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Method for industrially producing sec-butyl lithium

A technology of sec-butyllithium and lithium particles, which is applied in the field of industrialized production of sec-butyllithium, can solve the problems of reduced quality and yield of sec-butyllithium, flammability and explosion of metal lithium, and easy residual white oil in products, and achieves The effect of shortening the production cycle, no white oil residue, and suppressing side reactions

Pending Publication Date: 2021-12-03
GANFENG LITHIUM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The preparation of lithium sand requires high temperature and rapid cooling, which requires high equipment and cumbersome operation; white oil is easy to remain in the product, which affects product quality
Moreover, it is difficult to achieve rapid cooling in large-scale production, and metal lithium is easy to agglomerate. If cold water or frozen brine is used to cool down, because metal lithium is flammable and explosive when it meets water, there is a great safety hazard.
At the same time, due to the reaction temperature and amplification effect, the production of sec-butyllithium is prone to Wurtz side reaction, which leads to the reduction of the quality and yield of sec-butyllithium

Method used

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  • Method for industrially producing sec-butyl lithium
  • Method for industrially producing sec-butyl lithium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Dry clean 2000L reactor charge argon gas for 3 times, add 1000L cyclohexane solvent. 60kg of lithium particles are putter into the feeder, and the air is placed 2 times, and the lithium particles are placed in the reactor. The reactor was stirred, and 225 l 2-chlorobutane was added dropwise to the argon atmosphere of 0 to 0.05 MPa, and the completion of 2 h was added. The reaction is released, the temperature is raised to 30 ° C, and the reactor jacket and the reflow condenser are cooled to cool the oil, and the temperature control temperature is 30 to 40 ° C. The dropping end, 30 to 40 ° C insulation reaction for 3 h, and the reaction was pressed into the intermediate tank after the reaction was completed. The material of the intermediate tank was pressed into the filter with argon to remove the lithium chloride solid, 100 L cyclohexane washing the filter residue, resulting in a cyclohexane solution of 1200L pale yellow transparent sec-butyllithium, concentration: 14.0%, a...

Embodiment 2

[0042]700L cyclohexane solvent was added to the 2000L reactor. 32kg lithium particles are puttering the feeder, and the air is discharged from the gas. The lithium particles are placed in the reactor. The reactor was stirred, and 225 l 2-chlorobutane was added dropwise to the argon atmosphere of 0 to 0.05 MPa, and the completion of about 3 h hetero. The reaction is released, the temperature is raised to 30 ° C, and the reactor jacket and the reflow condenser are cooled to cool the oil, and the temperature control temperature is 30 to 40 ° C. The dropping end, the reaction was held at 30 to 40 ° C for 2 h, and after the reaction was completed, the reaction mixture was pressed into the intermediate can. Pressure of the bottle in the intermediate tank to remove the silicon chloride solid, 100L cyclohexane washing filter residue with argon, to give 900L pale-yellow transparent sec-butyristyl cyclohexane solution, concentration: 18.5%, activity: 98.7% , Oxine: 0.16%, covalent chlorine:...

Embodiment 3

[0044] 800L n-hexane solvent was added to the 2000L reactor. 30 kg of lithium particles are puttering the feeder, and the air is discharged from the air 3 times, and then the lithium particles are placed in the reaction kettle. The reactor was stirred, and 225 l 2-chlorobutane was added dropwise to the argon atmosphere of 0 to 0.05 MPa, and the completion of 2 h was added. The reaction is released, the temperature is raised to 30 ° C, and the reactor jacket and the reflow condenser are cooled to cool the oil, and the temperature control temperature is 30 to 40 ° C. End of dropwise, at 3 0 to 40 ° C for 2 h, and after the reaction was completed, the reaction mixture was pressed into the intermediate can. The material of the intermediate tank was pressed into the filter with argon to remove the lithium chloride solid, 100 L n-hexane washing filter residue, obtained 1000 L of colorless and transparent sec-butyristyl, concentration of 18.6%, activity: 98.4%, butter : 0.20%, covalent c...

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Abstract

The invention provides a method for industrially producing sec-butyl lithium. The method for industrially producing sec-butyllithium comprises the following steps: (1) replacing air in a reaction kettle with argon, and adding a solvent; (2) putting lithium particles into a feeder, replacing air with argon, and putting all the lithium particles into the reaction kettle; (3) starting stirring, dropwise adding 2-chlorobutane through a metering pump to react with the metal lithium, and controlling the reaction temperature through the reaction kettle jacket and the feeding speed of the 2-chlorobutane; (4) keeping the temperature for 2-4 hours, pressing the reaction liquid into an intermediate tank by using argon, and leaving excessive metal lithium in the reaction kettle; and (5) pressing the material liquid in the intermediate tank into a filter by using argon to remove the lithium chloride solid, thereby obtaining colorless to faint yellow transparent clear liquid, namely the sec-butyllithium solution. According to the method, excessive metal lithium particles and 2-chlorobutane react in a solvent at a certain temperature to produce sec-butyllithium, so that side reaction is effectively avoided, and the yield is increased.

Description

Technical field [0001] The present invention relates to the field of chemical processes and petrochemical technology, and more particularly to a method of industrially producing sec-butyllithium. Background technique [0002] Butyzide is the most important organic lithium compound, and the industrial production has positive butyllithium, sec ... lithium t-butyl lithium. Butyl lithium has good reaction properties, mainly used in polymer industries, is an excellent initiator and catalyst of synthetic rubber. Butyl lithium is also widely used for organic synthesis, has the advantages of complete reaction, less by-products, easy separation of products, and is used to prepare many valuable organic compounds and drugs. [0003] The secondary-buthake is relatively active, and the initiator is used as the initiator to the polymerization monomer, so when using sec-butyl lithium to polymerization initiator, there is no need to add a polar solvent such as tetrahydrofuran, simplifying the so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C1/26C07C9/12
CPCC07C1/26C07C9/12
Inventor 李良彬文本华袁晶张永飞王强廖志刚肖涛胡婷婷胡萍
Owner GANFENG LITHIUM CO LTD
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