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Method for preparing rhodium triiodide

A technology of rhodium triiodide and rhodium iodide acid, which is applied in the field of catalyst preparation, can solve the problems of complex preparation technology operation, non-environmental protection rhodium conversion rate, difficult batch production, etc., and achieve the effect of complex operation, low cost and complete reaction

Inactive Publication Date: 2015-06-10
KUNMING BOREN PRECIOUS METALS
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AI Technical Summary

Problems solved by technology

[0005] In the prior art, the synthetic method of rhodium triiodide mainly contains solution method, direct synthetic method and solution method conversion rhodium hydroxide synthetic method, and its preparation technology is constantly perfected and improved, and the report total yield has also been improved to 98.5%, but The disadvantage is that it is limited by the process conditions. These preparation technologies are complex in operation, harsh in conditions, high in cost, not environmentally friendly, and the conversion rate of rhodium is not high, so it is difficult to achieve mass production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0024] Preparation example one: the preparation of nanometer rhodium powder:

[0025] At room temperature, dissolve rhodium trichloride (0.1mol) in 100ml of water, add ethylenediamine (0.25mol) to react for 0.5h under continuous stirring to obtain an aqueous solution of ethylenediamine and rhodium complex, slowly drop 100g of formaldehyde with a concentration of 37% forms a suspension, slowly adds 0.5M sodium hydroxide solution to the suspension until the pH of the suspension is 14, and then uses ultrasonic vibration for 20 minutes, and then the suspension Put the liquid into a microwave oven with a power of 800W for 5 minutes, and then place the suspension at room temperature to cool naturally, so that the ethylenediamine and rhodium complexes are reduced to nano-rhodium powder and precipitate in the suspension. The precipitate is separated from the suspension, washed with ethanol and deionized water, and vacuum-dried to obtain nano-rhodium powder. The particle size range of ...

preparation Embodiment 2

[0026] Preparation example two: the preparation of nanometer rhodium powder

[0027] Add 200ml of PEG300 and 30ml of rhodium trichloride aqueous solution with a concentration of 50mg / ml into a 500ml round-bottomed flask in turn, and shake for 15 minutes with the assistance of an ultrasonic oscillator. After the rhodium trichloride is evenly dispersed, heat it in an 800W microwave oven 5 minutes, be cooled to room temperature, obtain suspension, separate and obtain precipitate from this suspension in centrifugal mode, wash with ethanol, deionized water, vacuum-dry, obtain nanometer rhodium powder 0.73g, measure nanometer rhodium powder particle size by TEM The diameter range is 1.5-4.5nm.

Embodiment 1

[0028] Embodiment 1: the method for preparing rhodium triiodide

[0029]Take by weighing 5.0g particle size scope and be that the nano-rhodium powder of 15nm-100nm is put into the U-shaped electrolytic cell of glass material, add the hydroiodic acid saturated solution of 100ml iodine, the concentration of the hydroiodic acid used for configuring this solution is 8mol / L . An alternating current of 60 volts was applied between the electrodes of the two graphite rods, the magnitude of the current was 25 amperes, and the electrolytic reaction was carried out for 7 hours, and the temperature of the electrolyte was kept at 90° C. After electrolysis finishes, filter electrolytic solution, wash, distill excess hydrogen iodide and water in the filtrate, obtain iodorhodium acid H 3 RhI 6 Concentrated solution, the rhodium content of rhodium iodide acid concentrated solution is 1.2mol / L, puts iodorhodium acid concentrated solution into crystallization furnace and crystallizes at 350 DE...

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Abstract

The invention provides a method for preparing rhodium triiodide, belonging to a noble metal catalyst and mainly solving the problems of economical efficiency and environment friendliness in preparation of the rhodium triiodide catalyst. The rhodium triiodide is generated by nano rhodium powder and a hydroiodic acid solution by electrolysis. The method comprises the following steps: 1, adding a potassium iodide solution of iodine and the nano rhodium powder into a U-shaped electrolytic cell, and loading alternating current between two electrodes, till the rhodium powder is dissolved to generate a rhodium iodate solution; 2, filtering the electrolyte, washing, distilling the filtrate to separate out excessive hydrogen iodide and water from the filtrate and obtain a rhodium iodate concentrate, and then crystallizing the rhodium iodate concentrate in a crystallization furnace to obtain rhodium triiodide; and 3, recycling the distilled hydroiodic acid solution and water. In the preparation method of the rhodium triiodide, the primary reaction conversion rate of rhodium is high (more than or equal to 99.9%), the yield and the purity are high; and the method is economic, environment-friendly, simple in operation and low in cost.

Description

technical field [0001] The invention discloses a preparation method of a precious metal rhodium catalyst, in particular to a method for preparing rhodium triiodide. Background technique [0002] Rhodium triiodide is an important noble metal homogeneous catalyst, which is mainly used in the production of acetic acid prepared by methanol carbonylation. As an important chemical raw material, acetic acid has an annual global demand of nearly 10 million tons in recent years. Among them, the methanol carbonylation method accounts for more than 65% of the total production capacity of acetic acid, and it is increasing year by year. Along with annual demand of acetic acid and methanol carbonylation account for the total production capacity of acetic acid increases year by year, the rhodium triiodide catalyst needed in its production process also increases year by year. Due to the complex operation, harsh conditions, low yield, high cost, and non-environmental protection of the domes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
Inventor 高传柱王天帅李琰
Owner KUNMING BOREN PRECIOUS METALS
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