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Treatment method of rhodium-containing catalyst and rhodium-containing catalyst

A technology of rhodium catalyst and treatment method, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, rhodium organic compounds, etc., can solve the problems of low recovery rate of rhodium treatment, improve recovery effect, reduce production cost, and realize recovery and the effect of recycling

Pending Publication Date: 2021-12-03
CHINA PETROLEUM & CHEM CORP +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a kind of processing method of rhodium-containing catalyst in order to overcome the low problem of the treatment recovery rate of rhodium in the rhodium-containing catalyst existing in the prior art, use this method to improve the recovery effect of rhodium

Method used

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  • Treatment method of rhodium-containing catalyst and rhodium-containing catalyst
  • Treatment method of rhodium-containing catalyst and rhodium-containing catalyst
  • Treatment method of rhodium-containing catalyst and rhodium-containing catalyst

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preparation example Construction

[0101] The preparation of triphenylphosphinecarbonyl rhodium acetylacetonate in the present invention can adopt following method to carry out: the rhodium trichloride that reclaims obtains and acetylacetone carry out the first reaction under the existence of solvent A, obtain acetylacetonate dihydroxy rhodium; Acetone dihydroxyrhodium and the recovered triphenylphosphine are subjected to a second reaction in the presence of solvent B to obtain triphenylphosphinecarbonyl rhodium acetylacetonate.

[0102] According to the present invention, in the first reaction, the recovered rhodium trichloride can be dissolved in solvent A, then mixed with acetylacetone, heated and reacted and then cooled to precipitate dihydroxyrhodium acetylacetonate crystals. The solvent A may be selected from N,N-dimethylformamide and / or N,N-dimethylacetamide, preferably N,N-dimethylformamide. The volume to mass ratio of solvent A to rhodium trichloride may be 30-100:1 mL / g, preferably 30-60: 1 mL / g, more...

Embodiment 1

[0112] 1) 1000g of acetylacetonate triphenylphosphine carbonyl rhodium acetylacetonate solution produced in the process of oxo alcohol (mainly butanol / octanol) is subjected to vacuum distillation, the temperature of the vacuum distillation is 120°C, and the pressure is -0.09MPa, The time was 4 hours, and 644 g of a rhodium-containing catalyst solution was obtained, wherein the concentration of rhodium was 300 ppm. After adding formaldehyde with a mass ratio of 1:1 to the rhodium-containing catalyst solution, a hydrochloric acid solution with a concentration of 10% by weight was added to adjust the pH of the formaldehyde and rhodium-containing catalyst solution to 3. The mixture was extracted at 120° C. for 1 h, and aqueous phase A and oil phase A were obtained by separation;

[0113] 2) Adjust the pH of the aqueous phase A to 9 with sodium carbonate, and filter to obtain a solid phase. Hydrochloric acid with a concentration of 10% by weight was added to the solid phase to adj...

Embodiment 2

[0123] Carry out according to the method for embodiment 1, difference is, the mass ratio of the formaldehyde added in step 1) and rhodium-containing catalyst solution is 0.8:1; Step 2) in the mass ratio of methanol and solid phase is 2.4:1; Step 3 ) in the mass ratio of isothiazolinone and oil phase A is 0.4:1. As a result, the recovery rate of the obtained triphenylphosphine was 98.3%, the total recovery rate of rhodium was 99.7%, and the crystal yield of triphenylphosphinecarbonyl rhodium acetylacetonate was 98.4%.

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Abstract

The invention relates to the technical field of catalysts, and discloses a treatment method of a rhodium-containing catalyst and the rhodium-containing catalyst prepared by using triphenylphosphine and / or rhodium obtained by the treatment method as raw materials. The method comprises the following steps: 1) extracting a rhodium-containing catalyst solution with aldehyde and an inorganic acid solution A, and separating to obtain a water phase A and an oil phase A; 2) adjusting the pH value of the water phase A to be more than 7, and carrying out solid-liquid separation to obtain a solid phase; and 3) reacting the oil phase A with an oxidant under an acidic condition to obtain an oxidation product, extracting the oxidation product by using an inorganic acid solution B and a water-soluble rhodium extraction agent, and separating to obtain the water phase B and the oil phase B. By using the method, the rhodium recovery effect can be improved.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a method for treating a rhodium-containing catalyst and a rhodium-containing catalyst prepared from triphenylphosphine and / or rhodium obtained by treating the method. Background technique [0002] Rhodium-containing catalysts are widely used in hydroformylation, formylation and hydroxylation, but they are expensive and have high production costs. In large-scale industrial production, a large amount of rhodium-containing catalyst waste liquid will be produced. If the rhodium-containing catalyst in this waste liquid can be treated and recycled, the recycling of resources will be realized and the production cost of enterprises will be reduced. [0003] He Yulian's "Extraction-Solvent Recrystallization Method Recovers Triphenylphosphine from Carbonyl Catalyst Waste Liquid" ("Industrial Catalysis", Supplement to Volume 12 in 2014, Pages 389-390) discloses a method to recover triphen...

Claims

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Application Information

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IPC IPC(8): C07F9/50C01G55/00C07F15/00B01J31/24B01J31/20
CPCC07F9/5022C01G55/005C07F15/008B01J31/2404B01J31/20B01J2531/822B01J2531/0238
Inventor 蒋绍洋伊红亮张玉景苑志伟陆贤史建公胡学武陆建军张寒张鑫杰孙岩颜明俊
Owner CHINA PETROLEUM & CHEM CORP
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