Synthetic method of palladium tetra-ammino sulfate

A technology of tetraammonium palladium sulfate and synthesis method, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve the problem that product yield and quality are difficult to control, and the process flow is long. , excessive sulfuric acid and other problems, to achieve the effect of high product yield, good selectivity and large exchange capacity

Active Publication Date: 2014-01-22
GUIYAN RESOURCE YIMEN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 ammonium sulfate is produced, which is mixed with tetraammonia palladium sulfate. An additional product separation process is required, and the process flow is long. Product yield and quality are more difficult to control

Method used

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  • Synthetic method of palladium tetra-ammino sulfate

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example 1

[0024] Take 200 g of reagent palladium chloride in a flask, add 600 mL of reagent grade ammonia water, heat in a water bath, keep the temperature constant at 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 the temperature for 3 hours, a large amount of solids precipitated out in the flask. The solid was separated by filtration, washed with pure water, the filtrate and washing water were collected for treatment, 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-yellow solid.

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

example 2

[0033] Take 200 g of reagent palladium chloride in a flask, add 500 mL of reagent grade ammonia water, heat in a water bath, keep the temperature constant at 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 the temperature for 3 hours, a large amount of solids precipitated out in the flask. The solid was separated by suction filtration, washed with a small amount of water, the filtrate and washing water were collected for treatment, 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-yellow solid.

[0034] The solid was dissolved in water, and the concentration of palladium in the solution was adjusted to be 10 g / 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 through the resin slowly at...

example 3

[0042] Take 1000g of palladium chloride as a reagent in a 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 are dissolved, and a light yellow transparent solution is obtained. Adjust the temperature to 85°C and keep the temperature for 5 hours, a large amount of solids precipitated out in the flask. The solid was separated by suction filtration, washed with water, the filtrate and washing water were collected for treatment, the solid was transferred to an oven, the temperature was controlled at 100°C, and the temperature was kept constant for 4 hours to obtain an orange-yellow solid.

[0043] The solid is dissolved in water, and the concentration of palladium in the solution is adjusted to be about 20 g / 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 through the resin slowly at a flow rat...

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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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Patent Type & Authority Patents(China)
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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