CN106905543A - 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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Publication number
CN106905543A
CN106905543A CN201710154332.9A CN201710154332A CN106905543A CN 106905543 A CN106905543 A CN 106905543A CN 201710154332 A CN201710154332 A CN 201710154332A CN 106905543 A CN106905543 A CN 106905543A
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nano silver
fluorescent solutions
preparation
gel fluorescent
polyacrylamide
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CN201710154332.9A
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CN106905543B (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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    • 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
    • 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
    • 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
    • CCHEMISTRY; METALLURGY
    • 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
    • C09K11/02Use of particular materials as binders, particle coatings or suspension media therefor
    • CCHEMISTRY; METALLURGY
    • 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

Abstract

The invention discloses a kind of preparation method of nano silver gel fluorescent solutions, polyacrylamide solution and silver nitrate solution are mixed, ultra violet lamp is reacted under dark surrounds, obtains nano silver gel fluorescent solutions.The present invention is template with PAMA prepares nano silver gel fluorescent solutions, and polyacrylamide itself carries amino and carboxyl, with weak reproducibility, it is not necessary to extraly add reducing agent and stabilizer;The polyacrylamide amine molecule of macromolecule occupies very big space in aqueous, absorption Ag that can be tightly+And prevent it from reuniting, therefore stabilization, the nano-Ag particles of uniform particle diameter can be formed.

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 technology
It is social fast-developing at this stage, economizing on resources, the energy and environmental protection turn into the emphasis in this epoch.Receive Rice material receives the favor of people as a kind of new material, and nanoscale science and technology turns into the also leading skill as this century Art.On the other hand, most of metal ion can suppress the activity of bacterium, remove harmful heavy metal ion, silver The bactericidal action of grain is most strong, and current most study is the antiseptic containing Argent grain.Therefore, nano silver material becomes everybody and grinds The focus studied carefully.
The small-size effect and skin effect of nano-Ag particles are notable, with very strong penetration power and antibacterial activity.Its The aspects such as security, antibiotic property, persistence, heat resistance have advantage, therefore obtain extensive in biological medicine, anti-biotic material Using.At present, the preparation of Nano Silver is broadly divided into Physical and chemical method:Physical needs to use laser, electron beam irradiation etc. Method, the Nano Silver grain size that it is prepared is more uniform, but technical sophistication, equipment requirement are high;Chemical method be by reduce silver from Son obtains Nano Silver, and its simple to operate, cost is relatively low, but particle diameter is not easily controlled, and the nano-Ag particles of synthesis are unstable, easy group It is poly-.
In research field, mostly the comparing of Nano Silver preparation is chemical reduction method, and it mainly includes:Brust- Schiffrin methods, template, surface ligand induced corrosion method, microemulsion method, electrochemical process and Microwave-assisted synthesis method.These Method is required for adding certain reducing agent and stabilizer, and most reagent is all toxic.
The content of the invention
It is an object of the invention to provide a kind of preparation method of nano silver gel fluorescent solutions, the material non-toxic and without Extraly add reducing agent and stabilizer.
The technical solution adopted in the present invention is, a kind of preparation method of nano silver gel fluorescent solutions, by polyacrylamide Amine aqueous solution and silver nitrate solution mix, and ultra violet lamp is reacted under dark surrounds, obtains nano silver gel fluorescence molten Liquid.
The features of the present invention is also resided in,
Polyacrylamide solution is 500 with the volume ratio of silver nitrate solution: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 during ultra violet lamp, and irradiation time is 20min-30min.
The beneficial effects of the invention are as follows the present invention is solidifying to prepare Nano Silver for template with PAMA (APAM) Glue fluorescent solutions, polyacrylamide itself carries amino and carboxyl, with weak reproducibility, it is not necessary to extraly add reducing agent And stabilizer.The polyacrylamide amine molecule of macromolecule occupies very big space in aqueous, absorption Ag that can be tightly+And Prevent it from reuniting, therefore stabilization, the nano-Ag particles of uniform particle diameter can be formed.Polyacrylamide is non-toxic in itself, more ring Protect.In addition, easy to operate, the easy realization of the present invention, low cost, speed are fast.
Brief description of the drawings
Fig. 1 is the uv absorption spectra of the nano silver gel fluorescent solutions that the embodiment of the present invention 1 is prepared;
Fig. 2 is the fluorescence spectra of the nano silver gel fluorescent solutions that the embodiment of the present invention 1 is prepared;
Fig. 3 is the transmission electron microscope figure of the nano silver gel fluorescent solutions that the embodiment of the present invention 1 is prepared.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The preparation method of nano silver gel fluorescent solutions of the present invention, is that 0.3-0.55g/ml polyacrylamides are water-soluble by concentration Liquid and concentration are the mixing of 0.1mol/L silver nitrate solutiones, and its polyacrylamide solution is 500 with the volume ratio of silver nitrate solution: 3-100:1,20min-30min is being reacted with the ultra violet lamp that wavelength is 365nm under dark surrounds, obtain nano silver gel Fluorescent solutions.
Embodiment 1
Weigh the polyacrylamide that quality is 0.3g to be dissolved in 100ml deionized waters, make its complete under magnetic stirring Dissolving.After polyacrylamide is completely dissolved, it is the silver nitrate solution of 0.1mol/L to add 600 μ l concentration, is placed it in completely Under dark environment and with the ultra violet lamp that wavelength is 365nm, it is allowed in the condition that stir speed (S.S.) is 750r/min and 35 DEG C Under react completely, reaction observes its solution state when carrying 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 carried out into ultra-violet absorption spectrum, fluorescence spectrum and transmission electron microscope etc. Test, its ultra-violet absorption spectrum is at 400-600nm as shown in figure 1, there is obvious absworption 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 reflects the pattern of the nano-Ag particles of synthesis, and its particle diameter is about 6.83nm, is distributed more uniform.
Embodiment 2
Specific experiment step such as embodiment 1, wherein polyacrylamide are 0.40g.The result and reality of its ultra-violet absorption spectrum Apply the basic indifference of example 1;Intensity of the fluorescence intensity all than embodiment 1 at 400nm and 470nm 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 are 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 all than embodiment 1, embodiment 2 at 400nm and 470nm is high;Transmission electricity In mirror figure, its ion size is slightly smaller than embodiment 1 and embodiment 2.
Embodiment 4
Specific experiment step such as embodiment 1, wherein polyacrylamide are 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 all than embodiment 1 at 400nm and 470nm is high, but than embodiment 2, The low intensity of embodiment 3;In transmission electron microscope picture, its ion size is obvious with embodiment 1 and embodiment 2 to be become big and is distributed not Uniformly.

