A kind of preparation method of n-hexyllithium

A technology of n-hexyllithium and n-hexane, applied in the field of organometallic compound synthesis, can solve the problems of affecting application, reducing the purity of n-hexyllithium, reducing the yield of n-hexyllithium, etc., so as to improve the conversion rate and reduce the influence of amplification benefits. , the effect of reducing side effects

Active Publication Date: 2015-09-30
SHANGYU HUALUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This will not only reduce the yield of n-hexyllithium, but also reduce the purity of n-hexyllithium, affecting subsequent applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Under the protection of argon, put 250L of white oil and 21kg of lithium flakes into the 500L reactor, slowly stir and raise the temperature to 180℃, after stirring for 0.5h, increase the stirring speed of the reactor to 130 rpm, stir at 180℃ for 1h, turn on and cool to At room temperature, press filter to remove the white oil, transfer the n-hexane to the washing kettle, and rinse 2-3 times to obtain a relatively uniform lithium metal form (lithium sand).

[0030] Under the protection of argon, add 20kg of n-hexane to the 500L reactor, and while keeping the argon inside the reactor, put in 7kg of lithium sand and 58gL-proline, cover and maintain positive pressure, open the vent valve to maintain pressure balance , Add 80kg n-hexane to the reactor, slowly turn on the stirring; increase the temperature to 55℃, open the balance pipe valve, add 60kg chloro-n-hexane dropwise, control the temperature of the reactor at about 53-55℃; control the speed of the reactor at 130 rpm / M...

Embodiment 2

[0040] Under the protection of argon, put 250L of white oil and 21kg of lithium flakes into the 500L reactor, slowly stir and raise the temperature to 180℃, after stirring for 0.5h, increase the stirring speed of the reactor to 130 rpm, stir at 180℃ for 1h, turn on and cool to At room temperature, press filter to remove the white oil, transfer the n-hexane to the washing kettle, and rinse 2-3 times to obtain a relatively uniform lithium metal form (lithium sand).

[0041] Under the protection of argon, add 20kg of n-hexane into the 500L reactor, and while keeping the argon in the reactor, put in 7kg of lithium sand, cover and maintain the positive pressure, open the vent valve to maintain pressure balance, and add 80kg to the reactor Start the stirring slowly with n-hexane; increase the temperature to 55°C, open the balance pipe valve, add 60kg chloro-n-hexane dropwise, and control the temperature of the reactor to 53-55°C; control the speed of the reactor to 130 rpm. After dripp...

Embodiment 3

[0043] Under the protection of argon, put 250L of white oil and 21kg of lithium flakes into the 500L reactor, slowly stir and raise the temperature to 180℃, after stirring for 0.5h, increase the stirring speed of the reactor to 130 rpm, stir at 180℃ for 1h, turn on and cool to At room temperature, press filter to remove the white oil, transfer the n-hexane to the washing kettle, and rinse 2-3 times to obtain a relatively uniform lithium metal form (lithium sand).

[0044] Under the protection of argon, add 20kg of n-hexane into the 500L reactor, and while keeping the argon in the reactor, put in 7kg of lithium sand, cover and maintain positive pressure, open the vent valve to keep the pressure balanced, and add 80kg to the reactor N-hexane, slowly turn on the stirring; the temperature is raised to slight reflux, the balance pipe valve is opened, 60kg of chloro-n-hexane is added dropwise, the temperature of the reactor is controlled to 65-66°C; the speed of the reactor is controlle...

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PUM

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Abstract

The invention discloses a preparation method of n-hexyl lithium, which comprises the following steps of (1), placing a lithium sheet in an inert solvent under protection of inert gas, heating and stirring to allow the lithium sheet to be dispersed, cooling, removing the inert solvent, obtaining a lithium dispersoid, and (2), adding a liquid hydrocarbon solvent to the lithium dispersoid obtained in Step (1) under the protection of the inert gas, adding L-proline with a catalytic amount, stirring, heating, flowing back, dropwise adding chlorohexane, reacting completely, and obtaining a solution of n-hexyl lithium through treatment. According to the preparation method, after catalyst L-proline is coordinated with lithium, a yield of a product is increased, and a side reaction is reduced.

Description

Technical field [0001] The invention belongs to the field of organometallic compound synthesis, and specifically relates to a preparation method of n-hexyl lithium. Background technique [0002] Organolithium compounds are an important class of organometallic compounds. They were prepared by K. Ziegler by reacting organic halides with metallic lithium as early as 1929, and they were subsequently used in organic synthesis. Currently, organolithium compounds, as an important synthetic reagent, play an important role in basic theoretical research and industrial synthesis. [0003] The chemical properties of organolithium compounds are similar to alkylmagnesium halides, but they are more active and can react with metal halides, carbonyl-containing substances, halogenated hydrocarbons and compounds containing active hydrogen. N-hexyl lithium is an important organolithium compound, which can be used to remove many active hydrogens of hydrogen carbonate, and the more important applicatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F1/02
Inventor 李典正张江林何光明
Owner SHANGYU HUALUN CHEM
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