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Manufacturing method of granular potassium tert-pentylate

Potassium tert-amylate and its manufacturing method are applied in the fields of metal alcohol preparation and organic chemistry, which can solve the problems of production environment safety threats, health damage of operators, dust flammability and explosion, etc., so as to reduce production environment safety risks, The effect of extending the shelf life and simple production process

Active Publication Date: 2013-08-14
GENCHEM & GENPHARM CHANGZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Potassium tert-amyloxide is commonly used as a powder 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 potassium tert-amyloxide powder, potassium tert-amylate is usually made into a toluene solution for use, 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 four-necked reaction flask of dry 2000ml, mechanical stirring is housed, thermometer, feeding port, reflux condenser, add tert-amyl alcohol 238g (2.77mol), mix trimethylbenzene 477g, metallic potassium fritter 90g (2.31mol), in Under the protection of nitrogen, reflux reaction for 10 hours, metal potassium completely disappeared, use a distillation device instead, steam the excess tert-amyl alcohol at normal pressure, and steam the residual mixed trimethylbenzene under vacuum -0.095MPa, keep stirring at a speed of 20 rpm , when the mixed trimethylbenzenes are evaporated, uniform potassium tert-amylate particles of about 0.6mm are produced in the bottle, and the low-temperature nitrogen (-20°C) is blown into the bottom valve of the reaction kettle to cool to below 40°C, and the required granular tert-amyloxide is obtained. potassium pentoxide.

Embodiment 2

[0016] In a dry 2000L reactor, add 238kg (2.77kmol) of tert-amyl alcohol, mix 477kg of trimethylbenzene, put in 90kg (2.31kmol) of metal potassium block under the protection of nitrogen, close the reaction kettle 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 tank bottom valve several times, and after cooling to 38°C, potassium tert-amyloxide with a particle size of 0.4mm was obtained.

Embodiment 3

[0018] In a dry 2000L reactor, add 397kg (4.62kmol) of tert-amyl alcohol, mix 1191kg of trimethylbenzene, put in 90kg (2.31kmol) of metal potassium block 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 tank bottom valve several times, and after cooling to 38°C, potassium tert-amyloxide with a particle size of 0.4mm was obtained.

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Abstract

The invention discloses a manufacturing method of granular potassium tert-pentylate, comprising the following steps: taking potassium metal, tert-amyl alcohol and inert organic solvent as raw materials; adding tert-amyl alcohol and inert organic solvent into a kettle; then, adding potassium metal into the kettle; after reflowing for 8-40 hours under the protection of nitrogen, evaporating tert-amyl alcohol at normal pressure; after tert-amyl alcohol is completely evaporated, decompressing to -0.08--0.098 MPa, and evaporating residual organic solvent; then, regulating the stirring rate of the kettle to 10-80 turns / min; decompressing to evaporate inert organic solvent, and leaving granular potassium tert-pentylate products in the kettle; and cooling to be below 40 DEG C to obtain the granular potassium tert-pentylate. The invention can carry out production by using general chemical equipment, has moderate operation condition, simple production technology, convenient and abundant raw material, and stable and reliable product quality and can effectively prolong the quality guarantee period of the product.

Description

technical field [0001] The present invention relates to a kind of manufacturing method of fine chemical intermediate, particularly relate to a kind of manufacturing method of granular potassium tert-amylate. Background technique [0002] Potassium 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 medicines and dyes. Potassium tert-amyloxide is commonly used as a powder 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 body injury and safety problems caused by potassium tert-amyloxide powder, potassium tert-amyloxide is usually mad...

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
Owner GENCHEM & GENPHARM CHANGZHOU CO LTD
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