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Method for preparing tetraamminepalladium hydrogen carbonate

A technology of tetraammine palladium bicarbonate and sodium bicarbonate, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve high cost, long operation process, discomfort Due to problems such as large-scale production, it achieves the effects of low pollution, simple operation and high purity

Active Publication Date: 2018-10-26
JINCHUAN GROUP LIMITED +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has a long operation process and high cost, and is also not suitable for large-scale production.

Method used

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  • Method for preparing tetraamminepalladium hydrogen carbonate
  • Method for preparing tetraamminepalladium hydrogen carbonate
  • Method for preparing tetraamminepalladium hydrogen carbonate

Examples

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Embodiment 1

[0023] Weigh 10g of tetraammine palladium sulfate (Pd: 39%), add 10mL of deionized water to dissolve, and prepare an aqueous solution of tetraammine palladium sulfate; weigh 9.38g of hydrated barium hydroxide, add 10mL of ammonia water to dissolve, and prepare the ammonia of barium hydroxide Aqueous solution: Slowly add the ammonia solution of barium hydroxide into the tetraammonia palladium sulfate aqueous solution, keep the pH of the reaction process at 11, and obtain 20mL containing BaSO after reacting for 30min 4 Precipitated suspension. Aqueous ammonia 20mL was added, and the reaction was stirred for 2h. Add an aqueous solution containing 6.2g of sodium bicarbonate, continue to stir and react for 2 hours, filter with slow filter paper, distill the filtrate at 60°C under negative pressure (P=-0.08MPa) until a crystal film appears, and place it in an ice-water bath to crystallize , the crystals were filtered and dried to obtain tetraammine palladium bicarbonate product wit...

Embodiment 2

[0027] Weigh 10g of tetraammine palladium sulfate (Pd: 39%), add 10mL of deionized water to dissolve, and prepare an aqueous solution of tetraammine palladium sulfate; weigh 17.49g of hydrated barium hydroxide, add 10mL of ammonia water to dissolve, and prepare the ammonia of barium hydroxide Aqueous solution: Slowly add the ammonia solution of barium hydroxide into the tetraammonia palladium sulfate aqueous solution, keep the pH of the reaction process at 12, and obtain 20mL containing BaSO after reacting for 30min 4 Precipitated suspension. Aqueous ammonia 20mL was added, and the reaction was stirred for 2h. Add an aqueous solution containing 24.9g of sodium bicarbonate, continue to stir and react for 2 hours, filter with slow filter paper, distill the filtrate at 60°C under negative pressure (P=-0.08MPa) until a crystal film appears, and place it in an ice-water bath to crystallize , the crystals were filtered and dried to obtain tetraammine palladium bicarbonate product w...

Embodiment 3

[0031] Weigh 100g of palladium tetraammine sulfate (Pd: 39%), add 100mL of deionized water to dissolve, and prepare an aqueous solution of tetraammine palladium sulfate; weigh 105g of hydrated barium hydroxide, add 100mL of ammonia water to dissolve, and prepare an ammonia solution of barium hydroxide ; The ammonia solution of barium hydroxide is slowly added in the tetraammonia palladium sulfate aqueous solution, the pH that keeps reaction process is 12, after reacting 30min, obtain 200mL containing BaSO 4 Precipitated suspension. Ammonia water 200mL was added, and the reaction was stirred for 2h. Add an aqueous solution containing 155.5g of sodium bicarbonate, continue to stir and react for 2.5h, filter with slow filter paper, distill the filtrate at 40°C under negative pressure (P=-0.06MPa) until a crystalline film appears, and place it at 0°C crystallized, and the crystals were filtered and dried to obtain tetraammine palladium bicarbonate product with a yield of 92.5%. ...

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Abstract

The invention discloses a method for preparing tetraamminepalladium hydrogen carbonate, belonging to the technical field of chemical synthesis. The method comprises the following steps: (1) in a palladium tetramine sulfate solution, slowly adding an ammonia water solution of barium hydroxide so as to obtain a suspension with a great amount of precipitate BaSO4, wherein the mole ratio of palladiumtetramine sulfate to barium hydroxide is 1:(0.8-1.5), and the ammonia water concentration is greater than 1mol / L; (2) adding ammonia water of which a volume is same as that of the suspension and the concentration is greater than 1mol / L, and stirring to carry out a reaction; (3) adding sodium bicarbonate which is 2-4 times of the mole amount of the palladium tetramine sulfate, and continuously stirring to carry out the reaction for more than 2 hours; and (4) carrying out filtration separation, carrying out spinning evaporation on the filtrate, and crystallizing, thereby obtaining tetraamminepalladium hydrogen carbonate. The method disclosed by the invention is simple to operate, high in yield, high in product purity and applicable to on-scale production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a preparation method of tetraammine palladium bicarbonate, in particular to a preparation method of tetraammine palladium bicarbonate for electroplating. Background technique [0002] Palladium nickel plating has been used in the field of electronic connectors for many years. In the existing palladium plating process, palladium ammonia complex is generally used as the main electroplating salt, and the anion generally uses SO 4 2- , Cl - , NO 2 - Wait. However, with the addition of electroplating salt, the level of salt in the electrolyte increases, thus shortening the life of the electroplating solution, while HCO 3 - with CO 3 2- ion is considered an ideal palladium salt. [0003] Chinese patent CN 102015744 A discloses a method for synthesizing a palladium salt coordinated by bicarbonate and ethylenediamine. By adding palladium in the form of carbonate (hydro...

Claims

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Application Information

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IPC IPC(8): C01G55/00
CPCC01G55/002C01P2006/80
Inventor 常全忠刘国旗张静白延利任志勇王红梅李欢郅欢欢
Owner JINCHUAN GROUP LIMITED
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