Technique for synthesizing triethylaluminum

A triethylaluminum, synthesis process technology, applied in the field of triethylaluminum synthesis process, can solve the problems of complex process, small scale, low production capacity, etc.

Inactive Publication Date: 2008-07-16
王学力
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Triethylaluminum products have been produced in some domestic enterprises, and the scale is too small to meet market demand
This production state has the characteristics of backward technology, complex process and low production capacity

Method used

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  • Technique for synthesizing triethylaluminum

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) The titanium powder catalyst is melted in the aluminum powder:

[0021] After dissolving the aluminum ingot in the melting furnace, add titanium powder (below 200 mesh) into the dissolved aluminum and stir to make the titanium evenly dispersed in the dissolved aluminum, atomize and spray the dissolved aluminum to obtain 0.25% titanium-containing ( 0.2-0.3% can be) titanium-containing aluminum powder.

[0022] 2) Hydrogenation reaction is carried out in a magnetically driven reaction hydrogenation kettle: 4 tons of triethylaluminum retention solution is reserved in the kettle as a seed, and the pressure is 12MPa, and 175 kilograms of aluminum powder containing the above-mentioned catalyst is added to the kettle under nitrogen protection, The temperature was raised to 132° C. under stirring, and hydrogenation was continued for 7 hours under a pressure of 10 MPa to complete the reaction.

[0023] 3) Direct ethylation in the hydrogenation kettle: After the hydrogenation...

Embodiment 2

[0035] The reaction of step 3) can be carried out in the ethylation reactor, and others are with embodiment 1.

[0036] A spiral ethylation reactor is used. There is a 100-meter spiral tube with an inner diameter of 200 mm in the shell side (the above-mentioned materials are passed inside). The tube inlet is where the hydrogenated material and ethylene are mixed. The reactants react in the 100-meter tube, and the shell Hexane is housed in the process, and when the reaction temperature rises, the hexane vaporizes in the shell, and returns to the shell after being cooled by the shell-and-tube condenser (water cooling) above the shell, and the vapor pressure of the hexane is controlled to be 0.15MPa. The reaction temperature was 100°C. Get 150 kg / hour of crude triethylaluminum.

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Abstract

The invention relates to a synthesizing process of aluminum triethide. The process contains the following procedures: continuous hydrogenation in a hydrogenation reactor for hydrogenation of titanium-containing aluminum powder for six to seven hours under the protection of inert gas and a pressure of 10-12MPa with aluminum triethide as the seed; continuous ethylene introduction under 0.5-3 pressure to acquire crude aluminum triethide after reaction completion within five to six hours; vaporizing distillation to separate impurities and ethylene transformation reaction to get aluminum triethide; dilution of residual impurity solution after distillation with hexane; hydrolization; and hexane recovery. The hydrogenation pressure of the invention is low, decreased from 28MPa to 10MPa. Adopting the body catalysis with aluminum triethide seed to disperse aluminum powder, the invention has simple process flow, All the equipment are localized. No pollution is caused. The cost is low while the yield is over 85-90 percent and the product quality is high.

Description

technical field [0001] The invention relates to an organic synthesis process, in particular to a synthesis process of triethylaluminum Background technique [0002] Triethylaluminum, molecular formula: (C 2 h 5 ) 3 Al (Aluminum triethyl) is mainly used in organic synthesis, especially as an important part of the catalyst in the polymerization of ethylene and propylene, and is also used as rocket fuel. There are two synthesis techniques of triethylaluminum, which are indirect synthesis method and direct synthesis method. Most of the research in some domestic laboratories adopts indirect production methods. The direct synthesis method is to hydrogenate diethyl aluminum hydride in the presence of triethyl aluminum seeds and aluminum powder, and diethyl aluminum hydride is passed into ethylene to form triethylaluminum. Industrial application has not yet been realized. At present, almost all the triethylaluminum needed in the country is imported, and 80% of its product mark...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06
Inventor 王学力
Owner 王学力
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