CS203125B2 - Method for the continuous production of sesquialkylhalogenaluminium - Google Patents

Description

The present invention relates to a process for the continuous production of a sesguialkylhaloaluminum of the general formula R 1 -AlgXp in which

R is lower alkyl;

X denotes halogne.

These compounds are used as catalysts for the polymerization of alkenes, as catalysts of the Friedel-Crafts type and also as intermediates for oroanole or organic compounds, for example in the preparation of tetrahydro-long-chain alcohols.

Until now, the alkyl alkyl halide is obtained by introducing into the reactor flushed with nitrogen a corresponding aluminum mono-matrix and then, after its activation, the alkyl halide is introduced. At the end of the process, reaction foam catalysed decomposition reactions begin to dominate, resulting in a large range of gaseous products, making it impossible to fully propagate aluminum. It is also known to carry out a fixed aluminum alkali halide with an overlapped reaction product. However, this procedure is only suitable for laboratory scale use.

The above-mentioned disadvantages of the prior art are largely eliminated in the process for the continuous production of a halogen alkyl of the formula R @ 1 -Al-X- in which R is C1 -C4 alkyl and X is halogen, by reacting aluminum with alkenyl halosiums, optionally in the lithium catalysts, According to the invention, the principle of the invention is that aluminum or its alloys are introduced into the reaction network under constant agitation at 80-120% of the stoichiometric quantity and below the alkali metal of the formula RX, in which R and X are previously treated. as defined above, and the final product is continuously removed together with the reaction foam. Preferably, at least one of the reaction components is fed to the reaction salt with the addition of a reaction catalyst, for example an alkyl bromide or alkyl aluminum, and the aluminum or its alloys and the alkyl allogenide are fed to the reaction mixture at a temperature of 1 to 60 ° C. The advantages of the process according to the invention are, inter alia, that it is possible to achieve a yield close to theory in a very short reaction time. The apparatus used for this method is very simple and furthermore the method according to the invention is suitable for use on a technical scale.

According to the invention, a process for the continuous production of a sesguialkylhaloaluminum of the formula R ^Al ^Xp is carried out in which R X and X mají are as previously defined by feeding aluminum, preferably in a stoichiometric amount, into a vertical tube reactor filled with susguialkylhaloaluminum. or an alloy thereof and an alkyl halide of the formula RX in which R and X are as previously defined.

The alkyl halide bubbles that enter the intensive mixing zone, where the amount of aluminum is present, do not bubble normally, but achieve controlled transverse movement, thereby extending their contact time with the aluminum considerably. This strongly exothermic process is conducted under constant temperature and pressure conditions, preferably such that the temperature does not exceed 60 ° C at atmospheric pressure.

In order to increase the reaction rate, optionally known reaction catalysts are used, such as iodine or bromine compounds, and can be introduced into the reaction medium either with aluminum or its alloys or with an alkyl halide. The resulting reaction foam is continuously removed along with the end product, which is then purified by distillation.

The invention is explained in more detail in the examples.

He did

In a vertical, tubular reactor with a propeller stirrer, 500 cc, 300 cc of sesguiethylchloroaluminum was introduced. After reaching a temperature of 60 ° C with vigorous stirring, aluminum dust was added through the top throat and iodine vapor ethyl chloride was added through the bottom throat. Aluminum was added to the reactor at a rate of 11 gh @ -1 and ethyl chloride at a rate of 39 gh @ -1. Iodine was added in an amount of 1% by weight relative to the amount of aluminum added. Sesguiethylchloroaluminum was taken at 47 cnP.h ^-1 . The reactor was cooled by blowing air so that the reaction temperature did not exceed 60 ° C. The product obtained was distilled at 1 mmHg at 70 ° C. The distillation residue was a reaction foam. The synthesis yield was 98% by weight and the product contained 54% by weight of ethyldichloroaluminum.

Example 2

Aluminum was fed to the reactor of Example 1 at a rate of 33 gh ^-1 and ethyl chloride at a rate of 117 gh ^-1 . Ethyl bromide was added in an amount of 3% by weight relative to the aluminum feed. Sesguiethylchlorhliník amount was taken at 145 cm ^ .h ^"first The reactor was cooled with membrane toluene. The product obtained was purified as in Example 1. The yield of synthesis was 97% by weight and the product contained 53% by weight of ethyldichloroaluminum.

Example 3

Into the reactor of Example 1 filled with 300 cm @ sesguimethylchlorhliníku aluminum was fed at 11 ^_1 gh and gh methylchorid speed of 31 ~ 4 J.ód was added with aluminum in an amount of 1% by weight. Sesguimethylchlorhliník was taken at a rate of 40 crn ^ .h ^"first The reactor was cooled with dry ice. The product obtained was distilled at atmospheric pressure at 120 ° C. The yield of the synthesis was 98.5% by weight and the product contained 57% by weight of methyldichloroaluminum.

Example 4

To a reactor as in Example 1 filled with 300 cm @ sesguiethylbromhliníku aluminum was fed at 11 g * hour ^_1 and ethyl bromide speed 66 gh ^first Sesguiethylbromhliník was taken at 74 cm mnnOství \ h ^_1. The reactor was cooled by membrane toluene. The product obtained was distilled. The yield of the synthesis was 99% by weight and the product contained 59% by weight of aluminum dibody aluminum.

Example 5

To the reactor of Example 1 charged with 300 cm @ 3 of ethyl iodoaluminum was added aluminum at a rate of 11 g.h @ -1 and ethyl iodide at a rate of 94 g.h @ -1. Sesguiethyl iodoaluminum was taken at 102 cb.h '. The reactor was cooled with dry ice. The yield of the synthesis was 100% and the product contained 61% of the mono-di-iodo-amino acids. .

Example 6

Into the reactor of Example 1 filled with 300 cm @ sesguibethylrгobhliníku aluminum was fed at 14 gh ^"1 methylbrobid rate 57.3 Uh ^first The reactor was removed at 67 cm @ 3 / h. The reactor was cooled with toluene. The product obtained was distilled. The yield of the synthesis was 99% by weight and the product contained 62% by weight of sesguimetlyl-aluminum-aluminum.

Example 7

Aluminum was fed at a rate of 11 gh @ -1 and 0 * X @ -1 @ -1 @ 1-50010 at a rate of 85 g @ ^-1 into the reactor of Example 1 packed with 30. Sesguibbtnlllódhlioík was obtained at a rate of 84 ctb.h ¹ . The reactor was cooled with dry ice. The product obtained was distilled. The synthesis yield was 100% by weight and the product contained 64% by weight of sesguibethyl iodoaluminum.

SUBJECT OF THE INVENTION

Claims (3)

SUBJECT OF THE INVENTION CLAIMS 1. A process for the continuous production of a sesylic halogen halide of the general formula R @ 1 A @ X -, in which: R is C 1 -C 4 alkyl; X represents a halogen atom by reaction of aluminum with alkyl halides, optionally in the presence of catalysts, characterized in that aluminum or its alloys and a lower alkyl halide of the formula RX are fed to the reaction mixture with stirring at 80 to 120% stoichiometric charge and below wherein R and X are as previously defined, and the final product is continuously removed together with the reaction foam. 2. The process of claim 1 wherein at least one of the reactants is fed to the reaction mixture with the addition of a reaction catalyst such as an alkyl bromide or an alkyl iodide. 3. The process of claim 1 wherein the aluminum or its alloys and the alkyl halide are fed to the reaction mixture at a temperature of from 1 to 60 ° C. Sevarogralie, n. P. Plant 7, Most