Preparation method of rhodium complex

A rhodium complex and reactor technology, applied in the directions of rhodium organic compounds, chemical instruments and methods, platinum group organic compounds, etc., can solve the problems of high production cost, unfavorable environment and safety, high rhodium price, etc. The effect of production time, increased utilization, and easy operation

Active Publication Date: 2020-03-31
铜陵欣诺科新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation method of triphenylphosphinecarbonyl rhodium acetylacetonate needs to use a large amount of solvents and needs to be distilled, which is very unfavorable to the environment and safety, and the steps are cumbersome and costly.
[000...

Method used

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  • Preparation method of rhodium complex

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Experimental program
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Effect test

Embodiment 1

[0024] Dissolve 1 mole of rhodium chloride in pure water; dissolve 1.05 moles of acetylacetone and 1.05 moles of triphenylphosphine in N,N-dimethylformamide and toluene (1:1); use hydroxymethylpolyphenyl Ethylene (CAS 66072-40-0) was filled into the two-stage 5L reactor; at 120°C, the rhodium trichloride solution and the acetylacetonate triphenylphosphine solution were added according to the reaction ratio and passed through the two-stage reactor at 5ml / min; The product uses condensed water for condensation and crystallization, and the liquid is transferred to the previous step for the next reaction. The obtained product was analyzed by an elemental analyzer as C 58.6%, H 4.5%, Rh content 20.82%, product purity over 99%, and primary yield 89%.

Embodiment 2

[0026] 1 mole of rhodium chloride was dissolved in pure water; 1.05 moles of acetylacetone and 1.05 moles of triphenylphosphine were dissolved in the reaction solution of Example 1; p-hydroxystyrene was used to fill the two-stage 5L reactor; at 120 ℃, add rhodium trichloride solution and triphenylphosphine acetylacetonate solution according to the reaction ratio and pass through the two-stage reactor at 5ml / min; the product uses condensed water for condensation crystallization, and the liquid is transferred to the previous step for the next reaction. The obtained product is analyzed by an elemental analyzer as C58.6%; H4.5%, Rh content is 20.82%, product purity is more than 99%, and primary yield is 90%.

Embodiment 3

[0028] Dissolve 1 mole of rhodium chloride in pure water; dissolve 1.05 moles of acetylacetone and 1.05 moles of triphenylphosphine in N,N-dimethylformamide and toluene (1:1); use hydroxymethylpolyphenyl Ethylene (CAS 66072-40-0) is filled into the two-stage 50L reactor; at 120°C, the rhodium trichloride solution and the triphenylphosphine acetylacetonate solution are added in proportion and passed through the two-stage reactor at 150ml / min; the product Condensed water is used for condensation crystallization, and the liquid is transferred to the previous step for the next reaction. The obtained product was analyzed by an elemental analyzer as C 58.6%, H 4.5%, Rh content 20.82%, product purity over 99%, and yield 88%.

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Abstract

The invention provides a preparation method of rhodium complex acetylacetonatocarbonyltriphenylphosphine rhodium. The preparation method comprises the following steps of: S1, dissolving rhodium metalsalt into pure water; S2, adding acetylacetone and triphenylphosphine into the same solvent, and performing uniform stirring; S3, filling a reactor with self-made redox resin; S4, adding a rhodium trichloride solution in S1 and the mixed solution of acetylacetone and triphenylphosphine in S2 into the reactor in proportion at a proper speed; and S5, after the reaction is finished, pumping the reactor solution into a condenser for solid-liquid separation to obtain the rhodium complex acetylacetonatocarbonyltriphenylphosphine rhodium. According to the preparation method of the rhodium complex, the production process is continuous, the production time is shortened, operation is easy and convenient, distillation is not needed, the utilization rate of metal rhodium is remarkably increased, the product purity is high, the yield is 88% or above, and the product purity reaches 99% or above.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to the technical field of preparation of noble metal complex catalysts, in particular to a preparation method of a rhodium complex triphenylphosphinecarbonylrhodium acetylacetonate. Background technique [0002] The basic organic synthesis and the three major raw material synthesis industries in modern petrochemistry are mainly based on the chemistry of alkynes and alkenes, and organometallic complex catalysis is widely used. Among them, the hydroformylation reaction is the industry and the aldehyde or alcohol. important method. Olefin formylation reaction, also known as OXO reaction, refers to the reaction of olefins and synthesis gas (CO and H2) to form aldehydes under the action of a catalyst. The resulting aldehydes, alcohols and their derivatives are widely used as plasticizers, fabric additives, surfactants, solvents and fragrances. In laboratory-scale studies, mos...

Claims

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Application Information

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IPC IPC(8): C07F15/00
CPCC07F15/0073Y02P20/584
Inventor 李娟
Owner 铜陵欣诺科新材料有限公司
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