Self-catalyzed one-step synthesis method of high-purity aluminum isopropoxide

An aluminum isopropoxide, self-catalysis technology, applied in organic chemistry, metal alcohol preparation, etc., can solve the problems of complicated operation and poor safety, and achieve the effect of simple operation, reliable raw material guarantee, and improved purity

Active Publication Date: 2015-02-18
SHANDONG HENGJING NEW MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The autocatalytic synthesis method of high-purity aluminum isopropoxide is rarely reported, and the operation is complicated and the safety is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: the method for autocatalytic one-step synthesis of high-purity aluminum isopropoxide

[0020] (1) Weigh 24g of high-purity Al into a three-necked flask;

[0021] (2) Add 130g Al(OPr iso ), heated to 60°C and stirred evenly, then added to a three-necked round-bottomed flask;

[0022] (3) Use an electric heating mantle to adjust the temperature to 100°C, keep the temperature of the reaction system at 85°C for 2 hours, and stop heating after the reaction starts.

[0023] (4) The reaction continued, and the evaporated product was condensed and refluxed for 6 hours, the temperature of the system dropped, and the reaction ended.

[0024] The reaction is an exothermic reaction, and after the reaction is started, the heat released by itself can fully satisfy the continuation of the reaction.

[0025] (5) After the reaction is over, turn on the heating mantle again, increase the temperature of the reaction system by 120°C, and keep it warm for 2 hours to fully c...

Embodiment 2

[0027] Embodiment 2 self-catalyzed one-step method for synthesizing high-purity aluminum isopropoxide

[0028] (1) Weigh 24g and place it in a three-necked flask;

[0029] (2) Add 200g Al(OPr iso ), heated to 80°C and stirred evenly, then added to a three-necked round-bottomed flask;

[0030] (3) Adjust the temperature of the electric heating mantle to 110°C. When the temperature of the reaction system reaches 85°C, reflux the evaporator for 4 hours, and the reaction ends.

[0031] (4) After the reaction is over, raise the temperature of the reaction system to 140°C to fully complete the reaction.

[0032] The whole synthesis process takes 8 hours, and the conversion rate of the synthesis reaction is 98%. The purity of the obtained high-purity aluminum isopropoxide is 99.996%. After vacuum distillation, the purity of aluminum isopropoxide can reach 99.9994%.

Embodiment 3

[0033] Embodiment 3 self-catalyzed one-step method for synthesizing high-purity aluminum isopropoxide

[0034]Add high-purity aluminum flakes (purity ≥ 99.996%) and isopropanol (rectified to remove impurities) into the reaction kettle, add high-purity aluminum isopropoxide (as a catalyst, high-purity aluminum isopropoxide is high-purity aluminum After catalyzed synthesis of flakes and anhydrous isopropanol, aluminum isopropoxide with a purity of ≥99.999% obtained by distillation under reduced pressure, with a concentration of 4mol / L) was used as a catalyst; h, start the reaction, and condense and reflux the evaporator for 5 hours. After the reaction, raise the temperature of the reaction system to 135° C. to fully react the remaining isopropanol, and then obtain high-purity aluminum isopropoxide in one step.

[0035] The whole synthesis process takes 6 hours, and the conversion rate of the synthesis reaction is 99.2%. The purity of the obtained high-purity aluminum isopropoxid...

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Abstract

The invention discloses a self-catalyzed one-step synthesis method of high-purity aluminum isopropoxide. The high-purity aluminum isopropoxide is synthesized in an autocatalysis manner by use of the high-purity aluminum isopropoxide as the catalyst. The high-purity aluminum isopropoxide is taken as the catalyst instead of HgCl2, AlCl3, I2, CuCl2 and the like to realize the autocatalysis of the aluminum isopropoxide synthesis process, and no impurity element is introduced so that the purity of the aluminum isopropoxide can be improved; and as a result, reliable raw material guarantee is provided for subsequent production of related high-purity materials by use of the aluminum isopropoxide.

Description

technical field [0001] The invention relates to a synthesis method of high-purity aluminum isopropoxide, in particular to a one-step self-catalyzed synthesis method of high-purity aluminum isopropoxide, which belongs to the field of catalytic synthesis of organic aluminum alcohols. Background technique [0002] In recent years, the chemical synthesis of metal alkoxides has developed rapidly. There are more than 60 elements in the periodic table that can synthesize alkoxides, of which 41 elements have been used to prepare advanced ceramic materials by sol-gel method. Aluminum alkoxides, also known as aluminum alkoxides, can be divided into: low-carbon aluminum alkoxides, generally low-carbon alcohols with 1 to 4 carbon atoms; and alcohols with more than 4 carbon atoms Atoms are called higher carbon alcohol aluminum. Among them, the low-carbon aluminum alkoxide of aluminum isopropoxide is widely synthesized, which can be widely used in dehydrating agents, catalysts, etc. In r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/32C07C29/70
CPCC07C29/70C07C31/32
Inventor 殷剑龙范光磊
Owner SHANDONG HENGJING NEW MATERIAL CO LTD
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