CN106363191B - A kind of preparation method of platinum powder or platinum-rhodium alloy powder - Google Patents

A kind of preparation method of platinum powder or platinum-rhodium alloy powder Download PDF

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CN106363191B
CN106363191B CN201610856089.0A CN201610856089A CN106363191B CN 106363191 B CN106363191 B CN 106363191B CN 201610856089 A CN201610856089 A CN 201610856089A CN 106363191 B CN106363191 B CN 106363191B
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platinum
powder
rhodium alloy
solution
acid
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CN106363191A (en
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彭辉
张胜明
石映奔
牟冉冉
邹东清
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CHENGDU GUANGMING PAITE PRECIOUS METAL Co Ltd
Chengdu Guangming Optoelectronics Co Ltd
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CHENGDU GUANGMING PAITE PRECIOUS METAL Co Ltd
Chengdu Guangming Optoelectronics Co Ltd
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    • 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

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Abstract

The invention belongs to platinum-rhodium alloy fields, and in particular to the preparation method of a kind of platinum powder or platinum-rhodium alloy powder.Technical problem to be solved by the invention is to provide the preparation methods of a kind of platinum powder or platinum-rhodium alloy powder, comprising the following steps: A, pre-treatment: using salt acid soak platinum or platinum-rhodium alloy, washes after taking-up, then be placed into the mixed solution of concentrated hydrochloric acid and concentrated nitric acid;B, it dissolves: system temperature being risen into 90~110 DEG C of sufficiently reactions, then sufficiently drives nitric acid away with concentrated hydrochloric acid, is then diluted to solution 30~80g/L containing noble metal;C, restore: when system temperature rises to 80~90 DEG C, being alternately added concentration is sufficiently to react after 20~60g/L polyvinylpyrrolidone ethanol solution and hydrazine hydrate, and then plus alkali neutralization is to neutrality;D, it post-processes: 30~80g/L ammonium bicarbonate aqueous solution is added, standing sedimentation is dried after washing of precipitate.Small granularity purity is high, particle, uniform platinum powder or platinum-rhodium alloy powder can be prepared in the method for the present invention.

Description

A kind of preparation method of platinum powder or platinum-rhodium alloy powder
Technical field
The invention belongs to platinum-rhodium alloy fields, and in particular to the preparation method of a kind of platinum powder or platinum-rhodium alloy powder.
Background technique
Ultrafine Platinum Powder or platinum-rhodium alloy powder material are the raw material for preparing platinum or platinum rhodium disperse material.In the prior art by platinum The method that gold or platinum-rhodium alloy are prepared into powder is roughly divided into physical method and chemical method, and wherein physical method has the sides such as induction atomization Method there are equipment requirement height, puts into the disadvantages such as expensive, yield rate is low;Wherein chemical method has the methods of hydrazine hydrate reduction method, Have the shortcomings that yield rate is low.
Summary of the invention
In view of the above-mentioned drawbacks of the prior art, the present invention is based on hydrazine hydrate reduction methods to be researched and analysed, to mention The preparation method of a kind of new platinum powder or platinum-rhodium alloy powder is supplied.It is below in 0.25mm that the method for the present invention is able to produce out granularity Ultrafine Platinum Powder or platinum-rhodium alloy powder material, finished product sieving rate is up to 70% or more.
Technical problem to be solved by the invention is to provide a kind of methods for preparing platinum powder or platinum-rhodium alloy powder.This method packet Include following steps:
A, pre-treatment: salt acid soak platinum or platinum-rhodium alloy are used, is washed after taking-up, then be placed into acid solution;Described Acid solution is the mixed solution of concentrated hydrochloric acid and concentrated nitric acid;
B, it dissolves: system temperature being risen into 90~110 DEG C of sufficiently reactions, then sufficiently drives nitric acid away with concentrated hydrochloric acid, it is then dilute It releases to solution 30~80g/L containing noble metal;
C, it restores: system temperature is risen to 80~90 DEG C, being alternately added concentration is 20~60g/L polyvinylpyrrolidone second Alcoholic solution and hydrazine hydrate sufficiently react, then plus alkali neutralization to neutrality;
D, it post-processes: 30~80g/L ammonium bicarbonate aqueous solution is added, standing sedimentation is dried after washing of precipitate.
