Method for preparing spherical dinitroso diammineplatinum by hydrothermal method and application

A technology of dinitrosodiammine platinum and hydrothermal method is applied in the field of preparing spherical dinitrosodiammine platinum by hydrothermal method, which can solve the problem of structural instability, uneven morphology of P salt, affecting product plating quality, etc. problem, to achieve the effect of good electroplating quality, convenient operation method and good crystallization

Active Publication Date: 2022-02-18
XIAN UNIV OF SCI & TECH
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  • Abstract
  • Description
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Problems solved by technology

[0004] The problem existing in the existing preparation method is that the structure is unstable, and the shape of the generated P salt is not uniform, which is likely to affect the quality of the product when it is electroplated.

Method used

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  • Method for preparing spherical dinitroso diammineplatinum by hydrothermal method and application
  • Method for preparing spherical dinitroso diammineplatinum by hydrothermal method and application
  • Method for preparing spherical dinitroso diammineplatinum by hydrothermal method and application

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preparation example Construction

[0032] The preparation method of spherical dinitrosodiammine platinum provided by the invention comprises the following steps:

[0033] 1) Precipitation of potassium chloroplatinate is prepared by reacting chloroplatinic acid with potassium chloride;

[0034] 2) Sodium nitrite reduction substitution:

[0035] Sodium nitrite is used as a reducing agent to reduce potassium chloroplatinate. The process is to dissolve the precipitated potassium chloroplatinate in water, add sodium nitrite solution for reduction after heating, no yellow-brown gas is produced in the final reaction, and the solution is transparent yellow-green, natural After cooling to room temperature, filter;

[0036] The specific method is to dissolve the potassium chloroplatinate precipitate in water, heat the oil bath to 85-100°C, add the sodium nitrite solution dropwise, control the reaction system at 100-110°C, and continue stirring for 1.5-2 hours after the dropwise addition , to obtain a yellow-green trans...

Embodiment 1

[0055] 1) Precipitation of potassium chloroplatinate by reaction of chloroplatinic acid and potassium chloride

[0056] 1.1) Take 50g of chloroplatinic acid solids in a beaker with an electronic balance, and prepare a chloroplatinic acid solution with a mass fraction of 10%;

[0057] 1.2) Weigh 1.5g of potassium chloride solid in a beaker, add 15ml of pure aqueous solution to obtain a 0.1g / ml potassium chloride solution;

[0058]1.3) Transfer 15ml potassium chloride solution to a 250ml three-neck flask, heat the oil bath to 90°C, slowly add 50ml of the prepared 10% potassium chloroplatinate solution dropwise, continue stirring for 1 hour after the dropwise addition, and cool to 5°C , filtered with suction and washed with ice-pure water, dried at 80°C, and the product was a yellow precipitate of potassium chloroplatinate;

[0059] 2) In a 250ml flask, 2.5g of potassium chloroplatinate precipitate was mixed with 5ml of pure water to make a paste; the oil bath was heated until t...

Embodiment 2

[0064] 1.1) Take 50g of chloroplatinic acid solids in a beaker with an electronic balance, and prepare a chloroplatinic acid solution with a mass fraction of 10%;

[0065] 1.2) Weigh 3g of potassium chloride solid in a beaker, add 30ml of pure aqueous solution to obtain 30ml of potassium chloride solution;

[0066] 1.3) Transfer 30ml of potassium chloride solution to a 250ml three-necked flask, heat the oil bath to 85°C, slowly add 100ml of the prepared 10% potassium chloroplatinate solution dropwise, continue stirring for 1 hour after the dropwise addition, and cool to 0°C , suction filtered and washed with ice-pure water, dried at 85°C, and the product was a yellow precipitate of potassium chloroplatinate;

[0067] 2) In a 250ml flask, mix 5g of potassium chloroplatinate solid with 10ml of pure water to make a paste; heat the oil bath until the reaction system is 85°C, start adding 50ml of the prepared sodium nitrite solution dropwise, and control the reaction system to 110°...

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Abstract

The invention belongs to the technical field of platinum compound preparation, and relates to a method for preparing spherical dinitroso diammineplatinum through a hydrothermal method and application. The method comprises the following steps: 1) preparing a potassium chloroplatinate precipitate from chloroplatinic acid and potassium chloride; 2) dissolving the potassium chloroplatinate precipitate in water, heating in an oil bath, dropwise adding a sodium nitrite solution, and stirring for 2 hours to obtain a yellow green transparent solution; 3) dropwise adding ammonia water into the yellow green transparent solution at 70-80 DEG C, and stirring to obtain yoghourt-like solid; and 4) transferring the yoghourt-like solid into a hydrothermal reaction kettle for reaction, cooling the reaction kettle, taking precipitate and washing for multiple times, and freeze-drying to obtain yellowish powder, namely the spherical dinitroso diammineplatinum. The method has the characteristics of uniform phase, high purity, good crystallization and high yield, the spherical P salt with controllable morphology is prepared, the spherical P salt can be used for cyanide-free electroplating, and the electroplating quality is ensured.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and relates to a method and application for preparing spherical dinitrosodiammine platinum by a hydrothermal method. Background technique [0002] Dinitrosodiammine platinum [Pt(NH 3 ) 2 (NO 2 ) 2 ] Commonly known as P salt, the molecular weight is 321.15, the appearance is white powder, insoluble in cold water, soluble in hot water and ammonia water; it is the most commonly used platinum-transfer reagent in cyanide-free electroplating, and the obtained coating has high hardness and low resistance. Brazing is often used for platinum plating on the surface of electronic components. [0003] Usually the preparation method of P salt is: metal platinum is dissolved in aqua regia to prepare chloroplatinic acid, and then reacts with potassium chloride to generate a yellow precipitate of potassium chloroplatinate; the potassium chloroplatinate precipitate is dissolved in water into a pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00C25D3/50
CPCC01G55/00C25D3/50C01P2004/32C01P2004/03C01P2002/72C01P2004/61Y02P10/20
Inventor 巩加芳杨凡贾伟航褚佳
Owner XIAN UNIV OF SCI & TECH
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