN201710154332 A CN 201710154332A CN 106905543 B CN106905543 B CN 106905543B
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nano silver
polyacrylamide
fluorescent solutions
gel fluorescent
silver gel
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CN106905543A (en
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程有亮
王开晔
方长青
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Xian University of Technology
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Xian University of Technology
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
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    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02Use of particular materials as binders, particle coatings or suspension media therefor
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/58Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2333/24Homopolymers or copolymers of amides or imides
    • C08J2333/26Homopolymers or copolymers of acrylamide or methacrylamide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0806Silver
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

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  • Organic Chemistry (AREA)
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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a kind of preparation methods of nano silver gel fluorescent solutions, polyacrylamide solution and silver nitrate solution are mixed, ultraviolet light irradiation is reacted under dark surrounds, obtains nano silver gel fluorescent solutions.The present invention prepares nano silver gel fluorescent solutions with anionic polyacrylamide is template, and polyacrylamide itself has amino and carboxyl, has weak reproducibility, does not need extraly to add reducing agent and stabilizer;The polyacrylamide amine molecule of macromolecule occupies very large space in aqueous solution, can absorption Ag tightly+And its reunion is prevented, therefore can be formed and be stablized, the nano-Ag particles of uniform particle diameter.

Description

A kind of preparation method of nano silver gel fluorescent solutions
Technical field
The invention belongs to technical field of material, and in particular to a kind of preparation method of nano silver gel fluorescent solutions.
Background technique
It is social fast-developing at this stage, economize on resources, the energy and protection environment become the emphasis in this epoch.It receives Rice material receives the favor of people as a kind of new material, and nanoscale science and technology becomes the leading skill for also becoming this century Art.On the other hand, most of metal ion is able to suppress the activity of bacterium, removes the heavy metal ion being harmful to the human body, silver The bactericidal effect of grain is most strong, and most study is the antibacterial agent containing Argent grain at present.Therefore, nano silver material becomes everybody and grinds The focus studied carefully.
The small-size effect and skin effect of nano-Ag particles are significant, have very strong penetration power and antibacterial activity.Its Safety, antibiotic property, persistence, heat resistance etc. have advantage, therefore obtain widely in biological medicine, anti-biotic material Using.Currently, the preparation of nano silver is broadly divided into physical method and chemical method: physical method needs to use laser, electron beam irradiation etc. The nano silver particle size of method, preparation is more uniform, but technology is complicated, equipment requirement is high;Chemical method be by reduction silver from Son obtains nano silver, easy to operate, cost is relatively low, but partial size is not easily controlled, and the nano-Ag particles of synthesis are unstable, easy group It is poly-.
In research field, the more of nano silver preparation is chemical reduction method, specifically includes that Brust- Schiffrin method, template, surface ligand induced corrosion method, microemulsion method, electrochemical process and Microwave-assisted synthesis method.These Method requires that certain reducing agent and stabilizer is added, and most reagent is all toxic.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano silver gel fluorescent solutions, the material non-toxic and do not have to Extraly add reducing agent and stabilizer.
The technical scheme adopted by the invention is that a kind of preparation method of nano silver gel fluorescent solutions, by polyacrylamide Amine aqueous solution and silver nitrate solution mixing, ultraviolet light irradiation is reacted under dark surrounds, and it is molten to obtain nano silver gel fluorescence Liquid.
The features of the present invention also characterized in that
The volume ratio of polyacrylamide solution and silver nitrate solution is 500:3-100:1.
The concentration of polyacrylamide solution is 0.3-0.55g/ml.
The concentration of silver nitrate solution is 0.1mol/L.
Wavelength is 365nm, irradiation time 20min-30min when ultraviolet light irradiation.
The invention has the advantages that the present invention is that template is solidifying to prepare nano silver with anionic polyacrylamide (APAM) Glue fluorescent solutions, polyacrylamide itself have amino and carboxyl, have weak reproducibility, do not need extraly to add reducing agent And stabilizer.The polyacrylamide amine molecule of macromolecule occupies very large space in aqueous solution, can absorption Ag tightly+And Its reunion is prevented, therefore can be formed and be stablized, the nano-Ag particles of uniform particle diameter.Polyacrylamide itself is non-toxic, more ring It protects.In addition, operation of the present invention is easy, Yi Shixian, at low cost, speed is fast.
