Production process of lithium alcoholate

A production process, lithium alkoxide technology, applied in metal alkoxide preparation, organic chemistry, etc., can solve problems such as easy to catch fire, difficult to achieve industrialized production, explosion, etc.

Inactive Publication Date: 2012-06-06
曹衍军
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the reaction between alcohol and metal lithium is an instantaneous reaction, the reaction is generally completed in 1-15 minutes, and a large amount of hydrogen and heat are released during the reaction, which is easy to catch fire and explode, which is very dangerous, so that the product is not easy to achieve industrial production.

Method used

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  • Production process of lithium alcoholate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] figure 1 It is a schematic diagram of the structure of the reaction device, which is intended to facilitate the description of the process of the present invention. Add 15kg lithium metal and 1000kg ethanol measured in the 2000L liter reaction tank. Before starting the dropwise addition, first turn on the ice water to cool down, the temperature drops to -20~-26°C, start to drop the measured alcohol (usually within 7 hours), and start dropping slowly through the metering tank , when it is added dropwise to 200L, close the ice water cooling valve, so that the temperature begins to rise slowly, and the temperature is controlled at 60-80 degrees (preferably 65-70 degrees C). During the reaction process, all 4 exhaust valves must be opened. The cooling valves of the stage condensers are fully opened. The gas components are condensed through the condenser, and the alcohol in it is condensed and refluxed through the collection tank to the reaction tank. After normal operati...

Embodiment 2

[0021] Different from Example 1, 15kg lithium metal was added to the reaction tank, and 900kg methanol was added to the alcohol metering tank. The mass content of lithium methoxide in the liquid lithium methoxide is 29%.

[0022] In the rake dryer, the vacuum degree is controlled to be 0.01-0.1Mpa, the temperature is 120°C, and the drying time is 14 hours. Lithium methoxide was obtained as a white crystalline powder solid. After testing, the mass content of lithium methoxide is 98.9%, the free alcohol is less than 0.5%, and the moisture content is zero.

Embodiment 3

[0024] Different from Example 1, 15kg lithium metal was added into the reaction tank, and 950kg n-butanol was added into the alcohol metering tank. The mass content of lithium n-butoxide in the liquid lithium n-butoxide is 28.5%.

[0025] In the rake dryer, the vacuum degree is controlled to be 0.01-0.1Mpa, the temperature is 100°C, and the drying time is 12 hours. Lithium n-butoxide was obtained as a white crystalline powder solid. After testing, the mass content of lithium n-butoxide is 98.8%, the free alcohol is less than 0.5%, and the moisture content is zero.

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Abstract

The invention relates to a technique for producing lithium alkoxide, which is characterized by comprising the following steps: adding lithium metal into a reactor, dripping ethanol slowly at a temperature of between 20 and 30 DEG C, providing ice water outside the reactor to reduce reaction temperature to between 60 and 80 DEG C in a reaction process, and after finishing dripping the ethanol, keeping the temperature to make full reaction to obtain liquid lithium alkoxide; and then conveying the liquid lithium alkoxide to a closed drier, condensing and drying the liquid lithium alkoxide to obtain solid lithium alkoxide. Reaction of the liquid lithium alkoxide is finished in the reactor firstly, and then materials are conveyed to the drier to be condensed and dried so as to obtain the solidlithium alkoxide. The technique is suitable for industrialized production of lithium methoxide, lithium ethoxide, lithium n-butylate, lithium tert-butylate, lithium isopropoxide or other lithium alkoxides; and the obtained product has high purity.

Description

technical field [0001] The invention belongs to the production technology of chemical products, in particular to a production process of lithium alkoxide. Background technique [0002] Lithium methoxide, lithium ethoxide, lithium n-butoxide, lithium tert-butoxide, lithium isopropoxide, used in medicine, chemical industry, organic synthesis, phase transfer catalyst, oxyacid inhibitor (used), basically not seen in the market High-purity (content: ≧98%) solid product. Since the reaction between alcohol and metal lithium is an instantaneous reaction, generally the reaction is completed in 1-15 minutes, and a large amount of hydrogen and heat are released during the reaction, which is easy to catch fire and explode, which is very dangerous, so that the product is not easy to achieve industrial production. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a production process of lithium alkoxide, industrialized producti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/30C07C29/70
Inventor 曹衍军
Owner 曹衍军
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