Method for preparing high-purity anhydrous indium trichloride

An anhydrous indium trichloride, high-purity technology, applied in the direction of chloride preparation, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of expensive reagents, environmental pollution, difficult post-processing, etc., achieve good chemical stability, No pollution price, good product quality effect

Inactive Publication Date: 2008-09-03
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These preparation methods have their own advantages and disadvantages. Some methods have higher requirements on the purity of raw material reagents, stricter temperature control, complex equipment, and lower output. Some methods are difficult to post-process and serious environmental pollution, etc.
Although foreign existing literature reports utilize organic solvents such as amine, formamide and kerosene to remove crystal water in crystalline chloride to prepare anhydrous chloride, but also because the processes involved in these reactions are often more complicated, the reaction time is long, The experimental conditions are demanding, the reagents are expensive, there are organic reagents that are polluted and dangerous, the equipment is large in size, high in energy consumption, difficult to operate, few in resources, and high in cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: Take 11.48g of 99.99% pure metal indium (In) and add 50ml of hydrochloric acid (HCl) with a concentration of 36% by weight, heat up to 45°C, and continue stirring until the metal indium is completely dissolved to obtain InCl 3 aqueous solution, and the aqueous solution was evaporated to obtain indium trichloride tetrahydrate (InCl 3 4H 2 O) white crystal; Add n-butanol (BuOH) 245ml in crystal, the ratio of its n-butanol and water of crystallization (BuOH / H 2 O) is 35, under the condition of temperature 100 ℃, carries out normal pressure distillation dehydration, obtains pasty product indium trichloride n-butanol complex (InCl 3 mBuOH); raise the temperature to 180°C, the paste complex (InCl 3 mBuOH) was distilled under reduced pressure for 10min, and the vacuum degree was 8kPa to obtain anhydrous indium trichloride (InCl 3 ); At this time, the temperature is raised to 350 ° C for anhydrous indium trichloride (InCl 3 ) was sublimated and purified for 10 mi...

Embodiment 2

[0013] Example 2: Take 99.99% pure metal indium (In) 11.48g and add 50ml of hydrochloric acid (HCl) with a concentration of 36% by weight, heat up to 45°C, and continue stirring until the metal indium is completely dissolved to obtain InCl 3 aqueous solution, and its aqueous solution was evaporated to obtain indium trichloride tetrahydrate (InCl 3 4H 2 O) white crystal; Add the mixture of n-butanol 105ml and n-heptane 105ml in the crystal, under the condition of temperature 95 ℃, carry out normal pressure distillation dehydration, obtain pasty unstable indium trichloride and n-butanol and Mixed complexes of n-heptane (InCl 3 mBuOH); the paste complex (InCl 3 mBuOH), distilled under reduced pressure at a temperature of 150°C for 8min, with a vacuum of 8kPa, to obtain white flaky anhydrous indium trichloride (InCl 3 ); anhydrous indium trichloride (InCl 3 ) was sublimated and purified at a temperature of 350°C for 10 minutes to obtain a white fluffy needle-shaped high-purity...

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PUM

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Abstract

The invention relates to a preparation method of high purity anhydrous indium trichloride, which belongs to the technology field of rare metal fine chemical industry. The preparation method includes: Using 99.99-99.999% Indium metal and 36% hydrochloric acid as the material and using organic solvents including n-butyl alcohol and n-heptane as the dehydrant, that is, using more unstable complex to replace more stable compound, the stable hydrated indium trichloride is replaced with the more unstable complex of the indium trichloride organic solvent; adopting a manner of microwave heating and gradually heating up including three steps of distillation dehydration at normal pressure, distillation de-reagent at reduced pressure and sublimation and purification of the anhydrous indium trichloride; and finally obtaining the high purity anhydrous indium trichloride (InCl3), which is white with a purity of up to 99.99-99.999% and a production rate of 97%-98%.

Description

1. Technical field: [0001] The invention relates to a method for preparing high-purity anhydrous indium trichloride, belonging to the technical field of rare metal fine chemicals. 2. Background technology [0002] High-purity anhydrous indium trichloride (InCl 3 ) is the main raw material for the preparation of ITO thin films and III-V semiconductor materials. It is one of the important solar cell materials and the basic raw material for the synthesis of organic indium series compounds. It can be used as a catalyst for organic reactions. In terms of organic synthesis and electronics industry Has a wide range of applications. my country is a country with large indium resources, and the annual smelting of indium metal can reach 400 tons, ranking first in the world. But InCl 3 The production of the current domestic production can only produce InCl 3 4H 2 O and InCl 3 , while high-purity anhydrous InCl 3 Must be imported and expensive. Although the preparation of anhydro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G15/00C01B9/02
Inventor 宋宁戴永年马文会杨斌姜宏伟严玉环
Owner KUNMING UNIV OF SCI & TECH
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