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Method for digesting spent rhodium catalyst in carbonyl group synthetic reaction

A technology for oxo synthesis and rhodium catalyst, applied in the field of catalysis, can solve problems such as reducing digestion efficiency and prolonging digestion time, and achieves the effects of improving digestion efficiency, increasing rhodium yield and shortening digestion time

Inactive Publication Date: 2012-06-13
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, nitric acid, perchloric acid, and hydrochloric acid described in this method are all volatile acids, and are generally sold in the form of aqueous solutions. Concentrated acids such as fuming nitric acid, due to the rapid decomposition of nitric acid in the digestion process, a considerable amount of water will also be generated into the digestion system, and the presence of water in the digestion process will greatly reduce the digestion efficiency and prolong the digestion time; It will decompose and volatilize rapidly under high temperature conditions, and the acid that actually acts on the digestion reaction is less

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 60g rhodium-containing waste catalyst (rhodium content 1750ppm) in the there-necked flask, place in oil bath, install stirring and tail gas absorption bottle, after adding the full carbonization of concentrated sulfuric acid (no bubbles emerge in the absorption bottle), add sodium nitrate solid, Adding speed control system continues to emit bubbles slowly, and control temperature at 170°C-175°C. After 8.0 hours, the system solution is clear and transparent. Take a sample and add water to test that the solution is still clear. At this time, the spent catalyst is completely digested, and rhodium becomes soluble rhodium salt. After analysis, detection and calculation, the yield of rhodium is 99.3%.

[0022] Rhodium yield adopts following formula to calculate:

[0023] Rhodium yield=(mass of solution after digestion×mass percentage of rhodium in solution after digestion) / (mass of rhodium-containing waste catalyst×mass percentage of rhodium of waste catalyst)×100%

[00...

Embodiment 2

[0026] The raw materials, raw material amounts, devices and steps are the same as in Example 1, except that the temperature is controlled at 180° C. to 185° C. After 6.5 hours, the system solution is clear and transparent, and the rhodium yield is 99.5%.

Embodiment 3

[0028] Different from Example 2, after adding concentrated sulfuric acid and fully carbonizing (no bubbles emerge in the absorption bottle), potassium nitrate solid is added, and the addition speed control system continues to slowly emit bubbles. After 6.8 hours, the system solution was clear and transparent, and the rhodium yield 99.4%.

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Abstract

The invention discloses a method for digesting spent rhodium catalyst in carbonyl group synthetic reaction, which is characterized by adding concentrated sulfuric acid into the spent rhodium catalyst in carbonyl group synthetic reaction for carbonization; and then adding alkali metal nitrate solid for digestion until solution of a system is clear and transparent; at this moment, organic matters are digested and removed in a format of carbon dioxide, and rhodium exists in acidic solution in a format of soluble salt. The method disclosed by the invention is high in recovery rate of rhodium, environment-friendly, moderate in operating condition, and high in efficiency.

Description

Technical field: [0001] The invention relates to the technical field of catalysis; it is a method for digestion of spent rhodium catalysts for oxo synthesis reactions, more precisely, it provides a method for eliminating organic components in waste rhodium catalysts for oxo synthesis reactions and turning rhodium into soluble salts . 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. Because rhodium resources are scarce and expensive, it is extremely important in indust...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B11/00
CPCY02P10/20
Inventor 蒋凌云于海斌李晨李继霞李俊
Owner CHINA NAT OFFSHORE OIL CORP
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