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Phosphine ligand as well as preparation method thereof, application thereof and method of extracting high-purity alkyl aluminum compound

A technology of phosphine ligands and alkylaluminum, which is applied in the field of purification of metal aluminum organic compounds, can solve the problems of difficult waste disposal and difficult regeneration of complexes, and achieve the effects of simple operation, suitable for large-scale production, and simple recycling process

Inactive Publication Date: 2018-05-08
JIANGXI JIAYIN PHOTOELECTRIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to provide a new type of phosphine ligand to overcome the disadvantages of difficult regeneration of complexes and difficult disposal of waste in the process of alkylaluminum purification in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1 prepares 1# phosphine ligand

[0027] The preparation method of 1# phosphine ligand, its step comprises,

[0028] (1) Dissolve 2000g of polystyrene with a crosslinking degree of 2% in 4000g of dichloromethane solvent, add 20g of aluminum chloride catalyst, then dropwise add 700g of liquid bromine halogenating agent, and react at room temperature for 24 hours;

[0029] (2) The product was washed with saturated sodium carbonate alkali and saturated saline successively, separated, then evaporated under reduced pressure to remove the solvent, washed with methanol, water and methanol in sequence, and dried in vacuum to obtain 2140g of light yellow brominated polystyrene solid;

[0030] (3) Dissolve 500g of chlorodiphenylphosphine in 4000g of THF, under nitrogen protection, add 500g n - Buli solution and 1500g of brominated polystyrene prepared in the previous step, under the protection of an oxygen barrier atmosphere, heated to reflux at 50°C for 4h, then stir...

Embodiment 2

[0033] Embodiment 2 prepares 2# phosphine ligand

[0034] The preparation method of 2# phosphine ligand, its step comprises,

[0035] (1) Dissolve 2000g of styrene-divinylbenzene copolymer with a crosslinking degree of 5% in 4000g of dichloromethane solvent, add 50g of aluminum acetate catalyst, and then dropwise add 1000g of elemental iodine halogenating agent, and react at room temperature for 24 hours;

[0036] (2) Wash the product successively with saturated sodium carbonate alkali and saturated brine, separate and then evaporate under reduced pressure to remove the solvent, then wash with methanol, water and methanol in sequence, and dry in vacuum to obtain 2070g of light yellow iodized polystyrene solid;

[0037] (3) Dissolve 500g of chlorinated diphenylphosphine in 4000g of THF, under nitrogen protection, add 60g of high-activity magnesium powder and 1500g of iodized polystyrene prepared in the previous step, heat and reflux at 70°C for 1h, and heat at 30°C Under stir...

Embodiment 3

[0040] Example 3 Preparation of 3# phosphine ligand

[0041] The preparation method of 3# phosphine ligand, its step comprises,

[0042] (1) Dissolve 2000g of polystyrene with a cross-linking degree of 8% in 4000g of dichloromethane solvent, add 100g of titanium acetate catalyst, then dropwise add 1000g of N-bromosuccinimide halogenating agent, and react at room temperature for 24 hours;

[0043] (2) The product was washed with saturated sodium carbonate alkali and saturated saline successively, separated, then evaporated under reduced pressure to remove the solvent, washed with methanol, water and methanol in sequence, and dried in vacuum to obtain 2070g of light yellow brominated polystyrene solid;

[0044] (3) Dissolve 500g of chlorinated diphenylphosphine in 4000g of THF, under nitrogen protection, add 60g of high-activity magnesium powder and 1500g of brominated polystyrene prepared in the previous step, heat and reflux at 40°C for 2h, then heat at 20°C Stir the reactio...

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Abstract

The invention discloses phosphine ligand loaded on a styrene polymer as well as a preparation method thereof, application thereof and a method of extracting a high-purity alkyl aluminum compound by utilizing the phosphine ligand. According to the technical scheme adopted by the invention, phosphine ligand loaded on polystyrene is good in stability, and purity of alkyl aluminum is not lower than amass fraction of 99.99995% after distribution and rectification; and the phosphine ligand loaded on polystyrene is simple in regeneration operation in a later stage. The method can remarkably increaseuse times of the ligand and can solve the defect that the ligand is not liable to regenerate. The method has the advantages of being simple in a ligand circulating process in purification of alkyl aluminum crude products such as trimethyl aluminum and triethyl aluminum, reducing cost, being suitable for large-scale production and the like.

Description

technical field [0001] The invention belongs to the technical field of purification of metal aluminum organic compounds, and in particular relates to a preparation method of a phosphine ligand for the purification of metal aluminum organic compounds. The invention also relates to a method for extracting high-purity alkylaluminum compounds from alkylaluminum crude products such as trimethylaluminum and triethylaluminum by using a phosphine ligand. Background technique [0002] As the precursor of aluminum nitride, high-purity alkylaluminum compounds are widely used in the growth of semiconductor thin film materials, and are the basic raw materials for the third generation of semiconductors. When the purity of high-purity alkylaluminum compounds is lower than 99.9999%, it will seriously restrict the improvement of the performance of the third-generation semiconductors. At present, the purification of alkyl aluminum crude products mainly uses amines and phosphine ligands for r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06C08F8/40C08F8/22C08F8/18C08F112/08
CPCC08F8/40C08F8/22C08F112/08C08F8/18
Inventor 廖维林邱曾烨谢贤清马玉峰陈飞彪雷志伟
Owner JIANGXI JIAYIN PHOTOELECTRIC MATERIAL
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