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Preparation method of iridium acetate

A kind of technology of iridium acetate and iridium hydroxide, applied in the field of catalyst preparation, can solve the problems such as not taking into account the problem of iridium valence, the increase of impurity content, the reduction of iridium acetate yield

Active Publication Date: 2020-03-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] However, the above preparation methods do not take into account the valence of iridium
As can be seen from the structural formula of the above-mentioned iridium acetate, in iridium acetate, iridium exists in a trivalent form, which means that iridium in a tetravalent form may lead to a decrease in iridium acetate yield or an increase in impurity content

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Embodiment 1-3

[0060] Wherein, the content of iridium in the product iridium (III) acetate was measured by inductively coupled plasma mass spectrometry (ICP) (model Agilent 7500cx).

[0061] The product yield was calculated by formula (2).

[0062] Product yield = (m t ×w / m i )×100% Formula (2)

[0063] Among them, m t - product quality; The content of the iridium in the w-iridium acetate (III) powder; m i - the mass of iridium in the aqueous solution containing iridium(IV).

Embodiment 1

[0066] Weigh 5g of chloroiridic acid and put it in a three-necked flask, add 50ml of deionized water to dilute. Under the condition of stirring, pass high-purity nitrogen gas (gas flow rate: 100ml / min) into the solution to purge for 30 minutes to obtain an aqueous solution containing iridium (IV).

[0067] Afterwards, 2.2 g of ascorbic acid was added to the aqueous solution containing iridium (IV), and the solution was heated to 98 ° C under stirring conditions, and refluxed at this temperature for 3 h to complete the reduction treatment and obtain an aqueous solution of iridium (III).

[0068] Then, the aqueous solution of iridium (Ⅲ) is cooled to 60 ℃, and in the aqueous solution of iridium (Ⅲ), sodium hydroxide solution (mass concentration is 30%) is added dropwise, and the pH of the aqueous solution of iridium (Ⅲ) is monitored during the dropping process value. When the pH value of the aqueous solution of iridium (Ⅲ) increased to 11, stop the dripping of sodium hydroxide ...

Embodiment 2

[0073] Weigh 5g of chloroiridic acid and put it in a three-necked flask, add 50ml of deionized water to dilute. Under the condition of stirring, high-purity nitrogen gas (gas flow rate: 200ml / min) was passed into the solution for purging for 30 minutes to obtain an aqueous solution containing iridium (IV).

[0074] Afterwards, 0.9 g of hydrazine hydrate was added to the aqueous solution containing iridium (IV), and the solution was continued to be heated to 98° C. with stirring, and refluxed at this temperature for 3 h to complete the reduction treatment and obtain an aqueous solution of iridium (III).

[0075] Then, the aqueous solution of iridium (Ⅲ) is cooled to 80 ℃, and in the aqueous solution of iridium (Ⅲ), sodium hydroxide solution (mass concentration is 30%) is added dropwise, and the pH of the aqueous solution of iridium (Ⅲ) is monitored during the dropping process value. When the pH value of the iridium (III) aqueous solution increased to 11, the dropwise addition ...

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Abstract

The invention provides a preparation method of iridium acetate. The method comprises the following steps: providing an iridium (IV)-containing aqueous solution, and carrying out reduction treatment onthe iridium (IV)-containing aqueous solution by using a reducing agent to obtain an aqueous solution of iridium (III); carrying out precipitation treatment and aging treatment on the aqueous solutionof iridium (III) by using an aqueous solution of an alkaline compound to obtain an iridium (III) hydroxide precipitate; dissolving the iridium hydroxide (III) precipitate in an aqueous acetic acid solution to obtain an iridium (III) acetate solution; and concentrating and drying the iridium (III) acetate solution to obtain iridium (III) acetate. By adopting the method, the final product is closeto standard iridium (III) acetate, and product yield is relatively high.

Description

technical field [0001] The invention relates to the field of preparation of catalysts, in particular to a preparation method of iridium acetate. Background technique [0002] Among platinum group metal elements, iridium has many unique physicochemical properties. It has the characteristics of high density, high melting point, high elastic modulus, good high temperature stability, chemical inertness and resistance to oxygen diffusion. Since iridium has a d orbital, it has a strong spin-orbit coupling after coordination with the ligand, which can produce phosphorescent emission. At the same time, iridium (Ⅲ) has a d2sp3 orbital hybrid, which can accept lone pair electrons to form a strong metal- Metal bonds and metal-coordination bonds, exhibiting catalytic activity, are widely used in the field of catalysis, especially as catalysts in isomerization reactions, hydroformylation reactions, and carbonylation reactions. [0003] Many researchers are studying the synthesis and ap...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C53/10
CPCC07C51/412C07C53/10
Inventor 李彤王世亮吕顺丰秦燕璜
Owner CHINA PETROLEUM & CHEM CORP
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