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Method for preparing rhodium chloride hydrate from oxo synthesis waste rhodium catalyst

A technology of oxo synthesis and rhodium catalyst, applied in the field of precious metal recovery, which can solve the problems of large loss of rhodium, harsh temperature control conditions, and low efficiency of the full liquid phase method

Active Publication Date: 2017-01-11
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The present invention aims at the deficiencies in the above-mentioned prior art, and the purpose is to provide a method for reclaiming rhodium from the spent rhodium catalyst of oxo synthesis reaction to prepare rhodium chloride hydrate, to overcome the low efficiency of the full liquid phase method and the existing incineration method or Disadvantages of large loss of rhodium, harsh temperature control conditions or complicated post-treatment, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Take by weighing 20g rhodium-containing waste catalyst (rhodium content 1750ppm) with 100ml quartz crucible, add 30g graphite powder, mix evenly, cover the quartz crucible lid and leave appropriate exhaust slit, place in the muffle furnace roasting, be heated up to 350 ℃, Keep the temperature constant for 3 hours, then raise the temperature to 550°C, keep the temperature constant for 2 hours, cut off the air, continue to raise the temperature to 1150°C, keep the temperature constant for 1 hour, turn off the heating, cut off the air and cool to room temperature to obtain 31.4g of rhodium ash.

[0033] Add rhodium ash to a 1L three-necked flask, place it in an oil bath, add 450ml of hydrochloric acid with a mass concentration of 37%, start stirring, add dropwise 300ml of hydrogen peroxide with a mass concentration of 30%, dissolve the active rhodium in the rhodium ash, filter it with a sand core funnel, The filter residue was washed with distilled water, and the filtrate w...

Embodiment 2

[0039] The raw material, raw material amount, device and steps are the same as in Example 1, except that 15g of activated carbon is added, and the roasting temperature control is as follows: the temperature is raised to 350°C, kept at a constant temperature for 2.5 hours, then raised to 500°C, kept at a constant temperature for 1.5 hours, isolated from the air, and continued to heat up to 1100°C, keep the temperature constant for 1 hour, turn off the heating, and cool to room temperature with the isolation of air to obtain 11.2 g of rhodium ash. The amount of hydrochloric acid with a mass concentration of 37% was 120ml, and the amount of 30% hydrogen peroxide was 80ml.

[0040] Analysis and detection 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 99.6%.

Embodiment 3

[0042] The raw material, raw material amount, device and steps are the same as in Example 2, except that 10g of charcoal powder is added, and the temperature control of roasting is: raise the temperature to 350°C, keep the temperature constant for 2 hours, then raise the temperature to 500°C, keep the temperature constant for 1 hour, cut off the air, and continue to heat up To 1100°C, keep the temperature constant for 0.5 hours, turn off the heating, and cool to room temperature with air isolation to obtain 9.5 g of rhodium ash. The amount of hydrochloric acid with a mass concentration of 37% was 80ml, and the amount of 30% hydrogen peroxide was 50ml.

[0043] 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%.

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Abstract

The invention discloses a method for preparing rhodium chloride hydrate from oxo synthesis waste rhodium catalyst through recycling rhodium, comprising the steps of adding certain amount of carbon into oxo synthesis reaction waste rhodium catalyst and then putting the catalyst into high temperature furnace, burning the catalyst based on certain temperature control program under the aerobic condition, keeping the temperature constant for certain time at the end of procedure to ensure the basic carbonization of the material, turning into anaerobic high temperature roasting,isolating the air and cooling the temperature to the room temperature after high-temperature roasting to obtain the active rhodium ashes, adding concentrated hydrochloric acid, dropping hydrogen peroxide while stirring, dissolving the active rhodium therein to obtain the coarse rhodium chloride acid solution,using the ion exchange method well known in this field to remove such ionic impurities as Fe, Ni and Ca in the coarse rhodium chloride acid solution, and then obtaining the rhodium chloride hydrate after concentration and drying. The filter residues generated from filtration are the carbon residues and used after being returned. This method is characterized by high efficiency, simple operation and small rhodium loss with rhodium yield exceeding 99%.

Description

[0001] Technical field: [0002] The invention relates to the technical field of precious metal recovery, and more precisely provides a method for recovering rhodium from waste rhodium catalysts of oxo synthesis reaction to prepare rhodium chloride hydrate. [0003] Background technique: [0004] 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-phosphine complex catalyst is the most commonly used catalyst for olefin oxo synthesis. In industrial production operations, rhodium-phosphine complex 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. Economical and efficient recovery of spent catalysts The rhodium in is very necessary. Rhodium chloride hydrate is the basic raw materi...

Claims

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Application Information

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IPC IPC(8): C22B1/02C22B7/00C22B11/00
CPCC22B1/02C22B7/007C22B7/009C22B11/048Y02P10/20
Inventor 蒋凌云李晨于海斌孙彦民李继霞郝婷婷王鹏飞王本雷
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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