The method of preparation of the catalyst complex to obtain oligoelement

 

(57) Abstract:

The inventive method obtain a homogeneous catalyst complex without precipitation, provides for the reduction of time for its preparation, and its increased activity. In the interaction of aluminum chloride and diphenyloxide in aromatic solvent as modifying additives using ethyl acetate in a weight ratio of aluminum chloride: diphenyloxide: ethyl acetate- 1: 0,4 - 0,7: 0,1 - 0,3.

The invention relates to catalytic chemistry, in particular for the catalytic complex (CPC) based on the aluminum chloride and diphenyloxide, upon receipt of oligoelement that can be used for the production of varnishes, paints, enamels, plasticizers, alloying additives to oils.

A known method of producing oligomers of butylene in various solid catalysts (U.S. Pat. USA N 3875075, op. 1.04.75 g). The disadvantage is the complicated technology of their preparation and subsequent use for polymerization.

The closest in technical essence is a method of preparation of the catalyst complex according to which in toluene with vigorous stirring, aluminum chloride, and then diphenylacetic rubber piperylene and oxidized liquid synthetic rubber piperitenone (linseed oil "Pentel"). Index of regulations Tr 1.03290-87).

The disadvantage of this method is the formation in the preparation of the catalyst complex is insoluble precipitate, causing the clogging of the equipment and reduce the rate of polymerization, and a long period of preparation of the catalyst.

The aim of the invention is to obtain a homogeneous catalyst complex without sediment, reduction of time for its preparation, and its increased activity.

This goal is achieved by the fact that in the known method of preparation of the catalyst complex, involving the interaction of aluminum chloride and diphenyloxide in aromatic solvent as a modifying additive is ethyl acetate in a mass ratio of aluminum chloride: diphenyloxide acid ethyl ester 1:(0,4-0,7):(0,1-0,3).

The ethyl acetate is a product that allows you to obtain the homogeneous solution of the catalyst without sediment in less time due to the formation of a complex catalyst complex of aluminum chloride, diphenyloxide and ethyl acetate.

P R I m e R 1 (the prototype).

In laboratory conditions in a reactor with a stirrer and a thermometer at 35-40aboutWith zag the activities preparation of complex 11-12 o'clock After preparation of the catalytic complex checking its activity. Activity refers to the content of active aluminum chloride, which came into complex diphenyloxide, excluding aluminum chloride, which entered into complexation with toluene. According to the results of the analysis of the prepared catalytic complex of the content of active aluminum chloride 65-70% of the total concentration of loaded aluminum chloride in solution. The number of the formed precipitate is 75 grams or 0.73% of the loaded AlCl3.

P R I m m e R 2 (the proposed method).

In laboratory conditions in a reactor with a stirrer and a thermometer at 20-25aboutTo download under vigorous stirring 164,5 kg of toluene, 2.5 kg of ethyl acetate, 5 kg of diphenyloxide and 10.2 kg aluminum chloride. The weight ratio of AlCl3:FEFD:ethyl acetate 1:0,492:0,246. The cooking time of the catalytic complex 4 o'clock On the results of the analysis of the prepared catalytic complex of the content of active aluminum chloride 87.2% of the total concentration of loaded aluminum chloride in solution. The amount of the formed precipitate UTS.

P R I m e R s 3-6. The same as in example 2 is as acetic acid in the specified proportions of the components allows to obtain the solution of the catalyst complex without sediment. The content of active aluminum chloride from the total concentration of downloadable AlCl3increases from 65-70% to 86% of the cooking time and reduces the complex with 11-12 hours to 3-3,5 hours

The METHOD of preparation of the CATALYST COMPLEX TO OBTAIN OLIGOELEMENT by reacting aluminum chloride and diphenyloxide in aromatic solvent, characterized in that interaction using advanced modifying additive ethyl acetate in a mass ratio of aluminum chloride as diphenyloxide acid ethyl ester 1 (0,4 0,7) (0,1 0,3).

 

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