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Novel method for synthesizing trimethylaluminum

A technology of trimethylaluminum and a new method, which is applied in the chemical industry, can solve the problems of large amount of waste slag and difficulty in slag discharge, and achieve the effect of improving safety

Pending Publication Date: 2020-04-28
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

Methylaluminum chloride is highly active and spontaneously ignites immediately when exposed to air, metal sodium and aluminum powder are flammable, sodium chloride agglomerates and sticks to the wall, the amount of waste slag is large, and slag removal is difficult
Special equipment is required for slag discharge, special technology and consumable materials are required for safe deactivation of waste slag, and stacking of deactivated waste slag is also a problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1 is made trimethyl aluminum by dimethyl aluminum chloride

[0036]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. 92.5 grams (1.00 moles) of dimethylaluminum chloride and 170 milliliters of mesitylene are placed at the bottom of the bottle, stirred and heated to 100 ° C, the pressure of methyl chloride is maintained at 1000 Pa (about 7 mmHg), and 46 grams (2.00 moles) of molten sodium start Add dropwise, at this time, the heat is violently exothermic, and the gas intake can be observed in the bubbling bottle of methyl chloride. The flask and condenser are cooled with a silicone oil bath, and the sodium drop rate is adjusted to maintain the temperature in the bottle at 100-120°C. Add sodium dropwise for about Af...

Embodiment 2

[0037] Embodiment 2 is made trimethyl aluminum by methyl aluminum dichloride

[0038] 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. 112.9 grams (1.00 moles) of methyl aluminum dichloride and 350 ml of mesitylene were heated to 80°C for complete melting, then added to the flask, stirred and heated to 100°C, the pressure of methyl chloride was maintained at 1000Pa (about 7mmHg), and the molten sodium was 92 gram (4.00 moles) began to drop, at this time, it exothermic violently, its gas intake can be observed in the methyl chloride bubbling bottle, the flask and condenser are cooled with a silicone oil bath, and the sodium drop rate is adjusted to maintain the temperature in the bottle at 100-120 ℃, the sodium was added dropwise f...

Embodiment 3

[0039] Embodiment 3 sesquimethylaluminum chloride and n-heptane system trimethylaluminum

[0040] 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 sesquimethyl aluminum chloride, its components are 0.52 moles of methyl aluminum dichloride and 0.48 moles of dimethyl aluminum chloride, 260 ml of n-heptane, add to the flask, stir and heat up to 100 ° C, chlorine The methane air pressure is maintained at 670Pa (about 5mmHg), and 70 grams (3.04 moles) of molten sodium start to drop. The rate of sodium addition is such that the temperature in the bottle is maintained at 105-115°C. The sodium is added dropwise for about 7 hours, and stops when the methyl chloride is no longer absorbed after the addition is completed. Cool...

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PUM

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Abstract

The invention provides a novel method for synthesizing trimethylaluminum. The reaction is carried out according to the following chemical reaction equation: CH3AlCl2. (CH3) 2AlCl + 6Na + 3CH3Cl = 2 (CH3) 3Al + 6NaCl, chloromethane is added to methyl aluminum chloride and sodium reaction system at the same time, trimethylaluminum is generated through the main reaction, the byproduct nascent-state elemental aluminum immediately reacts with chloromethane to regenerate methylaluminum chloride in situ, and the methylaluminum chloride continues to react with sodium to generate trimethylaluminum. Themethod solves the problems that the byproduct aluminum covers the metal sodium and adheres to the wall of the reactor, the sodium and the methylaluminum chloride react completely, and the yield of the trimethylaluminum is doubled by calculating the fed methylaluminum chloride. The preparation process improves the safety and is environment-friendly.

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 the wide use of trimethylaluminum, it has been paid more and more attention. [0003] A batch of trimethylaluminum patents that appeared earlier had a common disadvantage that the by-products were large and useless, so emission became a problem. [0004] U.S. Patent US2,744,127 (1952, Ziegler) proposed a relatively simple process, using magnesium-aluminum alloys in proportion to Mg 3 Al 2 to Mg 2 Between Al, when no ether exists, react with methyl bromide to obtain 60-75% yield of trimethylaluminum (magnesium-aluminum alloy method). [0005] US Patent No. 2...

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