CN105880628A - Preparation method of bright silver powder used in jewelry industry - Google Patents

Preparation method of bright silver powder used in jewelry industry Download PDF

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Publication number
CN105880628A
CN105880628A CN201610320064.9A CN201610320064A CN105880628A CN 105880628 A CN105880628 A CN 105880628A CN 201610320064 A CN201610320064 A CN 201610320064A CN 105880628 A CN105880628 A CN 105880628A
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CN
China
Prior art keywords
silver powder
preparation
bright
jewelry industry
powder
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Application number
CN201610320064.9A
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Chinese (zh)
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CN105880628B (en
Inventor
周全法
黄继忠
王自伟
孙洪波
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Jiangsu University of Technology
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Jiangsu University of Technology
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Priority to CN201610320064.9A priority Critical patent/CN105880628B/en
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Classifications

    • 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
    • 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
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Cosmetics (AREA)

Abstract

The invention relates to a preparation method of bright silver powder used in the jewelry industry. The preparation method of the bright silver powder used in the jewelry industry comprises the steps of (1) preparing a silver nitrate solution with the concentration of 1-1.5 mol/L; (2) adding a sodium hydroxide solution with the mass fraction of 5-10% into the silver nitrate solution and adjusting the pH value to 8-12; (3) dropping a triethanolamine solution into the silver nitrate solution in step (2) to obtain a silver powder serous fluid; (4) adding a stearic acid anhydrous ethanol solution with the mass fraction of 5-10% into the silver powder serous fluid for ultrasonic dispersion and drying; and (5) conducting ball-milling on the dried silver powder to obtain the bright silver powder. According to the preparation method of the bright silver powder used in the jewelry industry, ball-milling is conducted after the silver powder is dried, and it is ensured that the prepared bright silver powder is bright in color and luster, large in density, good in mechanical property, large in specific surface area, and capable of being used in the jewelry industry as well as being used in the fields of silver coating, conductive resin and the like. The preparation method of the bright silver powder used in the jewelry industry is simple, low in production cost, easy to produce in mass, and suitable for industrial large-scale production.