Preferably, the above-mentioned method for preparing platinum powder or platinum-rhodium alloy powder, comprising the following steps:
A, pre-treatment: salt acid soak platinum or platinum-rhodium alloy are used, is washed after taking-up, then be placed into acid solution;Described Acid solution is the mixed solution of concentrated hydrochloric acid and concentrated nitric acid;
B, it dissolves: system temperature being risen into 95~105 DEG C of sufficiently reactions, then sufficiently drives nitric acid away with concentrated hydrochloric acid, it is then dilute It releases to solution 40~60g/L containing noble metal;
C, it restores: system temperature is risen to 82~85 DEG C, being alternately added concentration is 30~50g/L polyvinylpyrrolidone second Alcoholic solution and hydrazine hydrate sufficiently react, and then plus alkali neutralization is to neutrality;
D, it post-processes: 40~60g/L ammonium bicarbonate aqueous solution is added, standing sedimentation is dried after washing of precipitate.
Preferably, in above method step B, described drive away after nitric acid further includes that water is added to drive a large amount of salt away before dilute solution Acid.
Preferably, in above method step A, the size of the platinum or platinum-rhodium alloy is long 400mm or less, width 150mm Below, thickness 0.2mm or less.
Preferably, in above method step A, the hydrochloric acid is that concentrated hydrochloric acid and water are formulated according to 1 ︰ 2~8 of volume ratio.
Preferably, in above method step A, the content of rhodium is below 20% in the platinum-rhodium alloy.
Preferably, in above method step A, the soaking time is 0.5~1h.
Preferably, in above method step A, the acid solution is that concentrated hydrochloric acid and concentrated nitric acid are prepared according to 2~8 ︰ 1 of volume ratio It forms.
Preferably, described to be diluted to solution 50g/L containing noble metal in above method step B.
Preferably, in above method step C, the concentration of the polyvinylpyrrolidone ethanol solution is 40g/L.
Preferably, in above method step C, the additional amount of the polyvinylpyrrolidone ethanol solution is 1~1.1L/kg Noble metal.
Preferably, in above method step C, the additional amount of the hydrazine hydrate is 0.7~0.8L/1kg noble metal.
Preferably, in above method step C, described neutralize is carried out using ammonium hydroxide.
Preferably, in above method step D, the concentration of the ammonium bicarbonate aqueous solution is 50g/L.
Preferably, in above method step D, the additional amount of the ammonium bicarbonate soln is 2.3~2.5L/1kg noble metal.
The platinum powder or platinum-rhodium alloy Powder Particle Size that the method for the present invention is prepared 0.25mm sieving rate below up to 70% with On;When further reasonably optimal control response parameter, granularity 0.25mm sieving rate below is up to 90% or more, or even into one Step can reach 99% or so.Platinum powder or platinum-rhodium alloy powder are the raw material for preparing platinum or platinum rhodium disperse material, so, the present invention Method provides a kind of better raw material for the preparation of disperse material.
