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Method for preparing granular potassium tert-butoxide

Potassium tert-butoxide and its manufacturing method are applied in the fields of metal alkoxide preparation and organic chemistry, which can solve problems such as equipment requirements and harsh operating conditions, and achieve the effects of prolonging the shelf life, mild operating conditions, and simple production processes

Active Publication Date: 2011-02-02
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 potassium tert-butoxide (US6870071). In this type of method, Dzgussa company first made potassium tert-butoxide into tetrahydrofuran solution, and then heated it at 150-250°C. The method of spraying the tetrahydrofuran solution of potassium tert-butoxide into the fluidized bed granulator under nitrogen sweeping, but the operating conditions of this method are harsh and have extremely high requirements on the 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 mechanical stirring, thermometer, feeding port, and reflux condenser, add 270g (3.65 moles) of tert-butanol, select 1,2,4-trimethylbenzene, 1,3,5- The mixture of trimethylbenzene and 1,2,3-trimethylbenzene (referred to as mixed trimethylbenzene) 1100g, metal potassium small pieces 90g (2.31 moles), under the protection of nitrogen, reflux reaction for 10 hours, metal potassium disappeared completely, and the distillation device was used instead , steam the excess tert-butanol under normal pressure, steam the residual mixed trimethylbenzene under vacuum -0.095MPa, keep stirring at a speed of 20 rpm, and when the mixed trimethylbenzene is evaporated, a uniform tert-butyl alcohol of about 0.6mm will be produced in the bottle Potassium alkoxide 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 potassium ter...

Embodiment 2

[0016] In a dry 2000L reactor, add 270kg (3.65k moles) of tert-butanol, mix 1100kg trimethylbenzene, put 90kg (2.52k moles) of metal potassium block under nitrogen protection, close the reaction kettle after feeding, and reflux reaction under nitrogen protection After 15 hours, excess tert-butanol was evaporated under normal pressure, residual mixed trimethylbenzenes were evaporated under vacuum -0.098MPa, and the stirring speed was maintained at 20 rpm. After the mixed trimethylbenzenes were evaporated, the reactor jacket was introduced into cooling water While cooling, nitrogen gas (-20°C) was blown through the gap of the valve at the bottom of the tank for several times, and after cooling to 38°C, potassium tert-butoxide with a particle size of 0.4 mm was obtained.

Embodiment 3

[0018] In a dry 2000L reactor, add 256kg (3.46k moles) of tert-butanol, mix 1152kg trimethylbenzene, and put 90kg (2.52k moles) of metal potassium block under the protection of nitrogen, close the reaction kettle after feeding, and reflux reaction under the protection of nitrogen After 15 hours, excess tert-butanol was evaporated under normal pressure, residual mixed trimethylbenzenes were evaporated under vacuum -0.098MPa, and the stirring speed was maintained at 20 rpm. After the mixed trimethylbenzenes were evaporated, the reactor jacket was introduced into cooling water While cooling, nitrogen gas (-20°C) was blown through the gap of the valve at the bottom of the tank for several times, and after cooling to 38°C, potassium tert-butoxide with a particle size of 0.4 mm was obtained.

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Abstract

The invention discloses a method for preparing granular potassium tert-butoxide, which comprises the following steps of: with metal potassium, tertiary butanol and an inert organic solvent as raw materials, charging the tertiary butanol and the inert solvent into a reactor, charging the metal potassium into the reactor and carrying out reflux reaction under the protection of nitrogen for 8-40 hours; evaporating the tertiary butanol at normal pressure; after the tertiary butanol is completely evaporated, decompressing to minus 0.08-minus 0.098MPa; evaporating residual inert organic solvent; then adjusting the stirring speed of the reactor to 10-80RPM; decompressing and evaporating the inert organic solvent; retaining a granular potassium tert-butoxide rough product in the reactor; and cooling to below 40 DEG C to obtain needed granular potassium tert-butoxide. The invention has the advantages of production by utilizing universal chemical equipment, more mild operation condition, simpleproduction process, convenience and easy acquisition of raw material use, stable and reliable product quality and effective extension of quality guarantee period of products.

Description

technical field [0001] The invention relates to a manufacturing method of a fine chemical intermediate, in particular to a manufacturing method of granular potassium tert-butoxide. Background technique [0002] Potassium 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. Commonly used potassium tert-butoxide products are powdery substances. Due to the strong corrosiveness and strong hygroscopicity of this product, the dust generated during operation and feeding will cause great damage to the health of operators. In addition, the characteristics of dust are flammable and explosive. Threats to the security of the production environment. In order to prevent human body injury and safety problems caused by potassium tert-butoxide powder, some foreign companies have tried to make potassium tert-butoxi...

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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