Atomization synthesizer and application thereof in synthesis of alkylaluminoxane

Abstract

The invention discloses an atomization synthesizer which comprises a reaction kettle (11) with a stirring device (12), a high-position visible water storage tank (10), a liquid flowmeter (8), an atomizer (9), a water inlet pipe (5), a central gas inlet pipe (6) and a peripheral gas inlet pipe (7), wherein the atomizer (9) is mainly composed of a central barrel (9-b), an outer barrel (9-a) and an annular nozzle (9-c); the outer barrel (9-a) is in an cylindrical / inverted V-shaped round table composite structure, and the length-to-diameter ratio is 8-10 on the basis of the diameter of the cylindrical part; the central barrel (9-b) and outer barrel (9-a) are coaxial and concentric, the central barrel (9-b) and the cylindrical part of the outer barrel (9-a) are of the same height, the bottom end of the central barrel (9-b) is closed, and the length-to-diameter ratio of the central barrel (9-b) is 8-10; the side wall on the middle and lower parts of the central barrel (9-b) is uniformly distributed with pinholes (9-d), wherein the density of the pinholes is 1-2 / mm<2>, and the sizes of the pinholes are 0.4-0.6mm; the bottom end of the outer barrel (9-a) is provided with the annular nozzle (9-c) which has the same diameter as the central barrel, and the clearances of the pinholes in the annular nozzle are 0.5-0.8mm; the water inlet pipe (5) and central gas inlet pipe (6) are inserted into the central barrel (9-b); and the peripheral gas inlet pipe (7) is connected between the outer barrel (9-a) and the central barrel (9-b). The atomization synthesizer has the advantages of controllable pressure, favorable water atomization effect and low cost, is safe and easy for operation, can be well applied to direct hydrosynthesis reaction of alkylaluminoxane, and greatly increases the yield of alkylaluminoxane as compared with the indirect hydrosynthesis technique.

Description

technical field [0001] The invention relates to an atomization synthesis device and its application in the synthesis of alkyl aluminoxane, in particular to an atomization device for synthesis of alkyl aluminoxane in direct water process and its application. Background technique [0002] There are many preparation methods of alkylaluminoxane, which can be summarized into two categories: indirect water process and direct water process. The indirect water process usually uses the reaction of crystalline hydrates with aluminum alkyls. The yield of this synthetic method target product is lower, generally below 45%, causes the cost of final product higher (US5099050, US5041583, EP393358A 2 , EP383255A 2 , EP208561A 2 , US5248801, US5015749). [0003] The direct water process refers to controlling certain process conditions and introducing water (ice, liquid water, water vapor) in various states into the reactor to react with the solution of aluminum alkyl / inert solvent through...

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Problems solved by technology

The problem is that the nozzle is easy to block, and because the water is added very slowly, and the heating of the reactor uses a thermocouple, and the cooling uses a jacket, the operation of the equipment is complicated, the energy consumption is huge, and the operation is dangerous, so it is not suitable for industrial production. , similarly, US5043942 also proposed

[0006] In short, the reaction between alkylaluminum and water in the direct water process is very violent, and the reaction is difficult to control. Therefore, there are extremely high requirements for the control of reaction conditions and synthesis equipment. It is necessary to obtain a higher reaction yield of the target product and reduce production. The danger of the process often requires the design of various special equipment, and the cost of the device is greatly increased.

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