Specific embodiment
A kind of preparation method of platinum powder or platinum-rhodium alloy powder, comprising the following steps:
A, pre-treatment: platinum or platinum-rhodium alloy are impregnated to remove certain impurity contained therein with hydrochloric acid solution, is then taken It is rinsed with water completely, is transferred in acid solution out;The acid solution is concentrated hydrochloric acid and concentrated nitric acid mixed solution;Wherein, institute Stating hydrochloric acid solution is that concentrated hydrochloric acid and water are formulated according to 1 ︰ 2~8 of volume ratio;The acid solution be concentrated hydrochloric acid and concentrated nitric acid by It is formulated according to 2~8 ︰ 1 of volume ratio;
B, dissolve: system temperature, which is warming up to 90~110 DEG C, reacts acid solution sufficiently to nothing with platinum or platinum-rhodium alloy Solid exists;Since heating hydrochloric acid and nitric acid can volatilize in reaction process, so needing optionally to supplement addition acid in reaction process Solution;Or reaction unit is closed, only stays waste emission pipeline;
In the presence of no solid, as reaction terminates;Then concentrated hydrochloric acid is added in two portions and sufficiently drives nitric acid away to no yellow Cigarette generates;Meanwhile in order to save it is subsequent neutralize consumed aqueous slkali, drive away and add pure water after nitric acid and drive a large amount of hydrochloric acid away, so Dilute solution is to containing 30~80g/L of noble metal afterwards;Solution is maroon at this time;
C, it restores: system being warming up to 80~90 DEG C, polyvinylpyrrolidone ethanol solution is alternately added and hydrazine hydrate fills It is colourless for point being restored to solution, then being neutralized to pH with ammonium hydroxide is 6~7, places cooling;The polyvinylpyrrolidone ethanol solution Concentration be 20~60g/L;
D, post-process: the ammonium bicarbonate soln of 30~80g/L is added in stirring, and quiescent settling is extracted out after supernatant clarification Recycling, precipitating are dried at 120 DEG C after acetone, dehydrated alcohol, pure water cleaning.
Noble metal described in above method step B is platinum or platinum-rhodium alloy, when raw material is platinum, herein expensive Metal is platinum;When raw material is platinum-rhodium alloy, noble metal herein is the total amount of platinum and rhodium.
The finished product platinum powder or platinum-rhodium alloy Powder Particle Size being prepared by the above method in 0.25mm to assign 70% or more, Other performances are able to satisfy requirement.Obtained platinum or platinum-rhodium alloy powder disperse means can be added by conventional method and Disperse material is prepared.
Preferably, the above-mentioned method for preparing platinum powder or platinum-rhodium alloy powder, comprising the following steps:
A, pre-treatment: salt acid soak platinum or platinum-rhodium alloy are used, is washed after taking-up, then be placed into acid solution;Described Acid solution is the mixed solution of concentrated hydrochloric acid and concentrated nitric acid;
B, it dissolves: system temperature being risen into 95~105 DEG C of sufficiently reactions, then sufficiently drives nitric acid away with concentrated hydrochloric acid, it is then dilute It releases to solution 40~60g/L containing noble metal;
C, restore: when system temperature rises to 82~85 DEG C, being alternately added concentration is 30~50g/L polyvinylpyrrolidone second It is sufficiently reacted after alcoholic solution and hydrazine hydrate, then plus alkali neutralization is to neutrality;
D, it post-processing: 40~60g/L ammonium bicarbonate aqueous solution is added, standing sedimentation extracts recycling out after supernatant clarification, Precipitating is dried at 120 DEG C after acetone, dehydrated alcohol, pure water cleaning.
The finished product platinum powder or platinum-rhodium alloy Powder Particle Size being prepared by the above method in 0.25mm to assign 90% or more, Other performances are able to satisfy requirement.Obtained platinum or platinum-rhodium alloy powder disperse means can be added by conventional method and Disperse material is prepared.
In above method step A, in order to sufficiently remove impurity contained in platinum or platinum-rhodium alloy, and do not waste time, The soaking time is 0.5~1h.
In above method step B, if the concentration after diluting is lower than 30g/L, the sequential reduction time can be extended, reduce finished product Rate;Such as it is higher than 80g/L, will lead to reduction particle and become larger, reduce yield rate;So need to control dilution after solution containing noble metal 30~ 80g/L.Preferably 40~60g/L.More preferably 50g/L.
In above method step C, be neutralized to it is neutral conventional aqueous slkali can be used, such as sodium hydroxide, potassium hydroxide, but should Impurity can be brought in the process, influence purity.It is advantageous to use ammonium hydroxide.
In above method step C, if the concentration of polyvinylpyrrolidone ethanol solution is lower than 20g/L, reduction will lead to Grain granularity becomes larger, and reduces yield rate;If the concentration of polyvinylpyrrolidone ethanol solution is higher than 60g/L, reduction particle will lead to It is meticulous, extend subsequent operation time, reduction not exclusively, reduces yield rate;So polyvinylpyrrolidone ethanol solution need to be controlled Concentration be 20~60g/L.Preferably 30~50g/L.More preferably 40g/L.
