Rhodium triiodid preparation method

A technology of rhodium triiodide and hydriodic acid, which is applied in iodide preparation, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of uncontrollable reaction conditions, unavoidable chlorine, etc., and achieve easy washing and filtration, and less loss of rhodium Effect

Active Publication Date: 2007-05-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction conditions of this method are not easy to control, and there is inevitably a certain amount of chlorine in the product, so it is not suitable for the production of rhodium-based catalysts required for the carbonylation of methanol to acetic acid

Method used

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  • Rhodium triiodid preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add the hydroxide of 5g trivalent rhodium in the there-necked flask, then add 30ml of HI solution with a mass percent concentration of 45%, stir, heat to boiling, keep for 2 hours, then filter while hot, wash the filter cake, remove soluble impurities, When the conductivity in the washing solution is lower than 50 μS / cm, place the obtained product rhodium triiodide in an oven and carefully dry it. The final product obtained is gray black powder with a rhodium content of 22.3% and a single-pass yield of 75%. . It can be seen from Figure 1 that the particles have a loose porous structure with a diameter of less than 5 μm and uniform size.

[0022] The reaction filtrate can be directly recycled. Add 45% HI solution to the filtrate and repeat the previous process to convert the trivalent rhodium hydroxide in the filtrate into products. The total yield of rhodium can be close to 100% after determination.

Embodiment 2

[0024] Change the amount of HI solution to 40ml, and other operations are the same as in Example 1, the rhodium content is 21.3%, and the yield per pass is 78.5%.

Embodiment 3

[0026] Change the reaction time to be 4 hours, other operations are the same as in Example 2, the rhodium content is 19.5%, and the yield per pass is 92.0%.

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Abstract

The invention provides a method for preparation of rhodium triiodide, which contains: using trivalent rhodium hydroxide and hydriodic acid as reactive raw material, adding proper hydriodic acid solution of certain concentration into said trivalent rhodium hydroxide, heating up to 60-100Deg. C and mixing, keeping for 2-6 hours, and filtering, washing and drying to prepare product. The prepared rhodium triiodide is cinereous and porous, and it is easy to wash and filter; the rhodium content in the product is about 19.5-21.5%, and the impurity is almost negligible; and the product is especially suitable to be a catalyst for synthesis of acetic acid by carbonylation of methanol.

Description

technical field [0001] The invention relates to a preparation method of a rhodium compound. Background technique [0002] Acetic acid is an important organic chemical raw material. In 2000, the global demand reached 6.3 million tons, and it is increasing year by year. At present, the production route of acetic acid is dominated by methanol carbonylation, accounting for more than 65% of the total production capacity of acetic acid. With the development of methanol carbonylation to produce acetic acid, the rhodium-based catalyst it needs increases year by year, and the demand for rhodium triiodide, the precursor for producing rhodium-based catalyst, also increases year by year. [0003] The traditional preparation method of rhodium triiodide is to first place elemental rhodium in hydrochloric acid solution for electrolysis, separate and purify to obtain rhodium trichloride solution, then add a certain concentration of potassium iodide solution, stir and heat, wash and filter ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G55/00C01B9/06
Inventor 何海龙黄凤兴贺黎明马京生郝玉春王伟
Owner CHINA PETROLEUM & CHEM CORP
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