Method for preparing cyclohexanol by hydrolyzing cyclohexyl formate

A technology of cyclohexyl formate and cyclohexanol, which is applied in the chemical industry, can solve problems such as catalyst loading and replacement difficulties, and reduce the reaction rate, and achieve large-scale industrial production, flexible operation control, and short process flow.

Inactive Publication Date: 2016-10-12
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the traditional reactive distillation coupling is carried out in the same column, the negative pressure operation of the reactive distillation column causes the temperature of the reaction tray to be 15-30°C, which greatly reduces the reaction rate, and the loading and unloading of the catalyst on the rectification tray It is difficult to replace

Method used

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  • Method for preparing cyclohexanol by hydrolyzing cyclohexyl formate
  • Method for preparing cyclohexanol by hydrolyzing cyclohexyl formate
  • Method for preparing cyclohexanol by hydrolyzing cyclohexyl formate

Examples

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Effect test

Embodiment 1

[0034] When the number of knapsack reactors is 1, with cyclohexyl formate and water as raw materials, adopt such as figure 1 Said technological process hydrolyzes and prepares cyclohexanol. The total plate number of described rectifying tower is 16 trays (reaction rectification area tray number 1, stripping area tray number 15); Rectification tower operating pressure is 15kPa; Tower diameter is 0.09m The first knapsack reactor was equipped with 700 g (the catalyst loading was 47.9% of the total mass of cyclohexyl formate and water freshly fed per hour) ion exchange resin Amberlyst 15. The volume of the reactor is 20L. Cyclohexyl formate and water are continuously fed into the first knapsack reactor according to the molar ratio of 1:1. The feed flow rate is 10mol / h. The ion exchange resin Amberlyst 15 is used as the acidic catalyst. At normal pressure, the reaction temperature is 60°C, the reaction liquid enters the reactive distillation zone of the rectification tower, the ga...

Embodiment 2

[0038] The number of knapsack reactors is 2, and the acidic catalyst is acidic molecular sieve HZSM-5, and the loading capacity of the first knapsack reactor is 350g (catalyst loading in the first knapsack reactor is 1 / 2 of fresh feed per hour. 24.0% of cyclohexyl formate and water gross mass), the reactor volume is 20L; The filling capacity of the second knapsack reactor is 300g (catalyst loading is the fresh charge per hour in the second knapsack reactor 20.5% of the total mass of cyclohexyl formate and water), the reactor volume is 20L; the total number of trays in the rectification tower is 13 (the number of trays in the reaction distillation area is 5, and the number of trays in the stripping area is 8) , The operating pressure of the reactive distillation tower is 10kPa, and the diameter of the distillation tower is 0.12m.

[0039] Water and cyclohexyl formate are fed in a molar ratio of 1:1, and the feed flow rate is 10mol / h; cyclohexyl formate is continuously fed into ...

Embodiment 3

[0044] The number of knapsack reactors is 2, and the acidic catalyst is acidic ion exchange resin D072H, and the loading capacity of the first knapsack reactor is 450g (catalyst loading capacity is 1 / 2 of fresh feed per hour in the first knapsack reactor). Cyclohexyl formate and 30.8% of the total mass of water), the reactor volume is 25L; the loading capacity of the second knapsack reactor is 350g (catalyst loading is 1 / 2 of fresh feed per hour in the second knapsack reactor 24.0% of the total mass of cyclohexyl formate and water), the reactor volume is 20L; the total number of trays in the rectification tower is 12 (the number of trays in the reaction distillation zone is 4, and the number of trays in the stripping zone is 8) , The operating pressure of the reactive distillation column is 10kPa, and the diameter of the distillation column is 0.09m.

[0045] Water and cyclohexyl formate are fed in a molar ratio of 1:1, and the feed flow rate is 10mol / h; cyclohexyl formate is ...

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Abstract

The invention discloses a new "backpack" reactive distillation process for preparing cyclohexanol by hydrolyzing cyclohexyl formate and water as raw materials. The backpack reactor is placed outside the rectification tower, and the first Cyclohexyl formate is continuously fed into the knapsack reactor for hydrolysis reaction, and the feed to the rest of the knapsack reactors comes from the upper tray of the rectification tower, and then enters the next tray of the rectification tower after reaction , obtain the product that cyclohexanol mole fraction is more than 95%. The "backpack" reaction and the rectification tower are both interconnected and independent. This coupling method can not only maintain the advantages of the integrated reaction distillation technology, but also make the operating conditions of the reactor and the rectification tower independent of each other. The process flow is short, the operation control is flexible, the production cost is low, and the economic benefit is high. At the same time, the volume of the reactor and the reaction volume can be adjusted freely, which realizes the best match between the reaction capacity and the separation capacity, and is conducive to the realization of large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a new production process of cyclohexanol, in particular to a method for preparing cyclohexanol by hydrolysis of cyclohexyl formate, which is a method of using cyclohexyl formate and water as raw materials, through "backpack type "The method of preparing cyclohexanol by the coupling process of reaction and rectification in the reactor. Background technique [0002] Cyclohexanol is an important chemical intermediate used in the production of nylon, adipic acid, caprolactam and other chemical products. In my country, cyclohexanol is mainly used as an intermediate in the production of adipic acid and amine compounds. [0003] The traditional preparation methods of cyclohexanol mainly include cyclohexane oxidation method and phenol hydrogenation method. At present, cyclohexane oxidation method is mainly used in industry. Patent CN102627541A introduces a process and equipment for prepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C27/00C07C27/28C07C29/09C07C29/80C07C35/08C07C51/09C07C51/44C07C53/02
CPCC07C29/095C07C29/80C07C51/09C07C51/44
Inventor 汤吉海乔旭王振松许戈陈献费兆阳崔咪芬李云鹏陆佳伟
Owner NANJING UNIV OF TECH
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