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Method for preparing rhodium chloride through recovering rhodium from incinerated waste rhodium residues

A technique of rhodium chloride and roasting, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum halides, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, etc. , deal with complex, harsh temperature control conditions and other issues, to achieve the effect of promoting dissolution, simplifying subsequent operations, and improving roasting conditions

Active Publication Date: 2018-04-06
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although these methods can increase the yield of rhodium, the harsh temperature control conditions have too high requirements for industrial production operations, which is not conducive to production stability, and based on the consideration of rhodium overburning, there are still some organics that cannot be removed by incineration. deal with complex

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take by weighing 20g (rhodium content 2.54%) batching rhodium slag with 100ml quartz crucible, cover the quartz crucible cover and leave appropriate exhaust slit, place in the high-temperature furnace with gas inlet and outlet, the gas outlet is connected to the tail gas detection device, the gas inlet Air was added, the temperature was raised to 980° C., and roasted at a constant temperature. After the tail gas was detected to be free of carbon oxides, the heating was turned off and cooled to room temperature to obtain 10.91 g of rhodium ash.

[0025] Add rhodium ash into a 500ml four-necked PTFE flask, place it in an oil bath, connect the tail gas absorption device, add 35ml of 40% hydrofluoric acid, start stirring, heat up to 60°C, stir at constant temperature for 2 hours, add 60% perchloric acid Add 120ml of 36% hydrochloric acid, dropwise add 60ml of 30% hydrogen peroxide while stirring, stir until the rhodium ash is completely dissolved, filter with a sand core fun...

Embodiment 2

[0031] The raw material, raw material quantity, device and steps are the same as in Example 1, except that 54ml of 50% hydrofluoric acid is added, stirring is started, heating is raised to 70°C, stirring at constant temperature for 2 hours, 20ml of 70% perchloric acid is added, and stirring and heating are continued To emit white smoke, add 160ml of 37% hydrochloric acid, dropwise add 160ml of 50% hydrogen peroxide while stirring, and stir until the rhodium ash is completely dissolved.

[0032] Analysis and testing results show that the total amount of impurity elements in rhodium trichloride is 0.048%, which meets the first-grade product quality index of YS / T593-2006, and the calculated rhodium yield is 99.3%.

Embodiment 3

[0034] Raw material, raw material amount, device and steps are the same as Example 1, the difference is that 47ml of 50% hydrofluoric acid is added, stirring is started, heating is raised to 65°C, constant temperature is stirred for 2 hours, 14ml of 70% perchloric acid is added, and stirring and heating are continued To white smoke, add 140ml of 36.5% hydrochloric acid, add dropwise 112ml of 50% hydrogen peroxide while stirring, and stir until the rhodium ash is completely dissolved.

[0035] Analysis and detection results show that the total amount of impurity elements in rhodium trichloride is 0.045%, which meets the first-grade product quality index of YS / T593-2006, and the calculated rhodium yield is 99.5%.

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PUM

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Abstract

The invention provides a method for preparing rhodium chloride through recovering rhodium from incinerated waste rhodium residues. The method comprises the steps of firstly carrying out aerobic high-temperature roasting on waste catalyst roasting rhodium residues with incompletely removed organic matters, thus thoroughly removing the organic matters, and obtaining rhodium ash; then adding hydrofluoric acid and perchloric acid into the rhodium ash for pretreating, adding hydrochloric acid and hydrogen peroxide for directly dissolving the rhodium residues, and filtering to obtain a coarse rhodium acid solution; finally adopting an ion exchange method for the coarse chlororhodic acid solution to remove ion impurities such as Fe, Ni and Ca, and then concentrating and drying to obtain rhodium chloride hydrate. According to the method provided by the invention, a roasted rhodium residue post-treatment process is simplified, the efficiency is high, the rhodium loss is less, and the rhodium yield is larger than 99 percent.

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 incinerated waste rhodium slag to prepare rhodium chloride hydrate. Background technique: [0002] Oxylation technology has become one of the most active frontier fields in the development of catalytic technology, and has become the development direction of modern chemical industry. Rhodium catalyst is the most commonly used catalyst for the oxo reaction of olefins. In industrial production operations, rhodium catalysts are easily poisoned by trace impurities and deactivated. The deactivated rhodium-containing catalyst waste liquid needs to be discharged at regular intervals. Rhodium resources are scarce and expensive, and rhodium in spent catalysts must be recovered. Rhodium chloride hydrate is the basic raw material for preparing rhodium compounds such as rhodium catalysts, and it is of great significance to recl...

Claims

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Application Information

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IPC IPC(8): C01G55/00
CPCC01G55/005
Inventor 蒋凌云王本雷李晨李继霞郝婷婷王鹏飞
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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