Claims (5)

1. a kind of preparation method of nano silver gel fluorescent solutions, it is characterised in that by polyacrylamide solution and silver nitrate Solution mixes, and ultra violet lamp is reacted under dark surrounds, obtains nano silver gel fluorescent solutions.
2. the preparation method of nano silver gel fluorescent solutions according to claim 1, it is characterised in that polyacrylamide aqueous amine Solution is 500 with the volume ratio of silver nitrate solution:3-100:1.
3. the preparation method of nano silver gel fluorescent solutions according to claim 1 and 2, it is characterised in that polyacrylamide The concentration of amine aqueous solution is 0.3-0.55g/ml.
4. the preparation method of nano silver gel fluorescent solutions according to claim 1 and 2, it is characterised in that silver nitrate is molten The concentration of liquid is 0.1mol/L.
5. the preparation method of nano silver gel fluorescent solutions according to claim 1, it is characterised in that during ultra violet lamp Wavelength is 365nm, and irradiation time is 20min-30min.
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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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1509206A (en) * 2001-04-30 2004-06-30 ѧУ��������Ī˹�ƴ�ѧУ Colloid solution of metal nanoparticles, metal-polymer nanocompositions and method for preparation thereof
CN104646683A (en) * 2015-02-28 2015-05-27 湖南汇通科技有限责任公司 Spherical silver powder with controllable granularity and preparation method thereof
CN104815990A (en) * 2015-04-20 2015-08-05 西安理工大学 Method for preparing nanometer sliver colloid with liquid phase reduction method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1509206A (en) * 2001-04-30 2004-06-30 ѧУ��������Ī˹�ƴ�ѧУ Colloid solution of metal nanoparticles, metal-polymer nanocompositions and method for preparation thereof
CN104646683A (en) * 2015-02-28 2015-05-27 湖南汇通科技有限责任公司 Spherical silver powder with controllable granularity and preparation method thereof
CN104815990A (en) * 2015-04-20 2015-08-05 西安理工大学 Method for preparing nanometer sliver colloid with liquid phase reduction method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王立英: ""贵金属-聚合物复合纳米材料的制备、表征及其光学性质的研究"", 《万方学位论文数据库》 *
覃爱苗等: ""聚丙烯酰胺存在下微波高压合成银纳米粒子及其光谱特性"", 《分析化学研究简报》 *

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