CN104014804A - Preparation method of nanometer silver powder with particles controllable - Google Patents
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Abstract
The invention discloses a preparation method of nanometer silver powder with particles controllable. The method includes the following steps that silver nitrate and dispersants are mixed with water in sequence in proportion so that an oxidizing mixed solution A can be obtained; reducing agents are added into water and stirred to be dissolved, then the pH value of the solution is regulated to range from 7.5 to 13.5 through small molecular amine, and a reducing solution B is obtained after stirring and dissolving; the oxidizing mixed solution A and the reducing solution B are pumped into a spraying nozzle according to the volume ratio ranging from 1:10 to 10:1, the oxidizing mixed solution A and the reducing solution B are sprayed into a spraying drying tower through hot air at the temperature ranging from 35 DEG C to 150 DEG C at the speed ranging from 1 kg/h to 8000 kg/h, and powdery solids are formed and subside to the bottom of the drying tower; powder airflow obtained through the reaction is pumped into a separation tower to be further separated, and finally, silver powder and redundant reducing agents are separated so that the nanometer silver powder can be obtained. The preparation method has the advantages of being simple in process, convenient to operate and capable of achieving mass production fast.
Description
Technical field
The present invention relates to the preparation method of the controlled nano-silver powder of a kind of particle.
Background technology
Argent has excellent physicochemical characteristics, as optimum normal temperature electric conductivity, thermal conductivity, and the strongest reflection characteristic, photosensitive imaging characteristic, anti-inflammation characteristics 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, and 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, active high, can effectively regulate and improve the parameters such as viscosity, rheological characteristic, thixotropy and sintering activity of conductive silver slurry, light, little, thin trend along with electric development, makes nano-silver powder become one of main application direction in microelectronics industry field; 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 still there is a difficult problem at aspects such as production equipment design, technology controlling and process, the silver powder particle diameter that what is more important Physical is produced is substantially all between several microns to tens of microns, and particle diameter distributes wide, yield is low, cannot effectively control its particle diameter, the more difficult preparation that realizes nanometer-level silver powder, has therefore limited its application (referring to CN1164452A).Chemical reduction method is to be academia and industrial quarters research is more thorough, the preparation method of most widely used nano-silver powder up to now, its required production equipment is simple, technological process is simple and easy to control, especially for the preparation of nano-silver powder, utilize the nucleation of crystal in solution phase and the stable and dispersion theory of growth control and nano-colloid particle, the control that can realize particle morphology and size is synthetic.Nearly ten years, liquid phase chemical reduction legal system has obtained plentiful and substantial achievement in research for nano-silver powder, by regulator solution concentration, pH value, reaction temperature, reducing agent kind, reducing agent, add the conditions such as speed, whipped form, the size Control that has realized silver nano material is synthetic (referring to Angew. Chem. Int. Ed. 2009,48,60).But current liquid phase is prepared nano-silver powder and is still had some defects.First, most method need adopt the control devices such as organic solvent, pyroreaction or microwave, ultraviolet lighting, in water solution system, the nano-silver powder that different size is prepared in normal temperature and pressure reaction is still a challenge (referring to Chem. Eur. J. 2005,11,454); Secondly, control for particle size, before obtaining experimental result, can only do qualitative estimation (as size becomes large or diminishes) to product size, can't design in advance and by regulation and control response parameter, realize accurate and quantitative control and synthesize (referring to Acc. Chem. Res. 2007 product size, 40,1067); In addition, for obtaining nano-silver powder, control growing up of silver-colored particle in solution phase, often adopt the silver-colored precursor solution of low concentration, production efficiency obviously decline (referring to CN1653907A).In order to solve above problem, Chinese patent CN102407342B has adopted seeded growth, and substep control method is to realize the accurate production control of nano-silver powder size.Although this patent has solved silver powder particle diameter and has controlled the problem of growing, but the method that the seeded growth adopting, substep are controlled seems too loaded down with trivial details, and can not too high this natural defect due to the predecessor concentration of seeded growth, production efficiency is not effectively promoted.Therefore, develop a kind of preparation method simple, quick, efficient and the nano-silver powder that product cut size is controlled and seem very necessary.
Summary of the invention
The invention provides the preparation method of the controlled nano-silver powder of a kind of particle.
