CN1817524A - Production of nanometer silver powder by liquid-phase and solid-liquid separating method - Google Patents
Production of nanometer silver powder by liquid-phase and solid-liquid separating method Download PDFInfo
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- CN1817524A CN1817524A CN 200610020119 CN200610020119A CN1817524A CN 1817524 A CN1817524 A CN 1817524A CN 200610020119 CN200610020119 CN 200610020119 CN 200610020119 A CN200610020119 A CN 200610020119A CN 1817524 A CN1817524 A CN 1817524A
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Abstract
A solid-liquid separation method for preparing Ag nanoparticles by liquid phase process includes such steps as preparing nano-class Ag sol by liquid-phase reduction method of sodium hypophosphite, adding regulator in ultrasonic field, laying aside for several hours, and separating Ag nanoparticles by gravitational deposition or vacuum filtering.
Description
Technical field
The present invention relates to a kind of solid-liquid separating method that is used for the solid-liquid separation technique that liquid phase method prepares nano-powder material, particularly production of nanometer silver powder by liquid-phase, belong to the nanosecond science and technology field.
Background technology
Nano-powder typically refers to grain graininess at 1～100nm, small solid particle between microcosmic particle and macro object.Liquid phase method is to be a kind of method that decentralized photo prepares nano-powder with water, ethanol or other organic reagent.Because the granularity of nano particle is very little, its in liquid phase easily with the comparatively stable colloid of decentralized photo formation, and along with reducing of nano particle granularity, the colloid of formation tends towards stability.
The method of traditional Separation of Solid and Liquid powder mainly contains settling methods, filtration method etc.Because the colloid that nano-powder forms is highly stable, nano particle almost can not sedimentation in gravitational field, and therefore traditional settling methods can't the Separation of Solid and Liquid nano-powder.The particle diameter of nano particle less than 50nm after, the filter phenomenon usually appears wearing during with common filter paper isolated by filtration, can't form filter cake, make that traditional filter method also can't the Separation of Solid and Liquid nano particle.
Liquid phase method is the method the most commonly used of preparation nano-silver powder.Production of nanometer silver powder by liquid-phase mainly in two steps, the first step is to prepare nano silver colloidal sol in liquid phase, second step was to separate the pure Nano Silver dry powder of preparation from silver sol.The nano silver colloidal sol particle diameter of liquid phase method preparation is little, colloidal stability good.But the nano-silver powder of isolating solid from liquid phase is the outstanding difficult problem of production of nanometer silver powder by liquid-phase.(the hypophosphites liquid phase reduction prepares nano-silver powder to Gu Daming etc. fast; " fine chemistry industry "; 2002; 19 (11)); (electrochemistry of Nano Silver is synthetic for Liao Xuehong etc.; " SCI ", 2000, (12)) all be to adopt high speed decanter type centrifugal the separation (centrifugal rotational speed is greater than 6000r/min).But this ultracentrifugal solid-liquid separating method energy consumption is big, and the silver powder after the separation can be bonded at the centrifuge tube bottom firmly, is difficult for taking out, and the loss amount of silver powder is bigger, and productive rate is low, and this method is high to the equipment requirement, is not suitable for large-scale industrialization and produces nano-silver powder.
Summary of the invention
The objective of the invention is to design a kind of solid-liquid separating method of simple nano-silver powder, solve the problem of the separation difficulty that occurs when liquid phase method prepares nano particle, in enormous quantities, the large-scale production of nano-silver powder provides feasibility.
The Separation of Solid and Liquid of production of nanometer silver powder by liquid-phase of the present invention realizes by process once:
1. the preparation of nano silver colloidal sol
With the sodium hypophosphite is reducing agent, and polyvinylpyrrolidone (PVP) is a macromolecule dispersant, and silver nitrate is a raw material, adopts the liquid phase chemical reduction legal system to be equipped with nano silver colloidal sol.
2. the preparation of conditioning agent
1) concentration of conditioning agent is 0.5～10% (mass fraction);
2) conditioning agent can be one or both in the reagent: NaOH, ammoniacal liquor, polyvinylamine, triethylamine, ethylenediamine, polyacrylamide, dimethylethanolamine, aluminium polychloride, bodied ferric sulfate.
3. stir nano silver colloidal sol in the ultrasonic field high speed, simultaneously to wherein adding conditioning agent, to pH be 1～5.
