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Preparation method of rhodium trichloride hydrate

A technology of rhodium trichloride and hydrate, which is applied in the field of catalyst synthesis, can solve the problems of complicated process, unsuitable for batch production, and long processing cycle, and achieve the effect of improving reaction yield and reducing waste liquid

Pending Publication Date: 2022-03-01
浙江微通催化新材料有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a simple process, but the treatment cycle is too long, chlorine gas is likely to be generated during the electrolysis process to pollute the environment, and it is not suitable for mass production
[0006] In the prior art, rhodium hydroxide precipitation is usually obtained first, then impurity ions are removed by washing, and finally hydrochloric acid is added to dissolve to obtain rhodium trichloride hydrate. The process is relatively complicated, requires a large amount of reagent consumption and produces a large amount of waste water; The cycle is long, the processing capacity is small and a large amount of waste gas is generated

Method used

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preparation example Construction

[0027] The invention provides a kind of preparation method of rhodium trichloride hydrate, comprising the following steps:

[0028] 1) reacting the chlororhodium salt solution and a reducing agent to obtain rhodium powder;

[0029] 2) Rhodium powder and chlorine are reacted to obtain a rhodium-containing mixture;

[0030] 3) After reacting the rhodium-containing mixture with hydrochloric acid, filter to obtain a chlororhodium acid solution;

[0031] 4) The chlororhodium acid solution is subjected to rotary evaporation to obtain rhodium trichloride hydrate.

[0032] Step 1) of the present invention preferably adjusts the pH value of the chlororhodium salt solution to obtain a mixed solution; the mixed solution preferably includes a clarified solution and a precipitate; the reducing agent is slowly added to the boiled precipitate for reaction to obtain rhodium powder; adjust the pH value The reagent used is preferably an alkali solution; the pH value is preferably adjusted to ...

Embodiment 1

[0060] With the sodium hydroxide solution that mass concentration is 5%, the pH value of the aqueous solution of 100g sodium chlororhodium acid (in the aqueous solution of sodium chlororhodium acid, the mass fraction of rhodium is 5%) is adjusted to 7.5, obtains the mixed solution, leaves standstill clarification . Decant the supernatant in the mixed solution, boil the remaining precipitate, add 15.0g of sodium formate dihydrate at a rate of 3g / min at 130°C for reduction, filter to obtain rhodium powder after the reduction, and deionize the rhodium powder with deionized water Wash until neutral, vacuum-dry at 70°C and 85KPa for 2 hours before use.

[0061] Put the obtained rhodium powder in a quartz boat, then place the quartz boat in a medium-temperature chlorination furnace, and react with chlorine gas with a flow rate of 1L / min at 400°C for 2h to obtain a mixture of anhydrous rhodium trichloride and rhodium powder . Put the mixture into a positive pressure reactor, add 11...

Embodiment 2

[0065] The 15.0g sodium formate dihydrate in embodiment 1 is changed into 8.4g formic acid, and other conditions are identical with embodiment 1.

[0066] The quality of the rhodium trichloride hydrate in Example 2 is 12.0 g, the rhodium content is 39.6% after detection, and the yield is 95.04%.

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Abstract

The invention belongs to the technical field of catalyst synthesis. The invention provides a preparation method of rhodium trichloride hydrate, which comprises the following steps: reacting a chlororhodate solution with a reducing agent to obtain rhodium powder; reacting rhodium powder with chlorine to obtain a rhodium-containing mixture; reacting the rhodium-containing mixture with hydrochloric acid, and filtering to obtain a chlororhodium acid solution; and carrying out rotary evaporation on the chlororhodium acid solution to obtain the rhodium trichloride hydrate. According to the invention, an intermediate product sodium chlororhodate or potassium chlororhodate in a rhodium recovery process is adopted as a raw material, and the rhodium powder with relatively high activity is prepared through a reducing agent, so that the single reaction yield is improved; water-insoluble rhodium trichloride is directly converted into a water-soluble rhodium chloride acid solution by using the positive pressure reactor, and the rhodium trichloride hydrate can be obtained through rotary evaporation, so that washing by using a large amount of deionized water can be avoided, and the generation of waste liquid is reduced.

Description

technical field [0001] The invention relates to the technical field of catalyst synthesis, in particular to a preparation method of rhodium trichloride hydrate. Background technique [0002] Rhodium trichloride hydrate is an important catalyst precursor. Since metal rhodium is very insoluble in various acids, many important rhodium catalysts, such as triphenylphosphine rhodium chloride, triphenylphosphine acetylacetonate carbonyl rhodium, Rhodium acetate and the like are prepared from rhodium trichloride. The most commonly used preparation method of rhodium trichloride is to obtain sodium chlororhodium (potassium) by rhodium powder and sodium chloride (potassium) medium temperature chlorination, then add alkali to obtain the hydroxide precipitation of rhodium, and the chloride ion in the precipitation After washing, add hydrochloric acid to dissolve and evaporate to obtain. There is also rhodium powder dissolved with sodium bisulfate (potassium) to obtain sodium sulfate (p...

Claims

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Application Information

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IPC IPC(8): C01G55/00
CPCC01G55/005
Inventor 魏青刘斌谢智平潘剑明马银标王冠群陈华黄鹏杨立强王惟鞠景喜施春苗
Owner 浙江微通催化新材料有限公司
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