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Method for preparing rhodium chloride hydrate by recovering rhodium from dead rhodium catalyst of oxo synthesis

A rhodium catalyst, a technology for carbonyl synthesis, applied in chemical instruments and methods, inorganic chemistry, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, etc., can solve complex post-processing, low efficiency of all liquid phase methods, and loss of rhodium. Large and other problems, to achieve the effect of simple operation, avoiding rhodium entrainment loss, and small rhodium loss

Active Publication Date: 2014-05-07
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims at the deficiencies in the above-mentioned prior art, and provides a method for reclaiming rhodium from the waste rhodium catalyst of oxo synthesis reaction to prepare rhodium chloride hydrate, which overcomes the low efficiency of the full liquid phase method and the existing incineration method. Or the shortcomings of large loss of rhodium, or complicated post-treatment, etc., absorbing the advantages of incineration and liquid phase methods, high efficiency, simple operation, small loss of rhodium, and recovery of rhodium in the form of rhodium chloride hydrate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 20g of rhodium-containing waste catalyst (rhodium content 1750ppm) in a 100ml quartz crucible, add 30g of silica powder, mix well, cover the quartz crucible with a proper venting gap, place it in a muffle furnace for dry distillation and roasting, and heat up to 400°C , keep the temperature for 2 hours, then raise the temperature to 600° C., and keep the temperature for 1 hour to get 32.2 grams of rhodium ash.

[0026] Add rhodium ash to a 1L three-neck flask, place it in an oil bath, add 700ml of concentrated hydrochloric acid, start stirring, heat to 100°C, pass through ozone and oxidize until there are no gray and black particles in the material system, filter it with a sand core funnel, and use distilled water Wash the filter residue and collect the filtrate. The filtrate is purified by a cation exchange resin to obtain a refined rhodium chloride acid solution, and the refined rhodium chloride acid solution is concentrated and dried to obtain high-purity rhodi...

Embodiment 2

[0032] The raw material, raw material amount, device and steps are the same as in Example 1, except that 18g of silicon dioxide powder is added; the temperature control of dry distillation and roasting is as follows: the temperature is raised to 400°C, kept at a constant temperature for 1.5 hours, then raised to 550°C, and kept at a constant temperature for 0.5 hours to obtain rhodium 20.4 grams of ash; the amount of hydrochloric acid added for acidification and oxidation was 360ml, and the temperature of acidification and oxidation was 90°C.

[0033] Analysis and detection results show that the total amount of rhodium trichloride impurity elements is 0.046%, which meets the first-grade product quality index of YS / T593-2006, and the calculated rhodium yield is 99.5%.

Embodiment 3

[0035] Use a 100ml quartz crucible to weigh 20g of rhodium-containing waste catalyst distilled rhodium slag (rhodium content 4.7%), add 6g of silica powder, mix well, cover the quartz crucible with a proper venting gap, and place it in a muffle furnace for dry distillation and roasting. Raise the temperature to 400°C and keep the temperature constant for 1 hour, then raise the temperature to 550°C and keep the temperature constant for 0.5 hour to obtain 8.1 g of rhodium ash.

[0036]Add rhodium ash into a 250ml three-neck flask, place it in an oil bath, add 100ml of concentrated hydrochloric acid, start stirring, heat to 80°C, pass through ozone and oxidize until there are no grayish black particles in the material system, filter it with a sand core funnel, and use distilled water Wash the filter residue and collect the filtrate. The filtrate is purified by a cation exchange resin to obtain a refined rhodium chloride acid solution, and the refined rhodium chloride acid solutio...

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Abstract

The invention discloses a method for preparing rhodium chloride hydrate by recovering rhodium from dead rhodium catalysts of oxo synthesis. The method is characterized by comprising: adding a certain amount of silica solid adsorbent in the dead rhodium catalysts of the oxo synthesis reactions, placing the mixture into a high-temperature furnace to perform destructive distillation baking through a certain temperature control program, adding a certain amount of concentrated hydrochloric acid into residue obtained through the destructive distillation baking, leading enough amount of ozone into the mixture by controlling the certain temperature until no charcoal grey particle exists in a system, and performing filtering washing to obtain coarse chlororhodic acid solution; and removing plasma impurities including Fe, Ni, Ca and the like in the chlororhodic acid solution by means of a well-known ion exchange method, and performing concentrating and drying to obtain the rhodium chloride hydrate.

Description

Technical field: [0001] The invention relates to the technical field of precious metal recovery, and more precisely provides a method for recovering rhodium from oxo synthesis spent rhodium catalysts to prepare rhodium chloride hydrate. 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. Due to the scarcity of rhodium resources and the high price, if the rhodium catalytic system is to be economically tenable, it depends on whether the rhodium in the spent catalyst can be ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G55/00
Inventor 蒋凌云于海斌李继霞李晨李俊郝婷婷
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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