Preparation method of aluminum acetylacetonate

A technology of aluminum acetylacetonate and acetylacetone, which is applied in the field of preparation of aluminum acetylacetonate, can solve the problems of large amount of acetylacetonate, large consumption of organic solvents, and low product purity, so as to promote the reaction, reduce the generation of waste water, and save solvents the effect of using

Active Publication Date: 2019-11-12
GUANGDONG UNIV OF PETROCHEMICAL TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method described in CN1903817A adopts isopropanol and acetone as solvent, adopts aluminum powder and acetylacetone to synthesize, and shortcoming is that organic solvent consumption is big, and reaction is slow, and the consumption of acetylacetone is excessive (aluminum powder: acetylacetone=1:12)
Gong Hong et al. (synthesis of aluminum acetylacetonate by solvent-free solid-phase grinding [J]. Chemical Research, 2006 (04): 31-34) reported a method for preparing aluminum acetylacetonate by solid-phase grinding, that is, solid base, acetylacetonate Acetone and aluminum salt are directly ground and reacted in a mortar. In this method, a large amount of alkali still needs to be added as a raw material during the grinding process, and there is a large amount of volatilization of acetylacetone. The residual unreacted product contains more inorganic salts and the product is not pure.

Method used

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  • Preparation method of aluminum acetylacetonate
  • Preparation method of aluminum acetylacetonate

Examples

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Comparison scheme
Effect test

Embodiment 1

[0038] This example prepares the technological process schematic diagram of aluminum acetylacetonate to see attached figure 1 . Refer below figure 1 , illustrate that this example prepares the method for aluminum acetylacetonate as follows:

[0039] Weigh 2.0g of aluminum powder and place it in the reactor, and add 50mL of methanol into the reactor from the methanol tank. Turn on the mixer to mix the aluminum powder evenly. Heat the reaction system to 65° C., maintain the temperature until the end of the reaction, and use formic acid to adjust the pH of the reaction solution to 3. Add 30.3mL of acetylacetone from the acetylacetone tank (the molar ratio of acetylacetone to aluminum powder is 4:1), drop it into the reaction kettle at a rate of 1-2 drops per second, until the aluminum powder is completely reacted (no Solid exists, and solvent can be replenished, and the reaction time at this stage is 12h). The reaction was continued for 4h, and the total reaction time was 16...

Embodiment 2

[0043] The preparation method of this example aluminum acetylacetonate is as follows:

[0044] Weigh 2.0g of aluminum powder and place it in the reaction kettle, and add 60mL of ethanol from the ethanol tank as a solvent. Turn on the mixer to mix the aluminum powder evenly. Heat the reaction system to 75° C., maintain the temperature until the end of the reaction, and use acetic acid to adjust the pH of the reaction solution to 4.0. Add 37.9 mL of acetylacetone from the acetylacetone tank (the molar ratio of acetylacetone to aluminum powder is 5:1), and drop it into the reaction bottle at a rate of 1-2 drops per second until the aluminum powder is completely reacted (no Solid exists, and the reaction time at this stage is 10h). The reaction was continued for 4h, and the total reaction time was 14h. Stop heating and cool to 30°C, add dropwise 2mol / L NaOH solution to adjust the pH to 7, so that aluminum acetylacetonate crystallizes out. The reaction solution was filtered, an...

Embodiment 3

[0047] The preparation method of this example aluminum acetylacetonate is as follows:

[0048] Weigh 2.0g of aluminum powder and place it in the reaction kettle, and add 60mL of ethanol from the ethanol tank as a solvent. Turn on the mixer to mix the aluminum powder evenly. Heat the reaction system to 75° C., maintain the temperature until the end of the reaction, and use formic acid to adjust the pH of the reaction solution to 3. Add 37.9mL of acetylacetone from the acetylacetone tank (the molar ratio of acetylacetone to aluminum powder is 5:1), drop it into the reaction bottle at a rate of 1-2 drops per second, and continuously add formic acid during the reaction to maintain the pH at 2 to 3, until the aluminum powder is completely reacted (no solid is observed in the reaction solution, and the reaction time at this stage is 14 hours). The reaction was continued for 4h, and the total reaction time was 18h. Stop heating and cool to 28°C, add dropwise 3mol / L NaOH solution t...

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Abstract

The invention discloses a preparation method of aluminum acetylacetonate, which comprises the following steps: 1) in a reactor, mixing aluminum powder with C1-C3 low-grade fatty alcohol, and adding organic acid to adjust the pH value to 2-4.5; 2) adding acetylacetone for reaction, and then adding alkali liquor to adjust the pH value to 6-7; and 3) filtering the product obtained in the step 2), andwashing and drying the filter residue to obtain the aluminum acetylacetonate. The method is free of water as a solvent, reduces the generation of wastewater, promotes the reaction by a small amount of organic acid as a pH value regulator, improves the utilization rate of the raw material acetylacetone, achieves the cyclic utilization of the solvent, and saves the cost.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of aluminum acetylacetonate. Background technique [0002] Aluminum acetylacetonate is a monoclinic crystal with good water resistance and lipophilicity. It is mainly used as a hardening accelerator for epoxy resins, a crosslinking agent for acrylic resins, and olefin polymerization for olefin polymerization, epoxy resins, and anhydride curing. , Catalyst for silane polymerization. Aluminum acetylacetonate can significantly improve the adhesion in white ink, transparent ink and other inks without causing the color to darken. [0003] The current industrial production method of aluminum acetylacetonate is to use aluminum chloride as the aluminum source, dissolve it in a large amount of water, then add acetylacetone, adjust the pH value with sodium hydroxide, and react to obtain aluminum acetylacetonate. A large amount of industrial waste w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/77C07C49/92
CPCC07C45/77C07C49/92
Inventor 曾兴业符锦铭王寒露吴世逵林存辉
Owner GUANGDONG UNIV OF PETROCHEMICAL TECH
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