WO2021002774A1 - Procédé de production de poudre à dispersion fine d'argent dans un électrolyte à base de nitrate - Google Patents

Procédé de production de poudre à dispersion fine d'argent dans un électrolyte à base de nitrate Download PDF

Info

Publication number
WO2021002774A1
WO2021002774A1 PCT/RU2020/000310 RU2020000310W WO2021002774A1 WO 2021002774 A1 WO2021002774 A1 WO 2021002774A1 RU 2020000310 W RU2020000310 W RU 2020000310W WO 2021002774 A1 WO2021002774 A1 WO 2021002774A1
Authority
WO
WIPO (PCT)
Prior art keywords
silver
powder
electrolyte
anode
nitrate
Prior art date
Application number
PCT/RU2020/000310
Other languages
English (en)
Russian (ru)
Inventor
Юрий Васильевич ТАРАСОВ
Original Assignee
Юрий Васильевич ТАРАСОВ
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=70415510&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=WO2021002774(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Юрий Васильевич ТАРАСОВ filed Critical Юрий Васильевич ТАРАСОВ
Publication of WO2021002774A1 publication Critical patent/WO2021002774A1/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells

Definitions

  • the invention relates to powder metallurgy, in particular, to electrolytic production of silver powders for the production of electrical contacts and other conductive products.
  • the precipitated silver has a coarse-crystalline structure and is sent for remelting into ingots, and the electrolyte is sent for periodic regeneration.
  • the closest to the claimed method in terms of the totality of features is the "Method of electrolytic production of fine silver powders" [5] using silver plates from Ag 99.99 as anodes in a nitrate electrolyte.
  • This method is taken as a prototype.
  • the size of the powder particles was controlled by changing the cathode current density and the composition of the electrolyte. To reduce the particle size of the powder, the current density was increased and the concentration of silver in the electrolyte was decreased. The latter factor is associated with the regeneration of the solution or its replacement and the associated difficulties in industrial implementation for controlling the dispersion of the powder.
  • a common property of electrolysis processes using only soluble anodes is the accumulation of metal in the solution during operation. When the permissible metal content is exceeded, the electrolyte is sent for regeneration to restore its original composition.
  • the solution is enriched in silver due to the fact that the cathodic current efficiency of the metal is lower anode current efficiency due to the fact that not only silver ions are discharged at the cathode, but also hydrogen ions with the release of nitric oxide in a nitrate solution according to the scheme:
  • waste on the sieve are considered recyclable waste and are returned after fusion to the head of the process: to the electrolysis bath for repeated anodic dissolution.
  • the volume of waste directly depends on the initial size of the semi-finished powder extracted from the bath.
  • the technical objectives of the invention are to increase the yield of silver powder, improve process controllability and increase the service life of the electrolyte.
  • the technical result of the proposed method for producing fine silver powder in a nitrate electrolyte is provided by the fact that electrolysis is carried out in combination with an insoluble anode, electrically directly connected to a soluble anode.
  • the insoluble anode taking on a part of the operating current, reduces the anode current output of the metal to the value of the cathodic current output of the metal, stabilizing the silver level in the electrolyte.
  • the directional effect of the insoluble anode on the silver level in the solution depends on the ratio of the cathodic and anodic current outputs of silver and the purity of the anode metal and is obviously manifested when the silver content in the anode is at least 90%.
  • the accumulation of impurity metals mainly copper
  • the service life of the electrolyte increases and becomes practically unlimited even at 99% purity of the anode silver.
  • stabilization of the electrolyte composition by Silver maintains consistent powder particle size and minimal waste, ensuring high product yields.
  • the silver content in the solution and the size of the powder particles are controlled by changing the current to the insoluble anode by changing the area of its contact with the solution due to its immersion depth.
  • the immersion depth of the anode is respectively increased or decreased by any available method: mechanical, automatic or manual.
  • the relationship between the particle size of the powder and the burial follows from the well-known laws of electrical engineering.
  • an increase in the immersion depth of the insoluble anode leads to a redistribution of currents between the anodes connected in parallel, namely: an increase in the current to it due to an increase in the contact area with the solution and, accordingly, a decrease in the current to the soluble anode and the anode current output of the powder at unchanged cathode output.
  • Nitric oxide released during electrolysis is captured in a ventilation trap, bubbling through the soda solution, turning into sodium nitrate - nitrogen fertilizer - without harm to the environment.
  • an insoluble anode was used, made of pyrocarbon [8] grade UPA-3 (pyrolytic reinforced carbon) produced by Novocherkassk
  • An example of industrial application of the method for producing finely dispersed silver powder PSr1 in a nitrate electrolyte using an insoluble anode solution composition - ⁇ g ⁇ + (50-400) g / l AgNCb + 10 g / l HNO 3 , temperature - 25-30 ° ⁇ , soluble anode - standard silver ingot 99.99%, operating current - 150 + 200 A, current to the insoluble anode - 10 + 20 A, initial dimensions of the insoluble anode - 50x300x10 mm, immersion depth - 100 + 200 mm.
  • Patent RU Ns 2210631 Patent RU Ns 2210631.
  • Patent RU a 2558325
  • Patent RU 2420613

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrolytic Production Of Metals (AREA)

