Method for producing alkyl lithium

A production method and technology of alkyl lithium, applied in the direction of lithium organic compounds, etc., can solve the problems of long reaction period, uneconomical process, low production capacity, etc., and achieve the effects of stable reaction, improved production capacity, and reduced consumption

Inactive Publication Date: 2003-09-24
CHINA PETROCHEMICAL CORP +1
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Problems solved by technology

Due to the constraints of exothermic reaction and side reactions, the reaction temperature is generally controlled at 35°C to 55°C, the reaction cycle is long, and the production capacity is low. In order to prevent the residual chlorinated alka

Method used

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  • Method for producing alkyl lithium

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comparative example 1

[0029] Comparative Example 1: Put 14.33kg of prepared lithium sand, 70L of dispersion medium white oil, and 600L of cyclohexane for washing the dispersion tank into the synthesis tank (the specific steps are the same as in Example 1). Add 93.8L of n-butyl chloride dropwise in the kettle (about 14% excess lithium than the theoretical value), control the reaction temperature to be 35-55°C, react and filter the rest according to Example 1 to obtain 430L of butyl chloride with a concentration of 1.10M light yellow and transparent Lithium solution with active C-Li content of 98.3%, residual BuCl content of 1.09%, Cl - The content is 275ppm. Add 800L cyclohexane into the settling tank, and after settling for 4 hours, pump the supernatant and filter to obtain a 0.26M concentration of butyllithium solution. The combined yield of the two is 76.6% based on chlorobutane. The lithium slag in the settling tank is discharged into the hydrolysis tank and then deactivated by hydrolysis.

comparative example 2

[0030] Comparative Example 2: 14.07kg of prepared lithium sand and 70L dispersion medium white oil, 600L industrial cyclohexane (composition is the same as Example 2) for washing the dispersion tank are put into the synthesis tank (the specific steps are the same as Example 1). Add 88.2L of n-butyl chloride dropwise into the kettle (about 19% excess lithium than theoretical value), control the reaction temperature to 35-55°C, react and filter the rest according to Example 1 to obtain 430L of butyl chloride with a concentration of 1.08M light yellow and transparent Lithium solution with active C-Li content of 98.7%, residual BuCl content of 0.89%, Cl - The content is 313ppm. Add 800L hexanaphthene in the settling tank, after the clear liquid is drawn out, the two are combined and the yield is 79.8% in terms of chlorobutane. The lithium slag in the settling tank is discharged into the hydrolysis tank and then deactivated by hydrolysis.

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Abstract

The present invention provides a production method of lithium alkylide, it includes the following steps: using white oil whose water value is 100 mg/kg-300 mg/kg as dispersing agent to disperser metal lithium ingot into lithium sand whose grain size is 20-400 micrometers under the closed condition; transferring the lithium sand into synthesis reactor, adding a certain quantity of hydrocarbon solvent and regulating its volume, adopting drop-additive mode to add a proper quantity of chlorohydrocarbon, controlling reaction temp. in 70-85 deg.C, controlling reaction time to make chlorohydrocarbonbe completely converted, after synthesis reaction, pressing the obtained material into settling tank, slanding still, taking upper layer of lithium alkylide, filtering and removing solid impurity so as to obtian the invented lithium alkylide solution.

Description

technical field [0001] The invention relates to a production method of alkyllithium. technical background [0002] Alkyllithium is mainly used as an initiator of anionic polymerization, and its demand is growing rapidly at present. In the prior art, there are many reports about the synthesis and preparation of alkyllithium, such as U.S.P. 5,332,533 (1994), 5,340,507 (1994), 5,567,474 (1996), 5,776,396 (1998) and so on in the United States patents in the past ten years. The synthesis of alkyllithium adopts the route of reacting chlorinated alkanes and metal lithium sand in hydrocarbon solvents. Due to the constraints of exothermic reaction and side reactions, the reaction temperature is generally controlled at 35°C to 55°C, the reaction cycle is long, and the production capacity is low. In order to prevent the residual chlorinated alkanes in the product from affecting the polymerization process, the relatively expensive The excess of lithium is 12%-25%, to ensure the comple...

Claims

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Application Information

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IPC IPC(8): C07F1/02
Inventor 曹志昂宁朝晖朱铁辉
Owner CHINA PETROCHEMICAL CORP
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