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The synthetic method of tetraammine palladium sulfate

A tetraammine 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 reaction, difficult to clean, difficult to separate and other problems, to achieve the effect of high reaction yield, high product purity and simple operation

Active Publication Date: 2016-07-06
烟台招金励福贵金属股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method introduces chloride ions and nitrate ions in the process of pickling and nitrate removal, but the chloride ions and nitrate ions are difficult to remove, and the residual chloride ions and nitrate ions form impurities such as dichlorotetraammonium palladium and ammonium nitrate with ammonia water. And difficult to separate, the yield is not high
Patent CN102616869A takes palladium chloride as the starting material to react with ammonia water to generate dichloro tetraammine palladium, and then quantitatively reacts with silver sulfate to generate sulfuric acid tetraammine palladium, but the solubility of silver sulfate is not good, and it reacts with dichloro tetraammine palladium The reaction is difficult to carry out, so the yield is not high

Method used

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  • The synthetic method of tetraammine palladium sulfate
  • The synthetic method of tetraammine palladium sulfate
  • The synthetic method of tetraammine palladium sulfate

Examples

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Embodiment 1

[0025] The synthetic method of tetraammine palladium sulfuric acid, weigh 10.00g (94.0mmol) palladium powder with beaker, add 200mL aqua regia in batches, cover watch glass and let palladium powder dissolve at 115 ℃ for 1h, then take Continue heating and add 10mL of hydrochloric acid with a mass fraction of 37% dropwise to facilitate the escape of nitrogen oxides. During the heating process, the liquid level is maintained at 20mL (the purpose of maintaining the liquid level is to prevent the palladium compound from being precipitated and then oxidized into Palladium oxide), if the liquid level drops, then add pure water to keep the solution volume constant), until no more yellow-brown gas escapes in the beaker, stop heating, and finish nitrating; after nitrating is completed, boil the solution volume to 10mL, Add 20mL of 30%wt sodium hydroxide solution, stir evenly; use a sand core funnel to suction filter, and wash the filter residue several times with pure water, recover the ...

Embodiment 2

[0029] Weigh 150.00 (1409.6mmol) palladium powder into a 1000mL beaker, add 500mL aqua regia in batches, cover the watch glass and heat at 130°C for 0.5h to dissolve the palladium powder, then take off the watch glass and continue heating and add dropwise from time to time Mass fraction is 10mL of hydrochloric acid of 37% to be beneficial to the escape of nitrogen oxides (during the heating process, the liquid level remains on 200mL, and keeping the liquid level is to prevent the palladium compound from being precipitated and then oxidized into palladium oxide). Add pure water to keep the volume of the solution constant, if the liquid level drops, add pure water to keep the volume of the solution constant), until no more yellow-brown gas escapes in the beaker, stop heating, and finish nitrating; The volume of the solution was boiled to 100mL, and 200mL of 30%wt sodium hydroxide solution was added, and stirred evenly; the filter residue was washed several times with pure water, ...

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Abstract

The invention discloses a synthetic method of palladium tetramminosulfate. The synthetic method comprises the following steps of: (1) dissolving palladium powder by using chloroazotic acid, and removing nitrate to obtain palladium chloride; (2) reacting the palladium chloride with sodium hydroxide to generate palladium hydroxide; (3) reacting the palladium hydroxide with measured sulfuric acid to generate palladium sulfate; (4) reacting the palladium sulfate with ammonium hydroxide to generate a palladium tetramminosulfate compound. The synthetic method has the advantages that the palladium powder is used as a starting raw material, and ([Pd(NH3)4]SO4), the operation is simple, the yield is high, and the obtained product has high purity.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and in particular relates to a synthesis method of a palladium complex, namely tetraammine palladium sulfate. Background technique [0002] Tetraammine palladium (II) compounds ([Pd(NH 3 ) 4 ]X 2 ) is an important class of palladium compounds, widely used in chemical catalysis and electroplating industries. Among them, tetraammine palladium (II) sulfate ([Pd(NH 3 ) 4 ] SO 4 ) is a new type of electroplating main salt, which has been widely used in the electronics industry for palladium plating due to its high electroplating efficiency, cleanness and environmental protection. In addition, tetraammine palladium (II) sulfate can also be used as a precursor compound of supported palladium catalyst due to its good water solubility and relatively stable chemical properties of the solution. [0003] The conventional synthesis method of tetraammine palladium (II) sulfate is to pre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G55/00
Inventor 朱振华李三梅
Owner 烟台招金励福贵金属股份有限公司