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Continuous production method of transition metal amido complex

A metal amine-based, production method technology, applied in the field of continuous production of transition metal amine-based complexes, can solve the problems of unsatisfactory industrial continuous production, low reaction efficiency, slow reaction speed, etc., and achieve short reaction time and high conversion rate High, stable and safe effect

Inactive Publication Date: 2019-12-20
合肥安德科铭半导体科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] It can be seen from the above that the preparation of transition metal amine complexes by stirring and mixing and batch reaction usually takes several hours to tens of hours, the reaction speed is slow, and the reaction efficiency is low, which cannot meet the needs of industrial continuous production.

Method used

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  • Continuous production method of transition metal amido complex
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  • Continuous production method of transition metal amido complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] The continuous production method of tetra(methylethylamino) hafnium:

[0081] 1) Mix n-butyllithium and n-hexane in proportion to form liquid A, and the volume concentration of n-butyllithium is 15%; mix ethylmethylamine (purity ≥ 99%) and n-hexane to form liquid B, and The molar concentration of methylamine is 15%; hafnium chloride (purity ≥ 99%) and n-hexane are mixed to prepare liquid C, and the mass concentration of hafnium chloride is 23%;

[0082] 2) Liquid A and Liquid B are respectively cooled to -15°C by a plunger pump and a precooler, and injected into a continuous flow reactor at a temperature of -15°C at a certain flow rate for 5-30 seconds to generate a solid containing The intermediate mixed solution of the product; the flow ratio of A liquid and B liquid is preferably 1:1, more preferably 40-50mL / min;

[0083] 3) The intermediate mixed liquid flows out from the outlet of the continuous flow reactor, and enters a dynamic tubular reactor with a temperature...

Embodiment 2

[0088] Continuous production method of penta(diethylamino)tantalum:

[0089] 1) Prepare tert-butyllithium and n-hexane in proportion to form liquid A, the volume concentration of tert-butyllithium is 12%; mix diethylamine (purity ≥ 99%) and n-hexane to form liquid B, ethyl methyl The molar concentration of amine is 12%; tantalum pentachloride (purity ≥ 99%) is mixed with n-hexane to prepare liquid C, and the mass concentration of tantalum pentachloride is 20.6%;

[0090] 2) Liquid A and liquid B are respectively cooled to -10°C by a plunger pump and a precooler, and injected into a continuous flow reactor at a temperature of -10°C at a certain flow rate to react for 5-30s to form a solid containing The intermediate mixed solution of the product; the flow ratio of A liquid and B liquid is preferably 1:1, more preferably 40-50mL / min;

[0091] 3) The intermediate mixed liquid flows out from the outlet of the continuous flow reactor, and enters the dynamic tubular reactor with a ...

Embodiment 3

[0096] The continuous production method of tetrakis (methyl ethyl amino) zirconium:

[0097] 1) Mix n-butyllithium and toluene solvent in proportion to prepare liquid A, and the volume concentration of n-butyllithium is 13%; mix ethylmethylamine (purity ≥ 99%) and toluene to prepare liquid B, ethyl The molar concentration of methylamine is 13%; ZrCl 4 (purity ≥ 99%) mixed with toluene to prepare liquid C, ZrCl 4 The mass concentration is 16.7%;

[0098] 2) Liquid A and Liquid B are respectively cooled to -15°C by a plunger pump and a precooler, and injected into a continuous flow reactor at a temperature of -15°C at a certain flow rate for 5-30 seconds to generate a solid containing The intermediate mixed solution of the product; the flow ratio of A liquid and B liquid is preferably 1:1, more preferably 40-50mL / min;

[0099] 3) The intermediate mixed liquid flows out from the outlet of the continuous flow reactor, and enters a dynamic tubular reactor with a temperature of -...

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Abstract

The invention provides a continuous production method of a transition metal amido complex. A solution A prepared from a metal alkyl compound and a solvent as main components in proportion and a solution B prepared from organic amine and a solvent as main components in proportion are cooled to the required temperatures and injected into a continuous flow reactor for a reaction, and an intermediatemixed solution containing a solid product enters a dynamic tubular reactor after flowing out of the continuous flow reactor; and a solution C prepared from main components adopting raw materials containing transition metal and a solvent in proportion is cooled to the temperature required for the reaction and enters the dynamic tubular reactor to react with the intermediate mixed solution, and a product mixed solution containing solids is generated, filtered and distilled. Compared with a stirring reaction with a reaction kettle, the method has higher yield, conversion rate and production efficiency, and meanwhile, a production device adopting a special mixing structure and formed by a heat exchange system and a pressure-resistant material has higher stability and safety.

Description

【Technical field】 [0001] The invention belongs to the field of semiconductor electronic chemicals, in particular to a continuous production method of a transition metal amine complex. 【Background technique】 [0002] Precursor is the main raw material of semiconductor thin film deposition process. It refers to a compound that is used in semiconductor manufacturing process, carries target elements, is in gaseous or volatile liquid state, has chemical and thermal stability, and has corresponding reactivity or physical properties. class of substances. In the semiconductor manufacturing process including thin film, lithography, interconnection, doping technology, etc., the precursor is mainly used in vapor deposition (including physical deposition PVD, chemical vapor deposition CVD and atomic vapor deposition ALD) to form semiconductor manufacturing requirements various thin film layers. In addition, the precursor can also be used for semiconductor epitaxial growth, etching, io...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/00C07F9/00B01J19/00B01D3/00B01D3/14
CPCB01D3/009B01D3/14B01J19/0046C07F7/00C07F7/003C07F9/005
Inventor 高雄张学奇李磊朱思坤李建恒
Owner 合肥安德科铭半导体科技有限公司
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