CN104014804B - A kind of preparation method of nano-silver powder of size tunable - Google Patents
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Abstract
The invention discloses a kind of preparation method of nano-silver powder of size tunable, comprise the following steps: in order silver nitrate, dispersant are carried out miscible with water in proportion, obtain oxidation mixed solution A; Reducing agent is added to the water and carries out stirring and dissolving, with Small molecular amine, solution ph is adjusted to 7.5-13.5 subsequently, after stirring and dissolving, obtains reducing solution B; Oxidation mixed solution A and reducing solution B by volume for 1:10-10:1 pumps in nozzle, and are that the hot-air of 35-150 DEG C sprays in spray drying tower with the speed of 1-8000 kg/hr by temperature, and form powdery solid to sedimentation bottom drying tower; Reaction gained powder air-flow is pumped into knockout tower be separated further, silver powder is separated can obtains nano silver powder with the reducing agent of surplus the most at last.Advantage is: this preparation method's technique is simple, easy to operate, can realize volume production fast.<!-- 2 --><!-- 3 -->
Description
Technical field
The present invention relates to a kind of preparation method of nano-silver powder of size tunable.
Background technology
Argent has excellent physicochemical characteristics, and as normal temperature electric conductivity, the thermal conductivity of optimum, the strongest reflection characteristic, photosensitive imaging characteristic, anti-inflammation characteristic etc., make it be widely used in modern industry field.Silver is also the noble metal of the most cheap resistance to high temperature oxidation, utilizes its electrical and thermal conductivity performance, silver powder is applied to electrocondution slurry, becomes the indispensable functional material of electronics industry.Because the particle diameter of nano-silver powder is little, activity is high, can effectively regulate and improve the parameters such as the viscosity of conductive silver slurry, rheological characteristic, thixotropy and sintering activity, along with light, little, the thin trend of electric development, nano-silver powder is made to become one of main application direction at microelectronics industry; In addition, utilize the anti-inflammation characteristic of Nano Silver, use it for the fields such as antibacterial fabric, plastics, pottery, coating, Medical dressing, also present tempting prospect.
The production method of silver powder can be divided into Physical and chemical method simply, and Physical comprises plasma gas phase condensation method, atomization (water atomization, aerosolization) etc., and chemical method comprises thermal decomposition method, liquid phase reduction etc.The feature of Physical is that output is large, product degree of crystallinity is high, but in production equipment design, technology controlling and process etc., still there is a difficult problem, the silver powder particle diameter that what is more important Physical is produced substantially all is between several microns to some tens of pm, and domain size distribution is wide, yield is low, cannot effectively control its particle diameter, the more difficult preparation realizing nanometer-level silver powder, because which limit its application (referring to CN1164452A).Chemical reduction method is the preparation method up to now for academia and more thorough, the most widely used nano-silver powder of industrial quarters research, production equipment needed for it is simple, technological process is simple and easy to manipulation, especially for the preparation of nano-silver powder, in utilizing solution mutually, the coring and increment control of crystal and the stable and dispersion theory of nano-colloid particle, can realize the control synthesis of particle morphology and size.Nearly ten years, solution phase chemical reduction is prepared nano-silver powder and is achieved plentiful and substantial achievement in research, the condition such as speed, whipped form is added by regulating solution concentration, pH value, reaction temperature, reducing agent kind, reducing agent, achieve the size Control synthesis of silver nano material (see Angew.Chem.Int.Ed.2009,48,60).But current liquid phase is prepared nano-silver powder and still be there are some defects.First, most method need adopt organic solvent, pyroreaction or the control device such as microwave, ultraviolet lighting, in water solution system, the nano-silver powder that normal temperature and pressure reaction controlling prepares different size is still a challenge (see Chem.Eur.J.2005,11,454); Secondly, for the control of particle size, before obtaining experimental result, qualitative estimation (become large as size or diminish) can only be done to Product size, can't design in advance Product size and realize accurate and quantitative control synthesis (see Acc.Chem.Res.2007 by regulation and control response parameter, 40,1067); In addition, for obtaining nano-silver powder, control solution mutually in the growing up of Argent grain, often adopt the silver-colored precursor solution of low concentration, production efficiency obviously declines (see CN1653907A).In order to solve above problem, Chinese patent CN102407342B have employed seeded growth, and substep control methods is to realize the accurate production control of nano-silver powder size.Although this patent solves the problem of silver powder size controlling growth, but the method that the seeded growth adopted, substep control seems too loaded down with trivial details, and due to the predecessor concentration of seeded growth can not this natural defect too high, production efficiency is not effectively promoted.Therefore, develop a kind of simple, fast, efficient and preparation method that the is nano-silver powder that product cut size is controlled seems very necessary.
