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A method of reclaiming rhodium from carbonylation reaction organic waste liquid

A technology of organic waste liquid and oxo synthesis, which is applied in the field of rhodium recovery, can solve the problems of short process, high rhodium recovery rate, difficult control of rhodium entrainment loss, etc., and achieve short time required, reduce energy waste, and reduce rhodium in intermediate steps churn effect

Inactive Publication Date: 2011-12-14
杭州凯大催化金属材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The purpose of the present invention is to aim at reasons such as strong binding ability between metallic rhodium and organic compounds, stable polynuclear rhodium complexes, extremely low rhodium concentration in organic waste liquid, and sticky waste liquid. It is not easy to use precipitant for rhodium in waste liquid in wet recovery. , reducing agent to react, can not be fully adsorbed by the adsorbent, fire method recovery has process amplification defects and rhodium entrainment loss is not easy to control and other reasons, to provide a method for reclaiming rhodium from carbonylation reaction organic waste liquid, the method does not need Vacuum distillation, easy for industrial production, suitable for the treatment of large quantities of organic waste liquid, simple equipment, short process, high recovery rate of rhodium

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]Get 5000 milliliters of rhodium-containing organic waste liquid (rhodium content 360ppm) of oxo-synthesizing butyl-octanol, add 50 milliliters of 67% nitric acid aqueous solution, acidify for 2 hours at 25 DEG C under stirring condition; Add 1000 milliliters of water, feed air (air flow rate 3000L / hr) to oxidize and break the complex, maintain the temperature at 80°C for 5 hours, transfer the reaction solution to the separatory funnel after the reaction, and then let it stand for 8 hours. The solution after standing is separated from oil and water. In the lower layer: 900 milliliters of water phase and 4900 milliliters of oil phase were obtained, and the rhodium content of oil phase was determined to be 1.5 ppm by atomic emission spectrometer (ICP, American Thermo Elemental Company, IRIS Intrepid ER / S). Add solid potassium hydroxide to the separated water phase under stirring conditions, adjust the pH value of the reaction solution to 8.0, then raise the temperature to 90...

Embodiment 2

[0032] Get 5000 milliliters of oxo-synthesis butyl octanol rhodium-containing organic waste liquid (rhodium content 510ppm), add 60 milliliters of 36% hydrochloric acid aqueous solution, acidify at 40 DEG C under stirring condition for 3 hours; add 1000 milliliters of 10% sodium hypochlorite solution again, maintain temperature at 90 DEG C Reacted for 3 hours, after the reaction, the reaction solution was transferred to a separatory funnel, and then left to stand for 8 hours; the solution after standing was separated from oil and water, the oil phase was in the upper layer, and the water phase was in the lower layer; 1000 ml of water phase and 4900 ml of oil phase were obtained , The rhodium content of the oil phase was determined to be 3.6ppm. The separated aqueous phase was stirred with solid sodium hydroxide to adjust the pH value of the reaction solution to 7.5, then heated up to 100°C, kept for 1 hour, left to separate and precipitate, and the precipitate was dried to obta...

Embodiment 3

[0034] Get 5000 milliliters of rhodium-containing organic waste liquids (rhodium content 510ppm) of oxo-synthesis butanol, add 50 milliliters of 50% sulfuric acid aqueous solution, and acidify at a temperature of 60°C under stirring conditions for 3 hours; add 1000 milliliters of 20% sodium peroxide aqueous solution, and maintain The temperature was reacted at 80° C. for 5 hours. After the reaction, the reaction solution was transferred to a separatory funnel, and then left to stand for 6 hours; the solution after standing was separated from oil and water, the oil phase was in the upper layer, and the water phase was in the lower layer; 1000 milliliters of the water phase were obtained. The oil phase is 4920 milliliters, and the rhodium content of the oil phase is determined to be 2.3 ppm. The separated aqueous phase was stirred with solid sodium hydroxide to adjust the pH value of the reaction solution to 9.0, then heated up to 100°C, kept for 2 hours, left to separate and pre...

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Abstract

The invention discloses a method for recovering rhodium from organic waste liquid produced in a carbonyl synthesis reaction. The method comprises: adding rhodium-containing organic waste liquid produced in a reaction for synthesizing octanol by using carbonyl into an inorganic acid; acidifying with stirring at 25 to 60 DEG C for 1 to 3 hours; adding oxidation accelerator after acidification, and reacting under a condition of a temperature of 50 to 100 DEG C for 1 to 5 hours; after the reaction is finished, standing reaction solution for 4 to 10 hours, demixing and obtaining a water phase and an oil phase; adding inorganic alkali into the water phase under a stirring condition; regulating the pH value of the reaction solution to 7.0 to 9.5; reacting at 60 to 110 DEG C for 1 to 2 hours; standing, precipitating, filtering out the precipitate, and drying; and thus, obtaining coarse rhodium. The maximum rhodium recovery rate reaches 99.4 percent, the oxidation accelerator may be oxygen, air, ozone, hydrogen peroxide, sodium peroxide, potassium peroxide or sodium hypochlorite; and the rhodium content in the rhodium-containing organic waste liquid is 100 to 600 ppm. The method disclosed by the invention can reduce energy waste, improve total metal rhodium recovery rate, has low equipment requirement, and is suitable for large-volume solution treatment, low in investment, simple in process flow, environment-friendly, quick, high in recovery rate and easy to industrialize.

Description

(1) Technical field [0001] The invention relates to a method for recovering rhodium, in particular to a method for recovering rhodium from organic waste liquid of oxo synthesis reaction. (2) Background technology [0002] At present, the production processes of butanol and octanol in the world are low-pressure improved rhodium propylene carbonyl synthesis, and these processes all use rhodium-phosphine complex catalysts. Because the price of the rhodium catalyst is very high, when the catalyst activity is reduced to a certain extent, the catalyst must be scrapped, the rhodium is reclaimed and processed into a fresh catalyst, which is conducive to the recovery of resources (recovery of precious metals) and environmental protection. [0003] The discarded rhodium-containing organic waste liquid discharged from the oxo reaction vessel is a very complex organic liquid, and rhodium mainly exists in the form of rhodium carbonyl complexes. In addition, the waste liquid also contains...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B11/00
Inventor 姚洪
Owner 杭州凯大催化金属材料股份有限公司
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