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Preparation method of tetraammine palladium hydrogen carbonate compound

A technology of palladium compound and bicarbonate, which is applied in the field of preparation of tetraammine palladium bicarbonate compound, can solve the problems of complex preparation process and high recycling cost, and achieve the effects of simple process, reduced production cost and reduced dosage

Active Publication Date: 2019-01-11
JINCHUAN GROUP LIMITED +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of preparation method of bicarbonate tetraammonium palladium compound, to solve the problems of complex preparation process, high product yield and high recovery cost

Method used

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Examples

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preparation example Construction

[0035] A kind of preparation method of bicarbonate tetraammine palladium compound, comprises the steps:

[0036] Step 1. Dissolving materials:

[0037] Use sponge palladium powder as raw material, add concentrated nitric acid and heat to dissolve at 50-80°C, preferably 60-70°C, wherein the molar ratio of concentrated nitric acid to palladium is 3.0-4.0:1, preferably 3.5:1, heat to dissolve and react The nitrogen oxides produced during the process are absorbed with 30% sodium hydroxide aqueous solution;

[0038] Step 2. Remove impurities:

[0039] The solution obtained in step 1 is filtered to remove insoluble solid impurities;

[0040] Step 3, nitrate concentration:

[0041] Heat the filtered palladium nitrate solution and concentrate it under vacuum to catch the nitrate. The concentration temperature is 110°C. Stop heating when it is concentrated until a layer of crystal film appears on the surface of the system and no obvious nitrogen oxides are produced. When the tempera...

Embodiment 1

[0047] Accurately weigh 10.0g of palladium sponge (Pd: 99.99%), add 19.6ml of concentrated nitric acid (mass fraction: 65%) under stirring, and raise the temperature to 50°C. until solid. Add powdered tetraammonium palladium nitrate into 20ml of ammonia water (mass fraction: 25%) in batches, maintain the pH of the system at 10.5 and stir at 30°C for 24 hours. The excess ammonia, with the volatilization of ammonia, the precipitation of tetraammonium palladium nitrate gradually dissolves in the system. When the temperature of the system drops to 40°C, 520ml of sodium bicarbonate solution (mass fraction: 3%) is added dropwise and boiled. At this time, the system Gradually tetraammine palladium bicarbonate precipitated out. After stirring for 1 hour, the system basically reacted completely. After the crystals were filtered, they were washed 4 times with deionized water and dried at 50°C for 8 hours to obtain a beige product. The yield of the target product was 95.2%. The metal pa...

Embodiment 2

[0049]Accurately weigh 10.0g of palladium sponge (Pd: 99.99%), add 19.6ml of concentrated nitric acid (mass fraction: 65%) under stirring, and heat up to 60°C. until solid. Add powdered tetraammonium palladium nitrate to 20ml of ammonia water (mass fraction: 25%) in batches, maintain the pH of the system at 11.5 and stir at 30°C for 24 hours. The excess ammonia, with the volatilization of ammonia, the precipitation of tetraammonium palladium nitrate gradually dissolves in the system. When the temperature of the system drops to 40°C, 520ml of sodium bicarbonate solution (mass fraction: 3%) is added dropwise and boiled. At this time, the system Gradually tetraammine palladium bicarbonate precipitated out. After stirring for 1 hour, the system basically reacted completely. After the crystals were filtered, they were washed 4 times with deionized water and dried at 50°C for 8 hours to obtain a beige product. The yield of the target product was 95.3%. The metal palladium content o...

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Abstract

The invention discloses a preparation method of a tetraammine palladium hydrogen carbonate compound, and belongs to the field of synthesis of electroplating compounds. The preparation method comprisesthe steps of material solution, impurity removal, saltpeter concentration, tetraammine palladium nitrate preparation and precipitation crystallization. According to the preparation method, during theprocess in which palladium nitrate is adopted as a starting material to react with ammonium hydroxide to prepare tetraammine palladium nitrate, ammonium hydroxide is added to synthesize tetraammine palladium nitrate, the intermediate product, tetraammine palladium nitrate, react with a sodium bicarbonate solution, a final product, tetraammine palladium hydrogen carbonate is obtained, the chemicalformula is [Pd(NH3)4](HCO3)2, and the palladium content of the target compound is 35% or above; and when the tetraammine palladium hydrogen carbonate compound is utilized to prepare a palladium replenishing liquid or prepare an electroplating liquid, the system acidity does not change, the addition amount of counter ions can be decreased, and the service life of the electroplating liquid can be greatly prolonged.

Description

technical field [0001] The invention belongs to the field of synthesis of electroplating chemicals, and in particular relates to a preparation method of tetraammine palladium bicarbonate compound. Background technique [0002] In the field of palladium-nickel alloy bonding or connector palladium plating, the main palladium electroplating salts used for many years are mostly compounds containing halogen or sulfate and nitrate, which are reported in Chinese patents CN1420947A, CN1289716C, CN101709462A, and CN1249366A. Most of the palladium-nickel electrolytes that have been used for many years contain chlorides, which will cause serious corrosion to the electroplating equipment and the substrate. quality. Tetraammine palladium bicarbonate is one of the latest palladium salts for electroplating. Due to its clean and environmentally friendly application and very high electroplating efficiency, it is gradually applied to the low-ammonia electroplating process of palladium and ni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D3/50
CPCC25D3/50
Inventor 常全忠曹笃盟任志勇张静白延利刘国旗马骞王红梅李欢郅欢欢何艳吴芳
Owner JINCHUAN GROUP LIMITED
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