4. separate after leaving standstill a few hours
Can take two kinds of methods when 1) separating: topple over upper strata stillness of night method, vacuumizing filtration method behind the gravitational settling;
2) filter paper is quantitative filter paper at a slow speed during vacuumizing filtration, before filtering with the conditioning agent infiltration of same concentration.
5. passivation, washing, drying get grey black Nano Silver dry powder.
Simple to operate, advantages such as energy consumption is low, economical and efficient that the present invention has.Adopt the nano-silver powder of the inventive method gained, the degree of growing up of silver particles is less before and after Separation of Solid and Liquid, the silver particles glomeration, and narrow diameter distribution, silver powder purity height has good dispersiveness in water, ethanol.
Description of drawings
Accompanying drawing 1 is the XRD spectra of the nano-silver powder of all embodiment preparations of the present invention
Accompanying drawing 2 is the TEM of the nano-silver powder of the embodiment of the invention 1 preparation, multiplication factor 100K
Accompanying drawing 3 is the TEM of the nano-silver powder of the embodiment of the invention 2 preparations, multiplication factor 100K
Accompanying drawing 4 is the TEM of the nano-silver powder of the embodiment of the invention 3 preparations, multiplication factor 100K
Accompanying drawing 5 is the TEM of the nano-silver powder of the embodiment of the invention 4 preparations, multiplication factor 200K
Accompanying drawing 6 is the TEM of the nano-silver powder of the embodiment of the invention 5 preparations, multiplication factor 100K
The specific embodiment
Embodiment 1: preparation liquor argenti nitratis ophthalmicus: take by weighing the 100g silver nitrate, use the 200mL deionized water dissolving; The preparation of reducing solution: sodium hypophosphite (NaH
2PO
2H
2O) 40g, PVP 150g, the H of 1.0mol/L
2SO
420mL, deionized water 1200mL; Reducing solution is placed the three-necked bottle of the 3000mL of stirring, 40 ℃ of water-baths heating; At rotating speed is that the speed with 1～2mL/min drips liquor argenti nitratis ophthalmicus under the 300r/min, after being added dropwise to complete, continues to stir 60 minutes; Make silver sol.The silver sol that makes is placed the ultrasonic wave container together with three-necked bottle, ultrasonic under the 300W, stir on one side down simultaneously with the 1000r/min rotating speed, be 5% ammonia spirit Yi Bian drip mass fraction, to colloidal sol pH be 2; Leave standstill 15min, with 5 layers of quantitative filter paper suction filtration at a slow speed, the filter paper mass fraction is that 5% ammoniacal liquor soaks into; Passivation, washing are in 50 ℃ of following vacuum drying.Gained silver powder has carried out XRD and TEM respectively and has detected, and shown in accompanying drawing 1,2, this product particle is spherical, good dispersion, average grain diameter 10nm, purity height.
Embodiment 2: as example 1 preparation nano silver colloidal sol.With nano silver colloidal sol 1000r/min high-speed stirred in ultrasonic field of preparation, be 0.5% polyacrylamide solution to wherein dripping mass fraction, be about 1.5 to pH; Leave standstill 8h, treat the silver sol layering after, topple over and fall supernatant liquor; After passivation, the washing, 50 ℃ of following vacuum drying.Gained silver powder detects through XRD and TEM, shown in accompanying drawing 1,3, and silver powder purity height, average grain diameter is about 10～20nm.
Embodiment 3: as example 1 preparation nano silver colloidal sol.The silver sol that makes is placed the ultrasonic wave container together with three-necked bottle, ultrasonic under the 300W, stir on one side down simultaneously with the 1000r/min rotating speed, be 10% ethylenediamine solution Yi Bian drip mass fraction, to colloidal sol pH be 3; Leave standstill 30min, with 5 layers of quantitative filter paper suction filtration at a slow speed, the filter paper mass fraction is that 10% ethylenediamine soaks into; Passivation, washing are in 50 ℃ of following vacuum drying.Gained silver powder has carried out XRD and TEM respectively and has detected, and shown in accompanying drawing 1,4, this product particle is spherical, average grain diameter 30nm, purity height.
