Method for preparing high-purity rhodium trichloride from carbonyl-synthetic-reaction waste rhodium catalyst degradation solution

A rhodium catalyst, a technology for carbonyl synthesis, applied in chemical instruments and methods, inorganic chemistry, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, etc. The effect and efficiency of impurity removal can reduce the burden of impurity removal and achieve the effect of efficient extraction.

Active Publication Date: 2015-03-11
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the digestion solution needs to be diluted to a lower concentration, the concentration of the precipitant added is also very low, and the amount of subsequent treatment solution is large; in addition, there is no pre-removal of cations, which leads to an excessive burden on ion exchange and affects ion exchange. The effect and efficiency of impurity removal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Get waste rhodium catalyst digestion solution (rhodium content 0.35%, sulfate radical content 75.20%, phosphate radical content 17.50%, iron content 0.040%, nickel content 0.0025%, calcium content 0.42%) 20 grams, dilute with 40 grams of deionized water to obtain Digestion diluent.

[0025] In addition, weigh 0.2 grams of analytically pure sodium sulfide and make a 12% solution with deionized water (in the form of S 2- gauge), heated to 60°C.

[0026] Control the temperature of the digestion diluent to 80°C, and slowly add the prepared hot sodium sulfide solution while stirring to carry out the precipitation reaction. After the precipitation is completed, filter and wash the precipitate with 6mol / L hydrochloric acid.

[0027] Separately take commercially available 37% analytically pure hydrochloric acid and commercially available 30% analytically pure hydrogen peroxide, and prepare a mixed solution at a volume ratio of 1:1.

[0028] Dissolve the precipitate with the p...

Embodiment 2

[0034] The operation process is the same as in Example 1, and the difference is that the digestion solution is diluted with 6 grams of water, and sodium sulfide is made into a 4% solution (in S 2- meter); the sodium sulfide solution was heated to 90°C, and the temperature of the digestion diluent was controlled to be 120°C;

[0035] Wash the rhodium sulfide precipitate with 12mol / L hydrochloric acid; dissolve the rhodium sulfide precipitate, hydrochloric acid and hydrogen peroxide mixture, and the ratio of hydrochloric acid volume to hydrogen peroxide volume is 3:1.

[0036] The analysis and detection results of the obtained rhodium trichloride showed that the total amount of impurity elements in the rhodium trichloride was 0.026%, which was in line with the first-grade product quality index of YS / T593-2006, and the rhodium yield was calculated to be 99.4%.

Embodiment 3

[0038] The operation process is the same as in Example 1, and the difference is that the digestion solution is diluted with 15 grams of water, and sodium sulfide is made into a 10% solution (in S 2- meter); the sodium sulfide solution was heated to 80°C, and the temperature of the digestion diluent was controlled to be 110°C;

[0039] Wash the rhodium sulfide precipitate with 10mol / L hydrochloric acid; dissolve the rhodium sulfide precipitate, hydrochloric acid and hydrogen peroxide mixture, and the ratio of hydrochloric acid volume to hydrogen peroxide volume is 2:1.

[0040] The analysis and detection results of the obtained rhodium trichloride showed that the total amount of impurity elements in the rhodium trichloride was 0.022%, which was in line with the first-grade product quality index of YS / T593-2006, and the rhodium yield was calculated to be 99.7%.

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Abstract

The invention discloses a method for preparing high-purity rhodium trichloride from a carbonyl-synthetic-reaction waste rhodium catalyst degradation solution. The method comprises: diluting a degradation solution obtained by using a sulfuric acid and nitric acid mixed solution or a sulfuric acid, nitric acid, hydrochloric acid and hydrogen peroxide mixed solution to degrade a carbonyl-synthesis waste rhodium catalyst, heating, adding excess water-soluble sulphurizing salt hot solution to precipitate rhodium, filtering, using a hydrochloric acid solution to washing the precipitate, adding a hydrochloric acid and hydrogen peroxide mixed solution to dissolve the precipitate, filtering, employing an ion exchange method known in the field to process the filtrate to remove Fe, Ni, Ca and other ionic impurities, concentrating and drying to obtain the high-purity rhodium trichloride.

Description

Technical field: [0001] The invention relates to the fields of waste catalyst recovery and precious metal chemical industry, more precisely, it provides a method for preparing high-purity rhodium trichloride from a waste rhodium catalyst digestion solution in an oxo synthesis reaction. Background technique: [0002] Carbonylation is an extremely important reaction in the chemical industry, including carbonylation of olefins to aldehydes, carbonylation of methanol to acetic acid, carbonylation of methyl acetate to acetic anhydride, etc. Rhodium-phosphine complex catalysts are the most commonly used catalysts for carbonylation reactions. In industrial production operations, rhodium-phosphine complex catalysts are often deactivated due to the presence of various high-boiling by-products and impurities in the raw materials during the reaction. The mass fraction of rhodium in the earth's crust is very low, it is difficult to mine and refine, and it is expensive. Therefore, it is...

Claims

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Application Information

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IPC IPC(8): C01G55/00
Inventor 蒋凌云李晨于海斌李继霞李俊于玺郝婷婷姜雪丹
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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