Summary of the invention
The invention provides a kind of preparation method of nano-silver powder of size tunable.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of nano-silver powder of size tunable, comprises the following steps:
(1) undertaken miscible by silver nitrate, dispersant and water in order, after dissolving, the concentration of silver nitrate is 0.005-1 mol/L, and dispersant concentration is 0.005-10 mM/l, obtains oxidation mixed solution A;
(2) be added to the water by reducing agent and carry out stirring and dissolving, with Small molecular amine, solution ph is adjusted to 7.5-13.5 subsequently, wherein the concentration of reducing agent is 0.01-5 mol/L, obtains reducing solution B after stirring and dissolving;
(3) by step (1) gained oxidation mixed solution A and step (2) gained reducing solution B by volume for 1:10-10:1 pumps in nozzle, and be that the hot-air of 35-150 DEG C sprays in spray drying tower with the speed of 1-8000 kg/hr by temperature, react and terminate rapidly within 1-2 second, and form powdery solid to sedimentation bottom drying tower;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower to be separated further, silver powder is separated can obtains nano silver powder with the reducing agent of surplus the most at last.
Further, in step (1), dispersant is one or more mixtures in polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, softex kw, hexadecyltrimethylammonium chloride, enuatrol, sodium laurate, sodium cinnamate, dodecyl sodium sulfate, neopelex.
Preferably, after mixing, the concentration of silver nitrate is 0.01-0.8 mol/L; The concentration of dispersant is 0.01-8 mM/l.
Further, in step (2), reducing agent is one or more mixtures in citric acid, ascorbic acid, tannic acid, tartaric acid, potassium citrate, sodium ascorbate, sodium oxalate, sodium metaphosphate, sodium hypophosphite, glucose.
Preferably, the concentration of reducing agent is 0.02-4 mol/L.
Further, step (2) small molecular amine is one or more mixtures in ammoniacal liquor, monomethyl amine, dimethylamine, trimethylamine, monoethyl amine, diethylamine, a propylamine, di-n-propylamine, isopropylamine.
Preferably, in step (3), the volume ratio of mixed solution A and mixed solution B is 1:5-5:1; Hot air temperature is 50-120 DEG C; Spray velocity is 5-4000 kg/hr.
Due to the utilization of technique scheme, compared with prior art, the advantage had is in the present invention:
(1) equipment is simple, reaction time is short, and method is easy, easy, unit interval reacting dose is large; (2) the nano-silver powder diameter that the method is obtained can regulate and control on a large scale; (3) this preparation method's technique is simple, easy to operate, can realize volume production fast; (4) adopt the gentle reducing agent of water, environment-friendly type, Small molecular amine can after completion of the reaction fast cleaned, decompose, avoid loaded down with trivial details post processing; (5) spray velocity fast, effectively compensate for the problem of reactant concentration deficiency; (6) micro-long-chain organic polymer uses as dispersant, not only aftertreatment technology can be simplified but also effectively can ensure that uniform domain size distribution (7) environment-friendly type, gentle reducing agent are introduced, at the reaction temperatures can slow releasing reducing property, thus avoid blocking spout, and evenly can induce formation and the growth of crystal grain; (8) spray drying tower has enough reaction settling heights, make reaction more fully, crystallinity is better; (9) introducing of cyclone separating tower, can make excessive reductant in last handling process effectively with nano-silver powder product separation, achieve the fast purifying of product, avoid loaded down with trivial details post processing, be easy to quick amplification.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation of cyclone separating tower.
Accompanying drawing 2 is silver powder transmission electron microscope (TEM) photo in embodiment one.
Accompanying drawing 3 is silver powder transmission electron microscope (TEM) photo in embodiment two.