Abstract

L'invention se rapporte au domaine du frittage, notamment à la production par un procédé électrolytique de poudres d'argent que l'on utilise dans l'industrie électro-technique et radio-électronique. Cette poudre d'argent à dispersion fine est obtenue dans un électrolyte à base de nitrate en utilisant de l'argent ayant une pureté d'au moins 90% en qualité d'anode soluble. L'électrolyse est effectuée en combinaison avec au moins une anode supplémentaire non soluble, et la teneur en argent de l'électrolyte et la taille des particules de poudre sont ajustées en modifiant la profondeur d'immersion de l'anode non soluble. Ce procédé permet d'augmenter la production de poudre d'argent, d'améliorer les caractéristiques de commande du processus et de prolonger la durée de vie de l'électrolyte.
PCT/RU2020/000310 2019-07-01 2020-06-26 Procédé de production de poudre à dispersion fine d'argent dans un électrolyte à base de nitrate WO2021002774A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2019120462 2019-07-01
RU2019120462A RU2720189C1 (ru) 2019-07-01 2019-07-01 Способ получения мелкодисперсного порошка серебра в нитратном электролите

Publications (1)

Publication Number Publication Date
WO2021002774A1 true WO2021002774A1 (fr) 2021-01-07

Family

ID=70415510

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/RU2020/000310 WO2021002774A1 (fr) 2019-07-01 2020-06-26 Procédé de production de poudre à dispersion fine d'argent dans un électrolyte à base de nitrate

Country Status (2)

Country Link
RU (1) RU2720189C1 (fr)
WO (1) WO2021002774A1 (fr)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU129447A1 (ru) * 1959-09-15 1959-11-30 В.И. Семерюк Способ электролитического получени порошка серебра из нерастворимых соединений
RU2420613C1 (ru) * 2010-04-13 2011-06-10 Открытое акционерное общество "УРАЛЬСКИЙ ЭЛЕКТРОХИМИЧЕСКИЙ КОМБИНАТ" Способ получения электролитических порошков металлов
RU2558325C1 (ru) * 2014-06-17 2015-07-27 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Способ электролитического получения мелкодисперсных порошков серебра

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0247208A (ja) * 1988-08-08 1990-02-16 Mitsui Mining & Smelting Co Ltd 高純度銀微粉末の製造方法
RU2534181C2 (ru) * 2013-02-19 2014-11-27 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Российский химико-технологический университет им. Д.И. Менделеева" (РХТУ им. Д.И. Менделеева) Способ получения электролитических порошков металлов

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU129447A1 (ru) * 1959-09-15 1959-11-30 В.И. Семерюк Способ электролитического получени порошка серебра из нерастворимых соединений
RU2420613C1 (ru) * 2010-04-13 2011-06-10 Открытое акционерное общество "УРАЛЬСКИЙ ЭЛЕКТРОХИМИЧЕСКИЙ КОМБИНАТ" Способ получения электролитических порошков металлов
RU2558325C1 (ru) * 2014-06-17 2015-07-27 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Способ электролитического получения мелкодисперсных порошков серебра

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
KATALOG OOO: "Donkarb Grafit", KATOD GRAFITOVYI. NAIDENO V INTERNET, 29 March 2017 (2017-03-29), Retrieved from the Internet <URL:https://doncarb.com/articles/katod-grafitovyy> *

Also Published As

Publication number Publication date
RU2720189C1 (ru) 2020-04-27

Similar Documents

Publication Publication Date Title
WO2001090445A1 (fr) Procede de production de metal de purete superieure
WO2013038927A1 (fr) Electrode positive de génération de chlore
CN104018186A (zh) 一种铜铟镓硒的回收方法
JP2014501850A (ja) チオ硫酸塩溶液からの金および銀の電気的回収
JP2010509050A (ja) 電気化学的方法により廃触媒から白金族金属を抽出する方法
KR101199513B1 (ko) Ｐｂ-ｆｒｅｅ 폐솔더로부터 유가 금속의 회수방법
US2273798A (en) Electrolytic process
CN112981433A (zh) 一种阳离子膜矿浆电解回收废旧磷酸铁锂正极材料的方法及回收得到的氢氧化锂
Ha et al. Electrowinning of tellurium from alkaline leach liquor of cemented Te
US3983018A (en) Purification of nickel electrolyte by electrolytic oxidation
GB2534332A (en) Method and apparatus for producing metallic tantalum by electrolytic reduction of a feedstock
WO2021002774A1 (fr) Procédé de production de poudre à dispersion fine d&#39;argent dans un électrolyte à base de nitrate
FI127028B (en) Method and apparatus for metal electrical recovery
RU2469111C1 (ru) Способ получения медных порошков из медьсодержащих аммиакатных отходов
JPH0445597B2 (fr)
US3382163A (en) Method of electrolytic extraction of metals
US4115222A (en) Method for electrolytic winning of lead
CN111826682A (zh) 金属粉末的回收方法
DE602004001677T2 (de) Verfahren zur elektrolytischen gewinnung von kupfer in salzsaurer lösung
JP2020055728A (ja) 硫酸溶液の製造方法
RU2553319C1 (ru) Способ получения порошка металла электролизом
CN109082686B (zh) 棒状形貌钛粉及其制备方法
DE19624024A1 (de) Verfahren zur Herstellung von Halogenen, Oxoverbindungen der Halogene sowie zur Herstellung von Peroxyverbindungen durch Elektrolyse
Mantell Electrodeposition of powders for powder metallurgy
RU2393943C2 (ru) СПОСОБ ПОЛУЧЕНИЯ СЕРЕБРЯНЫХ ПОРОШКОВ ПСр1 И ПСр2

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 20834216

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 20834216

Country of ref document: EP

Kind code of ref document: A1