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A kind of purification method of trimethylaluminum crude product

A technology of trimethylaluminum crude product and purification method, which is applied in the field of purification of trimethylaluminum crude product, can solve the problems of high cost and large liquid holding capacity, and achieve simple manufacturing process, improved heat transfer capacity and good corrosion resistance Effect

Active Publication Date: 2021-04-06
江西石华精细化工科技协同创新有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to obtain higher product purity, it is also necessary to optimize the pressure drop and the uniformity of gas distribution, and the cost of various new high-efficiency packing is relatively high and the liquid holding capacity is relatively large

Method used

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  • A kind of purification method of trimethylaluminum crude product

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for purifying trimethylaluminum crude product, comprising the following steps:

[0026] (1) The microchannel rectification tower is exchanged with inert gas, and the crude product of trimethylaluminum (purity 99.93%) is transferred to the rectification kettle;

[0027] (2) After the materials are transferred, close the feed valve and carry out rectification. Rectification pressure: 0.02MPa, rectification temperature: 80°C.

[0028] (3) intercept the distilled material with a boiling point of 125-127°C under standard atmospheric pressure, and collect it with a cold trap to obtain a high-purity trimethylaluminum product. Detected by ICP-MS and NMR, the purity of trimethylaluminum obtained by the method of this embodiment is calculated to be 7.0N (99.99999%).

[0029] The structure of the microchannel rectification tower is: the distillation column inside the rectification tower is two concentric column structures (inner tube 2 and outer tube 3), and the material...

Embodiment 2

[0031] A method for purifying trimethylaluminum crude product, is characterized in that, comprises the following steps:

[0032] (1) The microchannel rectification tower is exchanged with inert gas, so that the atmosphere of ultra-low water and oxygen content is maintained in the tower, and the crude product of trimethylaluminum (purity 99.93%) is transferred to the rectification kettle with a slight vacuum;

[0033] (2) After the materials are transferred, close the feed valve and carry out rectification. Rectification pressure: 0.05MPa Rectification temperature: 100°C.

[0034] (3) intercept the distilled material with a boiling point of 125-127°C under standard atmospheric pressure, and collect it with a cold trap to obtain a high-purity trimethylaluminum product. Detected by ICP-MS and NMR, it is calculated that the purity of trimethylaluminum obtained by the method of this embodiment is 7.3N (99.999993%).

[0035] The structure of the microchannel rectification tower is ...

Embodiment 3

[0037] A method for purifying trimethylaluminum crude product, comprising the following steps:

[0038] (1) The microchannel rectification tower is exchanged with inert gas, so that the atmosphere of ultra-low water and oxygen content is maintained in the tower, and the crude product of trimethylaluminum (purity 99.93%) is transferred to the rectification kettle with a slight vacuum;

[0039] (2) After the materials are transferred, close the feed valve and carry out rectification. Rectification temperature: 128°C, rectification pressure: 0.1MPa.

[0040] (3) intercept the distilled material with a boiling point of 125-127°C under standard atmospheric pressure, and collect it with a cold trap to obtain a high-purity trimethylaluminum product. Detected by ICP-MS and NMR, the purity of trimethylaluminum obtained by the method of this embodiment is calculated to be 7.2N (99.999992%).

[0041] The structure of the microchannel rectification tower is as follows: the distillation c...

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Abstract

The invention discloses a method for purifying trimethylaluminum crude products. The internal structure of the traditional distillation tower is improved, and the tray structure is replaced by a concentric column with a microchannel structure. After the rising gas is condensed, it spirals along two tubes The groove flows down, and its structure makes the two phases contact more fully. By strengthening its gas-liquid mass transfer and heat transfer process, the rectification process has a high separation efficiency and high-purity trimethylaluminum is obtained.

Description

technical field [0001] The invention belongs to the technical field of microelectronic materials, and in particular relates to a method for purifying crude trimethylaluminum. Background technique [0002] High-purity trimethylaluminum belongs to high-purity metal-organic compounds. It is a key supporting raw material for compound semiconductor thin film materials prepared by advanced metal-organic chemical vapor deposition (MOCVD) technology or atomic layer deposition thin film technology (ALD). It is widely used in LED equipment, new generation solar cells, phase change memory, semiconductor lasers, infrared detectors and supercomputers. [0003] As the raw material of microelectronic materials, the precursor of aluminum nitride requires a very high purity of 99.9999% or even 99.99999% for trimethylaluminum. Relatively speaking, there are many impurities and the difference between its boiling point is small, so it brings great difficulties to separation and purification. D...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/14B01D3/32C07F5/06
CPCB01D3/14B01D3/32
Inventor 廖维林陈飞彪谢贤清芮培欣刘德永涂媛红雷志伟
Owner 江西石华精细化工科技协同创新有限公司
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