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Method for synthesizing iron diacetone

A technology for the synthesis of iron acetylacetonate, which is applied to the preparation of aldehyde/ketone chelates, etc., can solve the problems of high equipment requirements, low yield, and many synthesis steps, and achieve low solvent consumption, high purity, and product selectivity high effect

Inactive Publication Date: 2011-04-06
YANGZHOU POLYTECHNIC INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It still cannot fundamentally solve its shortcomings such as many synthetic steps, low yield, and high equipment requirements, which brings great difficulties to its industrial production.

Method used

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  • Method for synthesizing iron diacetone
  • Method for synthesizing iron diacetone
  • Method for synthesizing iron diacetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 1.68g (30mmol) KOH and 3.00g (30mmol) acetylacetone into a mortar, grind for 10min, make it fully mixed, add 2.70g (10mmol) FeCl 3 ·6H 2 O, grind for 30 min, add 15 mL of deionized water, filter with suction, wash 3 times with 30 mL of deionized water, and dry at 75°C for 3 h to obtain a crude product. The crude product was recrystallized with acetone, and the acetone was recycled to obtain 3.06 g of the product with a yield of 86.7%. The melting point of the product was 180-182°C.

Embodiment 2

[0023] Put 1.20g (30mmol) NaOH, 3.00g (30mmol) acetylacetone into the mortar, grind for 10min, make it fully mixed, add 2.70g (10mmol) FeCl 3 ·6H 2 O, grind for 60 min, add 15 mL of deionized water, filter with suction, wash twice with 20 mL of deionized water, and dry at 75°C for 2.5 h to obtain a crude product. The crude product was recrystallized with absolute ethanol, and the ethanol was recycled to obtain 3.08 g of the product with a yield of 87.3%. The melting point of the product was 179-182°C.

Embodiment 3

[0025] Put 1.68g (30mmol) KOH and 4.00g (40mmol) acetylacetone into a mortar, grind for 10min, make it fully mixed, add 2.70g (10mmol) FeCl 3 ·6H 2 O, grind for 30 minutes, add 15 mL of deionized water, filter with suction, wash twice with 20 mL of deionized water, and dry at 60°C for 2.5 hours to obtain a crude product. The crude product was recrystallized with acetone, and the acetone was recycled to obtain 3.19 g of the product with a yield of 90.4%. The melting point of the product was 179-182°C.

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Abstract

The invention discloses a method for synthesizing iron diacetone, in particular relates to a method for preparing iron diacetone by using a solvent-free solid phase grinding method. The method has the advantages of simple preparation process, high product yield and high purity and is convenient to operate. The method comprises the following steps of: (1) mixing and grinding any one of Na2CO3, K2CO3, NaOH, KOH, (NH4)2CO3, NH4HCO3, NaHCO3 or KHCO3 and liquid diacetone; (2) adding the grinded mixture to any one of FeCl3.6H2O or Fe(NO3)3.9H2O to generate complexing reaction; and (3) adding water to a mortar, leaching and washing to obtain solid iron diacetone. In the invention, the iron diacetone is synthesized under room temperature by adopting the solvent-free solid phase grinding method. The invention mainly has the beneficial effects that: (1) the product has high selectivity, purity and utilization ratio; (2) the solvent consumption is low, and the adverse influence on complexes can be effectively eliminated; (3) the process is simple, the conditions are mild, the reaction speed is fast and the energy consumption is low; and (4) the method has no three wastes and is environmentally-friendly, green and free of pollution. The method is an ideal green synthesis method which has general practicability.

Description

technical field [0001] The invention relates to a method for preparing iron acetylacetonate by a solvent-free solid-phase grinding method. Background technique [0002] Iron acetylacetonate is an important metal-organic complex, which is dissolved in an organic solvent and prepared as an organic impregnating solvent to prepare a highly dispersed catalyst. The catalyst prepared by this method has a very high activity. Iron acetylacetonate can be used as resin crosslinking agent and curing accelerator, such as replacing traditional organometallic compounds such as lead, tin, zirconium and bismuth with iron acetylacetonate to catalyze the ring-opening polymerization of lactide, which not only has high catalytic activity, but also It avoids the gradual precipitation of toxic metal ions as the material degrades in the body, causing toxic and side effects to the human body; it is used as a catalyst for hydrogenation and carbonylation, such as catalyzing the selective hydrogenation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/92C07C49/14C07C45/77
Inventor 罗志臣王勤柴培培丁慧红
Owner YANGZHOU POLYTECHNIC INST
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