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Method for preparing alkoxy aluminum

A technology of aluminum alkoxide and aluminum powder, which is applied in the field of preparation of alkoxide aluminum, can solve problems such as large environmental impact, achieve the effect of reducing production cost and simplifying purification operation

Active Publication Date: 2013-06-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this system is that it uses easily sublimable iodine as a catalyst, which has a great impact on the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] In a reaction kettle with a volume of 25 liters, add 2.25 kilograms (2.87 liters) of isopropanol with a purity of 99.8% by mass, and put 12 grams of aluminum powder with a particle size of 99.9% by mass and a particle size of 1.6mm to 2.5mm. It is 852 grams of a monolithic aluminum ingot with 99.9 mass %. Purge the reaction system with nitrogen, then slowly raise the temperature to 70°C, and start the reaction after about 8 minutes. After the reaction is initiated, maintain the temperature at 68°C to 72°C, and continuously add 5.25 kg (6.69 liters) of isopropanol dropwise for 1 Hours, the dropwise addition was completed, and the reaction was continued at 70° C. for 4 hours. The reaction was completed, and the temperature was lowered to 25° C. to obtain 6.462 kilograms of aluminum isopropoxide, and the reaction conversion rate was 98.8 mass % (calculated by the conversion of metal aluminum, the same below).

example 2

[0025] In a reactor with a volume of 25 liters, add 3.826 kilograms (4.7 liters) of n-hexanol with a purity of 99.8 mass %, and put into 12 grams of aluminum powder with a particle size of 99.9 mass % and a particle size of 1.6 mm to 2.5 mm, with a purity of 852 grams of monolithic aluminum ingot with 99.9 mass %. Purge the reaction system with nitrogen, then slowly raise the temperature to 145°C, and the reaction starts after about 15 minutes. After the reaction is initiated, maintain the temperature at 135°C to 145°C, and continuously add 8.93 kg (10.97 liters) of n-hexanol dropwise for 1.5 hours After the dropwise addition, the reaction was continued at 135° C. for 5 hours to complete the reaction, and the temperature was lowered to 25° C. to obtain 10.434 kg of n-hexyl aluminum, and the reaction conversion rate was 98.6% by mass.

example 3

[0027] In a reaction kettle with a volume of 25 liters, add 4.88 kilograms (5.9 liters) of n-octanol with a purity of 99.8 mass %, and put 12 grams of aluminum powder with a particle size of 99.9 mass % and a particle size of 1.6 mm to 2.5 mm. It is 852 grams of a monolithic aluminum ingot with 99.9 mass %. Purge the reaction system with nitrogen, then slowly raise the temperature to 180°C, and the reaction starts after about 23 minutes. After the reaction is initiated, the temperature is maintained at 175°C to 185°C, and 11.38 kg (13.77 liters) of n-octanol is continuously added dropwise for 1.5 minutes. hours, the dropwise addition was completed, and the reaction was continued at 175° C. for 5 hours to complete the reaction, and the temperature was lowered to 25° C. to obtain 13.05 kg of n-octyloxyaluminum, and the reaction conversion rate was 98.3% by mass.

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Abstract

The invention discloses a method for preparing alkoxy aluminum. The method comprises the following steps: aluminium powder and / or aluminium yarns and aluminium ingots are put in a reaction vessel; fatty alcohol between C3-C10 is used for reacting in an inert environment, and is divided into two parts; the weight of one part is 10-35 percent of the total weight of the fatty alcohol; the first partof the fatty alcohol is added into the reaction vessel, and is contacted with the aluminium powder or aluminium yarns at the temperature which is 5-25 DEG C lower than the boiling point of the fatty alcohol for initiating the reaction; the second part of the fatty alcohol which is left is continuously added into the reaction vessel after the reaction is initiated, and is continuously reacted withthe aluminium powder or aluminium yarns until the reaction is fully carried out at the temperature which is lower than the boiling point of the fatty alcohol; and the weight of the aluminium powder or aluminium yarns is 0.5-5.0 percent of the total weight of the aluminium powder and / or aluminium yarns and the aluminium ingots. The method has the advantages that a catalyst is not used, the preparation is simple, and the reaction can be carried out fully, stably and fast.

Description

technical field [0001] The invention is a method for preparing aluminum alkoxide, specifically, a method for preparing aluminum alkoxide by using aluminum metal and fatty alcohol. Background technique [0002] Aluminum alkoxide is an important chemical intermediate. In addition to being used as a dehydrating agent, catalyst, and waterproofing agent, it also has important uses in chemical synthesis, special materials, and the preparation of high-purity aluminum hydroxide and alumina. [0003] As early as the 1950s, people carried out a lot of research on the preparation of alkoxide aluminum, using liquid alcohol and aluminum alloy or impure aluminum as raw materials, using HgCl 2 , CuCl 2 , FeCl 3 , SnCl 4 or BCl 3 Synthesize aluminum alkoxide as catalyst. USP2579251 discloses a method for synthesizing aluminum alkoxides. Aluminum-containing substances are pulverized and heated. Alcohol vapor is carried into the reactor by nitrogen or hydrogen and reacted at 200-300°C. T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/32C07C29/70
Inventor 蔡迎春马爱增杨彦鹏潘锦程
Owner CHINA PETROLEUM & CHEM CORP
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