Method for preparing lithium alkoxide

A technology of lithium alkoxide and lithium tert-butoxide, which is applied in the preparation of metal alkoxides, etc., can solve the problems of reduced yield, small atomic weight of metal lithium, and hidden dangers to the life safety of environmental operators.

Inactive Publication Date: 2011-04-27
SHANGHAI CHINA LITHIUM INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] ②. The reaction between metal lithium and alcohol is an exothermic reaction. When alcohol is added to metal lithium, as the reaction proceeds, the heat released by the reaction can violently volatilize the alcohol with a lower boiling point. Due to the by-product hydrogen and the volatilized alcohol Both are flammable and explosive. If lithium methoxide is produced, the volatilized methanol is very toxic and poses a great hidden danger to the environment and the life safety of operators.
Even if the ice water circulation cooling method is adopted outside the reactor, it may cause harm due to local overheating in actual production
[0008] ③. The atomic weight of metal lithium is small, only 6.941. Every kilogram of lithium consumed can generate 806L of hydrogen. According to the lower explosion limit of hydrogen at 10%, 806L of hydrogen can detonate 8060L of air, which has a huge potential for safe production risk
[0009] ④. The reaction between lithium metal and alcohol can release a lot of heat, and the reaction between lithium metal and alcohol accelerates rapidly with the increase of temperature. If the temperature cannot be controlled below the boiling point of alcohol, explosive reaction will easily occur and Groove phenomenon, resulting in waste of raw materials and reduced productivity

Method used

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  • Method for preparing lithium alkoxide
  • Method for preparing lithium alkoxide
  • Method for preparing lithium alkoxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 2000g of tetrahydrofuran into a 20L titanium bucket, and gradually add 800.5g of lithium tert-butoxide under stirring until the solution is completely clear. Under stirring, a total of 352.4 g of anhydrous methanol was added every half hour for 5 times. After the anhydrous methanol was completely added, the stirring was continued for 3 hours, and the material was transferred to a centrifuge under argon protection for separation. The separated solid was transferred to a vacuum oven for 8 hours at 120°C, and the vacuum degree was -0.074MPa. After crushing, a white powdery solid was obtained, weighing 375.2g. The mass analysis was carried out using (Shanghai enterprise standard), and the results were as follows:

[0021]

Embodiment 2

[0023] Weigh 1000g of tetrahydrofuran into a 20L titanium bucket, and gradually add 400.3g of lithium tert-butoxide under stirring until the solution is completely clear. Under stirring, a total of 253 g of absolute ethanol was added every half hour for 5 times. After complete addition of absolute ethanol, the stirring was continued for 2 hours, and then the material was transferred to a centrifuge under the protection of argon for separation. The separated solid was transferred to a vacuum oven at 120°C for 6 hours and the vacuum degree was -0.074MPa. After crushing, a light yellow powdery solid was obtained, weighing 255.5g. The mass analysis results were as follows:

[0024]

Embodiment 3

[0026] Weigh 2000g of tetrahydrofuran into a 20L titanium bucket, and gradually add 300.5g of lithium isopropoxide under stirring until the solution is completely clear. Under stirring, a total of 253 g of anhydrous ethylene glycol was added every half hour in 5 times. After the anhydrous ethylene glycol was completely added, the stirring was continued for 3 hours, and the material was transferred to a centrifuge under the protection of argon for separation. The separated solid was transferred to a vacuum oven at 150°C and dried for 12 hours with a vacuum degree of -0.074MPa. After crushing, a light yellow powdery solid was obtained, weighing 184.4g. The mass analysis results were as follows:

[0027]

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Abstract

The invention discloses a method for preparing lithium alkoxide, which comprises the following steps of: dissolving lithium tert-butoxide or lithium isopropoxide in an organic solvent, adding methanol, ethanol or ethylene glycol for reacting, collecting a solid matter in a reaction product, and drying to obtain the lithium alkoxide. In the method, the lithium tert-butoxide or lithium isopropoxide with strong alkalinity is taken as a raw material, so that metallic lithium is prevented from being subjected to side reaction with water, oxygen and nitrogen in air and causing low quality of a product, and the purity of the product is ensured while the yield is not reduced; and the lithium tert-butoxide or lithium isopropoxide is dissolved in tetrahydrofuran, the methanol (ethanol or ethylene glycol and the like) is added at normal temperature, and displacement reaction is completely performed with full stirring, so that reaction at normal temperature and normal pressure is performed, and potential safety hazard is reduced.

Description

technical field [0001] The invention relates to a preparation method of lithium alkoxide (ROLi). Wherein, R represents hydrocarbon groups such as CH3, CH3CH2. Background technique [0002] At present, the production method of lithium alkoxide is generally produced by the reaction of metal lithium and corresponding alcohol. Since lithium is an active metal, lithium can not only react with metal, but also react with oxygen, nitrogen and generated hydrogen in the air. , thereby reducing the quality of lithium alkoxide products. [0003] Chinese patent CN 101412659 discloses a kind of preparation method of lithium alkoxide, and this method comprises the following steps: [0004] Add metal lithium into the reactor, slowly add alcohol dropwise at 20-30°C, cool down the reactor with ice water outside the reactor during the reaction, keep the temperature of the reactor at 60-80°C, after adding the alcohol dropwise, keep warm until the reaction Completely, liquid lithium alkoxide ...

Claims

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Application Information

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IPC IPC(8): C07C29/70C07C31/30
Inventor 魏述彬米泽华
Owner SHANGHAI CHINA LITHIUM INDAL
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