Synthetic method of palladium tetra-ammino sulfate

A tetraammonium palladium sulfate and synthesis method technology, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve the difficult control of product yield and quality, and the increase of by-products , long technological process and other issues, to achieve high product yield, less side reactions, and good selectivity

Active Publication Date: 2012-11-21
GUIYAN RESOURCE YIMEN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process, a large amount of sulfuric acid needs to be used to drive away nitric acid. The excess of sulfuric acid is large, and the by-products increase. In addition, during the complexation process, a large amount of

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  • Synthetic method of palladium tetra-ammino sulfate

Examples

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Example Embodiment

[0023] Example 1

[0024] Take 200 g of reagent palladium chloride into the flask, add 600 mL of reagent grade ammonia water, heat in a water bath at a constant temperature of 50°C, stir for 30 minutes, all the solids are dissolved, and a light yellow transparent solution is obtained. Adjust the temperature to 85°C and keep it for 3 hours. A large amount of solids precipitated in the flask. The solid was separated by filtration, washed with pure water, the filtrate and washing water were collected for processing, the solid was transferred to an oven, the temperature was controlled at 100°C, and the temperature was kept constant for 2 hours to obtain an orange solid.

[0025] The solid is dissolved by adding water, and the concentration of palladium in the solution is adjusted to 5g / L. The volume of the ion exchange resin tube is 10L, and it is filled with about 7L of 201×7 anion exchange resin. The prepared solution flows slowly through the resin at a flow rate of 50mL / min. During...

Example Embodiment

[0032] Example 2

[0033] Take 200 g of reagent palladium chloride into the flask, add 500 mL of reagent grade ammonia water, heat in a water bath at a constant temperature of 50°C, stir for 30 minutes, all the solids are dissolved, and a light yellow transparent solution is obtained. Adjust the temperature to 85°C and keep it for 3 hours. A large amount of solids precipitated in the flask. The solid was separated by suction filtration, washed with a small amount of water, the filtrate and washing water were collected to be processed, and the solid was transferred to an oven, controlled at a temperature of 100°C, and kept constant for 2 hours to obtain an orange solid.

[0034] The solid is dissolved in water, and the concentration of palladium in the solution is adjusted to 10g / L. The volume of the ion exchange resin tube is 10L, and it is filled with about 7L of 201×7 anion exchange resin. The prepared solution flows slowly through the resin at a flow rate of 50mL / min. During th...

Example Embodiment

[0041] Example 3

[0042] Take 1000g of reagent palladium chloride into the flask, add 2000mL of reagent grade ammonia water, heat in a water bath, keep the temperature constant at 60°C, stir for 30 minutes, all the solids will be dissolved to obtain a light yellow transparent solution. Adjust the temperature to 85°C and keep it for 5 hours. A large amount of solids precipitated in the flask. The solid was separated by suction filtration, the solid was washed with water, the filtrate and washing water were collected to be processed, and the solid was transferred to an oven, controlled at a temperature of 100°C and kept constant for 4 hours to obtain an orange solid.

[0043] The solid is dissolved in water, and the concentration of palladium in the solution is adjusted to about 20g / L. The volume of the ion exchange resin tube is 10L, and it is filled with about 7L of 201×7 anion exchange resin. The prepared solution flows slowly through the resin at a flow rate of 200mL / min. Durin...

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Abstract

The invention discloses a synthetic method of palladium tetra-ammino sulfate, comprising the following steps of: (1) adding ammonia water in reagent level palladium chloride in order to dissolve palladium chloride; (2) concentrating and crystallizing the obtained solution, and drying the crystals to obtain orange solids; (3) confecting yellow solids into solution with a certain concentration; (4) flowing the solution through a negative ion exchange resin, exchanging repeatedly till Cl<-> ion cannot be detected in tail solution; (5) concentrating the exchanged solution to a certain concentration, adding sulfuric acid in a quantitative form, keeping on concentrating till crystals are generated; (6) separating out the crystals, re-crystallizing for 2-3 times, obtaining yellow crystals; and (7) drying crystals at a low temperature, so as to obtain faint yellow palladium tetra-ammino sulfate solids. The method has the following characteristics of simple process, few by-products, high product purity, and high product yield of more than 95%.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a synthesis method of tetraammonia palladium sulfate, and belongs to the coordination chemistry category. Background technique [0002] In order to manufacture parts with high stability and high wear resistance, it is usually necessary to deposit a layer of precious metals (such as gold plating, rhodium, palladium, etc.) on the coating. With the development of industrial technology, it is necessary to reduce the content of halogen elements in the plating solution. usage is increasing. [0003] Tetraammonia palladium sulfate is a new type of electroplating product, which is used for palladium plating in the electronics industry. It is mainly used for coating computer motherboards and network plugs, and manufacturing automotive catalytic crackers. Due to its high electroplating efficiency, halogen-free, clean and environmentally friendly, it can replace traditional halogen-containing...

Claims

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Application Information

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IPC IPC(8): C01G55/00
Inventor 贺小塘王欢韩守礼吴喜龙李勇李锟
Owner GUIYAN RESOURCE YIMEN
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