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Method for preparing potassium tetracyanoplatinate (ii) trihydrate by pressurized cyanidation

A technology of potassium acid trihydrate and tetracyanoplatinum, which is applied in the field of inorganic compound synthesis, can solve the problems of difficult control of reaction conditions, high production costs, and low total yield, and achieve easy control of reaction conditions and low total yield. Improvement, the effect that the response is sufficient

Inactive Publication Date: 2017-10-13
YUNNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to propose a short flow process and high reaction conditions for the long flow process that exists in the traditional preparation process of tetracyanoplatinate (II) potassium trihydrate, difficult to control reaction conditions, low total yield and high production cost. Easy to control, high yield, low cost pressurized cyanidation method for preparing potassium tetracyanoplatinate (II) trihydrate

Method used

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  • Method for preparing potassium tetracyanoplatinate (ii) trihydrate by pressurized cyanidation
  • Method for preparing potassium tetracyanoplatinate (ii) trihydrate by pressurized cyanidation
  • Method for preparing potassium tetracyanoplatinate (ii) trihydrate by pressurized cyanidation

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Effect test

Embodiment 1

[0023] Add the prepared 10wt% ascorbic acid solution dropwise to 200mL 25.62mmol / L H 2 PtCl 6 In the solution, the color of the solution changes from deep to light, from dark yellow to stable light yellow, at this time H 2 PtCl 6 The solution is converted to H 2 PtCl 4 solution. Then take 0.6g KOH and dissolve it in distilled water to make a 5wt% KOH solution, and add the KOH solution dropwise to the above H 2 PtCl 4 In the solution, the solution appeared precipitated. After the dropwise addition, continue to stir for 5 minutes to make the precipitation complete. Then weigh 1.7g KCN and add it to the above suspension. Dilute the suspension to 400 mL with distilled water and pour it into a 3-liter high-pressure reactor. , tighten the lid of the kettle, let in air, control the pressure at 2.0 MPa, raise the temperature to 110°C, keep the stirring speed at 400 r / min, cyanide at constant temperature and pressure for 2 hours, let the kettle body cool naturally for 1 hour, and...

Embodiment 2

[0025] Except that the following content is different from Example 1, all the others are the same.

[0026] h 2 PtCl 6 The concentration of the solution is 41.0mmol / L, the volume is 200mL, the amount of KOH is 1.0g, and it is made into a 5 wt% solution. The addition of KCN is 1.7g, and the suspension is diluted to 400mL with distilled water to finally obtain 7.90 mmolK 2 Pt(CN) 4 ·3H 2 O product, total recovery 96.3%, product element analysis result is shown in Table 1, does not detect the compound other than tetracyanoplatinate (II) potassium trihydrate.

Embodiment 3

[0028] Except that the following content is different from Example 1, all the others are the same.

[0029] h 2 PtCl 6 The concentration of the solution is 51.26mmol / L, the volume is 200mL, the amount of KOH is 1.2g, and it is made into a 5wt% solution. The addition of KCN is 1.7g, and the suspension is diluted to 400mL with distilled water to finally obtain 9.95mmolK 2 Pt(CN) 4 ·3H 2 O product, total yield 97.1%, product element analysis result is shown in Table 1, does not detect the compound other than tetracyanoplatinate (II) potassium trihydrate.

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Abstract

The invention relates to a method for preparing a potassium tetracyanoplatinate (II) trihydrate as a material intermediate. The method comprises the following steps: reducing H2PtCl6 to H2PtCl4 with an ascorbic acid solution, adding a potassium hydroxide solution, converting H2PtCl4 into a platinum hydroxide precipitate, and carrying out pressure cyanidation treatment on platinum hydroxide to obtain a K2Pt (CN) 4 3H2O product. The preparation process is short, and the yield of K2Pt (CN)4 3H2O is more than 96.0%. The platinum content of the potassium tetracyanoplatinate (II) trihydrate prepared by the method provided by the invention is 45.2 to 45.9% by elemental analysis.

Description

technical field [0001] The invention belongs to an inorganic compound synthesis method, in particular to a preparation method of potassium tetracyanoplatinate (II) trihydrate. Background technique [0002] Potassium tetracyanoplatinate (II) trihydrate is an important platinum group metal cyanide, an important intermediate for preparing phosphorescent materials and noble metal precursor materials for catalysts, and has a good market prospect. At present, only a few documents have reported the preparation method of potassium tetracyanoplatinate (II) trihydrate, which is mainly divided into the following steps: (1) using platinum as a starting material, firstly prepare hexabromoplatinate Platinic acid; (2) react hexabromoplatinic acid with potassium bromide to obtain potassium hexabromoplatinate (IV); (3) reduce potassium hexabromoplatinate (IV) to tetrabromoplatinate with hydrazine sulfate (4) Potassium tetrabromoplatinate (II) reacts with potassium cyanide solution to obtain...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01C3/06
CPCC01C3/06
Inventor 黄章杰韦群燕张金燕李荣陈慕涵吴胜杰杨荣清张琴
Owner YUNNAN UNIV