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Method for producing acetylacetone beryllium

A production method, the technology of acetylacetone, applied in the preparation of aldehyde/ketone chelate, organic chemistry, etc., can solve the problems of environmental pollution, complex process, beryllium toxicity, etc., reduce the difficulty of the process, reduce the number of process steps, and achieve high product purity Effect

Inactive Publication Date: 2012-09-12
YANGZHOU POLYTECHNIC INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: (1) The production method has low yield, and inorganic salts are formed in the reaction, which will pollute the environment if it is not handled properly; (2) Recrystallization is required before the product is obtained, the process is complicated and the production efficiency is low , and the yield is only 80-85%; (3) water is used as a solvent, which requires a large amount, difficult post-processing, difficult to recycle, and easy to cause adverse effects on the environment; (4) beryllium is very toxic and causes environmental pollution

Method used

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  • Method for producing acetylacetone beryllium
  • Method for producing acetylacetone beryllium
  • Method for producing acetylacetone beryllium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 45kg of isopropanol into the reaction kettle as a solvent, raise the temperature to 50-60°C, add 2.4kg of beryllium oxide powder into the reaction kettle under stirring, so that the beryllium oxide powder is evenly dispersed in isopropanol, and then add dropwise 22kg of acetylacetone, the temperature is controlled at 50-60°C until the dropwise addition is completed, the temperature of the reactor is properly raised, and the reaction is kept at 60°C for 5 hours, filtered while it is hot to remove a small amount of insoluble matter, and the filtrate is cooled and then filtered. Air-dried or vacuum-dried to obtain 18.38 kg of colorless crystals, which is the product, with a yield of 92.5%.

Embodiment 2

[0022] Add 50kg of ethanol as a solvent into the reaction kettle, raise the temperature to 50-60°C, add 2.5kg of beryllium oxide powder into the reaction kettle under stirring, so that the beryllium oxide powder is evenly dispersed in the ethanol, and then dropwise add 20kg of acetylacetone , the temperature is controlled at 50-60°C until the dropwise addition is completed, the temperature of the reactor is properly raised, and the reaction is kept at 70°C for 3.5 hours, filtered while hot to remove a small amount of insoluble matter, the filtrate is cooled and then filtered, and the filter cake is dried in the air or vacuum After drying, 18.94 kg of colorless crystals were obtained, which was the product, and the yield was 91.5%.

Embodiment 3

[0024] Add 55kg of ethanol as a solvent into the reaction kettle, raise the temperature to 50-70°C, add 2.5kg of beryllium oxide powder into the reaction kettle under stirring, so that the beryllium oxide powder is evenly dispersed in the ethanol, and then dropwise add 24kg of acetylacetone , the temperature is controlled at 50-70°C, until the end of the dropwise addition, the temperature of the reactor is properly raised, and the reaction is kept at 75°C for 4 hours, filtered while it is hot, and a small amount of insoluble matter is removed, and the filtrate is cooled and then filtered, and the filter cake is dried in the air or vacuum After drying, 19.42 kg of colorless crystals were obtained, which was the product, and the yield was 93.8%.

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Abstract

The invention relates to a method for producing a compound, in particular to a method for producing acetylacetone beryllium. The method comprises the steps of: dispersing beryllium oxide powder into solvent in a reaction kettle; adding acetylacetone into the reaction kettle, and carrying out reaction under the temperature condition of 50-80 DEG C; filtering while being hot, cooling filtrate and filtering again; and drying to obtain acetylacetone beryllium. The product obtained by the method is high in purity and fine in particles; and the yield is 90-95%, and the product purity reaches 99%. The method is fewer in steps, simple in technology, less in dosage of acetylacetone and low in production cost; and isopropanol or ethanol is used as solvent and can be recycled, so that the environment is not influenced.

Description

technical field [0001] The present invention relates to a production method of a compound. Background technique [0002] In the prior art, there is a compound whose Chinese name is: beryllium acetylacetonate; English name: Beryllium acetylacetonate, abbreviated as Be(acac) 2 ; CAS: NO 10210-64-7; Molecular formula: C 10 h 14 BeO 4 ; Molecular weight: 207.23; Physical and chemical properties: This product is colorless monoclinic crystal. Soluble in various organic solvents such as methanol, ethanol, acetone, ether, benzene, carbon disulfide, chloroform, etc., insoluble in water, but can be hydrolyzed by boiling water. The melting point is 109°C; the boiling point is 270°C. The relative density is 1.168. White crystal; Uses: It is an ideal precursor in the synthesis of CVD coating, carrier catalyst, beryllium-containing ceramics, beryllium-containing fibers, etc. It has broad application prospects in the fields of new materials and fine chemicals. [0003] The existing ...

Claims

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Application Information

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IPC IPC(8): C07C49/92C07C45/77
Inventor 于晓萍王斌
Owner YANGZHOU POLYTECHNIC INST
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