For achieving the above object, the technical solution used in the present invention is: the preparation method of the nano-silver powder that a kind of particle is controlled, comprises the following steps:
(1) in order silver nitrate, dispersant and water are carried out misciblely, 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) reducing agent is added to the water and carries out stirring and dissolving, by small molecule amine class, 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) step (1) gained is oxidized to mixed solution A and step (2) gained reducing solution B by volume for 1:10-10:1 pumps in nozzle, and by temperature, be that the hot-air of 35-150 ° of C sprays in spray drying tower with the speed of 1-8000 kg/hr, reaction finishes rapidly in second at 1-2, and forms powdery solid to drying tower bottom sedimentation;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower and carry out further separation, silver powder is separated with superfluous reducing agent the most at last can obtain nano silver powder.
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 ° of C; Spray velocity is 5-4000 kg/hr.
Due to the utilization of technique scheme, compared with prior art, the advantage having is in the present invention:
(1) equipment is simple, reaction time is short, and easy, the easy row of method, unit interval reacting dose are large; (2) the nano-silver powder diameter that the method makes can regulate and control on a large scale; (3) this preparation method's technique is simple, easy to operate, can realize fast volume production; (4) adopt water, the gentle reducing agent of environment-friendly type, small molecule amine class can be after reaction completes fast cleaned, decompose, avoided loaded down with trivial details post processing; (5) spray velocity fast, has effectively made up the problem of reactant concentration deficiency; (6) micro-long-chain organic polymer is used as dispersant, not only can simplify aftertreatment technology but also can effectively guarantee uniform particle diameter distribution (7) environment-friendly type, the introducing of gentle reducing agent, under reaction temperature, can slowly discharge reducing property, thereby avoid stopping up spout, and can evenly 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, realized the fast purifying of product, avoided loaded down with trivial details post processing, be easy to quick amplification.
Accompanying drawing explanation
The structural representation that accompanying drawing 1 is cyclone separating tower.
Accompanying drawing 2 is silver powder transmission electron microscope (TEM) photo in embodiment mono-.
Accompanying drawing 3 is silver powder transmission electron microscope (TEM) photo in embodiment bis-.
Accompanying drawing 4 is silver powder transmission electron microscope (TEM) photo in embodiment tri-.
Accompanying drawing 5 is silver powder transmission electron microscope (TEM) photo in embodiment tetra-.
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.
The specific embodiment
Below in conjunction with drawings and the specific embodiments, the present invention will be further described.
Embodiment mono-:
As depicted in figs. 1 and 2, the preparation method of the nano-silver powder that a kind of particle is controlled, comprises the following steps,
(1) in order silver nitrate, polyvinylpyrrolidone are carried out misciblely with water in proportion, 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, 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) step (1) gained is oxidized to mixed solution A and step (2) gained reducing solution B by volume for 1:1 pumps in nozzle, and by temperature, be that the hot-air of 50 ° of C sprays in spray drying tower with the speed of 200 kgs/hr, reaction finishes rapidly in second at 1-2, and forms powdery solid to drying tower bottom sedimentation;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower and carry out further separation, silver powder is separated with superfluous reducing agent the most at last can obtain nano silver powder, and the diameter of gained silver powder is 10 nanometers.
Embodiment bis-:
As shown in figures 1 and 3, the preparation method of the nano-silver powder that a kind of particle is controlled, comprises the following steps,
(1) in order silver nitrate, polyvinyl alcohol are carried out misciblely with water in proportion, 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, 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) step (1) gained is oxidized to mixed solution A and step (2) gained reducing solution B by volume for 1:2 pumps in nozzle, and by temperature, be 70 ° of C hot-air with double centner/hour speed in spray drying tower, spray into, reaction finishes rapidly in second at 1-2, and forms powdery solid to drying tower bottom sedimentation;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower and carry out further separation, silver powder is separated with superfluous reducing agent the most at last can obtain nano silver powder, and the diameter of gained silver powder is 20 nanometers.
Embodiment tri-:
As shown in Figure 1 and Figure 4, the preparation method of the nano-silver powder that a kind of particle is controlled, comprises the following steps,
(1) in order silver nitrate, polyvinylpyrrolidone are carried out misciblely with water in proportion, 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, 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) step (1) gained is oxidized to mixed solution A and step (2) gained reducing solution B by volume for 2:3 pumps in nozzle, and by temperature, be that the hot-air of 80 ° of C sprays in spray drying tower with the speed of 300 kgs/hr, reaction finishes rapidly in second at 1-2, and forms powdery solid to drying tower bottom sedimentation;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower and carry out further separation, silver powder is separated with superfluous reducing agent the most at last can obtain nano silver powder, and the diameter of gained silver powder is 35 nanometers.
