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A kind of production technology of next-wall reactive distillation to produce cyclohexyl formate

A cyclohexyl formate, production process technology, applied in the chemical industry, can solve the problems of low yield, high energy consumption, complicated process, etc., and achieve the effect of reducing production equipment, high purity and simple process

Active Publication Date: 2021-02-19
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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  • A kind of production technology of next-wall reactive distillation to produce cyclohexyl formate
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  • A kind of production technology of next-wall reactive distillation to produce cyclohexyl formate

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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 comprises 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 rectification 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 simulta...

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 process for producing cyclohexyl formate by reactive distillation in a partition, which comprises the following steps: (1) adding 50% by weight cyclohexyl formate and 25% cyclohexyl formate into the tank of the main rectification tower; Alcohol, 25% formic acid, add cyclohexanol in the side rectifying column tower kettle, the tower kettle liquid level all reaches 70%, open reboiler I and reboiler II, control tower internal pressure to be 10-15kPa; (2) When the temperature of the bottom of the main rectification tower reaches 90-100°C, add cyclohexanol and formic acid to the main rectification tower to react under the action of a solid acid catalyst, remove water from the top of the tower and recover cyclohexanol, and the main rectification tower The cyclohexyl formate is extracted from the still, and the cyclohexanol is extracted from the auxiliary distillation column and recycled. The process of the present invention is simple, reduces production equipment, saves production cost, solves the problems of complex energy consumption, high energy consumption and low yield of the original formic acid and cyclohexanol direct reaction production process of cyclohexyl formate, and the obtained cyclohexyl formate High purity.

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 Patents(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