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Preparation of organometallic compounds

A compound and metal technology, applied in 3/13 organic compounds without C-metal bonds, 4/14 organic compounds without C-metal bonds, organic chemistry, etc., can solve the problem of low yield of TMG

Inactive Publication Date: 2016-05-25
ROHM & HAAS ELECTRONICS MATERIALS LLC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the TMG yield reported in this patent application is still low, only 52%, not different from that reported in US6,495,707

Method used

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  • Preparation of organometallic compounds
  • Preparation of organometallic compounds
  • Preparation of organometallic compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The table below shows various organometallic compounds prepared according to this method. Suitable organic solvents are listed where such solvents are required or optionally used.

[0057] compound

[0058] Abbreviations have the following meanings: LAB = linear alkylbenzene; TDMA = tetrakis(dimethylamine) or [(CH 3 ) 2 N] 4 ; and TEMA=tetrakis(methylethylamine) or [(CH 3 )(CH 3 CH 2 )N] 4 .

Embodiment 2

[0060] In a reactor (which comprises a contact zone containing a first inlet and a second inlet, a plurality of heat transfer zones, a plurality of mixing zones with different radii of curvature and a reaction zone after each mixing zone), at 200- 300KPa, 10-30°C temperature, add a large amount at a flow rate of 10-20 units / h as the first reactant TMA liquid flow and at 200-300KPa, 10-30°C temperature, add a large amount at a flow rate of 20-40 units / h as the second reaction A liquid stream of tripropylamine ("TPA") was passed through the reactor inlet into a laminar flow environment. The flow rate was set to control the molar ratio of TPA to TMA slightly greater than 1 / 1. The two reactant streams are fed into the mixing zone of the reactor with concentric and substantially laminar flow. Each reactant stream entering the mixing zone has a Reynolds number 20 seconds. Upon leaving the reactor, the product (TMA-TPA adduct) stream is passed to a separation unit to remove impurit...

Embodiment 3

[0062] Into a reactor similar to the reactor used in Example 2, a large amount of the TMA-TPA liquid from Example 2 was added as the first reactant at a temperature of 200-300KPa, 40-60°C at a flow rate of 20-40 units / h Flow and add a large amount of gallium chloride in aromatic hydrocarbon solvent as the second reactant at a flow rate of 20-40 units / h at a temperature of 200-300KPa, 2-10°C to maintain the molar ratio of aluminum to gallium metal greater than 1 / 1 . The heat transfer zone of the reactor maintains the temperature at the outlet of the reactor at 85-100°C. The reactor was operated continuously for more than 24 hours, during which time the product (trimethylgallium or "TMG") was continuously purified in the separation unit to produce over 100 kg of high purity TMG in an overall yield of >85%.

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Abstract

Preparation of organometallic compounds. A method for continuously preparing an organometallic compound, the method comprising: providing an apparatus comprising a reactor unit comprising a plurality of mixing zones and one or more heat transfer zones; continuously flowing a first reactant stream and The second reactant stream is passed into the contacting zone having laminar flow to form a reaction mixture flow, wherein the first reactant stream and the second reactant stream are co-directional and substantially laminar, and wherein the first reactant is a metal-containing compound; divert the reaction mixture flow from a laminar mixing zone to a heat transfer zone and then into a mixing zone with turbulence promoting means; form the reaction mixture flow into an organometallic compound product stream; control the temperature and pressure of the product stream in the heat transfer zone to maintain the majority of the organometallic compound in a liquid phase; and transferring the product stream to a separation unit to separate the organometallic compound.

Description

technical field [0001] The invention relates to the field of metal-containing compounds, especially the field of preparing organometallic compounds. Background technique [0002] Metal-containing compounds are used in a variety of applications, such as catalysts and raw materials for the production of metal films. One use of these compounds is in the preparation of electronic devices, such as semiconductors. Many semiconductor materials are prepared from high-purity metal-organic (organometallic) compounds using well-established deposition techniques such as metal-organic vapor phase epitaxy, metal-organic molecular beam epitaxy, metal-organic chemical vapor deposition, and atomic layer deposition. [0003] Handling of many of these organometallic compounds or their starting materials poses significant challenges due to their air reactivity, pyrophoricity, and / or toxicity. Care must be taken in the production of these organometallic compounds. Common organometallic compou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00C07F5/06B01F23/10
CPCC07F5/00C07F7/003C07F7/00B03D1/004C07B61/00C07F5/003B01J19/2405B01J2219/00051B01J2219/24
Inventor R·S·迪克西特柏桦C·D·莫德特兰德R·A·韦尔J·G·小彭德格斯特C·P·克里斯滕森D·V·舍奈-卡特哈特A·阿曼奇安K·M·克鲁奇R·F·珀卡里
Owner ROHM & HAAS ELECTRONICS MATERIALS LLC