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Preparation method for tetraammineplatinum (II) acetate

A technology of acetic acid and calcium acetate, applied in chemical instruments and methods, platinum group organic compounds, platinum group organic compounds and other directions, can solve the problems such as the difficulty of obtaining dichlorotetraammine platinum, the high price of silver acetate, and the easy residual silver ions. , to achieve the effect of high yield, easy control and easy availability of raw materials

Active Publication Date: 2019-01-15
HOOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, because dichlorotetraammine platinum is not easy to obtain, the cost is high and the yield is not high; in addition, the price of silver acetate is relatively expensive, the consumption is large, and there are disadvantages such as easy residual silver ions in the product, therefore, the preparation method is limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of preparation method of tetraammoplatinum acetate (II), comprises the following steps:

[0021] Weigh 4.0g (0.044mol) of oxalic acid into a 300mL beaker, add 50mL of deionized water, stir to dissolve, then slowly add 10.0g (0.023mol) of ammonium chloroplatinate solid in portions, stir and react at 30°C for 2h, there is a little solid If it was not dissolved, the stirring was stopped, and it was allowed to stand for 10 minutes to filter to obtain a solution of diammonium platinum (II) oxalate (7.3 g). Slowly add 25mL (22.7g) of ammonia water to the diammonium oxalate (II) solution, control the temperature at 50-60°C, react for 2h, stop heating, cool to room temperature, dissolve 8g of calcium acetate in 25mL of deionized water to make Dissolve, and then slowly add calcium acetate solution to tetraammine platinum oxalate (8.0g) solution until no precipitate is formed, then add 5mL acetic acid, continue stirring for 0.5h, and let stand for 30min to obtain tetraammi...

Embodiment 2

[0024] A kind of preparation method of tetraammoplatinum acetate (II), comprises the following steps:

[0025] Weigh 50.0g (0.555mol) of oxalic acid into a 2000mL beaker, add 600mL of deionized water, stir to dissolve, then slowly add 100.0g (0.225mol) of ammonium chloroplatinate solid in portions, stir and react at 40°C for 1.5h, stop stirring , standing for 10min and filtering to obtain diammonium oxalate (II) solution (71.3g). Slowly add 320mL (291g) of ammonia water to the diammonium oxalate (II) solution, control the temperature at 50-60°C, react for 2h, stop heating, cool to room temperature, take 86.9g of calcium acetate and dissolve it in 300mL of deionized water to make Dissolve, then slowly add calcium acetate solution to tetraammonium platinum oxalate (79.0g) solution until no precipitate is formed, then add 30mL acetic acid, continue stirring for 0.5h, and let it stand for 30min to obtain tetraammonium acetate solution and white precipitate oxalic acid Calcium, fi...

Embodiment 3

[0028] A kind of preparation method of tetraammoplatinum acetate (II), comprises the following steps:

[0029] Weigh 140g (1.555mol) of oxalic acid into a 5000mL beaker, add 1000mL of deionized water, stir to dissolve, then slowly add 200g (0.451mol) of ammonium chloroplatinate solid in portions, stir and react at 50°C for 1h, stop stirring, and let stand After 10 minutes of filtration, a solution of diammonium platinum (II) oxalate (143.0 g) was obtained. Slowly add 785mL (715g) of ammonia water to the diammonium oxalate (II) solution, control the temperature at 50-60°C, react for 3h, stop heating, cool to room temperature, take 190g of calcium acetate and dissolve it in 600mL of deionized water to dissolve it , then slowly add calcium acetate solution to tetraammine platinum oxalate (158.3g) solution until no precipitate is formed, then add 50mL acetic acid, continue stirring for 0.5h, and let it stand for 30min to obtain tetraammine platinum acetate solution and white preci...

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Abstract

The invention discloses a preparation method for tetraammineplatinum (II) acetate. The preparation method comprises the following steps: reacting ammonium chloroplatinate (IV) with oxalic acid, ammonia water and calcium acetate respectively in three steps to form a tetraammineplatinum (II) acetate solution; then subjecting the tetraammineplatinum (II) acetate solution to concentration and separation through solvent-out crystallization so as to obtain a tetraammineplatinum (II) acetate crystal; and performing vacuum drying so as to obtain tetraammineplatinum (II) acetate with a purity of no less than 99.95%. According to the invention, the starting material, i.e., the ammonium chloroplatinate (IV) is a conventional compound of platinum and is easy to obtain and high in yield, and the otherauxiliary materials consisting of oxalic acid, concentrated ammonia water and calcium acetate are cheap, so production cost is greatly lowered; in addition, the method avoids residues of chloride ionsand nitrate ions and lowers residual silver ions in the produced tetraammineplatinum (II) acetate. The preparation method of the invention is carried out under normal temperature and normal pressure,is simple to operation and easy to control, has high reaction yield (more than 92%) and high product purity (no less than 99.95%), and is applicable to batch and industrial production of tetraammineplatinum (II) acetate.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysis, and in particular relates to a preparation method of tetraammonium platinum (II) acetate. Background technique [0002] Platinum catalysts are widely used in various fields such as petrochemical industry, pharmaceutical chemical industry, automobile exhaust and environmental treatment. However, due to the residual chloride ions and nitrate ions in the precursor compounds for the preparation of platinum catalysts, the high temperature resistance, activity and The service life of the equipment, as its usage increases, people have higher and higher requirements for platinum catalysts, and the lower the residual requirements for chloride ions and nitrate ions, the better. [0003] Tetraammine platinum (Ⅱ) compounds are an important class of platinum (Ⅱ) compounds, which are widely used in chemical catalysis and electroplating industries. Among them, tetraammine platinum(II) acetate (Pt(NH...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00
CPCC07F15/0093
Inventor 夏军李富荣索永喜李波易翔郭福田
Owner HOOTECH
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