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Synthetic method of Beta-diketone metal salt

A synthesis method and metal salt technology, which is applied in the field of synthesizing β-diketone metal salts, can solve the problems of high production equipment investment and production energy consumption, high solubility of β-diketone metal salts, high production investment and production energy consumption, etc. Reach the effect of reducing production equipment investment, shortening reaction time, and reducing production energy consumption

Active Publication Date: 2009-10-28
ANHUI JIAXIAN FUNCTIONAL AUXILIARY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unfortunately, when adopting the above-mentioned method to synthesize β-diketone metal salts, an organic solvent is required to be used as a reaction medium, so the application in industrial production has the following obvious disadvantages:
[0014] (1) Because the solubility of β-diketone metal salts in organic solvents is relatively large, the yield is low;
[0015] (2) Since the organic solvent recovery system must be configured, the production equipment investment and production energy consumption are relatively high;
[0016] (3) Since the organic solvent is toxic, flammable and explosive, the environmental protection and safety risks are relatively large;
[0017] (4) Due to the low yield, high production investment and production energy consumption, investment is needed to solve environmental protection and safety risks, so the production cost is high
This not only still has the problems of volatile organic compound recovery and environmental protection and safety risks, but also puts forward new requirements for the acid corrosion resistance of production equipment

Method used

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  • Synthetic method of Beta-diketone metal salt
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  • Synthetic method of Beta-diketone metal salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] At room temperature, add 224g of dibenzoylmethane (HDBM, 1mol), containing CaCl 2 55.5g (0.5mol) of calcium chloride aqueous solution and 40.0g (1mol) of NaOH containing sodium hydroxide aqueous solution, add water to the total mass of the solution is about 1000g, then stir, heat up to 80°C, control the constant temperature reaction for 30min, the reaction forms After filtration, washing and dehydration, the product was dried at 105°C under normal pressure to constant weight to obtain a yellow powder product with a yield of 99.3%. After analysis and determination, the melting point of the product is 227-228 °C, and the contents of Ca, C and H are 8.18%, 74.15% and 4.98% respectively, which is the same as the chemical formula Ca(DBM) 2 Consistent (the calculated values ​​of Ca, C, and H contents are 8.23%, 74.07%, and 4.93%, respectively).

Embodiment 2

[0041] At room temperature, add 224g dibenzoylmethane (HDBM, 1mol), MgSO 4 60.2g (0.5mol) of magnesium sulfate aqueous solution and 40.0g (1mol) of sodium hydroxide aqueous solution containing NaOH, add water until the total mass of the solution is about 1000g, then stir, heat up to 80°C, control the constant temperature reaction for 30min, the reaction product After filtering, washing with water and dehydration, it was dried at 105°C under normal pressure to constant weight to obtain a yellow powder product with a yield of 99.1%. After analysis and determination, the melting point of the product is 147-150°C, and the contents of Mg, C, and H are 5.25%, 76.79%, and 4.99% respectively, which is the same as the chemical formula Mg(DBM) 2 Consistent (the calculated values ​​of Mg, C, and H contents are 5.17%, 76.55%, and 5.10%, respectively).

Embodiment 3

[0043] At room temperature, add 224g dibenzoylmethane (HDBM, 1mol), ZnSO 4 80.8g (0.5mol) of zinc sulfate aqueous solution and 40.0g (1mol) of NaOH containing sodium hydroxide aqueous solution, add water until the total mass of the solution is about 1000g, then stir, heat up to 80°C, control the constant temperature for 30min, and the reaction product After filtering, washing with water and dehydration, it was dried at 105°C under normal pressure to constant weight to obtain a yellow powder product with a yield of 99.3%. After analysis and determination, the melting point of the product is 215-218°C, and the Zn, C, and H contents are 12.87%, 70.49%, and 4.66% respectively, which is the same as the chemical formula Zn(DBM) 2 Consistent (the calculated values ​​of Zn, C, and H contents are 12.79%, 70.39%, and 4.69%, respectively).

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Abstract

The invention discloses a synthetic method of Beta-diketone metal salt, which comprises the following steps: firstly, Beta-diketone, water soluble metal salt and alkali according to stoichiometric proportion are mixed with water as a reaction medium at the temperature of being lower than the melting point of the Beta-diketone and stirred; the temperature is adjusted for reaction; and the obtained product after the reaction is finished is filtered, washed, dehydrated and dried to obtain a Beta-diketone metal salt product. The invention realizes that water is taken as the reaction medium to synthesize the Beta-diketone metal salt; and compared with the prior art in which an organic solvent is taken as a reaction medium or acid aerial fog escapes in spite of no reaction medium, the operation is greatly simplified, the production ratio, the production efficiency, the environment protection property and the security are remarkably improved, and the production cost is reduced correspondingly.

Description

technical field [0001] The invention relates to a method for synthesizing beta-diketone metal salts, more specifically, the invention relates to a method for synthesizing beta-diketone metal salts in one step with water as a reaction medium. Background technique [0002] β-diketones are a class of organic compounds whose structure can be represented by the general formula (A): [0003] [0004] In formula (A), R 1 , R 2 may be the same or different groups. [0005] β-diketones can be converted to the enol structure by isomerization: [0006] [0007] Due to the acidity of the hydroxyl group in the enol structure, β-diketones can form metal salts [Formula (B)]: [0008] [0009] In the formula (B), M represents a metal element, n is equal to the charge number of the metal ion in the metal salt, and 1≤m≤n. [0010] Metal salts (also known as complexes) of β-diketones such as dibenzoylmethane [formula (C)] or fatty acylbenzoylmethane [formula (D)] are important he...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/92C07C45/77
Inventor 吴茂英赖文华毛芳
Owner ANHUI JIAXIAN FUNCTIONAL AUXILIARY
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