In above method step D, for the purposes of meeting sedimented particle granularity, need to control ammonium bicarbonate aqueous solution concentration is 30 ~80g/L.Preferably 40~60g/L.More preferably 50g/L.
Preferably, in above method step C, the additional amount of the polyvinylpyrrolidone ethanol solution is 1~1.1L/kg Noble metal.
Preferably, in above method step C, the additional amount of the hydrazine hydrate is 0.7~0.8L/1kg noble metal.
Preferably, in above method step D, the additional amount of the ammonium bicarbonate soln is 2.3~2.5L/1kg noble metal.
Embodiment 1
A, pre-treatment: platinum or platinum-rhodium alloy are impregnated with hydrochloric acid solution (volume ratio of concentrated hydrochloric acid and water is 1 ︰ 2), after taking-up It is rinsed well, is transferred in the reaction kettle containing acid solution (volume ratio of concentrated hydrochloric acid and concentrated nitric acid is 5 ︰ 1) with pure water;
B, dissolve: system temperature, which is warming up to 90 DEG C, makes acid solution sufficiently react to no solid with platinum or platinum-rhodium alloy It is existing, it concentrated hydrochloric acid is added in two portions sufficiently drives nitric acid to no yellow cigarette away and generate;Meanwhile in order to save the consumed alkali of subsequent neutralization, It drives away and adds pure water after nitric acid and drive a large amount of hydrochloric acid away, then dilute solution is to containing noble metal 30g/L;Solution is brown red at this time Color;
C, it restores: system is warming up to 80 DEG C, be alternately added polyvinylpyrrolidone ethanol solution and hydrazine hydrate sufficiently also It is colourless as far as solution, then being neutralized to pH with ammonium hydroxide is 6~7, places cooling;The polyvinylpyrrolidone ethanol solution it is dense Degree is 20g/L;The additional amount of the polyvinylpyrrolidone ethanol solution is 1~1.1L/kg noble metal;The hydrazine hydrate adds Entering amount is 0.7~0.8L/1kg noble metal;
D, post-process: the ammonium bicarbonate soln of 30g/L is added in stirring, and additional amount is 2.3~2.5L/1kg noble metal, static Sedimentation, extracts recycling out after supernatant clarification, and precipitating is dried at 120 DEG C after acetone, dehydrated alcohol, pure water cleaning.
The platinum powder or platinum-rhodium alloy Powder Particle Size being prepared by the above method in 0.25mm yield rate 68% below, He meets requirement at performance.
Embodiment 2
A, pre-treatment: platinum or platinum-rhodium alloy are impregnated with hydrochloric acid solution (volume ratio of concentrated hydrochloric acid and water is 1 ︰ 3), after taking-up It is rinsed well, is transferred in the reaction kettle containing acid solution (volume ratio of concentrated hydrochloric acid and concentrated nitric acid is 3 ︰ 1) with pure water;
B, dissolve: system temperature, which is warming up to 100 DEG C, reacts acid solution sufficiently to no solid with platinum or platinum-rhodium alloy Occur, concentrated hydrochloric acid is added in two portions sufficiently drives nitric acid to no yellow cigarette away and generate;Meanwhile being consumed to save subsequent neutralization Alkali drives away and adds pure water after nitric acid and drive a large amount of hydrochloric acid away, and then dilute solution is to containing noble metal 80g/L;Solution is brown at this time It is red;
C, reduction reaction: being warming up to 85 DEG C for system, is alternately added polyvinylpyrrolidone ethanol solution and hydrazine hydrate fills It is colourless for point being restored to solution, then being neutralized to pH with ammonium hydroxide is 6~7, places cooling;The polyvinylpyrrolidone ethanol solution Concentration be 60g/L;The additional amount of the polyvinylpyrrolidone ethanol solution is 1~1.1L/kg noble metal;The hydrazine hydrate Additional amount be 0.7~0.8L/1kg noble metal;
D, post-process: the ammonium bicarbonate soln of 80g/L is added in stirring, and additional amount is 2.3~2.5L/1kg noble metal, static Sedimentation, extracts recycling out after supernatant clarification, and precipitating is dried at 120 DEG C after acetone, dehydrated alcohol, pure water cleaning.
