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Preparation method of high-purity sponge palladium

A sponge palladium and high-purity technology is applied in the field of preparation of high-purity palladium sponge, which can solve the problems of long process flow and complicated steps, and achieve the effects of short process flow, simple steps and strong adaptability of raw materials.

Active Publication Date: 2020-03-24
XINJIANG RES INST OF NON FERROUS METALS
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  • Description
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AI Technical Summary

Problems solved by technology

However, several methods listed above all have problems such as long technological process and cumbersome steps.
[0004] Therefore, the research on how to reduce the loss on ignition of palladium powder in a more convenient way is still a hot spot and difficulty in this industry, and there are few research reports on this aspect at present

Method used

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  • Preparation method of high-purity sponge palladium
  • Preparation method of high-purity sponge palladium

Examples

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preparation example Construction

[0039] Such as figure 1 Shown, be the preparation method of high-purity palladium sponge of the present invention, it comprises steps:

[0040] S1: Dissolving in aqua regia: adding the crude palladium raw material into aqua regia, reacting at room temperature for 0.5-4h, dissolving the crude palladium raw material in aqua regia, filtering to obtain clear liquid A1 and solid slag B1;

[0041] S2: Nitrate removal: heat up the clear solution A1 to 40°C-100°C, add concentrated hydrochloric acid to remove the nitrate, and filter to obtain the clear liquid A2 and solid slag B2;

[0042] S3: Precipitating palladium: adding a precipitating agent and an oxidizing agent to the clear liquid A2, reacting at room temperature for 4-24 hours, and filtering to obtain clear liquid A3 and solid slag B3;

[0043] S4: The first ammonification: disperse the solid slag B3 into an appropriate amount of pure water, raise the temperature to 45°C-95°C and add ammonia water, ammoniate until the pH valu...

Embodiment 1

[0056] The present embodiment takes the crude palladium of the output of factory 1 as raw material (palladium content 83.7%), prepares high-purity sponge palladium, comprises steps:

[0057] ①The crude palladium is dissolved and filtered with aqua regia at room temperature;

[0058] ② Add concentrated hydrochloric acid to the filtrate at 80°C to catch the nitrate, and filter;

[0059] ③ Add precipitant and oxidant to the filtrate at room temperature, micro-oxidize and precipitate for 12 hours, and filter;

[0060] ④ Add water to the filter residue to make slurry, use ammonia water for the first ammoniation temperature of 65°C, keep warm for 2 hours until the pH value reaches 8-10, and filter;

[0061] ⑤ The filtrate is acidified with hydrochloric acid at room temperature to a pH value of 0.5-2, and filtered;

[0062] ⑥ Add water to the filter residue to adjust the slurry, use ammonia water for the second ammoniation, the ammoniation temperature is 65°C, keep warm for 2 hours...

Embodiment 2

[0067] The present embodiment takes the crude palladium of the output of factory 2 as raw material (palladium content 98.01%), prepares high-purity sponge palladium, comprises steps:

[0068] ①The crude palladium is dissolved and filtered with aqua regia at room temperature;

[0069] ②Add concentrated hydrochloric acid to the filtrate at 90°C to catch the nitrate, and filter;

[0070] ③ Precipitant and oxidant in the filtrate at normal temperature, micro-oxidized and precipitated for 8 hours, and filtered;

[0071] ④ Add water to the filter residue to adjust the slurry, use ammonia water for the first ammoniation temperature of 75°C, keep warm for 1h until the pH value reaches 8-10, and filter;

[0072] ⑤ The filtrate is acidified with hydrochloric acid at room temperature to a pH value of 0.5-2, and filtered;

[0073] ⑥ Add water to the filter residue to adjust the slurry, use ammonia water for the second ammoniation, the ammoniation temperature is 75°C, keep it warm for 1 ...

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Abstract

The invention discloses a preparation method of high-purity sponge palladium. The preparation method comprises the following steps that a palladium-containing material with the palladium content of greater than or equal to 35% is used as a raw material, the raw material is dissolved by using aqua regia at normal temperature, and filtration is carried out; the filtrate is heated, HCL is added to the heated filtrate for denitration, and filtration is carried out; a precipitant and an oxidizing agent are added in the filtrate, a precipitate is generated after normal temperature reaction, and filtration is carried out; water is added to filter residues for pulping, ammonization is carried out until the pH value is 8-10, and filtration is carried out; hydrochloric acid is added to the filtratefor acidification until the pH value is 0.5-2, and filtration is carried out; water is added to filter residues for pulping, so that the palladium content is 30-120 g / L, ammonization is carried out until the pH value is 8-10, and filtration is carried out; a reducing agent is added to the filtrate for reduction, cooling and filtration are carried out after reaction, and filter residues are dried to obtain palladium powder; and the palladium powder is dissolved by using nitric acid, filtration is carried out, denitration, oxidizing, ammonization, acidification, re-ammonization and reduction treatment are carried out on the filtrate repeatedly, filtration is carried out to obtain filter residues, and vacuum drying is carried out to obtain the high-purity sponge palladium with the content ofgreater than or equal to 99.95% and the burn loss rate of less than or equal to 0.1%. According to the preparation method of the high-purity sponge palladium, the raw material has high adaptability, the technological process is short, a national standard product can be prepared without calcining, so that the amount of waste water and waste gas is reduced, the loss of precious metal is reduced, andthe enterprise benefit is improved.

Description

technical field [0001] The invention relates to a preparation method of high-purity palladium sponge, belongs to the technical field of precious metal hydrometallurgy and refining, and in particular relates to a preparation method of high-purity palladium sponge. Background technique [0002] Palladium is a noble metal with high density, high melting point, and elegant color value. It is silvery white, and high-purity palladium powder is grayish white. It has good ductility and plasticity. At room temperature, 1 volume of palladium sponge can absorb 900 volumes of hydrogen gas, and hydrogen gas can pass through palladium freely. It has the ability to selectively pass through hydrogen gas. It is an important material for hydrogen storage and hydrogen permeability. At present, palladium is mainly used as a catalyst. In particular, hydrogenation or dehydrogenation catalysts can also be used to make resistance wires, alloys for watches, etc. [0003] At present, there are thre...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B11/00
CPCC22B7/006C22B11/04Y02P10/20
Inventor 曹毅臣邢诗雨刘力伊新辉孙哲王雪泓
Owner XINJIANG RES INST OF NON FERROUS METALS
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