Method for preparing ferric acetyl acetonade

A technology of iron acetylacetonate and acetylacetone, which is applied in the chemical field, can solve problems such as adverse environmental effects, low product yield, and low production efficiency, and achieve the effects of reducing production costs, high product purity, and cost reduction

Inactive Publication Date: 2010-10-13
扬州市兴业助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The weak point of this preparation method is (1) this production method productive rate is low, has hydrochloric acid to generate in the reaction, handles badly and can pollute environment; (2) needs recrystallization before obtaining product, and its process is complicated, and production efficiency Low, the productive rate is only 80~85%; (3) adopt water as solvent, its consumption is big, aftertreatment is difficult, easily causes adverse effect to environment
[0004] "Shanxi Chemical Industry" Volume 22, Issue 1 (Pages 7-8), Ren Xiaodong, Ma Guozhang and others disclosed the preparation method of iron acetylacetonate, using a t

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 150kg of isopropanol into the reaction kettle as a solvent, raise the temperature to 50-60°C, add 10kg of iron powder into the reaction kettle under stirring, so that the iron powder is evenly dispersed in the isopropanol, and then add iron powder with a mass of 0.2 % protonic acid catalyst 0.02kg, then dropwise add 62kg of acetylacetone, the temperature is controlled at 50-60°C, until the end of the dropwise addition, the reactor is properly heated, and at the same time, oxygen is added to the reactor by an oxygen increasing device, at 50°C Heat preservation reaction for 5 hours, remove the solvent after cooling, and dry to obtain 58.51 kg of product with a yield of 92.5%.

Embodiment 2

[0019] Add 105kg of toluene into the reaction kettle as a solvent, raise the temperature to 50-60°C, add 10kg of iron powder into the reaction kettle under stirring, so that the iron powder is evenly dispersed in isopropanol, and then add 1% of the iron powder mass Protonic acid catalyst 0.1kg, then add 65kg of acetylacetone dropwise, the temperature is controlled at 50-60°C, until the addition is completed, the reaction kettle is properly heated, and at the same time, oxygen is added to the reaction kettle through the oxygen increasing device, and the reaction is kept at 70°C After cooling for 3.5 hours, the solvent was removed, and the product was dried to obtain 58.82 kg, with a yield of 93.0%.

Embodiment 3

[0021] Add 52kg of toluene into the reactor as a solvent, raise the temperature to 50-60°C, add 5kg of iron powder into the reactor under stirring, so that the iron powder is evenly dispersed in isopropanol, and then add 1% of the iron powder mass Protonic acid catalyst 0.05kg, then add 33kg of acetylacetone dropwise, the temperature is controlled at 50-60°C, until the addition is completed, the reaction kettle is properly heated, and at the same time, oxygen is added to the reaction kettle through the oxygen increasing device, and the reaction is kept at 90°C After cooling for 3 hours, the solvent was removed, and the product was dried to obtain 29.98 kg with a yield of 94.8%.

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Abstract

The invention discloses a method for preparing ferric acetyl acetonade, which comprises the following steps of: adding isopropanol or methylbenzene serving as a solvent into a reactor, and raising the temperature to between 50 and 60 DEG C; adding iron powder into the reactor with stirring to make the iron powder uniformly dispersed in the isopropanol or methylbenzene; adding a protonic acid catalyst into the reactor, dripping diacetone, and controlling the temperature to between 50 and 60 DEG C until the dripping is finished; and raising the temperature of the reactor, adding oxygen into thereactor through an oxygenation device, keeping the temperature of between 50 and 90 DEG C, reacting for 3 to 5 hours, filtering, cooling, removing the solvent, and drying to obtain the product. The method has the advantages of high purity and fine particles of the product, the yield rate of 90 to 95 percent, less production steps, and simple process. Solution synthesis is adopted, mother liquor can be circularly used or recycled, the environmental protection requirement is met, the energy is saved, and the cost can be greatly reduced.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a method for preparing iron acetylacetonate. Background technique [0002] Iron acetylacetonate is mainly used as resin crosslinking agent, curing accelerator, rubber additive, petroleum cracking catalyst, fuel oil additive and organic synthesis catalyst, etc., and has a wide range of application fields. In recent years. With the development of my country's economy, the widespread use of agricultural mulch and domestic plastics has brought serious environmental pollution. As a high-efficiency photosensitizer for plastic photodegradation, iron acetylacetonate has been paid more and more attention at home and abroad, and has become the main subject of new market research. The research of this product is of great significance in industrial production and environmental chemistry. [0003] The common preparation method of iron acetylacetonate in the prior art is as follows: take acetone and...

Claims

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Application Information

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IPC IPC(8): C07C49/92C07C49/14C07C45/77
Inventor 于晓萍王斌
Owner 扬州市兴业助剂有限公司
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