Preparation method of trivalent rhodium acetate tripolymer

A technology of rhodium acetate trimer and glacial acetic acid, which is applied in the field of preparation of trivalent rhodium acetate trimer, can solve problems such as easy dehydration, poor solubility, and long synthesis time, so as to accelerate precipitation reaction, increase reaction rate, shorten The effect of the production cycle

Active Publication Date: 2022-03-15
浙江微通催化新材料有限公司
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Problems solved by technology

This method has the following problems: the raw material (divalent rhodium acetate dimer) itself is more difficult to obtain, and the synthesis time is long, the yield is low, and the product obtained by synthesis is mixed in a divalent state and a trivalent state and is difficult to separate
Compared with the divalent rhodium acetate dimer oxidation method, the raw material of the method of this patent is easy to obtain, and the yield is relatively high, but there are also the following two problems at the same time: one is that rhodium hydroxide reacts in weakly acidic ice Relatively poor solubility in acetic acid will adversely affect the yield and production cycle of the trivalent rhodium acetate trimer; the second is that rhodium hydroxide is easily dehydrated in the drying process, which will also adversely affect the follow-up reaction

Method used

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  • Preparation method of trivalent rhodium acetate tripolymer

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[0043] A preparation method of trivalent rhodium acetate trimer, comprising the following steps:

[0044] (1) After mixing the rhodium powder and potassium chloride, feed chlorine gas at a flow rate of 0.1 to 5 L / min, and react at 500 to 800° C. for 1 to 5 hours;

[0045] (2) Dissolve the product obtained in step (1) in water, filter, add 10-40wt% potassium hydroxide solution to the filtrate so that the pH value is between 7-10, react for 0.5-2h, filter and wash , obtain rhodium hydroxide;

[0046] (3) add water, 60~65wt% nitric acid and glacial acetic acid in rhodium hydroxide, the mass ratio of described rhodium hydroxide, water, nitric acid and glacial acetic acid is 1:2~30:0.5~3:1~5, React at 30-90° C. for 0.5-3 hours, evaporate the solution to dryness, use glacial acetic acid to remove the nitrate, and then use water to remove the acid to obtain trivalent rhodium acetate trimer.

[0047] Optionally, in step (2), before adding potassium hydroxide, add positively modified...

Embodiment 1

[0053] A preparation method of trivalent rhodium acetate trimer, comprising the following steps:

[0054] (1) Mix 30g of rhodium powder and 100g of potassium chloride evenly, put it into a quartz boat, transfer it to a medium-temperature tube furnace at 600°C, feed chlorine gas at a flow rate of 1L / min, and react for 3h.

[0055] (2) Dissolve the product obtained in step (1) in 0.5L water, filter, add 15wt% potassium hydroxide solution to the filtrate to adjust the pH to 8.0, react for 1h, filter, and wash with 2L deionized water several times to obtain Pure rhodium hydroxide. After detection, the yield of preparing rhodium hydroxide by potassium chlororhodate is 96.0%.

[0056] (3) Get rhodium hydroxide (0.100mol) containing 10.29g of rhodium, add 100g of deionized water to it, then add 29.08g of 65% analytically pure nitric acid and 28.00g of glacial acetic acid at the same time, stir and reflux at 60°C for 1h, filter , placed in an evaporating dish and evaporated to dryne...

Embodiment 2

[0058] A preparation method of trivalent rhodium acetate trimer, comprising the following steps:

[0059] (1) Mix 100g of rhodium powder and 200g of potassium chloride evenly, put it into a quartz boat, transfer it to a medium-temperature tube furnace at 650°C, feed chlorine gas at a flow rate of 4L / min, and react for 2h.

[0060] (2) Dissolve the product obtained in step (1) in 1L of water, filter, add 25wt% potassium hydroxide solution to the filtrate to adjust the pH to 9.0, react for 1.5h, filter, and wash with 6L of deionized water several times to obtain Pure rhodium hydroxide. After detection, the yield of preparing rhodium hydroxide by potassium chlororhodate is 96.1%.

[0061] (3) get the rhodium hydroxide (0.488mol) that rhodium content is 50.23g, add 400g deionized water wherein, add 65% analytical pure nitric acid 150.00g and glacial acetic acid 300.00g simultaneously again, 80 ℃ stir and reflux 1.5h, Filter, place in an evaporating dish and evaporate to dryness;...

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Abstract

The invention relates to the technical field of inorganic synthesis, and discloses a preparation method of a trivalent rhodium acetate tripolymer, which comprises the following steps: (1) mixing rhodium powder and potassium chloride, and introducing chlorine for reaction; (2) dissolving the product obtained in the step (1) in water, filtering, adding potassium hydroxide into the filtrate for reaction, filtering and washing to obtain rhodium hydroxide; and (3) adding water, nitric acid and glacial acetic acid into rhodium hydroxide for reaction, after the reaction is completed, evaporating the solution to dryness, performing nitrate removal with glacial acetic acid, and performing acid removal with water to obtain the trivalent rhodium acetate tripolymer. The nitric acid and the glacial acetic acid are adopted to dissolve rhodium hydroxide, and then the glacial acetic acid is used for removing nitrate, so that the reaction can be obviously accelerated, and the yield of the trivalent rhodium acetate tripolymer is improved.

Description

technical field [0001] The invention relates to the technical field of inorganic synthesis, in particular to a preparation method of trivalent rhodium acetate trimer. Background technique [0002] Trivalent rhodium acetate trimer is an important pharmaceutical catalyst that can catalyze various reactions of olefins and aromatic hydrocarbons. At the same time, trivalent rhodium acetate has good solubility in water and is an important rhodium precursor. It can be used as a rhodium source for supported catalysts, and a series of derivatives can be obtained by group substitution to adapt to different React environment. The molecular formula of trivalent rhodium acetate trimer is C 14 h 27 o 18 Rh 3 , the molecular weight is 792.07, and the structural formula is as follows: [0003] [0004] Known trivalent rhodium acetate trimer preparation method has following two kinds at present: [0005] 1. Utilize the divalent rhodium acetate dimer obtained by synthesis, add a sui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C08F292/00C08F220/34
CPCC07F15/008C08F292/00C08F220/34
Inventor 魏青马银标谢智平陈华杨立强黄鹏罗来彬陈小勤潘剑明
Owner 浙江微通催化新材料有限公司
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