Preparation method of acetylacetone triphenylphosphine carbonyl rhodium

A technology of acetone triphenylphosphine and acetylacetone, which is applied in the field of precious metal catalyst synthesis, can solve the problems of harsh reaction conditions, olefin conversion rate decline, catalyst poisoning, etc., and achieve the goal of increasing product yield, improving product purity and reducing by-products the effect produced

Pending Publication Date: 2022-06-07
JINCHUAN GROUP LIMITED +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the yield of triphenylphosphine rhodium acetylacetonate has been improved to a certain extent through technical improvement and condition control, due to the long reaction cycle and harsh reaction conditions, it is easy to introduce non-catalytically active rhodium black and chloride ions exceeding the standard, and the intermediate product uses Organic solvents are used for recrystallization, and product processing requires repeated washing with a large amount of water
[0006] In addition, a large number of domestic and foreign patents clearly point out that chlorine can cause triphenylphosphine carbonyl rhodium acetylacetonate poisoning
There are reports at home and abroad that the chloride ion in the olefin formylation unit exceeds the standard, resulting in a decrease in the conversion rate of olefins and even a catalyst poisoning that leads to production shutdown.
Rhodium is extremely rare in the earth's crust, and its mining and enrichment are difficult and costly. It is the most expensive metal of the platinum group metals. Due to the special chemical properties of rhodium, the cost of rhodium recovery and refining is relatively high

Method used

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  • Preparation method of acetylacetone triphenylphosphine carbonyl rhodium
  • Preparation method of acetylacetone triphenylphosphine carbonyl rhodium
  • Preparation method of acetylacetone triphenylphosphine carbonyl rhodium

Examples

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Effect test

Embodiment 1

[0025]Preparation method of acetylacetonone triphenylphosphinecarbonyl rhodium, comprising the following steps:

[0026] Step 1: In a three-mouth flask equipped with a reflux condenser, the rhodium content of 0.1g of rhodium oxide 0.122g is dissolved in 0.6g of acetylacetone solution, after stirring and mixing evenly, using a water ring vacuum pump, continuously evacuated under a vacuum degree of -0.08Mpa and injected nitrogen with a pressure of 0.02Mpa three times, the oxygen content in the three-mouth flask can be achieved less than 1000ppm;

[0027] Step 2, reflux: add 1ml of ammonia to the mixed solution prepared in step 1, heat up to 120 ° C, stir at the reflux temperature for 1.5h, when the solution is converted from black to brownish yellow, inject 0.28g triphenylphosphine and 0.05 g of anaerobic acetaldehyde, continue the reflux reaction at 120 °C, stir the reaction for 1.5 hours, stop heating, and cool the solution to room temperature;

[0028] Step 3, filtration washing:...

Embodiment 2

[0032] Preparation method of acetylacetonone triphenylphosphinecarbonyl rhodium, comprising the following steps:

[0033] Step 1, mixing: In the three-mouth flask equipped with a reflux condenser, the rhodium content of 0.1g of rhodium oxide 0.122g is dissolved in 1g of acetylacetonate solution, after stirring and mixing evenly, using a water ring vacuum pump, continuously evacuated under a vacuum degree of -0.08Mpa and injected nitrogen with a pressure of 0.02Mpa three times, the oxygen content in the three-mouth flask can be achieved less than 1000ppm;

[0034] Step 2, reflux: add 1ml of ammonia to the mixed solution prepared in step 1, heat up to 120 ° C, stir at the reflux temperature for 1.5h, when the solution is converted from black to brownish yellow, inject 0.31g triphenylphosphine and 0.08 g of anaerobic acetaldehyde at a time, continue the reflux reaction at 120 °C, stir the reaction for 1.5 hours, stop heating, and cool the solution to room temperature;

[0035]Step 3,...

Embodiment 3

[0039] Preparation method of acetylacetonone triphenylphosphinecarbonyl rhodium, comprising the following steps:

[0040] Step 1, mixing: In the three-mouth flask equipped with a reflux condenser, the rhodium content of 0.1g of rhodium oxide 0.122g is dissolved in 1g of acetylacetonate solution, after stirring and mixing evenly, using a water ring vacuum pump, continuously evacuated under a vacuum degree of -0.08Mpa and injected nitrogen with a pressure of 0.02Mpa three times, the oxygen content in the three-mouth flask can be achieved less than 1000ppm;

[0041] Step 2, reflux: add 1ml of ammonia to the mixed solution prepared in step 1, heat up to 120 ° C, stir at the reflux temperature for 1.5h, when the solution is converted from black to brownish yellow, inject 0.38g triphenylphosphine and 0.2 g of anaerobionaldehyde at a time, continue the reflux reaction at 120 °C, stir the reaction for 1.5 hours, stop heating, and cool the solution to room temperature;

[0042] Step 3, fil...

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Abstract

The invention discloses a preparation method of acetylacetone triphenylphosphine carbonyl rhodium, which comprises the following steps: stirring and mixing rhodium oxide and acetylacetone, adding an initiator, heating to reflux temperature, reacting, adding fatty aldehyde of triphenylphosphine when the system becomes brown yellow from black, and continuing reacting at reflux temperature to obtain acetylacetone triphenylphosphine carbonyl rhodium; after the reaction is finished, cooling, adding deionized water, filtering, washing a filter cake by using the deionized water, and carrying out vacuum drying on the filter cake to obtain acetylacetonatocarbonyl triphenylphosphine rhodium. The preparation method provided by the invention can be used for preparing acetylacetonatocarbonyltriphenylphosphine rhodium which causes the catalyst to be poisoned and has low chlorine impurity content, meanwhile, since acetylacetone is both a reactant and a solvent in the reaction, side reactions are reduced, and the obtained acetylacetonatocarbonyltriphenylphosphine rhodium product is high in yield and purity, does not need to be washed repeatedly, and is suitable for industrial production. And the product can be directly applied after drying.

Description

Technical field [0001] The present invention relates to the field of synthesis of precious metal catalysts, in particular to a method for preparing acetylacetone triphenylphosphinocarbonyl rhodium. Background [0002] Rhodium catalyst is an important catalytic material, which has been widely used in petrochemical, pharmaceutical chemical, fine chemical and environmental protection fields in the past 30 years. [0003] Acetylacetone triphenylphosphinocarbonyl rhodium with the formula Rh(C 5 H 7 O 2 )(CO)(PPh 3 ), referred to as ROPAC, is an oxygen - oxygen ligand ligand chelated rhodium organics, some olefin hydroformylation reaction has a high activity, high selectivity and positive isomerization ratio, and the reaction conditions are quite mild, less side reactions, is the current low-pressure carbonyl synthesis method used in the main catalyst. [0004] Acetylacetone triphenylphosphinecarbonyl rhodium is usually prepared from water and rhodium trichloride as raw materials. Acco...

Claims

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Application Information

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IPC IPC(8): C07F15/00
CPCC07F15/008Y02P20/584
Inventor 张静胡家彦白延利刘国旗曹笃盟任志勇李欢王红梅孟俊杰郅欢欢高嵩张宗磊王一帆朱婷高志磊
Owner JINCHUAN GROUP LIMITED
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