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Process for separating and purifying spongy platinum from ammonium chloroplatinate

A technology of ammonium chloroplatinate and sponge platinum, which is applied in the field of separation and purification of platinum metal, can solve the problems of excessive palladium in sponge platinum, and achieve the effects of overcoming palladium exceeding the standard, short cycle time and wide material adaptability

Active Publication Date: 2019-10-29
JIANGXI COPPER
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] The purpose of the present invention is exactly to aim at the above-mentioned problem existing in the technical process of refining platinum at present, a kind of platinum refining process method is provided, the present invention adopts acidic system sodium chlorate to oxidize and dissolve crude ammonium chloroplatinate, concentrates hydrolysis to remove impurity process, avoids Operations such as ammonium chloroplatinate calcining and aqua regia dissolving have overcome a series of problems such as insufficient palladium in sponge platinum caused by incomplete nitration, and the invention can obtain sponge platinum with a purity higher than 99.99%.

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  • Process for separating and purifying spongy platinum from ammonium chloroplatinate

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Effect test

Embodiment 1

[0043] (1) Weigh 500g of crude ammonium chloroplatinate solid, the mass fraction of ammonium chloroplatinate in the crude ammonium chloroplatinate is 92.6%, add 2L of water to slurry to obtain slurry, add hydrochloric acid to make the acidity reach 35g / L , heat the slurry to 93°C, add 200g of sodium chlorate while stirring, stir at constant temperature to completely dissolve the ammonium chloroplatinate solid, cool the solution to 60°C and filter;

[0044] (2) Heat the filtrate to a constant temperature of 95°C, add hydrochloric acid while stirring to catch chlorine, until no chlorine gas emerges, and the acidity reaches 3mol / L, the solution is cooled to 50°C, and 100g of ammonium chloride is added to precipitate platinum. Stir for 20 minutes, keep the stirring speed at 30 r / s, let it stand for clarification for 30 minutes, filter platinum yellow, wash with 3mol / L hydrochloric acid, 50g / L ammonium chloride mixture until the washing liquid is clear;

[0045] (3) Slurry the obta...

Embodiment 2

[0051] (1) Weigh 500g of crude ammonium chloroplatinate solid, the mass fraction of ammonium chloroplatinate in the crude ammonium chloroplatinate is 48.36%, add 2L of water to slurry to obtain a slurry, add hydrochloric acid to make the acidity reach 35g / L , heat the slurry to 93°C, add 150g of sodium chlorate while stirring, stir at constant temperature to completely dissolve the ammonium chloroplatinate solid, cool the solution to 60°C and filter;

[0052] (2) Heat the filtrate to a constant temperature of 95°C, add hydrochloric acid while stirring to catch chlorine, until no chlorine gas emerges, and the acidity reaches 3mol / L, the solution is cooled to 50°C, and 80g of ammonium chloride is added to precipitate platinum. Stir for 20 minutes, keep the stirring speed at 30 r / s, let it stand for clarification for 30 minutes, filter platinum yellow, wash with 3mol / L hydrochloric acid, 50g / L ammonium chloride mixture until the washing liquid is clear;

[0053] (3) Slurry the ob...

Embodiment 3

[0059] (1) Weigh 500g of crude ammonium chloroplatinate solid, the mass fraction of ammonium chloroplatinate in the crude ammonium chloroplatinate is 12.31%, add 2L of water to slurry to obtain a slurry, add hydrochloric acid to make the acidity reach 35g / L , heat the slurry to 93°C, add 35g of sodium chlorate while stirring, stir at constant temperature to completely dissolve the ammonium chloroplatinate solid, cool the solution to 60°C and filter;

[0060] (2) Heat the filtrate to a constant temperature of 95°C, add hydrochloric acid while stirring to catch chlorine, until no chlorine gas emerges, and the acidity reaches 3mol / L, the solution is cooled to 50°C, and 20g of ammonium chloride is added to precipitate platinum. Stir for 20 minutes, keep the stirring speed at 30 r / s, let it stand for clarification for 30 minutes, filter platinum yellow, wash with 3mol / L hydrochloric acid, 50g / L ammonium chloride mixture until the washing liquid is clear;

[0061] (3) Slurry the obt...

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Abstract

The invention provides a process for separating and purifying spongy platinum from ammonium chloroplatinate. The process includes the steps that water is added into crude ammonium chloroplatinate forpulpifying, hydrochloric acid is supplemented, the temperature is increased to 90-95 DEG C, sodium chlorate is added until solids are completely dissolved, the temperature is increased to 95-100 DEG Cfor chlorine driving, and cooling and filtering are carried out; after filtrate is heated to 40-65 DEG C, ammonium chloride is added for platinum settling, and filtering is carried out after coolingis completed; refining is repeated once, and NaOH is added into a secondary platinum dissolution for hydrolysis; the acidity of the hydrolyzed filtrate is adjusted back, and dimethylglyoxime is supplemented for palladium removing; and ammonium chloride is added into the filtrate, filtering is carried out, pure ammonium chloroplatinate is obtained and reduced with hydrazine hydrate, high-purity platinum powder is obtained, the high-purity platinum powder is boiled with nitric acid, and spongy platinum powder can be obtained. By means of the process, the spongy platinum meeting SM-99.99 can be stably generated, the flow of the process is simple, the raw material adaptability is high, the platinum recovery rate is high, the operation such as ammonium chloroplatinate calcination and aqua regiadissolution is further avoided, and a series of problems such as standard exceeding of platinum in the spongy platinum caused by incomplete nitrate driving are solved.

Description

technical field [0001] The invention belongs to the field of separation and purification of platinum metal, and in particular relates to a process for separating and purifying 99.99% sponge platinum from ammonium chloroplatinate materials. Background technique [0002] Platinum sponge is a chemical substance, black powder, soluble in aqua regia; insoluble in water and inorganic acids. Density: 5.78g / ml, melting point: 1769°C, boiling point: 3827°C, platinum sponge is mainly used to make catalysts. There are many platinum refining processes, and the main methods currently used in production are: aqua regia dissolution-ammonium chloride repeated precipitation method, oxidation hydrolysis method, carrier hydrolysis method, carrier hydrolysis-ion exchange method, alkali dissolution-reduction method, reduction- Dissolution method, reduction dissolution-ammonium chloride repeated precipitation method and extraction and refining method, etc. Based on the aqua regia dissolution-am...

Claims

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Application Information

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IPC IPC(8): C22B3/44C22B3/22C22B11/00
CPCC22B3/22C22B3/44C22B11/04Y02P10/20
Inventor 孙敬韬黄绍勇刘永平陈善文夏兴旺
Owner JIANGXI COPPER
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