Description

A kind of preparation method of the Bright Silver Powder for jewelry industry
Technical field
The present invention relates to the preparation method of a kind of argentum powder, a kind of Bright Silver Powder for jewelry industry Preparation method.
Background technology
Along with progress and the development of technology in epoch, metal surface technique is had an immense impact on by new technique, with Before the technological effect that cannot realize nowadays can put into effect.New technique has driven traditional metal surface technique Change, occur in that many new works, make the most time-consuming artisan craftsmanship taken a lot of work become easily quickly. New decorative pattern, mass production, more multicolour, more moulding, make metal surface technique have more business opportunity, Business opportunity itself has driven the progress of technological level, adds the change of technique itself.Powdery paints have energy-conservation, The characteristics such as the performance of VOC free discharge, good decorative property, use safety, the most domestic powder coating technology Quickly grow.Powdery paints is as decorative material, and along with improving constantly of living standard, people are the fullest It is sufficient to the decoration of powdery paints single color, protection, and has higher requirement, have outside bright metal The nanometer silver powder seen, by it has been recognized that for being the expensive goods in art of powder coatings, by jewelry, household electrical appliances, The favorable comment of the application such as furniture and automobile, and slowly popularization is come.
Argentum powder can be divided into flake silver powder and ball shape silver powder.Flake silver powder refers to the lamellar of one-dimensional thickness < 100nm Powder, its preparation method is different, can be divided into reduction ball-milling method, light inducible and chemical reduction method.Wherein also Former ball-milling method: be the nano-scale particle shape argentum powder prepared with chemical reduction method as raw material, be pressed into through ball milling Lamellar, thus the method obtaining flake silver powder.Bright Silver Powder bright in color prepared by ball grinding method, density is big, Good mechanical property, specific surface area are big.The report preparing flake silver powder about reduction ball-milling method is a lot, different It is to change the kind of reducing agent, reducing condition, ball milling condition etc. to prepare the flake silver powder of different requirement.This Invention first reduction prepares dendroid or spherical argentum powder, then the ball milling through certain time, makes the light of lamellar Silver lustre powder, can be widely used for jewelry industry, can be used for other fields such as silver coating, conducting resinl.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of Bright Silver Powder for jewelry industry, prepared light The mean diameter of bright flake silver powder is 2-12 μm, can be used for other fields such as silver coating, conducting resinl.
The technical solution adopted for the present invention to solve the technical problems is:
The preparation method of a kind of Bright Silver Powder for jewelry industry, comprises the following steps:
(1) preparation silver nitrate solution, in solution, the concentration of silver nitrate is 1-1.5mol/L;
(2) in the silver nitrate solution that step (1) is prepared, the sodium hydroxide that mass fraction is 5-10% is added molten Liquid, regulates pH to 9-12;
(3) triethanolamine solution is instilled in the silver nitrate solution of step (2) with the speed of 0.5-1mL/min, Prepare argentum powder serosity;
(4) first being filtered by the argentum powder serosity that step (3) obtains, adding mass fraction after washing is 5-10% Stearic acid ethanol solution, ultrasonic disperse 1-2h, be dried remove etoh solvent;
(5) a diameter of 1mm and 3mm that step (4) dried argentum powder and mass ratio are 1:3-5 is mixed Closing zirconia ball, put in hexagon ball grinder after mixing by the ratio of grinding media to material of 1:4-6, rotational speed of ball-mill is 80~100 R/min, ball milling 20h, obtain Bright Silver Powder.
Specifically, described step (2), the temperature constant of (3) system are 25-40 DEG C.
Specifically, in described step (3), the ratio of triethanolamine and the amount of the material of silver nitrate is (1.5-5): 1.
Specifically, in described step (4), stearic acid concentration in argentum powder serosity is 0.5-1.5%.
Specifically, the mean diameter of the flake silver powder that described step (5) obtains is 2-12 μm.
Beneficial effects of the present invention:
(1) present invention is when preparing ultrapure argentum powder, and any protective agent and dispersant, nothing need not be added in centre Any organic residual, meets the use demand of jewelry product.
(2) present invention is addition ball-milling additive before argentum powder is dried, and carries out ball milling after drying, it is ensured that preparation Bright Silver Powder bright in color.
(3) preparation method of the present invention is simple, and production cost is low, be prone to volume production, be suitable for industrial on a large scale Produce.
(4) ratio of grinding media to material is controlled at 1:4-6 by preparation method of the present invention, it is ensured that ball milling effect, and makes argentum powder Particle diameter distribution is in narrower scope.
Detailed description of the invention
Presently in connection with embodiment, the present invention is further detailed explanation.
Embodiment 1
The preparation method of a kind of Bright Silver Powder for jewelry industry, comprises the following steps:
(1) preparation silver nitrate solution, in solution, the concentration of silver nitrate is 1-1.5mol/L;
(2) in the silver nitrate solution that step (1) is prepared, the sodium hydroxide that mass fraction is 5-10% is added molten Liquid, regulates pH to 9-12;
(3) triethanolamine solution is instilled in the silver nitrate solution of step (2) with the speed of 0.5-1mL/min, Preparing argentum powder serosity, wherein triethanolamine is 1.5-5:1 with the ratio of the amount of the material of silver nitrate
(4) first being filtered by the argentum powder serosity that step (3) obtains, adding mass fraction after washing is 5-10% Stearic acid ethanol solution, ultrasonic disperse 1-2h, be dried remove etoh solvent;Stearic acid is in argentum powder serosity Concentration be 0.5-1.5%,
(5) a diameter of 1mm and 3mm that step (4) dried argentum powder and mass ratio are 1:3-5 is mixed Closing zirconia ball, put in hexagon ball grinder after mixing by the ratio of grinding media to material of 1:4-6, rotational speed of ball-mill is 80~100 R/min, ball milling 20h, obtain Bright Silver Powder, and mean diameter is 2-12 μm;
Wherein, step (2), the temperature constant of (3) system are 25-40 DEG C.
Embodiment 2-6 and other conditions of scheme with embodiment 1, difference such as following table:
With the above-mentioned desirable embodiment according to the present invention for enlightenment, by above-mentioned description, related work Personnel can carry out various change and amendment completely in the range of without departing from this invention technological thought. The content that the technical scope of this invention is not limited in description, it is necessary to according to right Determine its technical scope.

