Method for synthesizing acetylacetone metallic compound

A technology of metal compounds and acetylacetone, which is applied in the field of preparation of metal acetylacetone compounds, can solve the problems of variable reaction time, complicated operation, and great human injury, and achieves the goals of improving the preparation efficiency, simplifying the preparation process, and shortening the reaction time Effect

Inactive Publication Date: 2009-08-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of this method includes two processes, and the operation is relatively complicated.
At present, there are not many reports on metal acetylacetonate compounds, and there are many shortcomings in the existing preparation methods, such as complex preparation equipment, many operation steps, long time-consuming, high production cost, great harm to human body, low yield, and long reaction time
[0005] Literature [3] CN1358691 reported that the preparation of nano-hydrotalcite in a fully back-mixed liquid film reactor can completely mix the reactants in the co-precipitation reaction instantly, make them nucleate synchronously, achieve the uniformity of nucleated particles, and make the particle size of the product reach nanometers Level, which solves the shortcomings of traditional reactors such as uneven mixing, uneven particle size distribution, and different reaction times when reacting with other substances

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 68kg zinc chloride (ZnCl 2 ) mixed with 453.3kkg deionized water to make a zinc chloride solution with a concentration of 15wt%; 40kgNaOH was dissolved in 615kg deionized water to make a solution with a sodium hydroxide content of 6.5wt%, and added to the rotating liquid film reaction at the same speed In the device, the gap of the full back-mixed liquid film reactor is 0.02mm, and the rotating speed is 2000 revs / min. The slurry is moved to a container with a jacket and a stirring device; 150kg acetylacetone is added to the reactor to react with the above-mentioned mixture, at 800 The reaction was carried out for 45 minutes at a stirring rate of rev / min, and white acetylacetone crystals were generated. The mixture was suction filtered and the product was fully washed, and finally vacuum-dried at 70° C. to obtain 133.9 kg of product. After determination, the chemical formula of the product obtained was Zn(CH 3 COCHCOCH 3 ) 2 ·H 2 O, the product yield is 95.3%. ...

Embodiment 2

[0017] Weigh 55kg calcium chloride (CaCl 2 ) mixed with 366.7kg deionized water to make a zinc chloride solution with a concentration of 15wt%, 40kgNaOH was dissolved in 615kg deionized water to make a solution with a sodium hydroxide content of 6.5wt%, and added to the rotary liquid film reactor at the same speed Among them, the gap of the full back-mixing liquid membrane reactor is 0.04mm, and the rotating speed is 3000 rev / min. The slurry is moved to a container with a jacket and a stirring device; 250kg acetylacetone is added to the flask to react with the above mixture, and the The reaction was carried out for 45 minutes at a stirring rate of 1 minute, and white acetylacetone crystals were generated. The mixture was suction-filtered to fully wash the product, and finally vacuum-dried at 70° C. to obtain 113.9 kg of product. It was determined that the chemical formula of the product was Ca(CH 3 COCHCOCH 3 ) 2 Product yield is 96.1%

Embodiment 3

[0019] Weigh 66kg magnesium chloride (MgCl 2 6H 2 0) mix with 316.7kg deionized water and be made into the zinc chloride solution that concentration is 15wt%; 40kgNaOH is dissolved in 615kg deionized water and is made into the solution that sodium hydroxide content is 6.5%wt, joins the rotating liquid film with the same speed In the reactor, the gap of the full back-mixed liquid membrane reactor is 0.06mm, and the rotating speed is 4000 rev / min. The slurry is moved to a container with a jacket and a stirring device; 350kg of acetylacetone is added to the flask to react with the above-mentioned mixture. The reaction was carried out for 45 minutes at a stirring rate of rev / min, and white acetylacetone crystals were generated. The product was fully washed by suction filtration of the mixture, and finally vacuum-dried at 70° C. to obtain 106.3 kg of product. After determination, the chemical formula of the product obtained was Mg(CH 3 COCHCOCH 3 ) 2 , the product yield is 95.8...

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Abstract

The invention provides a method for preparing acetylacetone metallic compound, comprising soluble metal salt solution and aqueous alkali are quickly mixed together through a full back-mixing liquid membrane reactor to prepare precipitation grout of hydroxide with nanometer level, the precipitation of hydroxide is not needed to be separated and directly added with acetylacetone to react at the normal temperature to obtain the acetylacetone metallic compound. The method adopts the full back-mixing liquid membrane reactor to synthesize hydroxide with nanometer level, thus shortening the reaction time between the hydroxide and the acetylacetone and improving the preparation efficiency; meanwhile, by controlling the adding quantity of alkali and the acetylacetone in the crystal-transformation process, the reaction yield is greatly improved. The preparation method is simple in technique, convenient in operation and short in reaction time, and the obtained product has the yield being more than 95%.

Description

technical field [0001] The invention relates to a preparation method of metal acetylacetonate compounds. technical background [0002] The acetylacetone metal compound contains a β-diketone structure, which can quickly replace the allyl chloride generated during PVC processing through an alkylation reaction with PVC, so that the molecular chain of the conjugated polyene is interrupted and shortened, and it plays a good role in heat dissipation. Stabilization, especially in improving the initial colorability of PVC products, and can have a synergistic effect with various heat stabilizers. At the same time, it has a wide range of applications in catalysis and preparation of semiconductor materials. [0003] Document [1] CN1299392 reports a synthetic method of acetylacetonate. The method is to add a mixture of metal oxide and solvent acetone / methanol into a reactor, heat the mixture to reflux temperature, add acetylacetone after 1 hour, and keep the reaction in reflux state f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/77C07C49/92C07C49/14
Inventor 李殿卿林彦军刘青宝
Owner BEIJING UNIV OF CHEM TECH
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