Preparation method of high-purity rhodium iodide

A rhodium triiodide, high-purity technology, applied in the field of inorganic compounds, can solve the problems of low yield, complicated preparation method of rhodium triiodide, etc., and achieves high reactivity, increased mutual contact and collision, and high removal efficiency. Effect

Active Publication Date: 2013-07-03
陕西煤业化工技术开发中心有限责任公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0012] For this reason, what the present invention is to solve is that the preparation method of rhodium triiodide is complicated in the prior art, and the problem of low yield provides a kind of preparation method simple, high yield, the preparation method of rhodium triiodide with high purity

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  • Preparation method of high-purity rhodium iodide

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Effect test

Embodiment 1

[0035] Present embodiment is the preparation embodiment of high-purity rhodium triiodide, and concrete steps are:

[0036] S1. Take 98.4mL of rhodium trichloride aqueous solution with a rhodium concentration of 25g / L and 200g of HI solution with a concentration of 5% and place them in a microwave reactor, set the microwave power to 500W, and when the temperature reaches 100°C, continue the reaction at a constant temperature for 40min , to obtain a solution containing rhodium triiodide;

[0037] S2, after the end of the reaction, it is 20g / h of O that the flow rate is blown into the reaction solution 3 gas, maintain the reaction at 60°C, the generated I 2 Can further deepen the color of solution, stop reaction when the color of solution no longer deepens, and present embodiment shares 35min;

[0038] S3, the solid obtained after filtering the solution containing rhodium triiodide after the oxidizing gas treatment in step S2 is RhI 3 Crude product; washed with absolute ethano...

Embodiment 2

[0041] This embodiment is an example of preparing high-purity rhodium triiodide, and the preparation method is the same as in Example 1, specifically: 98.4 mL of rhodium trichloride aqueous solution with a rhodium concentration of 25 g / L and 65 g of HI solution with a concentration of 15% are placed In the microwave reactor, the microwave power was set at 150W, and when the temperature reached 80°C, the reaction was continued at a constant temperature for 60 minutes. O 3 Gas, maintain the reaction at 50°C for 30min. Then the reaction product is filtered; the obtained RhI 3 Wash with absolute ethanol until the washing solution is colorless and transparent. The washed material was dried at 120°C for 5 hours to obtain 11.521 g of high-purity rhodium triiodide, and the yield of rhodium iodide was 99.70%. The rhodium content measured by PerkinElmer7000DV inductively coupled plasma spectrometer is 20.92%, and the purity is high.

Embodiment 3

[0043]This embodiment is an example of preparing high-purity rhodium triiodide. The preparation method is the same as in Example 1, specifically: 98.4 mL of rhodium trichloride aqueous solution with a rhodium concentration of 25 g / L and 135 g of HI solution with a concentration of 7.5% are placed In the microwave reactor, the microwave power was set to 300W, and when the temperature reached 100°C, the reaction was continued at a constant temperature for 40 minutes. After the reaction was completed, the flow rate was 50g / h of O in the reaction solution. 2 Gas, maintain the reaction at 80°C for 30min. Then the reaction product is filtered; the obtained RhI 3 Wash with ethylene glycol until the washing solution is colorless and transparent. The washed material was dried at 120°C for 6 hours to obtain 11.533 g of high-purity rhodium triiodide, and the yield of rhodium iodide was 99.81%. The rhodium content measured by PerkinElmer7000DV inductively coupled plasma spectrometer is...

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Abstract

The invention provides a preparation method of high-purity rhodium iodide. The preparation method comprises the following steps: reacting rhodium chloride water solution with hydroiodic acid under a microwave radiation condition to obtain rhodium iodide, wherein the heat conduction process is not required in microwave radiation heating, the heating is uniform, and mutual contact and collision of molecules are increased, the conversion rate of the reaction product, namely rhodium iodide, is improved greatly, and the reaction process is easy to operate, quick and energy-saving; after the reaction is finished, continuously blowing oxidizing gases in reaction liquid to convert excess free I<-> ions in solution into I2 simple substances; and then filtering to obtain rhodium iodide, and washing I2 simple substances blended in rhodium iodide by organic solvent according to the characteristic that the I2 simple substances are easily dissolved in the organic solvent to obtain high-purity rhodium iodide. Rhodium iodide with high yield and high purity can be prepared by the preparation method, and the preparation method is simple to operate and low in cost.

Description

technical field [0001] The invention belongs to the field of inorganic compounds, in particular to a method for preparing high-purity rhodium triiodide using a microwave reactor. Background technique [0002] Rhodium triiodide (RhI 3 ) is a black crystalline powder with a Rh content of 19.5-21.3%, which is easily deliquescent in the air; as a catalyst for carbonylation reactions, it is widely used in the synthesis of acetic acid, acetic anhydride, and ethylene glycol. [0003] At present, the preparation methods of rhodium triiodide are mainly divided into three categories, namely solution method, direct synthesis method, and solution method conversion rhodium hydroxide synthesis method. [0004] The solution method is that rhodium trichloride reacts with hydroiodic acid in aqueous solution to generate rhodium triiodide; the reaction formula is: [0005] RhCl 3 +3KI=RhI 3 ↓+3KCl [0006] RhCl 3 +3HI=RhI 3 ↓+3HCl [0007] Specifically, an appropriate amount of potassi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
Inventor 张蕾杨凯宁唐应吉王振宇吴玉秀祈敏赵国静
Owner 陕西煤业化工技术开发中心有限责任公司
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