Claims (5)

1. it is used for a preparation method for the Bright Silver Powder of jewelry industry, comprises the following steps:
(1) preparation silver nitrate solution, in solution, the concentration of silver nitrate is 1-1.5mol/L;
(2) in the silver nitrate solution that step (1) is prepared, the sodium hydroxide that mass fraction is 5-10% is added molten Liquid, regulates pH to 9-12;
(3) triethanolamine solution is instilled in the silver nitrate solution of step (2) with the speed of 0.5-1mL/min, Prepare argentum powder serosity;
(4) first being filtered by the argentum powder serosity that step (3) obtains, adding mass fraction after washing is 5-10% Stearic acid ethanol solution, ultrasonic disperse 1-2h, be dried remove etoh solvent;
(5) a diameter of 1mm and 3mm that step (4) dried argentum powder and mass ratio are 1:3-5 is mixed Closing zirconia ball, put in hexagon ball grinder after mixing by the ratio of grinding media to material of 1:4-6, rotational speed of ball-mill is 80~100 R/min, ball milling 20h, obtain Bright Silver Powder.
A kind of preparation method of the Bright Silver Powder for jewelry industry, its feature It is: described step (2), the temperature constant of (3) system are 25-40 DEG C.
A kind of preparation method of the Bright Silver Powder for jewelry industry, its feature It is: in described step (3), triethanolamine is 1.5-5:1 with the ratio of the amount of the material of silver nitrate.
A kind of preparation method of the Bright Silver Powder for jewelry industry, its feature It is: in described step (4), stearic acid concentration in argentum powder serosity is 0.5-1.5%.
A kind of preparation method of the Bright Silver Powder for jewelry industry, its feature It is: the mean diameter of the flake silver powder that described step (5) obtains is 2-12 μm.
CN201610320064.9A 2016-05-13 2016-05-13 A kind of preparation method of Bright Silver Powder for jewellery industry Expired - Fee Related CN105880628B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001049309A (en) * 1999-08-13 2001-02-20 Dowa Mining Co Ltd Silver powder, its production and production of flaky silver powder
JP2003055701A (en) * 2001-08-10 2003-02-26 Fukuda Metal Foil & Powder Co Ltd Silver powder for conductive paste and its manufacturing method and conductive paste using the silver powder
JP2009242914A (en) * 2008-03-31 2009-10-22 Mitsui Mining & Smelting Co Ltd Flake silver powder, and method for producing the same
CN102784927A (en) * 2012-08-28 2012-11-21 苏州东旭弘业新材料科技有限公司 Method for preparing high-performance sheet silver powder
CN103143723A (en) * 2013-03-27 2013-06-12 深圳市中金岭南科技有限公司 Method for preparing flake silver powder with low bulk density
CN104308183A (en) * 2014-10-24 2015-01-28 昆明舒扬科技有限公司 Preparation method for flake silver powder for electronic paste

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001049309A (en) * 1999-08-13 2001-02-20 Dowa Mining Co Ltd Silver powder, its production and production of flaky silver powder
JP2003055701A (en) * 2001-08-10 2003-02-26 Fukuda Metal Foil & Powder Co Ltd Silver powder for conductive paste and its manufacturing method and conductive paste using the silver powder
JP2009242914A (en) * 2008-03-31 2009-10-22 Mitsui Mining & Smelting Co Ltd Flake silver powder, and method for producing the same
CN102784927A (en) * 2012-08-28 2012-11-21 苏州东旭弘业新材料科技有限公司 Method for preparing high-performance sheet silver powder
CN103143723A (en) * 2013-03-27 2013-06-12 深圳市中金岭南科技有限公司 Method for preparing flake silver powder with low bulk density
CN104308183A (en) * 2014-10-24 2015-01-28 昆明舒扬科技有限公司 Preparation method for flake silver powder for electronic paste

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