RU1799358C - Method of anhydrous aluminium chloride in anhydrous diethyl ether making - Google Patents

Abstract

Usage: in the production of an ethereal solution of anhydrous aluminum chloride. mini, Essence: anhydrous diethyl ether is saturated with hydrogen chloride to 3-5 M / L and stirred for 2-4 hours, followed by treatment with aluminum metal, taken in excess with respect to hydrogen chloride.

Description

The invention relates to the field of chemical technology, namely to the preparation of anhydrous aluminum chloride in the form of a solution in diethyl ether. Such a solution is one of the main reagents for a number of technological processes, for example, for the preparation of a Ziegler-Natta catalyst.

The purpose of the invention is to reduce the duration of the process, to reduce the fire hazard and toxicity of the process.

The proposed method is implemented as follows.

Example 1. The synthesis was carried out in a conical flask equipped with a reflux condenser. Granulated aluminum of qualification h and dried diethyl ether (medical) saturated with hydrogen chloride to a concentration of 3-5 M / L were used as starting reagents. The concentration of HC in ether is determined by potentiometric titration. The reaction mixture is stirred with a magnetic stirrer. For the introduction, iron chloride of the qualification part was used as an impurity.

3 g of aluminum metal are charged into a flask, 100 ml of an ethereal solution of hydrogen chloride with a content of 3 M / L HCI and 0.1 g / l of iron chloride are added and stirred for 4 hours at 25 ° C. The excess of aluminum metal is 11.1% of the theoretically calculated by the stoichiometry reaction 2AI + 6CH1-2A1C1z + ZN2. The product yield amounted to 85.% of theoretical, the content of iron chloride is less than 0.001 g / l.

Example 2. The synthesis of aluminum chloride is carried out as in example 1, except that 75 ml of a 4 M solution of HCI in diethyl ether are added, stirring is carried out for 2 hours. The product yield was 87% of theoretical, the content of iron chloride is less than 0.001 g / L.

PRI me R 3. The synthesis is carried out as in examples 1.2, only use 60 ml of 5 M HCI solution. The product yield was 85%, the content of iron chloride is less than 0.001 g / l.

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Example 4. The synthesis of aluminum chloride is carried out as in example 1, except that 50 ml of a 4M solution of NSH in diethyl ether are added to 3.81 g of aluminum, stirring is carried out for 4 hours. The excess aluminum metal is 112% of what is required for 100% conversion of HCI by reaction 2AI + + ZH2. The product yield was 85% of theoretical, the content of iron chloride is less than 0.001 g / l.

Example 5. The synthesis of aluminum chloride is carried out as in Example 1, except that 35 ml of a 4M solution of HCI in diethyl ether are added to 9.56 g of aluminum, stirring is carried out for 2 hours. The excess of aluminum metal is 659% of the required at 100% conversion of HCI in the reaction 2AI + b HCl2A1C1z + ZH2. The product yield was 87% of theoretical.

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the content of iron chloride is less than 0.001 g / l.

Claims (1)

SUMMARY OF THE INVENTION A method for producing anhydrous aluminum chloride in anhydrous diethyl ether, comprising dissolving hydrogen chloride gas in diethyl ether, treating the resulting solution with aluminum metal at room temperature, separating aluminum chloride from insoluble precipitate, characterized in that, in order to reduce fire hazard ™ and process toxicity , reducing its duration, the dissolution of hydrogen chloride in anhydrous diethyl ether lead to the content of hydrogen chloride 3- 5 M / L and the mixture is stirred with aluminum, taken in excess with respect to hydrogen chloride, for 2-4 hours.