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Preparation method of high-purity aluminum isopropoxide

A technology of aluminum isopropoxide and isopropanol, which is applied in the field of preparation of aluminum isopropoxide, can solve the problems of difficult reaction, difficult removal, and low reaction yield, and achieve the advantages of convenient reaction initiation, improved purity, and high purity Effect

Active Publication Date: 2019-02-22
SHANGYU SUNFIT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing method for preparing aluminum isopropoxide either needs to add various catalysts, thereby introducing additional impurities, which are difficult to completely remove and affect the purity of the product; if no additional catalysts are added, the reaction will be difficult to initiate, resulting in reaction Yield becomes lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Inject 40kg of isopropanol (AR) and 4.5kg of aluminum particles into the reaction kettle, stir at room temperature for 5 minutes, then heat to 50°C, and use different dropping equipment to slowly add 150g of tri-n-propylaluminum and 200g of aluminum isopropoxide was added dropwise for 30 minutes, then the temperature was raised to 85°C for reflux reaction, and the reaction was completed after 4 hours of reaction.

[0018] Atmospheric distillation was performed on the above reactants to remove isopropanol and by-product n-propane, and the distillation temperature was 90°C. Then, the contents in the still after atmospheric distillation were distilled under reduced pressure at 1333 Pa (absolute pressure), and fractions at 135° C. to 145° C. were collected to obtain aluminum isopropoxide.

[0019] After testing, the yield of aluminum isopropoxide is 95.8% (relative to aluminum), and the prepared high-purity aluminum isopropoxide has a purity greater than 99.99%, which meets...

Embodiment 2

[0021] Inject 40kg of isopropanol (AR) and 4.5kg of aluminum particles into the reaction kettle, stir at room temperature for 5 minutes, then heat to 50°C, and use different dropping equipment to slowly add 200g of tri-n-propylaluminum and 200g of aluminum isopropoxide was added dropwise for 30 minutes, then the temperature was raised to 85°C for reflux reaction, and the reaction was completed after 4 hours of reaction.

[0022] Atmospheric distillation was performed on the above reactants to remove isopropanol and n-propane, and the distillation temperature was 90°C. Then, the contents in the still after atmospheric distillation were distilled under reduced pressure at 1333 Pa (absolute pressure), and fractions at 135° C. to 145° C. were collected to obtain aluminum isopropoxide.

[0023] After testing, the yield of aluminum isopropoxide is 96.5% (relative to aluminum), and the prepared high-purity aluminum isopropoxide has a purity greater than 99.99%, meeting the quality re...

Embodiment 3

[0024] Embodiment 3 (comparative example 1)

[0025] Inject 40kg of isopropanol (AR) and 4.5kg of aluminum particles into the reaction kettle, stir at room temperature for 5 minutes, then heat to 50°C, slowly add 400g of aluminum isopropoxide to the reaction system for 30 minutes, and then raise the temperature to 85 ℃ reflux reaction, after 4 hours of reaction, the reaction was terminated.

[0026] Atmospheric distillation was performed on the above reactants to remove isopropanol and n-propane, and the distillation temperature was 90°C. Then, the contents in the still after atmospheric distillation were distilled under reduced pressure at 1333 Pa (absolute pressure), and fractions at 135° C. to 145° C. were collected to obtain aluminum isopropoxide.

[0027] After testing, the yield of aluminum isopropoxide is 54.8% (relative to aluminum).

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Abstract

The invention discloses a preparation method of high-purity aluminum isopropoxide. The preparation method comprises the following steps: mixing isopropanol and aluminum particles, stirring the mixture, dripping tri-n-propylaluminium and aluminum isopropoxide for initiating reaction, continuing to heat reaction liquid until the reaction is complete after the initiation is completed, and performingaftertreatment, so as to obtain the high-purity aluminum isopropoxide. According to the preparation method, a certain amount of aluminum isopropoxide and a certain amount of tri-n-propylaluminium areadded into the reaction system, so that the reaction is more easily initiated, and therefore, the addition of catalysts of CuCl2, HgCl2, AlCl3 and the like is avoided, and the product purity is improved.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for preparing aluminum isopropoxide. Background technique [0002] With the development of science and technology, the demand for ultra-fine high-purity alumina powder is increasing at home and abroad, and higher requirements are put forward for the particle size, purity and uniformity of high-purity alumina powder. At present, high-purity alumina is generally prepared by aluminum isopropoxide: aluminum isopropoxide is first hydrolyzed to obtain aluminum hydroxide, and then the aluminum hydroxide is further calcined to obtain high-purity alumina powder. Therefore, in order to obtain high-purity alumina powder, it is extremely critical to prepare high-purity aluminum isopropoxide. [0003] The synthesis process of aluminum isopropoxide is generally that aluminum and isopropanol generate aluminum isopropoxide under the action of a catalyst, and the commonly use...

Claims

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Application Information

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IPC IPC(8): C07C31/32C07C29/94C07C29/70C07C29/80
CPCC07C29/70C07C29/80C07C29/94C07C31/32
Inventor 黄生建陈炯明李文梁旭华
Owner SHANGYU SUNFIT CHEM
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