A kind of method for measuring rhodium content in bisphosphine ligand rhodium catalyst

A technology of rhodium catalyst and bisphosphine ligand, which is applied in the direction of measurement device, test sample preparation, color/spectral characteristic measurement, etc. It can solve the problems of unreported, cumbersome steps, complicated operation, etc., and shorten the processing time , good repeatability and simple operation

Active Publication Date: 2021-12-24
LIAOCHENG MEIWU NEW MATERIAL SCI & TECHCO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is complicated to operate and the steps are cumbersome
In the hydroformylation reaction, the catalytic activity and the selectivity of the bisphosphine ligand rhodium catalyst are better than the monophosphine ligand rhodium catalyst, but the detection method of rhodium content in the bisphosphine ligand rhodium catalyst in the prior art has not yet been seen. to report

Method used

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  • A kind of method for measuring rhodium content in bisphosphine ligand rhodium catalyst
  • A kind of method for measuring rhodium content in bisphosphine ligand rhodium catalyst
  • A kind of method for measuring rhodium content in bisphosphine ligand rhodium catalyst

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Experimental program
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Effect test

Embodiment 1

[0025] (1) Microwave digestion treatment of the sample: Weigh 0.10 g of the bisphosphine ligand rhodium catalyst and add it to the digestion tank, add 8 mL of nitric acid solution, put it into the microwave digestion instrument, set the digestion program for digestion, and perform acid removal treatment after the sample digestion is completed , cooled to room temperature, set aside, and make a blank at the same time.

[0026] Table 1 Microwave digestion program

[0027]

[0028] (2) Preparation of sample solution: Dilute the solution cooled to room temperature in step (1) with 1% nitric acid to prepare blank and sample solutions, dilute the blank and sample solutions, add 1mL LaCl 3 After the solution is constant volume, it is the solution to be tested.

[0029] (3) Preparation of rhodium standard solution: the rhodium standard solution with a concentration of 1000 μg / mL was diluted with 1% dilute nitric acid to 100 μg / mL for later use. A series of rhodium standard soluti...

Embodiment 2

[0036] Microwave digestion treatment of samples: Weigh 0.20g of bisphosphine ligand rhodium catalyst into the digestion tank, add 12mL of nitric acid, put it into the microwave digestion instrument, set the digestion program for digestion, after the sample digestion is completed, carry out acid removal treatment, and cool to room temperature , spare, and blank at the same time.

[0037] Table 3 Microwave digestion program

[0038]

[0039] (2) Preparation of sample solution: Dilute the solution cooled to room temperature in step (1) to prepare blank and sample solutions, dilute the blank and sample solutions with 5% dilute nitric acid, add 1mL LaCl 3 After constant volume, it is the solution to be tested.

[0040] (3) Preparation of rhodium standard solution: the rhodium standard solution with a concentration of 1000 μg / mL was diluted with 5% dilute nitric acid to 100 μg / mL for later use. A series of rhodium standard solutions with concentrations of 0.0, 1.0, 2.5, 5.0, 8....

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Abstract

The invention relates to a method for measuring rhodium content in a bisphosphine ligand rhodium catalyst, which mainly includes the following steps: (1) microwave digestion treatment of a sample: adding a bisphosphine ligand rhodium catalyst sample into a digestion tank, and adding nitric acid solution, Put it into the microwave digestion apparatus, set up the digestion program for digestion, after the sample is digested, carry out acid removal treatment, cool to room temperature, set aside, and make a blank at the same time. (2) Preparation of sample solution; (3) Preparation of rhodium standard solution; (4) Drawing of standard curve; (5) Determination of rhodium content. The method of the invention has the advantages of simple operation, rapidity, good repeatability, high accuracy, etc., and is suitable for the determination of metal elements in similar substances.

Description

technical field [0001] The invention relates to a method for measuring the rhodium content in a bisphosphine ligand rhodium catalyst, in particular to a method for measuring the rhodium content in a bisphosphine ligand rhodium catalyst by microwave digestion-flame atomic absorption spectrometry. Background technique [0002] At present, the methods for determining rhodium content in rhodium catalysts generally adopt gravimetric method and extraction method, and these two methods are complicated to operate and take too long (3h-4h). For example, the patent 201510460700.3 Method for Determination of Rhodium Content in Water-Soluble Rhodium-Phosphine Complexes discloses the technology of hexamminecobalt nitrate precipitation method to determine the rhodium content. It is necessary to process the digested solution in multiple steps, and then add hexamminecobalt nitrate precipitation agent. Multi-step washing, and finally drying to constant weight. The method is complicated to o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/31G01N1/44
CPCG01N1/44G01N21/3103
Inventor 孙彩虹庞玉娜尹萌萌冯庆霞宫斌
Owner LIAOCHENG MEIWU NEW MATERIAL SCI & TECHCO
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