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Clean process method for synthesizing trimethylaluminum

A technology of trimethylaluminum and process method, which is applied in the chemical industry to achieve the effect of good material fluidity

Inactive Publication Date: 2020-05-08
南京奥格美化学研究所有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The method of above-mentioned patent still has many defectives

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1, system trimethylaluminum.

[0045] A four-necked glass flask equipped with a magnetic stirrer, a reflux condenser, a thermometer, a methylaluminum chloride addition funnel, and a sodium dropping funnel; the methyl chloride inlet is placed on the top of the reflux condenser, and the air in the bottle is replaced with methyl chloride. 103.1 grams of sesquimethylaluminum chloride, whose components are 0.52 moles of methylaluminum dichloride and 0.48 moles of dimethylaluminum chloride, and 260 milliliters of o-dichlorobenzene are added to the flask, stirred and heated to 100 ° C, Chloromethane air pressure is maintained at 670Pa (about 5mmHg), and 70 grams (3.04 moles) of molten sodium begin to drip, and this moment exotherm is violent, can observe its air intake in the methyl chloride bubble bottle, and flask and condenser are cooled with silicone oil bath, Adjust the rate of sodium addition so that the temperature in the bottle is maintained at 110-120°C. Ad...

Embodiment 2

[0046] Embodiment 2, preparation of trimethylaluminum dechlorination process.

[0047] Phase 1, Synthesis.

[0048] A four-necked glass flask equipped with a magnetic stirrer, a reflux condenser, a thermometer, a methylaluminum chloride addition funnel, and a sodium dropping funnel; the methyl chloride inlet is placed on the top of the reflux condenser, and the air in the bottle is replaced with methyl chloride. 103.1 grams of sesquimethylaluminum chloride, whose components are 0.52 moles of methylaluminum dichloride and 0.48 moles of dimethylaluminum chloride, and 260 milliliters of o-dichlorobenzene are added to the flask, stirred and heated to 100 ° C, The air pressure of methyl chloride is maintained at 670Pa (about 5mmHg), and 70 grams (3.04 moles) of molten sodium are started to be added dropwise. At this time, the heat is released violently. The flask and condenser are cooled with a silicone oil bath, and the sodium drop rate is adjusted to maintain the temperature in t...

Embodiment 3

[0055] Example 3, continuous preparation of trimethylaluminum.

[0056] Preparation device configuration: The synthesis unit has two reactors for mixing and heat preservation, one reactor for the oxygen removal unit, one filter ball and one set of distillation unit for the trimethylaluminum unit, and these three units are connected in series. The filter residue processing unit is set up separately.

[0057] Unit 1, Synthesis.

[0058] The first 500ml four-neck glass flask is equipped with a magnetic stirrer, the reflux condenser and the thermometer are shared by a Y-shaped tube, the inlet of methyl chloride is placed on the top of the reflux condenser, and methylaluminum chloride and o-dichlorobenzene are shared One port and the sodium drop port are all inserted into the bottom of the bottle through the glass tube; one end of the discharge tube (overflow tube) is inserted from the bottle mouth to the 250 ml volume liquid level in the first bottle, and the other end is connect...

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Abstract

The invention relates to a clean process method for synthesizing trimethylaluminum. A trace amount of dimethyl aluminum chloride is generated in a reaction product of the following formula: 2Al + 3CH3Cl = CH3AlCl2.(CH3)2AlCl, a compound of formula MAl(CH3)4 is used to reduce the chlorine content of the trimethylaluminum, M is a Group IA element including lithium, sodium, and potassium; NaAl(CH3)4tetramethylaluminum sodium is adopted, and the dimethyl aluminum chloride is eliminated. Through removing the residual chlorine in the trimethylaluminum by using the tetramethylaluminum sodium, and recovering the tetramethylaluminum sodium, and converting the tetramethylaluminum sodium into methylaluminum chloride to be used as an initial raw material, the clean process method for synthesizing thetrimethylaluminum is a green process without three wastes.

Description

technical field [0001] The invention relates to the preparation of trimethylaluminum and belongs to the technical field of chemical industry. Background technique [0002] Trimethylaluminum is used to prepare methylalumoxane as a metallocene cocatalyst for olefin polymerization, for the preparation of semiconductor materials and the sealing layer of photovoltaic cells, for the production of nanomaterials, etc. Due to its wide application, trimethylaluminum is attracting more and more attention. [0003] The process route for preparing trimethylaluminum has successively appeared magnesium-aluminum alloy method, amalgam method and cryolite method, etc. These methods for preparing trimethylaluminum have high starting raw material prices, large amount of by-products and no use value of by-products , Due to the high reactivity of waste slag, the investment in waste slag treatment equipment is large and the cost is large. [0004] Thus, the alkali metal reduction method was deve...

Claims

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Application Information

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IPC IPC(8): C07F5/06
CPCC07F5/062
Inventor 庄建元庄中兴
Owner 南京奥格美化学研究所有限公司
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