The platinum powder or platinum-rhodium alloy Powder Particle Size being prepared by the above method in 0.25mm yield rate 72% below, He meets requirement at performance.
Embodiment 3
A, pre-treatment: platinum or platinum-rhodium alloy are impregnated with hydrochloric acid solution (volume ratio of concentrated hydrochloric acid and water is 1 ︰ 8), after taking-up It is rinsed well, is transferred in the reaction kettle containing acid solution (volume ratio of concentrated hydrochloric acid and concentrated nitric acid is 8 ︰ 1) with pure water;
B, dissolve: system temperature, which is warming up to 110 DEG C, reacts acid solution sufficiently to no solid with platinum or platinum-rhodium alloy Occur, concentrated hydrochloric acid is added in two portions sufficiently drives nitric acid to no yellow cigarette away and generate;Meanwhile being consumed to save subsequent neutralization Alkali drives away and adds pure water after nitric acid and drive a large amount of hydrochloric acid away, and then dilute solution is to containing noble metal 80g/L;Solution is brown at this time It is red;
C, reduction reaction: being warming up to 90 DEG C for system, is alternately added polyvinylpyrrolidone ethanol solution and hydrazine hydrate fills It is colourless for point being restored to solution, then being neutralized to pH with ammonium hydroxide is 6~7, places cooling;The polyvinylpyrrolidone ethanol solution Concentration be 40g/L;The additional amount of the polyvinylpyrrolidone ethanol solution is 1~1.1L/kg noble metal;The hydrazine hydrate Additional amount be 0.7~0.8L/1kg noble metal;
D, post-process: the ammonium bicarbonate soln of 50g/L is added in stirring, and additional amount is 2.3~2.5L/1kg noble metal, static Sedimentation, extracts recycling out after supernatant clarification, and precipitating is dried at 120 DEG C after acetone, dehydrated alcohol, pure water cleaning.
The platinum powder or platinum-rhodium alloy Powder Particle Size being prepared by the above method in 0.25mm yield rate 86% below, He meets requirement at performance.
Embodiment 4
A, pre-treatment: platinum or platinum-rhodium alloy are impregnated to remove with hydrochloric acid solution (volume ratio of concentrated hydrochloric acid and water is 1 ︰ 3) Impurity therein, is rinsed well after taking-up with pure water, transfers to that (volume ratio of concentrated hydrochloric acid and concentrated nitric acid is containing acid solution 3 ︰ 1) reaction kettle in;
B, dissolve: system temperature, which is warming up to 98 DEG C, makes acid solution sufficiently react to no solid with platinum or platinum-rhodium alloy It is existing, it concentrated hydrochloric acid is added in two portions sufficiently drives nitric acid to no yellow cigarette away and generate;Meanwhile in order to save the consumed alkali of subsequent neutralization, It drives away and adds pure water after nitric acid and drive a large amount of hydrochloric acid away, then dilute solution is to containing noble metal 45g/L;Solution is brown red at this time Color;
C, reduction reaction: being warming up to 83 DEG C for system, is alternately added polyvinylpyrrolidone ethanol solution and hydrazine hydrate fills It is colourless for point being restored to solution, then being neutralized to pH with ammonium hydroxide is 6~7, places cooling;The polyvinylpyrrolidone ethanol solution Concentration be 38g/L;The additional amount of the polyvinylpyrrolidone ethanol solution is 1~1.1L/kg noble metal;The hydrazine hydrate Additional amount be 0.7~0.8L/1kg noble metal;
D, post-process: the ammonium bicarbonate soln of 42g/L is added in stirring, and additional amount is 2.3~2.5L/1kg noble metal, static Sedimentation, extracts recycling out after supernatant clarification, and precipitating is dried at 120 DEG C after acetone, dehydrated alcohol, pure water cleaning.
The platinum powder or platinum-rhodium alloy Powder Particle Size being prepared by the above method in 0.25mm yield rate 94% below, He meets requirement at performance.
