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A kind of synthetic method of lithium methylate

A synthesis method and technology of lithium methoxide, applied in the preparation of alcohol metal, organic chemistry and other directions, can solve the problems of easy agglomeration of solid lithium methoxide, excessive residual solvent, and intense reaction between lithium and methanol, so as to ensure efficient drying and residual solvent. The effect of less and higher production safety

Active Publication Date: 2017-10-31
SHANGYU HUALUN CHEM
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  • Summary
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  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the defects of the existing invention that the reaction between lithium and methanol is intense, the generated solid lithium methylate is easy to agglomerate, and the residual solvent is too high, the present invention provides a synthetic method for lithium methylate

Method used

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  • A kind of synthetic method of lithium methylate

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Embodiment 1

[0053] Step (1): Turn on the jacket to freeze and lower the temperature, replace the reactor with argon for 3 times, then put 300kg of methanol (water content 0.3wt%) from the elevated tank, and add 14kg of lithium sand in batches under the protection of argon, each time 0.5-1kg, the temperature in the reactor is controlled to be lower than 60°C during the feeding process; after the feeding is completed, stir the reaction until the lithium sand is completely dissolved.

[0054] Step (2): reflux for 0.5-1h, distill 150kg of methanol, and concentrate the remaining liquid into a ribbon stirrer (preheated to 50°C) for drying. The stirring speed of the ribbon stirrer is 25rpm. The vacuum degree in the ribbon stirrer is 0.01-0.02MPa. The temperature in the ribbon stirrer was raised from 50°C to 70°C at a rate of 10°C / 30min, and then to 80°C at a rate of 5°C / 30min. After the treatment was completed, 70 kg of white solid powder of lithium methoxide was obtained, without agglomeration...

Embodiment 2

[0058] Step (1): Turn on the jacket to freeze and lower the temperature, replace the reactor with argon for 3 times, then put 300kg of methanol (water content 0.3wt%) from the elevated tank, and add 14kg of lithium sand in batches under the protection of argon, each time 0.5-1kg, the temperature in the reactor is controlled to be lower than 60°C during the feeding process; after the feeding is completed, stir the reaction until the lithium sand is completely dissolved.

[0059] Step (2): Reflux for 0.5-1h, distill 200kg of methanol, concentrate the remaining liquid and put it into a ribbon stirrer (preheated to 50°C) for drying, and the stirring speed of the ribbon stirrer is 15rpm. The vacuum degree in the ribbon stirrer is 0.07-0.09MPa. The temperature in the ribbon stirrer was raised from 50°C to 70°C at a rate of 15°C / 30min, and then to 80°C at a rate of 10°C / 30min. After the treatment was completed, 68kg of white solid powder of lithium methoxide was obtained, without ag...

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Abstract

The invention discloses a synthetic method of lithium methoxide. The method comprises the following steps: Step (1): in an inert gas atmosphere, pouring lithium into methanol, stirring and reacting; and Step (2): after the reaction, concentrating and recycling methanol, and transferring a concentrated residual liquid into a helical ribbon agitator and drying to prepare lithium methoxide, wherein pressure in the helical ribbon agitator is 0.01-0.09 MPa, and temperature in the helical ribbon agitator is 70-80 DEG C. The method has advantages of high production safety, simple operation and high production efficiency. High-quality recycling of methanol can be achieved. The prepared lithium methoxide dry product is not easy for caking, and there is few residual solvent.

Description

technical field [0001] The invention relates to the field of synthesis of chemical raw materials, in particular to a method for synthesizing lithium methoxide. Background technique [0002] Lithium methoxide is an important chemical product with strong alkalinity and high activity, and can be used as a pharmaceutical intermediate for the production of vitamin A, vitamin B, sulfadiazine, etc. [0003] Lithium methoxide products mainly have two forms: solid and liquid, and solid lithium methoxide can be prepared from liquid lithium methoxide. The production methods of lithium methoxide mainly include metal lithium method and alkali method. The metal lithium method refers to the direct reaction of metal lithium with methanol, and the obtained liquid lithium methoxide product has a higher purity. The alkaline method refers to dissolving lithium hydroxide in methanol and reacting with methanol to generate lithium methoxide, which is a reversible reaction. The alkalinity of lit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/70C07C31/30
CPCC07C29/70C07C31/30
Inventor 李典正赵大文黄光亮
Owner SHANGYU HUALUN CHEM
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