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Preparation method of indium acetate crystal

A technology of indium acetate and crystals, which is applied in the field of preparation of indium acetate crystals, can solve the problems of slow reaction speed between acetic acid and indium particles or indium strips, slow reaction between glacial acetic acid and indium, and reduced utilization rate of acetic acid, etc., so as to reduce volatilization, Effect of large specific surface area and improved utilization

Pending Publication Date: 2020-05-08
昆明先导新材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the indium industry, the reaction of elemental indium and glacial acetic acid is mainly used to prepare indium acetate solution, and indium acetate crystals are obtained through evaporation and crystallization. This method has the following disadvantages: acetic acid is volatile, and the equipment is easy to be corroded. At the same time, the utilization rate of acetic acid is reduced. ;The reaction speed between acetic acid and indium particles or indium strips is slow. Acetic acid is a weak acid. After heating, the reaction between glacial acetic acid and indium is very slow. Even if hydrogen peroxide is added, the dissolution period is still very long

Method used

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Examples

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Effect test

preparation example Construction

[0019] The present invention proposes a kind of preparation method of indium acetate crystal, it comprises the steps:

[0020] S1. Material preparation: The sponge indium and pure water are prepared according to a certain solid-to-liquid ratio, and the sponge indium is added to the pure water, then stirred and dispersed to form the first mixed solution, and the temperature of the first mixed solution is raised to 70~80°C;

[0021] S2. Prepare indium acetate solution: add glacial acetic acid to the first mixed solution until the pH of the first mixed solution is less than 1.8 to form a second mixed solution, then add hydrogen peroxide solution to the second mixed solution at a certain drop rate, and at the same time Continue to add glacial acetic acid to the second mixed solution so that the pH of the second mixed solution is between 1.0 and 1.8 to form the third mixed solution; keep the reaction at 70~80°C until the density of the third mixed solution is 1.10~1.20g / ml After th...

Embodiment 1

[0034] A preparation method for indium acetate crystals, comprising the steps of: first adding 1000g of indium sponge into a beaker with 1000g of pure water, stirring and dispersing to form a first mixed solution, and heating the first mixed solution to 75°C; In the first mixed solution, add glacial acetic acid until the pH=1.0 of the first mixed solution forms the second mixed solution, then add the hydrogen peroxide solution that mass fraction is 40% with the drop rate of 4g / 15min in the second mixed solution, simultaneously Continue to add glacial acetic acid to the second mixed solution to maintain the pH between 1.0 and 1.8 to form the third mixed solution; keep the reaction at 70-80°C for 10 hours, and then stop the reaction after the density of the third mixed solution is 1.16g / ml. The three mixtures are filtered until the solution is clear and transparent to obtain unreacted indium sponge and indium acetate solution; transfer the indium acetate solution to the evaporati...

Embodiment 2

[0037] A preparation method for indium acetate crystals, comprising the steps of: first adding 1000g of indium sponge into a beaker with 2000g of pure water, stirring and dispersing to form a first mixed solution, and heating the first mixed solution to 70°C; In the first mixed solution, add glacial acetic acid until the pH=1.3 of the first mixed solution forms the second mixed solution, then add the hydrogen peroxide solution that mass fraction is 70% with the drop speed of 5g / 15min in the second mixed solution, simultaneously Continue to add glacial acetic acid to the second mixed solution to maintain the pH between 1.0 and 1.8 to form the third mixed solution; keep the reaction at 70-80°C for 20 hours, stop the reaction after the density of the third mixed solution reaches 1.10 g / ml, and put The third mixed solution is filtered until the solution is clear and transparent to obtain unreacted indium sponge and indium acetate solution; the indium acetate solution is transferred...

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Abstract

The invention relates to a preparation method of indium acetate crystals, which comprises the following steps: S1, preparing sponge indium and pure water according to a certain solid-to-liquid ratio,adding the sponge indium into the pure water, stirring and dispersing the components to form a first mixed solution, and heating the mixture the first mixed solution to 70-80 DEG C; S2, adding glacialacetic acid into the first mixed solution until the pH value of the first mixed solution is less than 1.8 to form a second mixed solution, then adding a hydrogen peroxide solution into the second mixed solution at a certain dropping speed, and continuously adding glacial acetic acid into the second mixed solution to enable the pH value of the second mixed solution to be 1.0-1.8 to form a third mixed solution, keeping the temperature at 70-80 DEG C for continuous reaction until the density of the third mixed solution is 1.10-1.20 g / ml, stopping the reaction, and filtering the third mixed solution until the solution is clear and transparent to obtain an unreacted sponge indium and indium acetate solution; and S3, transferring the indium acetate solution to an evaporation kettle, adding acetic acid until the molar ratio of indium ions to free acetic acid in the solution is 1:(0.05-1), heating the solution for evaporation, cooling the solution, carrying out suction filtration, and dryingthe product to obtain indium acetate crystals.

Description

technical field [0001] The invention relates to the field of preparation of indium compounds, in particular to a method for preparing indium acetate crystals. Background technique [0002] The molecular formula of indium acetate is In(CH 3 COO) 3 , the molecular weight is 291.8, and the physical properties are white powder. It is used in the preparation of indium tin oxide nanopowder, the field of copper indium selenium quantum dots, and the field of dye solar cells. It is a product with great market value. [0003] At present, there are no related patents and literatures to disclose the synthesis method of indium acetate. In the indium industry, the reaction of elemental indium and glacial acetic acid is mainly used to prepare indium acetate solution, and indium acetate crystals are obtained through evaporation and crystallization. This method has the following disadvantages: acetic acid is volatile, and the equipment is easy to be corroded. At the same time, the utilizat...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C53/10
CPCC07C51/412C07C53/10
Inventor 王波康冶朱刘
Owner 昆明先导新材料科技有限责任公司
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