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Preparation method for lithium alkyl

A technology of alkyl lithium and lithium sand, which is applied in the field of preparation of alkyl lithium, can solve the problems of poor appearance and color, inability to recycle the mixture, turbid color, etc., and achieves the reduction of production cost and the improvement of product appearance and internal quality. Effect

Inactive Publication Date: 2007-11-28
CHINA PETROCHEMICAL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the existing alkyllithium production technology, white oil with a high initial boiling point is used as a dispersant for the dispersion of lithium metal. There are two problems: one is that the white oil contains some impurities, which makes it difficult to process or costly to process. It is very high and generally not treated, so that the prepared alkyllithium has a high impurity content and a poor appearance color, mainly manifested as turbidity and darker color; the second is that the mixture of white oil and organic hydrocarbon solvent (such as cyclohexane) cannot Recycling or recycling is costly and increases the production cost of alkyllithium

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Put 60 liters of refined cyclohexane with a water value less than 20 mg / kg in a clean pressure-resistant kettle, put in 14.5 kg of metal lithium rods under the protection of inert gas argon, then quickly seal the lithium injection port, and use argon to Replace the kettle three times, raise the temperature of the kettle to 230±15°C, and keep the temperature constant for 1 to 2 hours. After confirming that the metal lithium is completely melted, start the stirring motor, adjust the speed through the frequency converter, and investigate the dispersion of lithium sand under different speed conditions. After 10 minutes, the kettle temperature was lowered to 40° C. to obtain a cyclohexane suspension in which lithium metal was dispersed into lithium sand. Then, put the suspension into another reaction kettle, and after the materials are drained, rinse the dispersion kettle and pipeline with 40-60 liters of refined cyclohexane, and put them into the reaction kettle t...

Embodiment 2

[0024] Example 2: The preparation method is the same as in Example 1, the dispersant is adjusted from cyclohexane to a mixture of benzene, toluene, cyclohexane and n-hexane in different proportions, the stirring speed is fixed at 1500 rpm, and the experimental results are shown in Table 2.

[0025] Preface

[0026] It can be seen from Table 2 that using the mixture of benzene, toluene, cyclohexane and n-hexane in different proportions as the lithium metal dispersant can better disperse the metal lithium into lithium sand and synthesize the desired finished butyllithium.

Embodiment 3

[0027] Embodiment 3: The preparation method is the same as in Example 1, the stirring speed is fixed at 500rpm, and the reaction medium is adjusted from 1-chlorobutane to 1-chloroisobutane, 2-chloroisobutane, 1-bromobutane, 1-bromoisobutane, 2-bromoisobutane, the experimental results are shown in Table 3.

[0028] Preface

[0029] It can be seen from Table 3 that the alkyllithium with good quality can also be obtained by using different halogenated alkanes.

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Abstract

The present invention provides alkyl lithium producing process. The production process has the solvent for producing lithium polymer replacing white oil serving as the metal lithium dispersant. The production process can produce alkyl lithium with high purity, good appearance and color and high activity; and the dispersant may be recovered in a SBS solvent recovering system to lower the production cost of alkyl lithium.

Description

technical field [0001] The invention relates to a preparation method of alkyllithium. Background technique [0002] Alkyl lithium is an initiator for the production of lithium-based anionic polymers. Lithium-based anionic polymers are generally produced by solution polymerization, and the solvents are generally organic hydrocarbons such as cyclohexane, n-hexane, benzene, toluene, etc. In the existing preparation method of alkyllithium, firstly, under the protection of an inert gas (such as argon), block-shaped lithium metal is used as a dispersant with a white oil with an initial boiling point greater than 300°C, at a temperature greater than 190°C In the container, under the action of high-speed stirring, under the condition of ensuring the temperature and rotating speed, after a period of time (about 30 minutes), the metal lithium that has been melted into liquid state is dispersed into fine metal lithium sand; and then quickly lowered to normal temperature , normal press...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F1/02
Inventor 张红星陈韶文张家颂
Owner CHINA PETROCHEMICAL CORP
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