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Synthesis method of tetraamminepalladium sulfate (II)

A technology of tetraammine palladium sulfate and tetraammine palladium dichloride, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve the problem of increased by-products and excessive sulfuric acid Many, increase costs and other issues, to achieve the effect of simple operation

Inactive Publication Date: 2016-08-10
TITAN ADVANCED MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the process, sulfuric acid is needed to drive away the nitric acid in the palladium nitrate solution to obtain palladium sulfate. The excessive sulfuric acid will increase the by-products, which will produce a large amount of ammonium sulfate, which will affect the quality of the product.
Chinese patent (201210315379.6) adopts palladium chloride to react with ammonia water to generate dichloro tetraammine palladium solution, removes chloride ions through repeated anion exchange, and then reacts with sulfuric acid to generate tetraammine palladium sulfate, which can effectively remove chloride ions , to avoid the formation of ammonium sulfate by-products, but it needs to undergo ion exchange many times, which increases the workload, and some precious metals will be adsorbed on the ion resin, which increases the workload of subsequent recovery
Chinese patent (201210099564.6) adopts the reaction of palladium chloride and ammonia water to generate dichlorotetraammine palladium (II), and then reacts with silver sulfate to generate tetraammine palladium (II) sulfate. The method is simple to operate and no ammonium sulfate by-product is formed. , but the use of silver sulfate in production increases the cost, and there will be a certain amount of palladium residue in the silver chloride by-product, which increases the difficulty for the future recovery of precious metals
Chinese patent (201310312422.8) uses palladium chloride as a raw material, first generates palladium hydroxide with sodium hydroxide, reacts with sulfuric acid to generate palladium sulfate, and reacts palladium sulfate with ammonia water to generate sulfuric acid tetraammine palladium (II). Salt residue, but the reaction process is longer, and a large amount of ammonia water is used when palladium sulfate reacts with ammonia water, which has a greater impact on the environment

Method used

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  • Synthesis method of tetraamminepalladium sulfate (II)

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Embodiment 1

[0018] see figure 1 , in the embodiment of the present invention, respectively weigh 100 g of potassium chloropalladate and 55 g of ammonium acetate, dissolve in water and mix, add water to 6 L, adjust the pH value to 5 with acetic acid and reflux for 4 h, and filter the obtained solid after cooling, 62 g of cis-dichlorodiammine palladium (II) was obtained, with a yield of 96%.

[0019] Weigh 60g of cis-dichlorodiammine palladium (II), dissolve it with an appropriate amount of ammonia until the solution is transparent and clear, then concentrate the solution under reduced pressure to nearly dryness to obtain 68g of dichlorotetraammine palladium (II) solid, with a yield of 98 %.

[0020] Weigh 61.2g of dichlorotetraamminepalladium(II) and dissolve it in water, add 26.3mL of 10mol / L sulfuric acid solution, add water to 0.45L and then reflux for 5h, concentrate the solution to nearly dryness and then concentrate under reduced pressure to obtain 65.5g tetrasulfuric acid Ammonia ...

Embodiment 2

[0022] see figure 1 , in the embodiment of the present invention, respectively weigh 750 g of potassium chloropalladate and 450 g of ammonium acetate, dissolve in water and mix, add water to 38 L, adjust the pH value to 5 with acetic acid and reflux for 4 hours, and filter the obtained solid after cooling. 461 g of cis-dichlorodiammine palladium (II) was obtained, with a yield of 95%.

[0023] Take by weighing 460g cis-dichloro diammine palladium (II), dissolve it with an appropriate amount of ammonia until the solution is transparent and clear, then concentrate the solution under reduced pressure to near dryness to obtain 523g of dichloro tetraammine palladium (II) solid, with a yield of 98 %.

[0024] Weigh 490g of dichlorotetraamminepalladium (II) and dissolve it in water, add 220mL of 10mol / L sulfuric acid solution, add water to 4L and then reflux for 5h, concentrate the solution to near dryness and then concentrate under reduced pressure to obtain 518.4g of tetraamminepa...

Embodiment 3

[0026] see figure 1 , in the embodiment of the present invention, respectively weigh 1000 g of potassium chloropalladate and 600 g of ammonium acetate, dissolve them in water and mix them, add water to 55 L, adjust the pH value to 5 with acetic acid and reflux for 4 hours, and filter the obtained solid after cooling. 621 g of cis-dichlorodiammine palladium (II) was obtained, with a yield of 96%.

[0027] Take by weighing 620g cis-dichloro diammine palladium (II), dissolve it with an appropriate amount of ammonia until the solution is transparent and clear, then concentrate the solution under reduced pressure to near dryness to obtain 705g of dichloro tetraammine palladium (II) solid, with a yield of 98 %.

[0028] Weigh 612.5g of dichlorotetraamminepalladium(II) and dissolve it in water, add 263mL of 10mol / L sulfuric acid solution, add water to 5L and then reflux for 5h, concentrate the solution to nearly dryness and concentrate under reduced pressure to obtain 648g of tetraa...

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Abstract

The invention discloses a synthesis method of tetraamminepalladium sulfate (II). The method is composed of the following steps: dissolving potassium tetrachloroplatinate and ammonium acetate in water, then carrying out reflux reaction to synthesize cis-diamminedichloropalladium (II); reacting the cis-diamminedichloropalladium (II) with ammonia water to generate a tetraamminepalladium sulfate (II) compound. The method provided by the invention is easy to operate, can effectively remove chlorine ions, and has yield up to more than 90%.

Description

technical field [0001] The invention relates to the field of chemistry and chemical industry, in particular to a method for synthesizing tetraammine palladium (II) sulfate. 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 metal on the coating. Due to the continuous increase in product requirements, the requirements for residual halogen elements are getting lower and lower, and the amount of halogen-free electroplating solutions is increasing. [0003] Tetraammine palladium (Ⅱ) compounds are an important class of palladium compounds, which are 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 palladium plating in the electronics industry due to its high electroplating efficiency, cleanness and environmental...

Claims

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Application Information

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IPC IPC(8): C01G55/00
CPCC01G55/002C01P2006/80
Inventor 王庆琨王安之
Owner TITAN ADVANCED MATERIALS CO LTD
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