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Method for recovering rhodium to produce rhodium chloride hydrate from oxo synthesis reaction waste rhodium catalyst

A hydrated rhodium chloride, rhodium catalyst technology, applied in chemical instruments and methods, inorganic chemistry, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, etc., can solve the problem of low efficiency and complex post-processing of the all-liquid-phase digestion method , rhodium loss and other problems, to avoid rhodium loss, simple operation, high rhodium yield effect

Active Publication Date: 2017-03-29
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The present invention aims at the deficiencies in the above-mentioned prior art, and provides a method for preparing rhodium chloride hydrate by reclaiming rhodium from the spent rhodium catalyst of the oxo synthesis reaction, which overcomes the low efficiency of the full liquid phase digestion method and the existing incineration method. Or the shortcomings of large loss of rhodium, or complicated post-treatment, etc., its efficiency is high, the loss of rhodium is small, the post-treatment is simple, and rhodium is recovered in the form of rhodium chloride hydrate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 500g of rhodium-containing waste catalyst (rhodium content 1750ppm) and put it into a 1L two-necked flask, add 80g of dimethylformamide, place it in an oil bath with magnetic stirring, connect one port to the condensing device and the tail gas treatment device, and the other port to nitrogen , start stirring and mixing, slowly introduce nitrogen, and raise the temperature step by step: first, control the temperature of the oil bath to 90°C, and evaporate the light components; When no liquid drops flowed out again, the temperature of the oil bath was controlled to 180° C., and the temperature was kept constant for 1.5 hours to obtain 116.5 g of raffinate.

[0028] Add 120mL ethanol to the residual liquid to dilute, filter with a sand core funnel, wash the filter residue three times with 60mL ethanol, blow dry, add 37% hydrochloric acid 10mL, 30% hydrogen peroxide 5mL to dissolve the filter residue successively, and collect the rhodium chloride solution , after dilut...

Embodiment 2

[0034] The raw material, raw material quantity, device and steps are the same as in Example 1, except that 60g of dimethylformamide is added; the temperature is raised step by step: firstly, the temperature of the oil bath is controlled to 90°C, and the light components are evaporated; Control the temperature of the oil bath to 155°C; when there is no droplet flowing out of the evaporation and condensation device again, control the temperature of the oil bath to 185°C and keep the temperature constant for 2.0 hours. 102.8 g of raffinate was obtained.

[0035] Analysis and testing results show that the total amount of impurity elements in rhodium trichloride 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

[0037] Get 50g of rhodium-containing waste catalyst distillation rhodium slag (rhodium content 4.7%) and add in 500mL two-necked flask, add 120g of dimethylformamide, place in an oil bath with magnetic stirring, connect a condensing device and a tail gas treatment device at one port, Connect the other port with nitrogen, turn on stirring and mixing, slowly introduce nitrogen, and increase the temperature step by step: first control the temperature of the oil bath to 90°C, and evaporate the light components; when there is no liquid drop out of the evaporation and condensation device, control the temperature of the oil bath to 158°C ; When no liquid drops flow out from the evaporating and condensing device again, control the temperature of the oil bath to 185° C. and keep the temperature constant for 2 hours. 43.5 g of raffinate was obtained.

[0038]Add 50 mL of ethanol to the residual liquid to dilute, filter with a sand core funnel, wash the filter residue three times with 90...

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Abstract

The invention discloses a method for reclaiming rhodium from a waste rhodium catalyst of an oxo synthesis reaction to prepare a rhodium chloride hydrate. The method comprises the following steps: adding dimethyl formamide into a waste rhodium catalyst solution, uniformly stirring and mixing, and stepwise heating in the existence of nitrogen; collecting vapor by a condensing device, treating tail gas with a water spray absorption tower, diluting the residual liquid with ethanol, and filtering; washing the filter residues with ethanol to obtain a simple substance of active rhodium, adding concentrated hydrochloric acid and hydrogen peroxide into the simple substance of active rhodium, and dissolving to obtain a rhodium chloride solution; and removing iron, nickel, calcium and other impure ions with ionic exchange resin to obtain a refined chlororhodic acid solution, and concentrating and drying the refined chlororhodic acid solution to obtain high purity rhodium trichloride. The method has high efficiency, simple operation small rhodium loss and a rhodium yield of more than 99 percent.

Description

[0001] Technical field: [0002] The invention relates to the technical field of precious metal recovery, in particular to a method for preparing rhodium chloride hydrate by recovering rhodium from waste rhodium catalysts of oxo synthesis reaction. [0003] Background technique: [0004] 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 spen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G55/00
Inventor 蒋凌云李晨于海斌孙彦民李继霞郝婷婷王鹏飞
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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