A kind of preparation method of trivalent rhodium acetate trimer

A technology of rhodium acetate trimer and glacial acetic acid, applied in the field of preparation of trivalent rhodium acetate trimer, can solve problems such as poor solubility, long synthesis time, easy dehydration, etc., and achieves increasing reaction rate, shortening production cycle, accelerating The effect of the precipitation reaction

Active Publication Date: 2022-06-21
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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  • A kind of preparation method of trivalent rhodium acetate trimer

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

[0044] (1) after mixing rhodium powder and potassium chloride, feed chlorine gas at a flow rate of 0.1~5L / min, and react at 500~800 ℃ for 1~5h;

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

[0046] (3) in rhodium hydroxide, add water, 60~65wt% nitric acid and glacial acetic acid, the mass ratio of described rhodium hydroxide, water, nitric acid and glacial acetic acid is 1:2~30:0.5~3:1~5, The reaction is carried out at 30 to 90° C. for 0.5 to 3 hours, the solution is evaporated to dryness, and after nitrification is carried out with glacial acetic acid, the acid is carried out with water to obtain trivalent rhodium acetate trimer.

[0047] Optionally, in step (2), before adding potas...

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, pass chlorine gas at a flow rate of 1L / min, and react for 3h.

[0055] (2) dissolving the product obtained in step (1) in 0.5L water, filtering, adding 15wt% potassium hydroxide solution to the filtrate to adjust the pH to 8.0, reacting for 1h, filtering, and washing with 2L deionized water times to obtain Pure Rhodium Hydroxide. After testing, the yield of rhodium hydroxide prepared from potassium chlororhodate was 96.0%.

[0056] (3) get the rhodium hydroxide (0.100mol) that the rhodium content is 10.29g, add 100g deionized water to it, add 65% analytically pure nitric acid 29.08g and glacial acetic acid 28.00g simultaneously, 60 ℃ of stirring reflux 1h, filter , placed in an evaporating dish and evaporated to drynes...

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, pass chlorine gas at a flow rate of 4L / min, and react for 2h.

[0060] (2) dissolving the product obtained in step (1) in 1L water, filtering, adding 25wt% potassium hydroxide solution to the filtrate to adjust the pH to 9.0, reacting for 1.5h, filtering, and washing with 6L deionized water times to obtain Pure Rhodium Hydroxide. After testing, the yield of rhodium hydroxide prepared from potassium chlororhodate was 96.1%.

[0061] (3) get the rhodium hydroxide (0.488mol) that the rhodium content is 50.23g, add 400g deionized water to it, add 65% analytically pure nitric acid 150.00g and glacial acetic acid 300.00g simultaneously, 80 ℃ of stirring reflux 1.5h, Filtration, placed in an evaporating dish and evaporated t...

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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 trimer, comprising the following steps: (1) mixing rhodium powder and potassium chloride, and then introducing chlorine gas for reaction; (2) mixing The product obtained in step (1) is dissolved in water, filtered, potassium hydroxide is added to the filtrate for reaction, and rhodium hydroxide is obtained after filtering and washing; (3) water, nitric acid and glacial acetic acid are added to rhodium hydroxide Carry out the reaction, evaporate the solution to dryness after the reaction is completed, use glacial acetic acid to remove the nitrate, and then use water to remove the acid to obtain trivalent rhodium acetate trimer. The invention adopts nitric acid and glacial acetic acid to dissolve rhodium hydroxide, and then uses glacial acetic acid to catch up with the nitric acid, so that the reaction speed can be obviously accelerated, thereby increasing the yield of trivalent rhodium acetate trimer.

Description

technical field [0001] The invention relates to the technical field of inorganic synthesis, in particular to a preparation method of a trivalent rhodium acetate trimer. Background technique [0002] Trivalent rhodium acetate trimer is an important pharmaceutical catalyst, which 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 not only be used as a rhodium source for supported catalysts, but also a series of derivatives can be obtained by group substitution to adapt to different reaction 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] Currently known trivalent rhodium acetate trimer preparation methods have the following two: [0005] 1. Utilize the divalent rhodium acetate dimer obtained by ...

Claims

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Application Information

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Patent Type & Authority Patents(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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