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Preparation method of silyl ether alkyl lithium

A technology for silyl ether alkyl lithium and silyl ether substitution, which is applied in the field of polymerization initiator synthesis, can solve the problems of high alkyl lithium impurity content, poor appearance and color, and high processing cost, and achieves high yield, fast reaction process, and high synthesis rate. fully responsive effect

Active Publication Date: 2021-12-07
JIANGSU CHANGJILI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the lithium sand prepared by this method often contains more white oil
White oil contains some impurities, which are difficult or costly to deal with. Generally, no treatment is carried out, so that the prepared alkyllithium has high impurity content, poor appearance and color, and its application is limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of 3-(tert-butyl-dimethylsiloxy)-1-propyl lithium (molecular formula C 9 H 21 The preparation method of LiOSi, CAS No. 97057-70-0), comprises the following steps:

[0031] S1, lithium metal preparation

[0032] (1) Weigh Ni30Mn70 alloy powder and disperse it in a hot 1mol / L ammonium sulfate solution, keep it for 10h for etching, filter out, and disperse again in a mixed solution of 1g / 50mL of polyvinylpyrrolidone and glacial acetic acid After being dispersed for a few seconds, it was filtered out. The precipitate was washed with deionized water and anhydrous ethanol in turn. After vacuum drying, the obtained metal powder was placed in an alumina ceramic boat and moved into the middle of the tube furnace. The tube furnace was closed, and the tube was removed. Air, filled with argon, heated to 950°C at a rate of 5°C / min in an argon atmosphere, kept for 12 minutes, and then heated to 25:1 in Ar-H 2 The annealing treatment is carried out in a mixed atmosphere, and...

Embodiment 2

[0043] A kind of 3-(tert-butyl-dimethylsilyloxy)-1-propyllithium (molecular formula C 9 H 21 The preparation method of LiOSi, CAS No. 97057-70-0), comprises the following steps:

[0044] S1. Preparation of lithium metal

[0045] (1) Weigh Ni30Mn70 alloy powder and disperse it in hot 1mol / L ammonium sulfate solution, keep it standing for 10h for etching, filter it out, and disperse it again in a mixed solution of 1g / 50mL polyvinylpyrrolidone and glacial acetic acid , disperse for a few seconds and filter out, the precipitate is washed with deionized water and absolute ethanol in turn, after vacuum drying, the obtained metal powder is placed in an alumina ceramic boat and moved into the middle of the tube furnace, the tube furnace is closed, and the tube is pumped out. Air, filled with argon, heated to 950°C at a rate of 5°C / min in an argon atmosphere, kept for 12 minutes, and then heated in Ar-H with a volume ratio of 25:1 2 Annealing treatment is carried out in a mixed atmo...

Embodiment 3

[0057] A 1L four-necked round-bottom flask is used as the reaction kettle. The reaction kettle is placed in a magnetic stirring heating mantle, a mercury thermometer is inserted in the left port, and a reflux condenser (cooled with tap water) is inserted in the middle port. Seal, insert a 250mL dropping funnel into the right opening, use magnets and magnetic stirring; wash and dry flasks, dropping funnels, beakers for weighing, glass bottles for sampling, syringes and other instruments;

[0058] Put 17-23g of lithium sand (excess) and 400-450mL of mixed solvent of cyclopentane and n-hexane into the round bottom flask in sequence in the argon-sealed glove box, keep the reaction temperature at 51-70°C, add 140-150 g 3-(tert-butyl-dimethylsilyloxy)-1-chloropropane (85-90%).

[0059] After the reaction system is connected, the atmosphere is replaced with argon. The flask is first placed in a magnetic stirring heating mantle and heated to 50-60°C, then the heating is stopped but th...

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PUM

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Abstract

The invention provides a preparation method of silyl ether alkyl lithium, and belongs to the technical field of polymerization initiator synthesis. Nitrogen-doped few-layer graphene with a three-dimensional structure is prepared through a vapor deposition method by taking a porous nano nickel material with catalytic activity as a substrate and taking pyridine as a carbon source and a nitrogen source, the interlayer spacing is increased through layer expansion treatment, depositing is conducted on a carbon fiber paper substrate to obtain a film carrier with a high specific surface layer substructure, molten lithium loading is conducted, reacting with halogenated silyl ether in a non-polar solvent is conducted, and a reaction product is filtered to obtain silyl ether alkyl lithium. By preparing the film carrier and uniformly loading the molten lithium metal on the film carrier, the film carrier has good dispersity, so that the synthesis reaction is sufficient, and the film carrier has the characteristics of high yield, low impurity content and easiness in separation.

Description

technical field [0001] The invention relates to the technical field of synthesis of polymerization initiators, in particular to a preparation method of silyl ether alkyl lithium. Background technique [0002] Alkyllithium is used as an initiator for the production of lithium-based anionic polymers, which is a very important class of organic alkali metal compounds. Its unique properties are both covalent and ionic, which make it both soluble in polar It can also be dissolved in non-polar solvents. [0003] The preparation of lithium-based initiators for synthesizing hydroxyl-terminated polybutadiene liquid polymers is mostly prepared by reacting monohalogenated or dihalogenated organic compounds with metallic lithium. Monohalogenated organic compounds can synthesize initiators with protective groups, and dihalogenated organic compounds can synthesize organic dilithium initiators. Among them, alkyl lithiums with silyl ethers to protect hydroxyl groups are widely used. Silyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/1892
Inventor 周卫强储鹏史先桥程力伟蒋国群朱爱军曹沛栋谢云良董涛戴玉明吴晓明沈伟忠周月松钱东
Owner JIANGSU CHANGJILI NEW ENERGY TECH CO LTD