Accompanying drawing 4 is silver powder transmission electron microscope (TEM) photo in embodiment three.
Accompanying drawing 5 is silver powder transmission electron microscope (TEM) photo in embodiment four.
Accompanying drawing 6 is silver powder transmission electron microscope (TEM) photo in embodiment five.
Accompanying drawing 7 is silver powder transmission electron microscope (TEM) photo in embodiment six.
Detailed description of the invention
Below in conjunction with drawings and the specific embodiments, the present invention will be further described.
Embodiment one:
As depicted in figs. 1 and 2, a kind of preparation method of nano-silver powder of size tunable, comprises the following steps,
(1) carry out miscible with water in proportion by silver nitrate, polyvinylpyrrolidone in order, after dissolving, the concentration of silver nitrate is 0.02 mol/L, and polyvinylpyrrolidone concentration is 0.02 mM/l, obtains oxidation mixed solution A;
(2) environment-friendly type, gentle weak reductant ascorbic acid are added to the water and carry out stirring and dissolving, with monomethyl amine, solution ph is adjusted to 9 subsequently, wherein the concentration of reducing agent is 0.2 mol/L, obtains reducing solution B after stirring and dissolving;
(3) by step (1) gained oxidation mixed solution A and step (2) gained reducing solution B by volume for 1:1 pumps in nozzle, and be that the hot-air of 50 DEG C sprays in spray drying tower with the speed of 200 kgs/hr by temperature, react and terminate rapidly within 1-2 second, and form powdery solid to sedimentation bottom drying tower;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower to be separated further, silver powder is separated with the reducing agent of surplus and can obtains nano silver powder the most at last, and the diameter of gained silver powder is 10 nanometers.
Embodiment two:
As shown in figures 1 and 3, a kind of preparation method of nano-silver powder of size tunable, comprises the following steps,
(1) carry out miscible with water in proportion by silver nitrate, polyvinyl alcohol in order, after dissolving, the concentration of silver nitrate is 0.045 mol/L, and polyvinyl alcohol concentration is 0.025 mM/l, obtains oxidation mixed solution A;
(2) environment-friendly type, gentle weak reductant potassium citrate are added to the water and carry out stirring and dissolving, with ammoniacal liquor, solution ph is adjusted to 11 subsequently, wherein the concentration of reducing agent is 0.4 mol/L, obtains reducing solution B after stirring and dissolving;
(3) by step (1) gained oxidation mixed solution A and step (2) gained reducing solution B by volume for 1:2 pumps in nozzle, and by temperature be 70 DEG C hot-air with double centner/hour speed spray in spray drying tower, react and terminate rapidly within 1-2 second, and form powdery solid to sedimentation bottom drying tower;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower to be separated further, silver powder is separated with the reducing agent of surplus and can obtains nano silver powder the most at last, and the diameter of gained silver powder is 20 nanometers.
Embodiment three:
As shown in Figure 1 and Figure 4, a kind of preparation method of nano-silver powder of size tunable, comprises the following steps,
(1) carry out miscible with water in proportion by silver nitrate, polyvinylpyrrolidone in order, after dissolving, the concentration of silver nitrate is 0.05 mol/L, and polyvinylpyrrolidone concentration is 0.015 mM/l, obtains oxidation mixed solution A;
(2) environment-friendly type, gentle weak reductant tannic acid are added to the water and carry out stirring and dissolving, with the mixed solvent of ammoniacal liquor and dimethylamine, solution ph is adjusted to 11 subsequently, wherein the concentration of reducing agent is 0.4 mol/L, obtains reducing solution B after stirring and dissolving;
(3) by step (1) gained oxidation mixed solution A and step (2) gained reducing solution B by volume for 2:3 pumps in nozzle, and be that the hot-air of 80 DEG C sprays in spray drying tower with the speed of 300 kgs/hr by temperature, react and terminate rapidly within 1-2 second, and form powdery solid to sedimentation bottom drying tower;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower to be separated further, silver powder is separated with the reducing agent of surplus and can obtains nano silver powder the most at last, and the diameter of gained silver powder is 35 nanometers.
