Production technology for producing cyclohexyl formate by dividing wall reaction rectification

A technology of cyclohexyl formate and reactive distillation, which is applied in the field of production technology of cyclohexyl formate by reactive distillation next door, can solve the problems of low yield, high energy consumption, complicated process, etc., and achieve reduction of production equipment, purity High, simple process effect

Active Publication Date: 2018-09-11
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problems of complex process, high energy consumption and low yield of the original direct reaction of formic acid and cyclohexanol to produce cyclohexyl formate, and to provide a production process for the production of cyclohexyl formate by partition reaction distillation

Method used

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  • Production technology for producing cyclohexyl formate by dividing wall reaction rectification
  • Production technology for producing cyclohexyl formate by dividing wall reaction rectification
  • Production technology for producing cyclohexyl formate by dividing wall reaction rectification

Examples

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Effect test

Embodiment 1

[0024] A production process for producing cyclohexyl formate by reactive distillation in a partition, comprising the following steps:

[0025] (1) add the hexamethylene formate, 25% cyclohexanol, 25% formic acid that the percentage by weight is 50% in the main rectification tower still of next door reactive distillation column, add hexamethylene alcohol in the secondary rectification tower still, The liquid levels of the two towers and kettles both reached 70%, and a certain amount of zeolite was added to the tower kettles of the main rectifying tower and the auxiliary rectifying tower to prevent bumping, and the reboiler Ⅰ1 and reboiler Ⅱ2 were turned on, and the electric heating wire switch was turned on Carry out heat preservation, control the pressure in the reaction rectifying column next door to be 15kPa;

[0026] (2) When the temperature of the main rectifying tower still reaches 100°C, add formic acid to the feed port at the lower end of reaction section 4, and simulta...

Embodiment 2

[0033] A production process for producing cyclohexyl formate by reactive distillation in a partition, comprising the following steps:

[0034] (1) add the hexamethylene formate, 25% cyclohexanol, 25% formic acid that the percentage by weight is 50% in the main rectification tower still of next door reactive distillation column, add hexamethylene alcohol in the secondary rectification tower still, The liquid levels of the two towers and kettles both reached 70%, and a certain amount of zeolite was added to the tower kettles of the main rectifying tower and the auxiliary rectifying tower to prevent bumping, and the reboiler Ⅰ1 and reboiler Ⅱ2 were turned on, and the electric heating wire switch was turned on Carry out heat preservation, control the pressure in the reaction rectifying column next door to be 10kPa;

[0035] (2) When the temperature of the main rectifying tower still reaches 90°C, add formic acid to the feed port at the lower end of reaction section 4, and simultan...

Embodiment 3

[0043] A production process for producing cyclohexyl formate by reactive distillation in a partition, comprising the following steps:

[0044] (1) add the hexamethylene formate, 25% cyclohexanol, 25% formic acid that the percentage by weight is 50% in the main rectification tower still of next door reactive distillation column, add hexamethylene alcohol in the secondary rectification tower still, The liquid levels of the two towers and kettles both reached 70%, and a certain amount of zeolite was added to the tower kettles of the main rectifying tower and the auxiliary rectifying tower to prevent bumping, and the reboiler Ⅰ1 and reboiler Ⅱ2 were turned on, and the electric heating wire switch was turned on Carry out heat preservation, control the pressure in the reaction rectifying column next door to be 15kPa;

[0045] (2) When the temperature of the main rectifying tower still reaches 90°C, add formic acid to the feed port at the lower end of reaction section 4, and simultan...

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Abstract

The invention discloses a production technology for producing cyclohexyl formate by dividing wall reaction rectification. The technology comprises the following steps: (1) adding 50 wt% of cyclohexylformate, 25 wt% of cyclohexanol and 25 wt% of formic acid into a main rectification tower bottom, adding cyclohexanol into an auxiliary rectification tower bottom, starting a reboiler I and a reboilerII when the height of the liquid level in every tower bottom reaches 70% of the height of the corresponding tower bottom, and controlling the pressure in every tower to be 10-15 kPa; and (2) adding cyclohexanol and formic acid into a main rectification tower when the temperature of the main rectification tower bottom reaches 90-100 DEG C, performing a reaction under the action of a solid acid catalyst, removing water and recovering cyclohexanol from the tower top of the main rectification tower, extracting the cyclohexyl formate from the main rectification tower bottom, extracting the cyclohexanol from the auxiliary rectification tower bottom, and recycling the extracted cyclohexanol. The technology has the advantages of simplicity, reduction of production devices, production cost saving,solving of the problems of high complex energy consumption and low yield of original technologies for producing the cyclohexyl formate through directly reacting formic acid with cyclohexanol, and realization of high purity of the obtained cyclohexyl formate.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a production process for producing cyclohexyl formate through reaction distillation in a partition wall. Background technique [0002] Cyclohexyl formate is liquid at room temperature. It is popular because it is often used as a synthetic fragrance and as a dispersant in paints and inks with good results. Because its molecule contains reductive aldehyde groups, its synthesis used to be obtained by multi-step synthesis using boric acid, cyclohexanol and formic acid as raw materials. Although there have been many reports on its synthetic routes in the past ten years, most of them are improvements in conditions. Its synthesis is generally through the reaction of boric acid and cyclohexanol to obtain cyclohexyl borate, and then use formic acid for acid substitution reaction, or first by phosgene, and then by HCONMe 2 reacted. These reaction conditions are co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/54C07C69/06
CPCC07C67/08C07C67/54C07C2601/14C07C69/06Y02P20/10
Inventor 田晖邓帅胡明圆孙进超
Owner YANTAI UNIV
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