Embodiment tetra-:
As shown in Figure 1 and Figure 5, the preparation method of the nano-silver powder that a kind of particle is controlled, 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, 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) step (1) gained is oxidized to mixed solution A and step (2) gained reducing solution B by volume for 2:5 pumps in nozzle, and by temperature, be that the hot-air of 85 ° of C sprays in spray drying tower with the speed of 350 kgs/hr, reaction finishes rapidly in second at 1-2, and forms powdery solid to drying tower bottom sedimentation;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower and carry out further separation, silver powder is separated with superfluous reducing agent the most at last can obtain nano silver powder, and the diameter of gained silver powder is 50 nanometers.
Embodiment five:
As shown in Fig. 1 and Fig. 6, the preparation method of the nano-silver powder that a kind of particle is controlled, 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, 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) step (1) gained is oxidized to mixed solution A and step (2) gained reducing solution B by volume for 1:3 pumps in nozzle, and by temperature, be that the hot-air of 85 ° of C sprays in spray drying tower with the speed of 250 kgs/hr, reaction finishes rapidly in second at 1-2, and forms powdery solid to drying tower bottom sedimentation;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower and carry out further separation, silver powder is separated with superfluous reducing agent the most at last can obtain nano silver powder, and the diameter of gained silver powder is 80 nanometers.
Embodiment six:
As shown in Figure 1 and Figure 7, the preparation method of the nano-silver powder that a kind of particle is controlled, 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, 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) step (1) gained is oxidized to mixed solution A and step (2) gained reducing solution B by volume for 3:2 pumps in nozzle, and by temperature, be that the hot-air of 100 ° of C sprays in spray drying tower with the speed of 500 kgs/hr, reaction finishes rapidly in second at 1-2, and forms powdery solid to drying tower bottom sedimentation;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower and carry out further separation, silver powder is separated with superfluous reducing agent the most at last can obtain nano silver powder, and the diameter of gained silver powder is 200 nanometers.
In the present invention, (1) equipment is simple, reaction time is short, and easy, the easy row of method, unit interval reacting dose are large; (2) the nano-silver powder diameter that the method makes can regulate and control on a large scale; (3) this preparation method's technique is simple, easy to operate, can realize fast volume production; (4) adopt water, the gentle reducing agent of environment-friendly type, small molecule amine class can be after reaction completes fast cleaned, decompose, avoided loaded down with trivial details post processing; (5) spray velocity fast, has effectively made up the problem of reactant concentration deficiency; (6) micro-long-chain organic polymer is used as dispersant, not only can simplify aftertreatment technology but also can effectively guarantee uniform particle diameter distribution (7) environment-friendly type, the introducing of gentle reducing agent, under reaction temperature, can slowly discharge reducing property, thereby avoid stopping up spout, and can evenly 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, realized the fast purifying of product, avoided loaded down with trivial details post processing, be easy to quick amplification.
Claims (7)
1. a preparation method for the controlled nano-silver powder of particle, is characterized in that: comprise the following steps:
(1) in order silver nitrate, dispersant and water are carried out misciblely, 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) reducing agent is added to the water and carries out stirring and dissolving, by small molecule amine class, 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) step (1) gained is oxidized to mixed solution A and step (2) gained reducing solution B by volume for 1:10-10:1 pumps in nozzle, and by temperature, be that the hot-air of 35-150 ° of C sprays in spray drying tower with the speed of 1-8000 kg/hr, reaction finishes rapidly in second at 1-2, and forms powdery solid to drying tower bottom sedimentation;
(4) step (3) reaction gained powder air-flow is pumped into knockout tower and carry out further separation, silver powder is separated with superfluous reducing agent the most at last can obtain nano silver powder.
2. the preparation method of the controlled nano-silver powder of a kind of particle 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 controlled nano-silver powder of a kind of particle according to claim 1 and 2, is characterized in that: after 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 controlled nano-silver powder of a kind of particle 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. according to the preparation method of the controlled nano-silver powder of a kind of particle described in claim 1 or 4, it is characterized in that: the concentration of reducing agent is 0.02-4 mol/L.
6. the preparation method of the controlled nano-silver powder of a kind of particle 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 controlled nano-silver powder of a kind of particle 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 ° of C; Spray velocity is 5-4000 kg/hr.
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