Embodiment 5
A, pre-treatment: platinum or platinum-rhodium alloy are impregnated to remove with hydrochloric acid solution (volume ratio of concentrated hydrochloric acid and water is 1 ︰ 6) Impurity therein, is rinsed well after taking-up with pure water, transfers to that (volume ratio of concentrated hydrochloric acid and concentrated nitric acid is containing acid solution 7 ︰ 1) reaction kettle in;
B, dissolve: system temperature, which is warming up to 102 DEG C, reacts acid solution sufficiently to no solid with platinum or platinum-rhodium alloy Occur, concentrated hydrochloric acid is added in two portions sufficiently drives nitric acid to no yellow cigarette away and generate;Meanwhile being consumed to save subsequent neutralization Alkali drives away and adds pure water after nitric acid and drive a large amount of hydrochloric acid away, and then dilute solution is to containing noble metal 55g/L;Solution is brown at this time It is red;
C, reduction reaction: being warming up to 84 DEG C for system, is alternately added polyvinylpyrrolidone ethanol solution and hydrazine hydrate fills It is colourless for point being restored to solution, then being neutralized to pH with ammonium hydroxide is 6~7, places cooling;The polyvinylpyrrolidone ethanol solution Concentration be 46g/L;The additional amount of the polyvinylpyrrolidone ethanol solution is 1~1.1L/kg noble metal;The hydrazine hydrate Additional amount be 0.7~0.8L/1kg noble metal;
D, post-process: the ammonium bicarbonate soln of 48g/L is added in stirring, and additional amount is 2.3~2.5L/1kg noble metal, static Sedimentation, extracts recycling out after supernatant clarification, and precipitating is dried at 120 DEG C after acetone, dehydrated alcohol, pure water cleaning.
The platinum powder or platinum-rhodium alloy Powder Particle Size being prepared by the above method in 0.25mm yield rate 95% below, He meets requirement at performance.
Embodiment 6
A, pre-treatment: platinum or platinum-rhodium alloy are impregnated with hydrochloric acid solution (volume ratio of concentrated hydrochloric acid and water is 1 ︰ 5), after taking-up It is rinsed well, is transferred in the reaction kettle containing acid solution (volume ratio of concentrated hydrochloric acid and concentrated nitric acid is 5 ︰ 1) with pure water;
B, dissolve: system temperature, which is warming up to 100 DEG C, makes chloroazotic acid sufficiently react to no solid with platinum or platinum-rhodium alloy It is existing, it concentrated hydrochloric acid is added in two portions sufficiently drives nitric acid to no yellow cigarette away and generate;Meanwhile in order to save the consumed alkali of subsequent neutralization, It drives away and adds pure water after nitric acid and drive a large amount of hydrochloric acid away, then dilute solution is to containing noble metal 50g/L;Solution is brown red at this time Color;
C, reduction reaction: being warming up to 83 DEG C for system, is alternately added polyvinylpyrrolidone ethanol solution and hydrazine hydrate fills It is colourless for point being restored to solution, then being neutralized to pH with ammonium hydroxide is 6~7, places cooling;The polyvinylpyrrolidone ethanol solution Concentration be 40g/L;The additional amount of the polyvinylpyrrolidone ethanol solution is 1~1.1L/kg noble metal;The hydrazine hydrate Additional amount be 0.7~0.8L/1kg noble metal;
D, post-process: the ammonium bicarbonate soln of 50g/L is added in stirring, and additional amount is 2.3~2.5L/1kg noble metal, static Sedimentation, extracts recycling out after supernatant clarification, and precipitating is dried at 120 DEG C after acetone, dehydrated alcohol, pure water cleaning.
The platinum powder or platinum-rhodium alloy Powder Particle Size being prepared by the above method are 99% in 0.25mm ratio defective product below, Other performances meet requirement.

