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A kind of carbonylation catalyst reaction waste liquid treatment method

A technology for oxo synthesis and waste liquid treatment, which is applied in chemical instruments and methods, special compound water treatment, oxidized water/sewage treatment, etc. The effect of convenience, simple equipment and high organic removal rate

Active Publication Date: 2016-09-14
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention aims at the above disadvantages of high energy consumption, low economic benefit and secondary pollution of DMF in the treatment and recovery of wastewater, and proposes a new method for treating DMF-containing wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh the carbonyl rhodium acetylacetonate reaction waste liquid. It is known that the content of DMF is about 50g / L and the content of acetylacetone is 5g / L. After diluting ten times with deionized water, take 100ml into a 250ml flask and place it in an oil bath at 50°C , turn on the magnetic stirring, after the temperature is stable, add 10% Ru / Fe 2 o 3 Catalyst 5g / L, after reacting for 2 hours, stop heating, filter, get filtrate and measure metal ion content and COD value. The experiment was repeated three times, and the results were averaged. The leaching concentration of Ru ions in the filtrate was 0.3 mg / L, and the leaching concentration of Fe ions was 1 mg / L, and the COD removal rate of the solution reached 99.6%.

Embodiment 2

[0022] Weigh the reaction waste liquid of rhodium carbonyl acetylacetonate, known DMF content is about 50g / L, acetylacetone content is 5g / L, dilute ten times with deionized water, take 100ml into a 250ml flask, and place it in an oil bath at 80°C , turn on the magnetic stirring, after the temperature is stable, add 1%Pt / 20%CoO-79Fe 2 o 3 Catalyst 5g / L, after reacting for 1 hour, stop heating, filter, take filtrate and measure metal ion content and COD value. The experiment was repeated three times, and the results were averaged. The leaching concentration of Pt ions is 0.1 mg / L, the leaching concentration of Co ions is 0.1 mg / L, and the leaching concentration of Fe ions is 0.8 mg / L. The COD removal rate of the solution reaches 99.7%.

Embodiment 3

[0024] Weigh the carbonyl rhodium acetylacetonate reaction waste liquid. It is known that the DMF content is about 50g / L and the acetylacetone content is 5g / L. After diluting ten times with deionized water, take 100ml into a 250ml flask and place it in an oil bath at 30°C , turn on magnetic stirring, after the temperature stabilizes, add 1% Au / 42% CeO-57Fe 2 o 3 Catalyst 5g / L, after reacting for 3 hours, stop heating, filter, get filtrate and measure metal ion content and COD value. The experiment was repeated three times, and the results were averaged. The leaching concentration of Au ions is 0.2mg / L, the leaching concentration of Ce ions is 0.2mg / L, and the leaching concentration of Fe ions is 0.7mg / L. The COD removal rate of the solution reaches 99.7%.

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Abstract

The invention relates to an oxo catalyst reaction waste liquid treatment method. The method adopting an intermittent heterogeneous phase technology to process a waste liquid comprises the following steps: adding an iron oxide immobilized metal catalyst into an oxo catalyst reaction waste liquid, stirring at 30-80DEG C for 1-6h, filtering, and separating, wherein the oxo catalyst reaction waste liquid is a reaction waste liquid obtained after the preparation of acetylacetonatocarbonyl rhodium from dimethyl formamide (DMF); the pH value of the waste liquid is 1-6, and the waste liquid contains 5-20mass% of the DMF and 0.2-2mass% of acetylacetone; the iron oxide immobilized metal catalyst comprises a iron oxide immobilized metal single substance active component, the metal oxide is one or more of iron oxide, copper oxide, cobalt oxide and cerium oxide , and the metal single substance active component is one or more of ruthenium, palladium, platinum, gold and nickel; and the mass proportion of iron oxide in the catalyst is 40-95%, the mass proportion of other metal oxides in the catalyst is 20-60%, and the mass proportion of the metal simple substance active component in the catalyst is 1-10%.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of dimethylformamide wastewater, and relates to a method for purifying wastewater containing dimethylformamide, in particular to a method for treating oxo catalyst reaction waste liquid. Specifically, it is a method for treating wastewater containing dimethylformamide (DMF) by a heterogeneous Feton reagent method. technical background [0002] Olefin carbonylation reaction is an important method for industrial synthesis of aldehydes or alcohols. Propylene carbonylation of butanol and octanol is the most representative carbonylation technology. The existing domestic production capacity of butanol (octyl) alcohol exceeds 2000kt / a, and the average annual demand for catalysts The amount is more than 4000kg, and currently the acetylacetonate carbonyl phosphine-rhodium complex catalyst is mainly used. The synthesis of the catalyst intermediate rhodium acetylacetonate dicarbonyl main...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F1/72C02F101/38
CPCC02F1/725C02F2101/38C02F2305/026
Inventor 李继霞蒋凌云于海斌李俊姜雪丹李晨郝婷婷王鹏飞
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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