Method for preparing high purity rhodium trichloride by removing impurity from liquid phase digestion solution of waste rhodium catalyst

A technology of high-purity rhodium trichloride and rhodium catalyst is applied in the direction of improving process efficiency, can solve the problems of dilute concentration of the sample to be processed, high energy consumption for concentration, etc., and achieves the effects of mild process conditions, simple operation and easy industrialization.

Inactive Publication Date: 2014-01-22
CHINA NAT OFFSHORE OIL CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The impurity removal method of ion exchange resin requires the concentration of the sample to be treated to be extremely dilute, so that a large amount of water will be used, which will make the subsequent concentration consume more energy.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The first step is to take the spent rhodium catalyst digestion solution (rhodium content 0.02 ~ 0.5wt%, other metal impurities are: sodium 10 ~ 15wt%, calcium 0.01 ~ 0.06wt%, iron 0.01 ~ 0.04wt%, nickel 0.001 ~ 0.004wt% %,) 30g, adjust the rhodium salt solution pH=1.5 with sodium hydroxide. 130 g of sodium oxalate solution with a mass concentration of 1% was added under stirring. The above mixture was stirred for 30 minutes and filtered to obtain a clear filtrate.

[0022] In the second step, dilute the filtrate 10 times with deionized water and heat it to a slight boiling state. Slowly add 1wt% sodium hydroxide solution dropwise to adjust the pH=8. Fully washed with water to obtain rhodium gel. Prepare 6 mol / L hydrochloric acid to dissolve the rhodium gel, then evaporate, concentrate and dry the obtained rhodium salt solution to obtain rhodium trichloride. Analysis and testing results show that the total amount of impurity elements in rhodium trichloride is 0.046%, ...

Embodiment 2

[0028] The operation process is the same as in Example 1, except that the pH is adjusted to 3.5 in the first step. The obtained rhodium trichloride analysis and detection results show that the total amount of impurity elements in rhodium trichloride is 0.039%, which meets the first-grade product quality index of YS / T593-2006. After calculation, the rhodium yield is 99.8%.

Embodiment 3

[0030] The operation process is the same as in Example 1, except that pH=5 is adjusted in the first step. The obtained rhodium trichloride analysis and detection results show that the total amount of impurity elements in rhodium trichloride is 0.042%, which meets the first-grade product quality index of YS / T593-2006. After calculation, the rhodium yield is 99.4%.

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Abstract

The invention discloses a method for preparing high purity rhodium trichloride by removing impurities from a liquid phase digestion solution of a waste rhodium catalyst. The method is characterized by comprising the following steps: step one, taking liquid phase digestion solution obtained by digesting waste rhodium catalyst for carbonyl synthesis with concentrated sulfuric acid and nitrate, adjusting to pH value to 1-5 by using sodium hydroxide, dropwise adding a sodium oxalate solution with stirring so that the solution becomes turbid, continuing adding the sodium oxalate solution until complete precipitation, stirring for 20-40 min and filtering to obtain the filtrate, wherein the concentration of sodium oxalate solution is 1-10 wt%; and two, directly heating the filtrate obtained in the step one or diluting the filtrate with deionized water by 10 times and heating to a boiling state, adjusting the pH value to 8 with 1%-15% sodium hydroxide solution, stirring and filtering to obtain a rhodium gel; and dissolving the rhodium gel in 6 mol / L hydrochloric acid, and evaporating, concentrating and drying the solution to obtain high-purity three rhodium trichloride. The method of the invention is applicable to recovery of noble metal rhodium from the waste rhodium catalyst from carbonyl synthesis, and is economical and environment-friendly; and the method has the advantages of mild reaction conditions, simple operation and easiness for industrialization.

Description

technical field [0001] The invention relates to a method for preparing high-purity rhodium trichloride by removing impurity ions from the digestion solution of spent rhodium catalyst, more specifically, recovering precious metal rhodium from the liquid-phase digestion solution of waste rhodium catalyst for oxo synthesis to prepare high-purity rhodium trichloride Methods. Background technique [0002] As one of the most commonly used catalysts for oxo synthesis in the chemical industry, rhodium-phosphine complex catalysts have a series of advantages, such as high catalytic activity, mild catalytic reaction conditions, low equipment requirements, and the addition of an appropriate amount of phosphine ligands can Increase the normal isomerization ratio of the product and increase the output value. However, in the long-term industrial production process, external impurities will reduce the activity of the rhodium catalyst, and the formation of the rhodium cluster complex will d...

Claims

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Application Information

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IPC IPC(8): C22B11/00C22B7/00
CPCY02P10/20
Inventor 于海斌郝婷婷李晨蒋凌云李继霞李俊
Owner CHINA NAT OFFSHORE OIL CORP
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