Claims (17)

1. the method for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: the following steps are included:
A, pre-treatment: salt acid soak platinum or platinum-rhodium alloy are used, is washed after taking-up, then be placed into acid solution;The acid is molten Liquid is the mixed solution of concentrated hydrochloric acid and concentrated nitric acid;
B, it dissolves: system temperature being risen into 90~110 DEG C of sufficiently reactions, then sufficiently drives nitric acid away with concentrated hydrochloric acid, is then diluted to Solution 30~80g/L containing noble metal;
C, it restores: system temperature is risen to 80~90 DEG C, being alternately added concentration is that 20~60g/L polyvinylpyrrolidone ethyl alcohol is molten Liquid and hydrazine hydrate sufficiently react, then plus alkali neutralization to neutrality;
D, it post-processes: 30~80g/L ammonium bicarbonate aqueous solution is added, standing sedimentation is dried after washing of precipitate.
2. the method according to claim 1 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: the following steps are included:
A, pre-treatment: salt acid soak platinum or platinum-rhodium alloy are used, is washed after taking-up, then be placed into acid solution;The acid is molten Liquid is the mixed solution of concentrated hydrochloric acid and concentrated nitric acid;
B, it dissolves: system temperature being risen into 95~105 DEG C of sufficiently reactions, then sufficiently drives nitric acid away with concentrated hydrochloric acid, is then diluted to Solution 40~60g/L containing noble metal;
C, it restores: system temperature is risen to 82~85 DEG C, being alternately added concentration is that 30~50g/L polyvinylpyrrolidone ethyl alcohol is molten Liquid and hydrazine hydrate sufficiently react, and then plus alkali neutralization is to neutrality;
D, it post-processes: 40~60g/L ammonium bicarbonate aqueous solution is added, standing sedimentation is dried after washing of precipitate.
3. the method according to claim 1 or 2 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: in step B, institute State after driving nitric acid away further includes that water is added to drive a large amount of hydrochloric acid away before dilute solution.
4. the method according to claim 1 or 2 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: in step A, institute The size for stating platinum or platinum-rhodium alloy is long 400mm or less, width 150mm or less, thickness 0.2mm or less.
5. the method according to claim 3 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: in step A, the platinum The size of gold or platinum-rhodium alloy is long 400mm or less, width 150mm or less, thickness 0.2mm or less.
6. the method according to claim 1 or 2 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: in step A, institute Stating hydrochloric acid is that concentrated hydrochloric acid and water are formulated according to 1 ︰ 2~8 of volume ratio.
7. the method according to claim 3 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: in step A, the salt Acid is that concentrated hydrochloric acid and water are formulated according to 1 ︰ 2~8 of volume ratio.
8. the method according to claim 1 or 2 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: in step A, institute Stating acid solution is that concentrated hydrochloric acid and concentrated nitric acid are formulated according to 2~8 ︰ 1 of volume ratio.
9. the method according to claim 3 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: in step A, the acid Solution is that concentrated hydrochloric acid and concentrated nitric acid are formulated according to 2~8 ︰ 1 of volume ratio.
10. the method according to claim 2 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: described in step B It is diluted to solution 50g/L containing noble metal.
11. the method according to claim 3 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: described in step B It is diluted to solution 50g/L containing noble metal.
12. the method according to claim 2 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: described in step C The concentration of polyvinylpyrrolidone ethanol solution is 40g/L.
13. the method according to claim 3 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: described in step C The concentration of polyvinylpyrrolidone ethanol solution is 40g/L.
14. the method according to claim 2 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: described in step D The concentration of ammonium bicarbonate aqueous solution is 50g/L.
15. the method according to claim 3 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: described in step D The concentration of ammonium bicarbonate aqueous solution is 50g/L.
16. the method according to claim 1 or 2 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: in step C, institute The additional amount for stating polyvinylpyrrolidone ethanol solution is 1~1.1L/kg noble metal;The additional amount of the hydrazine hydrate be 0.7~ 0.8L/1kg noble metal;In step D, the additional amount of the ammonium bicarbonate soln is 2.3~2.5L/1kg noble metal.
17. the method according to claim 3 for preparing platinum powder or platinum-rhodium alloy powder, it is characterised in that: described in step C The additional amount of polyvinylpyrrolidone ethanol solution is 1~1.1L/kg noble metal;The additional amount of the hydrazine hydrate be 0.7~ 0.8L/1kg noble metal;In step D, the additional amount of the ammonium bicarbonate soln is 2.3~2.5L/1kg noble metal.
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