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Preparation of acetylacetone cobalt

A technology of cobalt acetylacetonate and acetylacetone, which is applied in the preparation field of cobalt acetylacetonate, can solve the problems of complicated operation, complicated preparation device, and many operation steps, and achieves the effects of simple preparation process, improved preparation efficiency, and improved yield.

Inactive Publication Date: 2006-03-15
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The feature of this method is that pure cobalt hydroxide must be prepared first, and then react with acetylacetone to generate cobalt acetylacetonate. The process includes two main processes, and the operation is relatively complicated.
At present, there are not many reports on acetylacetonate-based metal complexes, and the existing preparation methods have disadvantages such as complicated preparation equipment, many operation steps, long time-consuming, and low product yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 10kg crystalline cobalt chloride (CoCl 2 ·6H 2 0) mixed with 50kg deionized water to form a concentration of 16.7% crystalline cobalt chloride solution, and added to the reactor with stirring and heating device; 3.5kgNaOH was dissolved in 50kg deionized water to form a NaOH content of 6.5 % solution, add in the reactor and mix with crystalline cobalt chloride solution to generate cobalt hydroxide precipitation, after the precipitation reaction is completed, the pH value of the reaction mixture is 8; 25.2kg acetylacetone is added to the reactor and mixed with the above-mentioned precipitation reaction mixture, in At a stirring speed of 800 r / min, the temperature was raised to reflux temperature for 3 hours to generate pink cobalt acetylacetonate crystals. After cooling down, the reaction mixture was suction-filtered and the precipitate was fully washed, and finally vacuum-dried at 40° C. to obtain 11.7 kg of the product. After determination, the chemical formula ...

Embodiment 2

[0018] In Example 1, other conditions were kept unchanged, the amount of NaOH was reduced to 3.2 kg, and the pH value of the reaction mixture was 7 after the precipitation reaction was completed. Operate by the preparation method in Example 1, obtain 11.2kg product. After determination, the chemical formula of the product obtained is Co(CH 3 COCHCOCH 3 ) 2 2H 2 O, the yield is 90.8%.

Embodiment 3

[0020] Keeping other conditions unchanged in Example 1, the consumption of acetylacetone was increased to 33.6kg, and the preparation method in Example 1 was operated to obtain 11.3kg of product. After determination, the chemical formula of the product obtained is Co(CH 3 COCHCOCH 3 ) 2 2H 2 O, the yield is 91.7%.

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Abstract

Production of cobalt acetylacetone is carried out by reacting soluble ceramic cobalt blue solution with NAOH solution to generate cobaltous hydroxide deposit, and adding into acetylacetone to generate cobaltous acetylacetone crystal at 130 Deg C.. It achieves simple process, higher production efficiency and recovery rate.

Description

Technical field: [0001] The invention relates to a method for preparing cobalt acetylacetonate by directly adding acetylacetone to a reaction mixture of a soluble cobalt salt solution and an alkali solution for reaction. technical background: [0002] Cobalt acetylacetonate is a precious metal organic coordination compound, which can be dissolved in an organic solvent to prepare an organic impregnation solution to impregnate a porous carrier to prepare a highly dispersed cobalt catalyst. Because the catalyst prepared by organic solution impregnation method has high activity, cobalt acetylacetonate has been widely used in the field of catalysis. [0003] Document [1] US Patent USP 20040127690 reports a method for preparing cobalt acetylacetonate. The method is to first react the soluble cobalt salt solution with NaOH solution to form cobalt hydroxide precipitate, then fully wash the precipitate to completely remove the adsorbed alkali, and finally use pure cobalt hydroxide s...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 李殿卿段雪张法智张香梅李孟龙
Owner BEIJING UNIV OF CHEM TECH
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