Continuous synthesis method for acetylacetone metallic compound

A metal compound, acetylacetone technology, applied in the field of continuous synthesis of acetylacetonate metal compounds, can solve the problems of high equipment requirements, complicated operation process, low product purity, etc., and achieves wide application prospect, simple operation process, and product yield. high effect

Inactive Publication Date: 2012-06-20
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of this type of method are: (1) the yield is low, and salt is generated in the reaction process, resulting in low product purity; (2) to obtain a pure product, the product must be recrystallized, and the process is complicated; (3) Due to the introduction of a large amount of water during the adoption process, a large amount of waste liquid will be generated in the later stage, which will easily cause environmental pollution
The disadvantages of this type of method are: (1) the operation process is complicated, time-consuming, and the production cost is high; (2) for metals that are difficult to prepare hydroxides, or are difficult to obtain pure hydroxides, t

Method used

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  • Continuous synthesis method for acetylacetone metallic compound
  • Continuous synthesis method for acetylacetone metallic compound
  • Continuous synthesis method for acetylacetone metallic compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Add 8 g Fe to Reactor 1 2 o 3 , 20mL of xylene and 50mL of acetylacetone, add 50mL of acetylacetone to the product collector 3, start magnetic stirring, first heat the product collector 3 until the acetylacetone starts to reflux, then start heating the reactor 1 to reflux, stop after 2 hours of reaction Heated, and after the product collector 3 was cooled, it was placed in an ice bath, reddish-brown crystals were precipitated, filtered with suction, and reddish-brown iron acetylacetonate was obtained after precipitation and drying, with a yield of 90%. The purity of the obtained iron acetylacetonate was determined to be 98.5% by chelate titration. The infrared spectrogram of gained iron acetylacetonate is as image 3 shown.

Embodiment 2

[0059] 5 g Fe was added to batch reactor 1 2 o 3 , 50mL carbon tetrachloride and 50mL acetylacetone, start magnetic stirring, heat the reactor 1 to reflux, stop heating after 12 hours of reaction, filter while it is hot, put the filtrate in an ice bath, precipitate reddish-brown crystals, suction filter, precipitate After drying, reddish-brown iron acetylacetonate was obtained with a yield of 85%. The X-ray diffraction spectrogram of gained iron acetylacetonate is as attached Figure 4 shown.

Embodiment 3

[0061] Add 5 g of V to Reactor 1 2 o 3 , 35mL of cyclohexane and 35mL of acetylacetone, add 60mL of acetylacetone in the product collector 3, start magnetic stirring, feed 90mL / min of oxygen into the reactor 1, first heat the product collector 3 until the acetylacetone starts to reflux , then start to heat the reactor 1 to reflux, stop heating after reacting for 2 hours, place it in an ice bath after the product collector 3 is cooled, and precipitate blue crystals, suction filter, precipitate and dry to obtain blue acetylacetone Vanadyl, the yield is 87%. The purity of the obtained vanadyl acetylacetonate was determined to be 99% by chelate titration. The X-ray diffraction spectrogram of gained vanadyl acetylacetonate is as attached Figure 5 shown.

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Abstract

The invention relates to a continuous synthesis method and a synthesis device for an acetylacetone metallic compound. The method comprises the following steps of: adding a metallic compound and acetylacetone into a reactor; adding the acetylacetone into a product collector; uninterruptedly distilling the acetylacetone in the product collector into the reactor in the heating process, and reacting the distilled acetylacetone with the metallic compound; when a liquid level in the reactor is higher than a siphon, siphoning liquid comprising the acetylacetone metallic compound generated during reaction in the reactor into the product collector to separate a product from a reactant; distilling the acetylacetone which is not reacted in a product separator into the reactor, and continuously reacting the acetylacetone with the metallic compound; and reacting and refluxing for a certain period of time, stopping heating, cooling a solution in the product collector, precipitating, filtering, drying, and thus obtaining the product. The method has a simple process and universality, is high in product yield and is environment-friendly.

Description

technical field [0001] The invention relates to a method for continuously synthesizing metal acetylacetonate compounds and a synthesis device thereof, in particular to a method for continuously synthesizing metal acetylacetonate compounds using metal compounds and acetylacetone as raw materials and a synthesis device thereof. Background technique [0002] Metal acetylacetonate is a common organometallic complex, which has a wide range of applications in catalysts, catalyst preparation, organic synthesis, and material preparation. For example, vanadyl acetylacetonate can be combined with tert-butyl hydroperoxide (TBHP), and can be rapidly oxidized into a homogeneous pentavalent vanadium compound under the reaction system, which can effectively oxidize various organic functional groups; nickel acetylacetonate catalyst can not only be used as Oligomerization and polymerization catalysts for non-polar monomers such as propylene, styrene, dienes, and cycloolefins, and can also be...

Claims

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Application Information

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IPC IPC(8): C07C49/92C07C49/14C07C45/77B01J19/00
Inventor 余剑杨娟许光文
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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