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Method for preparing rhodium trichloride hydrate by using silica gel-polyamine resin

A technology for hydrating rhodium trichloride and silica gel polyamine, which is applied in chemical instruments and methods, inorganic chemistry, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, etc., can solve the difficulty of rhodium elution and cannot be directly prepared Problems such as hydrated rhodium trichloride, to achieve the effects of high rhodium adsorption rate, reduced rhodium loss, and simple steps

Active Publication Date: 2015-04-01
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When anion exchange resin is used to purify rhodium acid solution, it is difficult to elute the rhodium adsorbed on the resin, and it needs to be eluted with lye, so what is obtained is an alkaline solution containing rhodium, and rhodium trichloride hydrate cannot be directly obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 1000 g of concentrated sulfuric acid and nitric acid to digest rhodium slag to obtain rhodium acid solution, wherein the mass content of rhodium is 7.2% (0.70mol), the mass content of nitric acid is 3%, the mass content of sulfuric acid is 55%, and the rhodium acid solution is diluted with water When the acid molar concentration was 5.2 mol / L, 368 grams (6.29 mol) of sodium chloride solid was added, and then the solution was heated to reflux for 1 hour. After cooling, the rhodium solution was passed through a layer containing 2L of WP-1 silica gel polymerized amine resin at a linear velocity of 3m / h. After the rhodium in the solution is completely adsorbed by the resin, deionized water and 3mol / L hydrochloric acid solution are used to elute the small amount of sodium, iron, nickel, calcium and other metals remaining in the column and adsorbed on the resin, and then use a concentration of 10mol / L of 90°C hydrochloric acid elutes the rhodium adsorbed on the resin to ...

Embodiment 2

[0033] Take 1000 g of concentrated sulfuric acid and nitric acid to digest rhodium slag to obtain rhodium acid solution, wherein the mass content of rhodium is 1.6% (0.16 mol), the mass content of nitric acid is 5%, the mass content of sulfuric acid is 32%, and the rhodium acid solution is diluted with water To the acid molar concentration of 6.1 mol / L, add 140 grams (2.40 mol) of sodium chloride solid, and then heat the solution to reflux for 1 hour. After cooling, the rhodium solution was passed through a layer containing 2L of WP-1 silica gel polymerized amine resin at a linear velocity of 3m / h. After the rhodium in the solution is completely adsorbed by the resin, deionized water and 3mol / L hydrochloric acid solution are used to elute the small amount of sodium, iron, nickel, calcium and other metals remaining in the column and adsorbed on the resin, and then use a concentration of 6mol / L of 90°C hydrochloric acid elutes the rhodium adsorbed on the resin to obtain refined ...

Embodiment 3

[0035] Take 1000 g of concentrated sulfuric acid and nitric acid to digest rhodium slag to obtain rhodium acid solution, in which the mass content of rhodium is 10.5% (1.02 mol), the mass content of nitric acid is 4%, the mass content of sulfuric acid is 84%, and the rhodium acid solution is diluted with water When the acid molar concentration was 1.2 mol / L, 358 grams (6.12 mol) of sodium chloride solid was added, and the solution was heated to reflux for 1 hour. After cooling, the rhodium solution was passed through a layer containing 2L of WP-1 silica gel polymerized amine resin at a linear velocity of 3m / h. After the rhodium in the solution is completely adsorbed by the resin, deionized water and 3mol / L hydrochloric acid solution are used to elute the small amount of sodium, iron, nickel, calcium and other metals remaining in the column and adsorbed on the resin, and then use a concentration of 12mol / L of 60°C hydrochloric acid elutes the rhodium adsorbed on the resin to ob...

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Abstract

The invention relates to a method for preparing rhodium trichloride hydrate by using silica gel-polyamine resin. The method comprises the following steps: adding water to dilute a rhodium acid digestion solution obtained after digestion of rhodium residues by concentrated sulfuric acid and nitric acid, adding a sodium chloride solid, and heating to reflux the obtained solution; allowing the solution to go through an exchange column filled with silica gel-polyamine resin; and sequentially eluting a small amount of sodium, iron, calcium, nickel and other metals residual in the column and adsorbed to the resin by using deionized water and 1-6mol / L of a hydrochloric acid solution, eluting rhodium adsorbed to the resin by using 6-12mol / L of 50-90DEG C hydrochloric acid, and evaporating the eluted chlororhodic acid solution to obtain the rhodium trichloride hydrate. In the rhodium acid digestion solution, the rhodium content is 1-10wt%, the nitrate content is 1-5wt%, and the sulfuric acid content is 30-85wt%; a molar ratio of sodium chloride to rhodium in the digestion solution is 3-15; and the silica gel-polyamine resin is water soluble polyurethane, and is combined to resin formed on the surface of a silica gel carrier in a covalent bond mode. The method for preparing rhodium trichloride hydrate from the rhodium acid digestion solution has the characteristics of high recovery efficiency, simple process, mild process conditions and the like.

Description

Technical field: [0001] The invention relates to the field of precious metal recycling and utilization, and aims to provide a more efficient method for adsorbing and separating rhodium contained in a rhodium acid digestion solution and then preparing hydrated rhodium trichloride. Background technique: [0002] Rhodium homogeneous organic complex catalyst has the advantages of high catalytic activity and good selectivity. It has important applications in catalytic hydrogenation, olefin hydroformylation, and oxo synthesis catalysis, and many have been used in industrial production. For example: Tris(triphenylphosphine) rhodium chloride is used in industry as a highly efficient olefin hydrogenation catalyst. Acetylacetone dicarbonyl rhodium, triphenylphosphine acetylacetone carbonyl rhodium, tris(triphenylphosphine) carbonyl hydrogen rhodium, three [Tris(m-sulfonate phenyl)phosphine] carbonyl rhodium hydride, etc. are used as high-efficiency olefin hydroformylation catalysts in olef...

Claims

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Application Information

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IPC IPC(8): C01G55/00
Inventor 李晨于海斌蒋凌云李继霞郝婷婷王鹏飞姜雪丹张雪梅
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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