Embodiment 4: as example 1 preparation nano silver colloidal sol.Be 0.5% polyacrylamide with mass fraction with concentration be that the ethylenediamine equal-volume of 1.0mol/L mixes and is made into conditioning agent solution; Under the condition of stirring at low speed, with the preparation conditioning agent solution slowly pour in the nano silver colloidal sol, to pH be 2; Leave standstill a few hours, treat the colloidal sol layering after, topple over and fall supernatant liquor; Spend deionised water 5 times, after passivation, more once with deionized water, absolute ethyl alcohol, each washing of acetone; 50 ℃ of following vacuum drying.Gained silver powder has carried out XRD and TEM respectively and has detected, and shown in accompanying drawing 1,5, this product particle is spherical, average grain diameter 20nm, purity height.
Embodiment 5: as example 1 preparation nano silver colloidal sol.Be 0.5% polyacrylamide with mass fraction with concentration be that the ethylenediamine equal-volume of 1.0mol/L mixes and is made into conditioning agent solution; Under the condition of stirring at low speed, with the preparation conditioning agent solution slowly pour in the nano silver colloidal sol, to pH be 2; After leaving standstill 15min, with 3 layers of quantitative filter paper suction filtration at a slow speed, filter paper soaks into the ethylenediamine of 1.0mol/L; Passivation, washing are in 50 ℃ of following vacuum drying.Gained silver powder has carried out XRD and TEM respectively and has detected, and shown in accompanying drawing 1,6, this product particle is spherical, good dispersion, average grain diameter 10nm, purity height.
Claims (6)
1. the solid-liquid separating method of a production of nanometer silver powder by liquid-phase, the method comprises following continuous step:
At first, be reducing agent with the sodium hypophosphite, polyvinylpyrrolidone (PVP) is a macromolecule dispersant, silver nitrate is a raw material, adopts the liquid phase chemical reduction legal system to be equipped with nano silver colloidal sol; Then, stir nano silver colloidal sol, drip conditioning agent simultaneously in the ultrasonic field high speed; Separate after leaving standstill a few hours; Passivation, washing, 50 ℃ of vacuum drying.
2. according to the method for claim 1, it is characterized in that conditioning agent can be one or both in the reagent: NaOH, ammoniacal liquor, polyvinylamine, triethylamine, ethylenediamine, polyacrylamide, dimethylethanolamine, aluminium polychloride, bodied ferric sulfate.
3. according to the method for claim 1, the concentration that it is characterized in that conditioning agent is 0.5～10% (mass fraction).
4. according to the method for claim 1, it is characterized in that the pH adjustable range is 1～5.
5. according to the method for claim 1, can take two kinds of methods when it is characterized in that separating: topple over upper strata stillness of night method, vacuumizing filtration method behind the gravitational settling.
6. according to the method for claim 1, filter paper is quantitative filter paper at a slow speed when it is characterized in that vacuumizing filtration, before filtering with the conditioning agent infiltration of same concentration.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103331454A (en) * | 2013-07-02 | 2013-10-02 | 南京大学 | Nano-silver manufacturing technology |
| CN104174864A (en) * | 2013-05-21 | 2014-12-03 | 中国科学院理化技术研究所 | Preparation method of nano or sub-micron silver particle powder |
| CN105855562A (en) * | 2016-03-30 | 2016-08-17 | 湖南华信稀贵科技有限公司 | Method for preparing nanometer silver powder |
| CN106607180A (en) * | 2016-12-30 | 2017-05-03 | 广东工业大学 | Separation method of nanoparticles |
| CN111774583A (en) * | 2020-07-30 | 2020-10-16 | 金川集团股份有限公司 | Preparation method of superfine silver powder with high tap mass and high specific surface |
-
2006
- 2006-01-09 CN CN 200610020119 patent/CN1817524A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104174864A (en) * | 2013-05-21 | 2014-12-03 | 中国科学院理化技术研究所 | Preparation method of nano or sub-micron silver particle powder |
| CN103331454A (en) * | 2013-07-02 | 2013-10-02 | 南京大学 | Nano-silver manufacturing technology |
| CN105855562A (en) * | 2016-03-30 | 2016-08-17 | 湖南华信稀贵科技有限公司 | Method for preparing nanometer silver powder |
| CN106607180A (en) * | 2016-12-30 | 2017-05-03 | 广东工业大学 | Separation method of nanoparticles |
| CN106607180B (en) * | 2016-12-30 | 2019-02-22 | 广东工业大学 | A kind of separation method of nano particle |
| CN111774583A (en) * | 2020-07-30 | 2020-10-16 | 金川集团股份有限公司 | Preparation method of superfine silver powder with high tap mass and high specific surface |
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