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Method of preparing granular sodium tert-butoxide

A technology of sodium tert-butoxide and its manufacturing method, which is applied in the preparation of metal alcohols, organic chemistry, etc., can solve problems such as harsh operating conditions and equipment requirements, and achieve the effects of mild operating conditions, extended shelf life, and simple production processes

Active Publication Date: 2013-06-12
GENCHEM & GENPHARM CHANGZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2005, Dzgussa company published the first method for manufacturing granular sodium tert-butoxide (US6870071). In this type of method, Dzgussa company first made sodium tert-butoxide into tetrahydrofuran solution, and then heated it at 150~250°C Under nitrogen sweeping, spray the tetrahydrofuran solution of sodium tert-butoxide into the fluidized bed granulator for granulation, but this method has harsh operating conditions and extremely high requirements for equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In a dry 2000ml four-necked reaction flask equipped with a mechanical stirrer, a thermometer, a feeding port, and a reflux condenser, add 620g (8.38mol) of tert-butanol, select 1,2,4-trimethylbenzene, 1,3,5- The mixture of trimethylbenzene and 1,2,3-trimethylbenzene (mixed trimethylbenzene for short) 1100g, metal sodium wire 65g (2.83mol), under the protection of nitrogen, reflux reaction for 10 hours, metal sodium completely disappears, use distillation apparatus instead, Evaporate excess tert-butanol under normal pressure, and evaporate residual mixed trimethylbenzene under vacuum -0.095MPa, keep stirring at a speed of 20 rpm. Sodium particles are blown into low-temperature nitrogen (-20°C) through the bottom valve of the reaction tank to cool down to below 40°C to obtain the required granular sodium tert-butoxide.

Embodiment 2

[0016] In a dry 2000L reactor, add 620kg (8.38kmol) of tert-butanol, mix 540kg of trimethylbenzene, press in 65kg (2.83kmol) of sodium metal under the protection of nitrogen, close the reactor after feeding, and reflux for 12 hours under the protection of nitrogen , steam the excess tert-butanol at normal pressure, steam the residual 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 valve at the bottom of the tank several times, and after cooling to 38°C, sodium tert-butoxide with a particle size of 0.6mm was obtained.

Embodiment 3

[0018] In a dry 2000L reactor, add 522kg (7.05kmol) of tert-butanol, mix 470kg 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 12 After 1 hour, excess tert-butanol was steamed at 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 blow nitrogen gas (-20°C) several times from the gap of the valve at the bottom of the tank, and after cooling to 38°C, sodium tert-butoxide with a particle size of 0.6mm was obtained.

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Abstract

The invention discloses a method of preparing granular sodium tert-butoxide, which includes the following steps: using metal sodium, tert-butanol and an inert organic solvent as raw materials; adding the tert-butanol and the inert solvent into a reaction kettle and then adding the metal sodium into the reaction kettle; under the protection of a nitrogen gas, refluxing for 8-40 h; at a normal temperature, distilling the tert-butnaol; after totally distilling the tert-butanol, reducing the pressure to -0.08 to -0.098 MPa to distil the remained insert organic solvent; then adjusting the stirringrate of the reaction kettle to 10-80 r / min; reducing the pressure to distil the inert organic solvent; obtaining a residual granular sodium tert-butoxide product in the reaction kettle; cooling the product to less than 40 DEG C to obtain the required granular sodium tert-butoxide. The method can perform a production by using universal chemical equipment. An operation condition is moderate; a protection technique is simple; and the raw materials used are easily obtained. The quality of the product is stable and reliable. 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-butoxide. Background technique [0002] Sodium tert-butoxide is an intermediate widely used in fine chemicals. 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-butoxide product is a powdery substance. Due to the strong corrosiveness and strong hygroscopicity of the 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-butoxide powder, some foreign companies have tried to make sodium tert-butoxide int...

Claims

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Application Information

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