Check patentability & draft patents in minutes with Patsnap Eureka AI!

A device and method for removing impurities from circulating tert-butanol in a cyclohexanone ammoximation process

A technology of cyclohexanone amidoxime and tert-butanol, which is used in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc. The problems of high water content at the top of the alcohol recovery tower and the increased proportion of circulating tert-butanol water have achieved the effect of solving the difficulty of separation, avoiding a large number of side reactions, and high utilization of mass transfer space.

Active Publication Date: 2017-12-15
HUBEI SANNING CHEM
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This increases the difficulty of purification of raw materials such as cyclohexanone and hydrogen peroxide on the one hand, and also increases the consumption of hydrogen peroxide and gaseous ammonia on the other hand.
In addition, due to the tert-butanol-water azeotrope, the water content in the top of the tert-butanol recovery tower is high under high load, resulting in an increase in the proportion of water in the circulating tert-butanol, and this part of water increases the load of the reactor after being introduced into the reactor , and the larger the proportion of water in the system, the more unfavorable the oximation reaction
[0004] Therefore, it is necessary to seek a method for removing impurities in a cyclohexanone ammoximation device, and the existing cyclohexanone ammoximation device and method do not involve the device and method for recycling tert-butanol.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A device and method for removing impurities from circulating tert-butanol in a cyclohexanone ammoximation process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A device for removing impurities by circulating tert-butanol in a cyclohexanone ammoximation process, comprising a circulating tert-butanol storage tank 1 and a tert-butanol refining tower 2, and the top of the tert-butanol refining tower 2 is sequentially connected to a condenser 3, Reflux tank 4 and reflux pump 5, reflux pump 5 is respectively connected to tert-butanol refining tower 2 and new ring tert-butanol storage tank 6 by pipeline, and the tower bottom of described tert-butanol refining tower 2 passes through tower bottom discharge pump 7 Connect to waste water treatment unit 8.

[0024] Further, a feed pump 9 is provided between the circulating tert-butanol storage tank 1 and the tert-butanol refining tower 2 .

[0025] Further, the tert-butanol refining tower 2 adopted is a new vertical sieve tray tower.

[0026] Further, the number of trays of the tert-butanol refining tower 2 is 24 layers, the feed position connected to the circulating tert-butanol storage...

Embodiment 2

[0028] A method for removing impurities of circulating tert-butanol in a cyclohexanone ammoximation process, carried out according to the following steps:

[0029] a. The tert-butanol in the circulating tert-butanol storage tank is pumped to the tert-butanol refining tower through the feed of the tert-butanol refining tower, and the material flow rate is 2m 3 / h, the feed tray position is the 17th floor;

[0030] b. The reflux at the top of the tower is controlled at 1m 3 / h, reflux ratio 0.5, tower top temperature 80°C;

[0031] c. The steam feed rate at the bottom of the tower is 3t / h, and the temperature at the bottom of the tower is 90°C;

[0032] d. Based on the above control conditions, after analysis, the total impurities in the top tert-butanol 78%, and the bottom tert-butanol content < 0.5%.

Embodiment 3

[0034] A method for removing impurities of circulating tert-butanol in a cyclohexanone ammoximation process, carried out according to the following steps:

[0035] a. The tert-butanol in the circulating tert-butanol storage tank is pumped to the tert-butanol refining tower through the feed of the tert-butanol refining tower, and the material flow rate is 3m 3 / h, the feed tray position is the 17th floor;

[0036] b. The reflux at the top of the tower is controlled at 2m 3 / h, reflux ratio 0.67, tower top temperature 78°C;

[0037] c. The steam feed rate at the bottom of the tower is 5t / h, and the temperature at the bottom of the tower is 95°C;

[0038] d. Based on the above control conditions, after analysis, the total impurities in the top tert-butanol 80%, and the bottom tert-butanol content<0.1%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a device and method for circulating tertiary butanol impurity removal in a cyclohexanone ammoximation technology. The device comprises a circulating tertiary butanol storage tank and a tertiary butanol refining tower, the top of the tertiary butanol refining tower is sequentially connected with a condenser, a reflux tank and a reflux pump, the reflux pump is connected to the tertiary butanol refining tower and a newly-made circulating tertiary butanol storage tank through a pipeline, and the bottom of the tertiary butanol refining tower is connected to a wastewater treatment unit through a discharging pump at the bottom of the tower. By the adoption of the device, the water content in circulating tertiary butanol can be effectively reduced, the concentration of circulating tertiary butanol is increased to 80-85% from 72-75% before refining, the feeding load of a reaction kettle is reduced, and the reaction environment is improved; refining and impurity removing are performed on circulating tertiary butanol, the content of impurities of a reaction system is reduced, a lot of side reactions are avoided, and reaction selectivity is improved.

Description

technical field [0001] The invention belongs to the field of chemical technology and equipment, in particular to a device and method for removing impurities from circulating tert-butanol in a cyclohexanone ammoximation process. Background technique [0002] Cyclohexanone oxime is an important intermediate in the production of caprolactam. The main production method of cyclohexanone ammoximation is to use hydrogen peroxide, ammonia and cyclohexanone to react in the presence of titanium silicon molecular sieve catalyst and tert-butanol solvent. Cyclohexanone oxime, through the filtration system, filters out the molecular sieve catalyst to obtain the reaction liquid, and then recovers tert-butanol and extracts and rectifies to obtain high-purity cyclohexanone oxime. [0003] In the existing cyclohexanone ammoximation process, tert-butanol is recovered through a tert-butanol recovery tower in the tert-butanol recovery process, and the recovered tert-butanol is returned to the ox...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/80C07C31/12B01D3/16
CPCB01D3/16C07C29/80C07C31/12
Inventor 李万清周学军李军游华彬车小军万军严敏陈超
Owner HUBEI SANNING CHEM
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More