Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of silicon ether alkyllithium

A technology of silicon ether alkyllithium and silicon ether substitute, which is applied in the field of synthesis of polymerization initiators, can solve the problems of high impurity content of alkyllithium, high processing cost, poor appearance and color, etc., achieve high yield, sufficient synthesis reaction, The effect of fast reaction process

Active Publication Date: 2022-03-25
JIANGSU CHANGJILI NEW ENERGY TECH CO LTD
View PDF4 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 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:

[0031] S1. Preparation of lithium metal

[0032] (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 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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a preparation method of silyl ether alkyl lithium, which belongs to the technical field of synthesis of polymerization initiators. Through a vapor deposition method, a porous nano-nickel material with catalytic activity itself is used as a substrate, and pyridine is used as a carbon source and a nitrogen source to prepare Nitrogen-doped few-layer graphene with a three-dimensional structure is obtained, and then the interlayer spacing is increased by layer expansion treatment, and it is deposited on a carbon fiber paper substrate to obtain a film carrier with a high specific surface hierarchical structure. The ether is reacted in a non-polar solvent, and the reaction product is filtered to obtain the silyl ether alkyl lithium; by preparing the film carrier, the present invention uniformly supports the molten lithium metal on the film carrier, and has good dispersibility, so that the The synthesis reaction is sufficient, and it has the characteristics of high yield, low impurity and easy separation.

Description

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

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(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