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Manufacturing method of granular sodium tert-pentoxide

A technology of sodium tert-amylate and its manufacturing method, which is applied in the fields of metal alcohol preparation, organic chemistry, etc., can solve the problems of production environment safety threats, health damage of operators, dust flammability and explosion, etc., to reduce production environment safety risks, The raw materials are convenient and easy to obtain, and the production process is simple

Active Publication Date: 2011-04-06
GENCHEM & GENPHARM CHANGZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commonly used sodium tert-amylate product is a powdery substance. Due to the strong corrosiveness and strong hygroscopicity of this product, the dust generated during the operation and feeding will cause great damage to the health of the operators. In addition, the characteristics of the dust are flammable and explosive. Threat to the security of the production environment
In order to prevent human injury and safety problems caused by sodium tert-amylate powder, it is often used as a toluene solution, but the need to remove the solvent during use still brings a lot of inconvenience to users

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In the dry 2000ml four-necked reaction flask, equipped with mechanical stirring, thermometer, feeding port, and reflux condenser, add tert-amyl alcohol 747g (8.49mol), mix trimethylbenzene 523g, metallic sodium wire 65g (2.83mol), Under protection, the reflux reaction was carried out for 12 hours, and the sodium metal disappeared completely. The distillation device was used instead, and the excess tert-amyl alcohol was evaporated under normal pressure, and the residual mixed trimethylbenzene was evaporated under vacuum -0.095MPa, and the stirring speed was maintained at 20 rpm. When the mixed trimethylbenzenes are evaporated, uniform sodium tert-amylate particles of about 0.6 mm are produced in the bottle, and low-temperature nitrogen (-20°C) is blown into the bottom valve of the reaction kettle to cool down to below 40°C, and the desired granular tert-amyl alcohol is obtained. sodium alkoxide.

Embodiment 2

[0016] In a dry 2000L reactor, add 747kg (8.49kmol) of tert-amyl alcohol, mix 523kg of trimethylbenzene, press in 65kg (2.83kmol) of sodium metal under the protection of nitrogen, close the reactor after feeding, and reflux for 14 hours under the protection of nitrogen , steam the excess tert-amyl alcohol at normal pressure, steam the remaining mixed trimethylbenzenes under vacuum-0.098MPa, keep the speed of rotation at 20 rpm, and when the mixed trimethylbenzenes are evaporated, the reactor jacket is introduced into the cooling water for cooling. Simultaneously, nitrogen gas (-20°C) was blown into the gap of the bottom valve of the tank several times, and after cooling to 38°C, sodium tert-amyloxide with a particle size of 0.6mm was obtained.

Embodiment 3

[0018] In a dry 2000L reactor, add 1046kg (11.89kmol) of tert-amyl alcohol, mix 732kg of trimethylbenzene, press 65kg (2.83kmol) of metal sodium wire under the protection of nitrogen, close the reactor after feeding, and reflux reaction under the protection of nitrogen for 14 After 1 hour, excess tert-amyl alcohol was steamed under normal pressure, and residual mixed trimethylbenzenes were steamed under vacuum-0.098MPa, and the stirring rate was kept at 20 rpm. After the mixed trimethylbenzenes were evaporated, the reactor jacket was introduced into cooling water to cool , At the same time, nitrogen gas (-20°C) was blown into the gap of the bottom valve of the tank several times, and after cooling to 38°C, sodium tert-amyloxide with a particle size of 0.6mm was obtained.

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Abstract

The invention discloses a manufacturing method of granular sodium tert-pentoxide, which comprises the following steps: taking metal sodium, tert-amyl alcohol and inert organic solvent as raw materials, pouring the tert-amyl alcohol and the inert solvent into a reaction kettle, further pouring the metal sodium into the reaction kettle, carrying out reflux reaction for 8-40h under the protection of nitrogen, evaporating the tert-amyl alcohol under normal pressure, decompressing to minus 0.08-minus 0.098MPa after the tert-amyl alcohol is completely evaporated, evaporating the residual inert organic solvent, then regulating the stirring rate of the reaction kettle to 10-80 turns / minute, decompressing and evaporating the inert organic solvent, cooling a remaining granular sodium tert-pentoxide product in the kettle to below 40 DEG C, and finally obtaining the required granular sodium tert-pentoxide. The manufacturing method can carry out production by utilizing general chemical equipment, the operation conditions are mild, the production process is simple, the used raw materials are convenient and easy to obtain, the product quality is stable and reliable, and the shelf life of the product can be effectively prolonged.

Description

technical field [0001] The invention relates to a manufacturing method of a fine chemical intermediate, in particular to a manufacturing method of granular sodium tert-amylate. Background technique [0002] Sodium tert-amylate is an intermediate widely used in fine chemical industry. It is often used in various reactions of etherification, esterification, and carbonyl α position, and is used in the manufacture of pharmaceuticals and liquid crystals. The commonly used sodium tert-amylate product is a powdery substance. Due to the strong corrosiveness and strong hygroscopicity of this product, the dust generated during the operation and feeding will cause great damage to the health of the operators. In addition, the characteristics of the dust are flammable and explosive. Threats to the security of the production environment. In order to prevent human injury and safety problems caused by sodium tert-amylate powder, it is often used as a toluene solution, but the need to remov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/30C07C29/70
Inventor 王玉琴詹玉俊
Owner GENCHEM & GENPHARM CHANGZHOU CO LTD
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