Method for preparing palladium chloride by utilizing inactivated palladium nitrate

A technology of palladium nitrate and palladium chloride, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum halides, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, etc., can solve environmental problems. Heavy pollution, melting of palladium nitrate, high energy consumption of nitric acid, etc.

Active Publication Date: 2022-01-11
SHENYANG RES INST OF NONFERROUS METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Palladium nitrate is used as analytical reagent and oxidizing agent, and is also used for the separation of chlorine and iodine; but palladium nitrate is easy to absorb moisture, and if it is improperly stored, it is very easy to cause phenomena such as melting and deactivation of palladium nitrate. The current treatment method after dea

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Take 100 g of deactivated palladium nitrate and soak it in 500 ml of deionized water at 95°C for 10 min. Heat the palladium nitrate treatment solution at 100°C, and when steam appears from the solution, add 5 mL of perchloric acid solution into the system and stir. Then continue to heat, repeat 5 times, touch the bottom with a glass rod without solid insoluble matter, concentrate at 100°C for 45 min; maintain the temperature, add 15ml of hydrochloric acid and continue to concentrate at 110°C until the palladium nitrate solution is concentrated until a layer of crystals appears on the liquid surface. After the membrane, add 50 mL hydrochloric acid, repeat 5 times. After that, it was placed in a constant temperature water bath at 85°C, cured for 10 hours, ground, bottled, and assayed.

[0050] result:

[0051] Palladium nitrate conversion rate: 99.99%;

[0052] Product palladium chloride mass: 67 g;

[0053] Product palladium content: 59.6%;

[0054] Hydrochloric aci...

Embodiment 2

[0056] Take 100 g of deactivated palladium nitrate and soak it in 450 ml of deionized water at 100°C for 9 min. Heat the palladium nitrate treatment solution at 110°C, and when steam appears from the solution, add 6 mL of perchloric acid solution into the system and stir. Then continue heating, repeat 6 times, touch the bottom with a glass rod, concentrate at 120°C for 35 min; add 15ml hydrochloric acid to the palladium nitrate solution and concentrate at 110°C until a layer of crystal film appears on the liquid surface, add 70 mL hydrochloric acid, repeat 3 times. After that, it was placed in a constant temperature water bath at 95°C, cured for 8 hours, ground, bottled, and assayed.

[0057] result:

[0058] Palladium nitrate conversion rate: 99.99%;

[0059] Product palladium chloride mass: 68 g;

[0060] Product palladium content: 59.7%;

[0061] Hydrochloric acid insoluble test: qualified.

Embodiment 3

[0063] Take 100 g of deactivated palladium nitrate and soak it in 500 ml of deionized water at 100 °C for 8 min. Heat the palladium nitrate treatment solution at 110°C, and when steam appears from the solution, add 7.5 mL of perchloric acid solution into the system and stir. Then continue to heat, repeat 7 times, touch the bottom with a glass rod, concentrate at 110°C for 40 min; add 15ml of hydrochloric acid to the palladium nitrate solution and concentrate at 110°C until a layer of crystal film appears on the liquid surface, then add 60 mL of hydrochloric acid, repeat 4 times. After that, it was placed in a constant temperature water bath at 90°C, cured for 10 hours, ground, bottled, and assayed.

[0064] result:

[0065] Palladium nitrate conversion rate: 99.99%;

[0066] Product palladium chloride mass: 67.3 g;

[0067] Product palladium content: 59.7%;

[0068] Hydrochloric acid insoluble test: qualified.

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Abstract

The invention belongs to the technical field of precious metal metallurgy, and particularly relates to a method for preparing palladium chloride from inactivated palladium nitrate. The preparation method comprises the four steps of pretreatment of inactivated palladium nitrate, catalysis of dissolution of perchloric acid, removal of nitrate via hydrochloric acid and curing forming. According to the method, the inactivated palladium nitrate is pretreated, so impurities can be effectively removed, the purpose of wetting can be achieved, a follow-up palladium nitrate dissolution rate is increased, and palladium chloride yield is increased; perchloric acid is used for completely dissolving palladium nitrate, meanwhile, the activity of the palladium solution can be improved, and a good foundation is laid for improving a palladium nitrate conversion rate; and with the method disclosed by the invention, the inactivated palladium nitrate can be directly converted into the product palladium chloride with equivalent activity, a brand new method for converting the palladium nitrate into the palladium chloride is provided, and the palladium content of the converted palladium chloride is more than or equal to 59.6%.

Description

technical field [0001] The invention belongs to the technical field of precious metal metallurgy, and in particular relates to a method for preparing palladium chloride by using deactivated palladium nitrate. Background technique [0002] Palladium nitrate is used as analytical reagent and oxidizing agent, and is also used for the separation of chlorine and iodine; but palladium nitrate is easy to absorb moisture, and if it is improperly stored, it is very easy to cause phenomena such as melting and deactivation of palladium nitrate. The current treatment method after deactivation of palladium nitrate Mainly, palladium nitrate is reduced to palladium powder and then re-dissolved. In this method, metal palladium has a long dissolution time and a low dissolution rate. A large amount of nitric acid is required to dissolve metal palladium once, resulting in large energy consumption and heavy environmental pollution. [0003] The present invention uses deactivated palladium nitr...

Claims

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Application Information

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IPC IPC(8): C01G55/00
CPCC01G55/005Y02P10/20
Inventor 王大维李岩松徐飞飞肖雪关雪峰刘冬梅王靖涵
Owner SHENYANG RES INST OF NONFERROUS METALS
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