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Ammonia-palladium complex and preparing method thereof

A complex, ammonia palladium technology, applied in the field of ammonia palladium complex and its preparation, can solve the problems such as poor ability of electroplating solution or supplementary solution to counter ion salt, short service life of electroplating solution, low palladium content, etc. Facilitate large-scale production, increase service life, and increase the effect of palladium content

Inactive Publication Date: 2019-02-01
JINCHUAN GROUP LIMITED +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a kind of ammonia-palladium complex and preparation method thereof, to solve the problem that palladium content is lower in the existing four-ammonia palladium sulfate, and the ability of the prepared electroplating solution or supplementary liquid to counter ion salt is relatively poor, causing electroplating solution Problems with short lifespan

Method used

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Examples

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Effect test

preparation example Construction

[0032] A preparation method of ammonia palladium complex, comprising the steps of:

[0033] Step 1. Dissolving materials:

[0034] Using sponge palladium powder as raw material, add concentrated sulfuric acid with a mass fraction of 98% and concentrated nitric acid with a mass fraction of 68%, add 80-120mL of concentrated sulfuric acid to every 100g of sponge palladium powder, add 60-80mL of concentrated sulfuric acid to every 100g of sponge palladium powder Nitric acid, then heated to dissolve;

[0035] Step 2, preparation solution:

[0036] After the solution obtained in step 1 is heated at a temperature of 90-130°C to catch the nitrate, add deionized water to prepare solution A, and the concentration of palladium ions in solution A is 60-150g / L;

[0037] Step 3, pH adjustment:

[0038] Add ammonia water to the solution A to adjust the pH value to 7-10, and stir the reaction at room temperature for 0.5-1h;

[0039] Step 4, Precipitation and crystallization:

[0040] Add...

Embodiment 1

[0042] Weigh 100g of palladium sponge (Pd: 99.99%), add 80ml of concentrated sulfuric acid (mass fraction: 98%), 60ml of concentrated nitric acid (mass fraction: 68%), heat to 60°C and dissolve completely, then raise the temperature to 130°C to catch the nitric acid, Until no nitrogen oxide overflows. Add deionized water to prepare 1670ml of solution A, wherein the Pd content is 60g / L. Add an appropriate amount of ammonia water, adjust the pH to 10, stir for 30 minutes, and stop the reaction. Ammonia water 1000ml was added, the supernatant became colorless after stirring, the crystals were filtered, washed three times, and dried at 90°C for 8 hours to obtain the product with a yield of 95%, and the palladium content of the product was detected to be 48.23%.

Embodiment 2

[0044] Weigh 100g of palladium sponge (Pd: 99.99%), add 120ml of concentrated sulfuric acid (mass fraction: 98%), 80ml of concentrated nitric acid (mass fraction: 68%), heat to 80°C and dissolve completely, then heat up to 90°C to catch the nitric acid. Until no nitrogen oxide overflows. Add deionized water to prepare 670ml of solution A, wherein the Pd content is 150g / L. Add appropriate amount of ammonia water, adjust the pH value to 7, stir for 1 hour, and stop the reaction. Add 1000ml of ammonia water, the supernatant liquid becomes colorless after stirring, the crystals are filtered, washed three times, and dried at 90°C for 8 hours to obtain the product, the yield is 98%, and the palladium content of the product is detected to be 49.95%.

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PUM

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Abstract

The invention discloses an ammonia-palladium complex and a preparing method thereof and belongs to the technical field of chemical synthesis. The general formula of the ammonia-palladium complex is Pd(NH3)x Pd(SO4)2, and x=0.9-2.0. The preparing method comprises the steps of dissolving materials, preparing a solution, adjusting the pH value and carrying out sediment crystallization. The palladiumcontent of the ammonia-palladium complex reaches up to 48-50% and is obviously increased compared with that of electroplating palladium (Pd is about 39% in tetraamminepalladium sulfate) widely adoptedat present, the adding amount of counter ions can be correspondingly reduced when the ammonia-palladium complex is used for preparing palladium-contained electroplating fluid or replenishing fluid, and thus the service life of electroplating fluid can be prolonged. The productivity of the preparing method of the ammonia-palladium complex can reach to 98% which is close to 100%, no byproduct is generated, the operation flow is short, the reaction temperature is low, the production cost of electroplating palladium salt can be further reduced, and mass production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to an ammonia-palladium complex and a preparation method thereof. Background technique [0002] In the field of connectors, electroplating palladium or palladium-nickel alloy combined with thin gold process has been used for many years instead of hard gold plating. Commonly used palladium electroplating main salts are generally compounds containing ammonia or organic amines, as described in Chinese patents CN101709462A, CN1289716C, CN1249366A, and CN1420947A. The conventional palladium-nickel electrolyte contains chloride, which will cause strong corrosion to the substrate or electroplating equipment. Chloride ions may also cause cracks in the electroplated parts and affect the quality of electroplating. [0003] Tetraammonia palladium sulfate is a novel palladium salt for electroplating. Due to its high electroplating efficiency, cleanness and environmental ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D3/50
CPCC25D3/50
Inventor 张静曹笃盟刘国旗白延利马骞任志勇王红梅李欢郅欢欢何艳吴芳
Owner JINCHUAN GROUP LIMITED
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