Embodiment four:
As shown in Figure 1 and Figure 5, a kind of preparation method of nano-silver powder of size tunable, comprises the following steps,
(1) in order the mixture of silver nitrate, polyvinyl alcohol and softex kw is carried out miscible with water in proportion, after dissolving, the concentration of silver nitrate is 0.075 mol/L, the concentration of the mixture of polyvinyl alcohol and softex kw is 0.02 mM/l, obtains oxidation mixed solution A;
(2) environment-friendly type, gentle weak reductant potassium metaphosphate are added to the water and carry out stirring and dissolving, with the mixed solvent of ammoniacal liquor and monoethyl amine, solution ph is adjusted to 11 subsequently, wherein the concentration of reducing agent is 0.25 mol/L, obtains reducing solution B after stirring and dissolving;
(3) by step (1) gained oxidation mixed solution A and step (2) gained reducing solution B by volume for 2:5 pumps in nozzle, and be that the hot-air of 85 DEG C sprays in spray drying tower with the speed of 350 kgs/hr by temperature, react and terminate rapidly within 1-2 second, and form powdery solid to sedimentation bottom drying tower;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower to be separated further, silver powder is separated with the reducing agent of surplus and can obtains nano silver powder the most at last, and the diameter of gained silver powder is 50 nanometers.
Embodiment five:
As shown in figures 1 to 6, a kind of preparation method of nano-silver powder of size tunable, comprises the following steps,
(1) in order the mixture of silver nitrate, polyethylene glycol and softex kw is carried out miscible with water in proportion, after dissolving, the concentration of silver nitrate is 0.1 mol/L, the concentration of the mixture of polyethylene glycol and softex kw is 0.025 mM/l, obtains oxidation mixed solution A;
(2) environment-friendly type, gentle weak reductant glucose are added to the water and carry out stirring and dissolving, with the mixed solvent of ammoniacal liquor, solution ph is adjusted to 11 subsequently, wherein the concentration of reducing agent is 0.25 mol/L, obtains reducing solution B after stirring and dissolving;
(3) by step (1) gained oxidation mixed solution A and step (2) gained reducing solution B by volume for 1:3 pumps in nozzle, and be that the hot-air of 85 DEG C sprays in spray drying tower with the speed of 250 kgs/hr by temperature, react and terminate rapidly within 1-2 second, and form powdery solid to sedimentation bottom drying tower;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower to be separated further, silver powder is separated with the reducing agent of surplus and can obtains nano silver powder the most at last, and the diameter of gained silver powder is 80 nanometers.
Embodiment six:
As shown in Figure 1 and Figure 7, a kind of preparation method of nano-silver powder of size tunable, comprises the following steps,
(1) in order the mixture of silver nitrate, softex kw is carried out miscible with water in proportion, after dissolving, the concentration of silver nitrate is 0.025 mol/L, the concentration of the mixture of softex kw is 0.015 mM/l, obtains oxidation mixed solution A;
(2) environment-friendly type, gentle weak reductant ascorbic acid are added to the water and carry out stirring and dissolving, with the mixed solvent of monomethyl amine, solution ph is adjusted to 13.5 subsequently, wherein the concentration of reducing agent is 0.15 mol/L, obtains reducing solution B after stirring and dissolving;
(3) by step (1) gained oxidation mixed solution A and step (2) gained reducing solution B by volume for 3:2 pumps in nozzle, and be that the hot-air of 100 DEG C sprays in spray drying tower with the speed of 500 kgs/hr by temperature, react and terminate rapidly within 1-2 second, and form powdery solid to sedimentation bottom drying tower;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower to be separated further, silver powder is separated with the reducing agent of surplus and can obtains nano silver powder the most at last, and the diameter of gained silver powder is 200 nanometers.
