The method of obtaining dimethylzinc

 

(57) Abstract:

The invention relates to the production of Organoelement compounds, in particular dimethylzinc. The method is carried out by reacting iodotope bromide with alloy zinc-copper-silver. This is achieved by reducing the duration of the synthesis process dimethylzinc and increasing the yield of the target product.

The invention relates to the production of Organoelement compounds, in particular dimethylzinc.

A method of obtaining dimethylzinc by interaction iodotope bromide with zinc-copper alloy [1]. The alloy contains 8 - 10 wt.% copper and 90 - 92 wt. % zinc and is prepared by heating a mixture of powdered metals to a temperature of 420oC in an inert atmosphere. Air alloy rapidly loses its activity due to oxidation and therefore it is prepared just prior to synthesis dimethylzinc. The synthesis is carried out by introducing iodotope bromide to crushed zinc-copper alloy is added dropwise in an inert gas atmosphere with constant stirring of the reaction mass. The process proceeds in two stages, the first of which interact iodotope bromide with alloy education promezhutochnoC) and lasts for 9 to 15 hours Of which 3 hours is spent on the gradual addition iodotope methyl, and the remaining time to complete its interaction with the alloy and the formation of methylsergide

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In the second stage, the temperature of the reaction mixture rises to 60 - 65oC is the disproportionation of methylsergide education dimethylzinc:

2CH3ZnI _ (CH3)2Zn+Zn+I2< / BR>
Phase disproportionation continues for 7 to 9 h, the reaction mass Argonauts target product. Contained in the copper alloy of direct participation in the reaction does not accept or after the distillation dimethylzinc remains in a solid non-volatile reaction slurry.

The total duration of the process of obtaining dimethylzinc in a known manner (without taking into account the time of its isolation from the reaction mass reaches one-day (16 - 24 h). Despite guidance on quantitative (100%) the yield of the target product by a known method, its real reproducible value is only 70 - 80% of theoretical.

This known method of obtaining dimethylzinc selected by the authors as a prototype of the invention as closest to him tenia dimethylzinc is the long duration of the process, not a high yield of the target product, the impossibility of making alloy zinc-copper in advance due to its oxidation.

The problem solved by the invention is the increased activity of the zinc-copper alloy, leading to reduced synthesis time dimethylzinc and increase its output.

The problem is solved in that in the known method of obtaining dimethylzinc interaction iodotope bromide with zinc-copper alloy, the alloy further added silver in an amount of 0.1 to 1.0 wt.% when the following concentrations of all ingredients, wt.%:

Zinc - 89 - 91,9

Copper - 8 - 10

Silver - 0,1 - 1,0

Due to the introduction of silver in the zinc-copper alloy increases its chemical activity and stage of formation of the intermediate methylsergide significantly reduced in time and ends almost simultaneously with the completion of the addition iodotope bromide. After 0.5 h after boiling iodotope bromide in the reactor stops. Approximately 1.5 times (up to 5 - 6 h) and reduced phase disproportionation of methylsergide education dimethylzinc. The total duration of the process of obtaining dimethylzinc according to the invention, the composition is portsionirovaniem). Thus, the duration of the process of obtaining dimethylzinc reduced 1.7 - 2.8 times (8,5 - 9,5 h by the proposed method; 16 to 24 h in the prototype). Simultaneously, 87 - 95% of theoretical increases the yield of the target product, that is 1.2 - 1.3 times in comparison with the prototype. In addition, the addition to the alloy of silver in an amount of 0.1 to 1.0 wt.% increases its resistance to oxidation and contributes to the conservation of chemical activity in a long time. For example, the syntheses dimethylzinc carried out immediately after preparation of ternary alloy zinc-copper-silver and one month after its storage in the air gave the same results on the yield of the target product and the duration of the process. It allows you to separate in time the processes of preparation of the alloy and its use, that is, to produce the alloy in advance, which is particularly beneficial during production dimethylzinc.

Used according to the invention, an expensive noble metal (silver) after synthesis dimethylzinc and its distillation from the reaction mass remains in the sludge and can be selected from it for reuse in the preparation of the alloy.

The essential features offers the becoming of this alloy, wt. %: 89 - 91.9 zinc; 8 - 10 copper; 0.1 to 1.0 silver. These features combine to provide a positive effect, which consists in reducing the duration of the process of obtaining dimethylzinc and increase the yield of the target product. If the content of silver in the alloy is less than 0.1 wt.%, the specified positive effect is not achieved. Increasing the concentration of silver in the alloy above 1.0 wt.% does not increase the positive effect, and therefore impractical. Only the silver content in the concentration range of 0.1 - 1.0 wt.% provides maximum effect: reduce process time: 1.7 - 2.8 times and increase the yield of the target product 1.2 - 1.3 times.

Claimed in the present invention the combination of features - the presence of additional ingredient (silver) at a concentration of 0.1 - 1.0 wt.% - it is not known from open sources of scientific, technical and patent information and is new.

The following is a specific example of the invention:

Preparation of alloy zinc - copper - silver.

In a quartz Cup thoroughly mixed with 900 g of zinc powder, 95 g of copper powder and 5 g of silver powder. Cup us is with argon. After being dismissed from the office of air the mixture is heated to a temperature of 400 - 420oC and incubated for 30 to 45 minutes While the zinc is melted and forms a gray-black mass of the alloy, which after cooling is easily crushed to a granular powder.

The result is 1 kg of an alloy containing 90 wt.% zinc; 9,5% wt. % of copper and 0.5 wt.% silver.

Getting dimethylzinc.

In all-metal synthesis reactor with a capacity of 3 l was placed 500 g of crushed alloy. The reactor is equipped with a "face", which circulates liquid coolant (water), allow to heat it in the temperature range 5 - 80oC. Reactor provided with a mechanical agitator with electric and reflux condenser and addition funnel, completely made of metal and provided with viewing Windows to monitor the feed rate and the rate of boiling in the reactor liquid reagents.

In an addition funnel pour 367 g (161 ml) iodotope bromide, after which the reactor was rinsed with argon. Then into the reactor at a rate of 1 ml/min serves modesty methyl. The interaction of the reagent with a triple alloy zinc-copper-silver begins immediately. Since this reaction is exothermic, heat is was ivalsa. With this aim, adjust the feed rate to the reactor new portions iodotope bromide and temperature of the reactor due to its external cooling or heating. Within 3 hours into the reactor dropwise poured all modesty methyl. After this boiling iodotope methyl slows, and then stops. To complete the process of its interaction with alloy reactor is forcibly heated to a temperature of 42 - 45oC for half an hour. When boiling iodotope methyl again slows down, the reactor is heated to 60 - 65oC and maintained at these conditions for 6 hours After that, the reflux condenser is replaced by a direct and conduct the distillation dimethylzinc. Obtain 115 g of the target product.

Output dimethylzinc is 93% of theoretical (eudistoma the stands).

The method of obtaining dimethylzinc the interaction of methyl iodide with zinc-copper alloy, characterized in that the zinc - copper alloy additionally contains silver at the following ratio of ingredients, wt.%:

Zinc - 89 - 91,9

Copper - 8 - 10,0

Silver - 0,1 - 1,01

 

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