Method of preparing copper acetylacetone

A technology of copper acetylacetonate and acetylacetone, which is applied in the field of preparation of copper acetylacetonate, can solve the problems of benzene pollution to the environment, low production efficiency and conversion rate, low product purity, etc., achieve no organic solvent pollution, reduce production costs, The effect of high product purity

Inactive Publication Date: 2009-08-19
SHANDONG UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of this method: one is that there is an equimolar amount of by-product ammonium sulfate in the product, the separation of the product is difficult and the product purity is low; the other is that recrystallization is required, the production process is complicated, the production efficiency and conversion rate are low; There is secondary pollution in the crystallization so

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 100 kg of water to the reaction kettle, add 15 kg of copper oxide powder under agitation, so that the copper oxide powder is evenly dispersed in the water; heat to 75°C under agitation, and add 40 kg of acetyl Acetone; use hydrochloric acid to adjust the pH of the solution to 2.0, after adding acetylacetone dropwise, react at 75°C under stirring conditions for 2.0 hours; adjust the pH to 5.0 with ammonia water, and continue to react at 75°C under stirring conditions for 1.5 hours; Adjust the pH to 8.5, and continue to stir at 75°C for 0.5 hours; cool to room temperature, separate copper acetylacetonate, and repeatedly wash with water until the washing liquid is colorless, and obtain 47.5 kg of copper acetylacetonate after drying; the product purity is 98.2%. The conversion rate of copper was 95.0%.

Embodiment 2

[0024] Add 200 kg of water to the reaction kettle, add 30 kg of copper oxide powder under agitation, so that the copper oxide powder is evenly dispersed in the water; heat to 65°C under agitation, and add 90 kg of acetylene dropwise at 65°C under agitation Acetone; use sulfuric acid to adjust the pH of the solution to 1.0, after adding acetylacetone dropwise, react for 2.5 hours at 65°C under stirring conditions; adjust the pH to 7.0 with sodium hydroxide, and continue to react at 65°C under stirring conditions for 2.0 hours; Use sodium hydroxide to adjust the pH to 9.0, and continue stirring at 65°C for 1.0 hour; cool to room temperature, separate copper acetylacetonate, and repeatedly wash with water until the washing liquid is colorless, and obtain 97.5 kg of copper oxide after drying; the product The purity was 98.0%, and the conversion rate of copper oxide was 97.5%.

Embodiment 3

[0026] Add 150 kg of water to the reaction kettle, add 20 kg of copper oxide powder under agitation, so that the copper oxide powder is evenly dispersed in the water; heat to 85°C under agitation, and drop 55 kg of acetyl Acetone; use phosphoric acid to adjust the pH of the solution to 3.0, and after adding acetylacetone dropwise, react for 2.0 hours at 85°C under stirring conditions; adjust the pH to 6.0 with potassium hydroxide, and continue to react at 85°C under stirring conditions for 1.5 hours; Use potassium hydroxide to adjust the pH to 8.5, and continue to stir and react at 85°C for 0.25 hours; cool to room temperature, separate copper acetylacetonate, and repeatedly wash with water until the washing liquid is colorless, and obtain 64.0 kg of copper acetylacetonate after drying; product purity The conversion rate of copper oxide was 98.8%, and the conversion rate of copper oxide was 95.5%.

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Abstract

The invention belongs to the field of fine chemistry industry, and in particular relates to a method for preparing cupric acetylacetonate using cupric oxide powder to synthesize with acetylacetone, characterized in that water is used as solvent, and protonic acid is used as a catalyst and protonic base is used for regulating the acidity; the protonic acid is one of hydrochloric acid, sulphuric acid and phosphorous acid, and the protonic base is one of sodium hydroxide, potassium hydroxide and ammonia water. Compared with the prior art, the method has the by-products of trace soluble inorganic salts and simple production process, the product of cupric acetylacetonate with high purity can be obtained without special purification, and the yield is greater than 95 percent; using water as the solvent eliminates pollution from organic solvent; the mol ratio of reactant of cupric oxide to acetylacetone is 1.0:2.0 to 1.0:2.4, with low usage of acetylacetone, low production cost and high benefit.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a method for preparing copper acetylacetonate. Background technique [0002] Copper acetylacetonate is blue powder or needle crystal, easily soluble in chloroform, soluble in benzene, carbon tetrachloride and other organic solvents, insoluble in water. Copper acetylacetonate can be used as catalyst, resin crosslinking agent, etc. The existing production method of copper acetylacetonate uses water as the medium, and adopts copper sulfate and benzene for the synthesis of acetylacetone to carry out recrystallization. The disadvantages of this method: one is that there is an equimolar amount of by-product ammonium sulfate in the product, the separation of the product is difficult and the product purity is low; the other is that recrystallization is required, the production process is complicated, the production efficiency and conversion rate are low; There is secondary pollution in th...

Claims

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Application Information

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IPC IPC(8): C07C49/92C07C49/14C07C45/77B01J31/22C08K5/07
Inventor 管从胜
Owner SHANDONG UNIV
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