In the present invention, (1) equipment is simple, reaction time is short, and method is easy, easy, unit interval reacting dose is large; (2) the nano-silver powder diameter that the method is obtained can regulate and control on a large scale; (3) this preparation method's technique is simple, easy to operate, can realize volume production fast; (4) adopt the gentle reducing agent of water, environment-friendly type, Small molecular amine can after completion of the reaction fast cleaned, decompose, avoid loaded down with trivial details post processing; (5) spray velocity fast, effectively compensate for the problem of reactant concentration deficiency; (6) micro-long-chain organic polymer uses as dispersant, not only aftertreatment technology can be simplified but also effectively can ensure that uniform domain size distribution (7) environment-friendly type, gentle reducing agent are introduced, at the reaction temperatures can slow releasing reducing property, thus avoid blocking spout, and evenly can induce formation and the growth of crystal grain; (8) spray drying tower has enough reaction settling heights, make reaction more fully, crystallinity is better; (9) introducing of cyclone separating tower, can make excessive reductant in last handling process effectively with nano-silver powder product separation, achieve the fast purifying of product, avoid loaded down with trivial details post processing, be easy to quick amplification.
Claims (7)
1. a preparation method for the nano-silver powder of size tunable, is characterized in that: comprise the following steps:
(1) undertaken miscible by silver nitrate, dispersant and water in order, after dissolving, the concentration of silver nitrate is 0.005-1 mol/L, and dispersant concentration is 0.005-10 mM/l, obtains oxidation mixed solution A;
(2) be added to the water by reducing agent and carry out stirring and dissolving, with Small molecular amine, solution ph is adjusted to 7.5-13.5 subsequently, wherein the concentration of reducing agent is 0.01-5 mol/L, obtains reducing solution B after stirring and dissolving;
(3) by step (1) gained oxidation mixed solution A and step (2) gained reducing solution B by volume for 1:10-10:1 pumps in nozzle, and be that the hot-air of 35-150 DEG C sprays in spray drying tower with the speed of 1-8000 kg/hr by temperature, react and terminate rapidly within 1-2 second, and form powdery solid to sedimentation bottom drying tower;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower to be separated further, silver powder is separated can obtains nano silver powder with the reducing agent of surplus the most at last.
2. the preparation method of the nano-silver powder of a kind of size tunable according to claim 1, is characterized in that: in described step (1), dispersant is one or more mixtures in polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, softex kw, hexadecyltrimethylammonium chloride, enuatrol, sodium laurate, sodium cinnamate, dodecyl sodium sulfate, neopelex.
3. the preparation method of the nano-silver powder of a kind of size tunable according to claim 1 and 2, is characterized in that: after described step (1) mixing, the concentration of silver nitrate is 0.01-0.8 mol/L; The concentration of dispersant is 0.01-8 mM/l.
4. the preparation method of the nano-silver powder of a kind of size tunable according to claim 1, is characterized in that: in described step (2), reducing agent is one or more mixtures in citric acid, ascorbic acid, tannic acid, tartaric acid, potassium citrate, sodium ascorbate, sodium oxalate, sodium metaphosphate, sodium hypophosphite, glucose.
5. the preparation method of the nano-silver powder of a kind of size tunable according to claim 1 or 4, is characterized in that: the concentration of reducing agent is 0.02-4 mol/L.
6. the preparation method of the nano-silver powder of a kind of size tunable according to claim 1, is characterized in that: described step (2) small molecular amine is one or more mixtures in ammoniacal liquor, monomethyl amine, dimethylamine, trimethylamine, monoethyl amine, diethylamine, a propylamine, di-n-propylamine, isopropylamine.
7. the preparation method of the nano-silver powder of a kind of size tunable according to claim 1, is characterized in that: in described step (3), the volume ratio of mixed solution A and mixed solution B is 1:5-5:1; Hot air temperature is 50-120 DEG C; Spray velocity is 5-4000 kg/hr.
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| CN106312087B (en) | 2015-07-03 | 2019-02-22 | 王东 | Nano-metal particle and preparation method thereof |
| CN105710379A (en) * | 2016-02-26 | 2016-06-29 | 金川集团股份有限公司 | Method for spraying drying of superfine silver powder |
| CN106041352B (en) * | 2016-08-17 | 2018-05-01 | 武汉工程大学 | A kind of organic acid silver cladding nano-Ag particles and its preparation method and application |
| CN108247082B (en) * | 2018-04-04 | 2021-09-17 | 太原氦舶新材料有限责任公司 | Nano-silver concentrated solution and preparation method thereof |
| CN110883340A (en) * | 2018-09-10 | 2020-03-17 | 河南金渠银通金属材料有限公司 | Electronegative superfine silver powder and preparation method thereof |
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