Detailed description of the invention
Fig. 1 is the uv absorption spectra for the nano silver gel fluorescent solutions that the embodiment of the present invention 1 is prepared;
Fig. 2 is the fluorescence spectra for the nano silver gel fluorescent solutions that the embodiment of the present invention 1 is prepared;
Fig. 3 is the transmission electron microscope figure for the nano silver gel fluorescent solutions that the embodiment of the present invention 1 is prepared.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
Concentration is that 0.3-0.55g/ml polyacrylamide is water-soluble by the preparation method of nano silver gel fluorescent solutions of the present invention Liquid and concentration are that 0.1mol/L silver nitrate solution mixes, and the volume ratio of polyacrylamide solution and silver nitrate solution is 500: 3-100:1 reacts 20min-30min in the ultraviolet light irradiation for being 365nm with wavelength under dark surrounds, obtains nano silver gel Fluorescent solutions.
Embodiment 1
It weighs the polyacrylamide that quality is 0.3g to be dissolved in 100ml deionized water, makes it under magnetic stirring completely Dissolution.After polyacrylamide is completely dissolved, the silver nitrate solution that 600 μ l concentration are 0.1mol/L is added, places it in completely Under dark environment and be 365nm with wavelength ultraviolet light irradiation, allow its condition for being 750r/min and 35 DEG C in stirring rate Lower reaction completely observes its solution state when reaction carries out 30min or so, if solution becomes pink, reaction terminates, receives Rice silver gel fluorescent solutions are successfully prepared.
The nano silver gel fluorescent solutions of preparation are subjected to ultra-violet absorption spectrum, fluorescence spectrum and transmission electron microscope etc. Test, ultra-violet absorption spectrum is at 400-600nm as shown in Figure 1, there is apparent absorption peak, it was demonstrated that nano-Ag particles Successful synthesis.Fig. 2 is the fluorescence spectra of nano silver gel, when its excitation spectrum is 500nm, at 400nm and 470nm There is fluorescence spectrum respectively, this further demonstrates the formation of nano-Ag particles.Fig. 3 is the transmission electron microscope of synthesizing nano-silver gel Figure, the figure reflect the pattern of the nano-Ag particles of synthesis, and partial size is about 6.83nm, are distributed more uniform.
Embodiment 2
Specific experiment step such as embodiment 1, wherein polyacrylamide is 0.40g.The result and reality of its ultra-violet absorption spectrum Apply the basic indifference of example 1;Intensity of the fluorescence intensity at 400nm and 470nm all than embodiment 1 is high;Transmission electron microscope picture and implementation It is more uniform that example 1 compares particle distribution.
Embodiment 3
Specific experiment step such as embodiment 1, wherein polyacrylamide is 0.50g.The result of its ultra-violet absorption spectrum is than real The peak for applying example 1 is slightly lower;Fluorescence intensity of the fluorescence intensity at 400nm and 470nm all than embodiment 1, embodiment 2 is high;Transmission electricity In mirror figure, ion size is slightly smaller than embodiment 1 and embodiment 2.
Embodiment 4
Specific experiment step such as embodiment 1, wherein polyacrylamide is 0.55g.The result of its ultra-violet absorption spectrum is than real Apply example 1 peak is low and peak spectrum is narrow;Intensity of the fluorescence intensity at 400nm and 470nm all than embodiment 1 is high, but than embodiment 2, The intensity of embodiment 3 is low;In transmission electron microscope picture, ion size and embodiment 1 and embodiment 2 is obvious becomes larger and be distributed not Uniformly.

Claims (1)

1. a kind of preparation method of nano silver gel fluorescent solutions, which is characterized in that by anionic polyacrylamide aqueous solution and Silver nitrate solution mixing, ultraviolet light irradiation is reacted under dark surrounds, obtains nano silver gel fluorescent solutions;
The concentration of anionic polyacrylamide aqueous solution is 0.3-0.55g/ml;
The concentration of silver nitrate solution is 0.1mol/L;
The volume ratio of anionic polyacrylamide aqueous solution and silver nitrate solution is 500:3-100:1;
Wavelength is 365nm, irradiation time 20min-30min when ultraviolet light irradiation.
CN201710154332.9A 2017-03-15 2017-03-15 A kind of preparation method of nano silver gel fluorescent solutions Active CN106905543B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002087749A1 (en) * 2001-04-30 2002-11-07 Postech Foundation Colloid solution of metal nanoparticles, metal-polymer nanocomposites and methods for preparation thereof
CN104646683B (en) * 2015-02-28 2017-03-15 贵州大龙汇成新材料有限公司 Controllable ball shape silver powder of a kind of granularity and preparation method thereof
CN104815990B (en) * 2015-04-20 2017-05-03 西安理工大学 Method for preparing nanometer sliver colloid with liquid phase reduction method

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