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Method for recovering solvent from ammoximation reaction liquid

A technology for ammoximation reaction and solvent recovery, which is applied in oxime preparation, organic chemistry, etc., can solve problems such as environmental hazards, high energy consumption, and increased production cost of cyclohexanone oxime, and achieve the effect of saving production costs and reducing dosage

Inactive Publication Date: 2012-08-15
北京凯美信科科技开发有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have many intermediate steps, complex processes, and use a large amount of corrosive and heavily polluting raw materials, causing great harm to the environment.
[0003] The ammoximation reaction of cyclohexanone, ammonia and hydrogen peroxide using titanium silicon molecular sieve as a catalyst is a new process for preparing cyclohexanone oxime. This method has the characteristics of simple process and low pollution, but the ammoximation Use a large amount of solvents in the reaction process, and solvent is generally selected from alcohols, and wherein suitable is tert-butanol and Virahol, as in the disclosed method of U.S. Patent USP4794198 and USP5227525, needs 2~5 times of cyclohexanone Tert-butanol is used as solvent, and isopropanol is used as solvent in the disclosed method of CN1556098. Recycling and utilization of these solvents from the reaction product usually adopts the method of atmospheric distillation, which needs to consume a large amount of energy, which makes the production cost of cyclohexanone oxime increase

Method used

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  • Method for recovering solvent from ammoximation reaction liquid
  • Method for recovering solvent from ammoximation reaction liquid
  • Method for recovering solvent from ammoximation reaction liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] according to figure 1 The flow scheme shown is implemented. Among them, the inner diameter of the distillation towers a and b is 0.35 meters, with 8 meters of BX500 packing inside, equipped with reflux and feed distributors, reboilers E1 and E2 are vertical fixed tube-sheet heat exchangers, and the heat exchange area of ​​E1 is 14 square meters The heat exchange area of ​​E2 is 9 square meters, and the condenser E3 is a 2-tube fixed tube-sheet heat exchanger with a heat exchange area of ​​60 square meters.

[0040] The ammoximation reaction solution containing 2.8% of ammonia, 20.2% of cyclohexanone oxime, 41.3% of tert-butanol, 35.6% of water, and 0.08% of cyclohexanone is continuously passed into distillation tower a at a flow rate of 1237 kg per hour, and distilled Tower a maintains natural normal pressure, the material in the tower kettle is pumped and sent to distillation tower b, reboiler E2 is fed with 1.0MPa water vapor, the operating pressure of distillation t...

Embodiment 2

[0043] Repeat Example 1, the difference is that distillation tower a adopts 80kPa negative pressure operation, distillation tower b adopts 180kPa operation, ammonia-containing non-condensable gas 11 is boosted to normal pressure with booster pump c, and its main operating conditions and results are summarized in Table 1.

Embodiment 3

[0045] Repeat Example 1, the difference is that the operating pressure of distillation tower a is 150kPa, and the operating pressure of distillation tower b is 450kPa, and its main operating conditions and results are summarized in Table 1.

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PUM

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Abstract

The invention provides a method for recovering a solvent from an ammoximation reaction liquid. The method comprises the following steps: feeding a reaction liquid containing ammonia, the solvent, cyclohexanone oxime, water and cyclohexanone into a primary distillation tower (a), and evaporating out partial solvent containing ammonia and water from a tower top; and feeding materials in a tower kettle into a secondary distillation tower (b), and carrying out pressure distillation by utilizing exterior heat source so as to obtain high-temperature vapor containing the solvent from the tower top and obtain a material containing cyclohexanone oxime, water and cyclohexanone from the tower kettle, wherein the high-temperature vapor containing the solvent serves as the distillation heat source for the primary distillation tower (a). By using the method, the energy consumption for the solvent recovery can be reduced.

Description

technical field [0001] The invention relates to a method for recovering a solvent from an ammoximation reaction solution. More specifically, it relates to the separation of the ammoximation reaction solution and the preparation of cyclohexanone oxime. Cyclohexanone oxime is mainly used in the production of caprolactam and is an important intermediate in the production of caprolactam. Background technique [0002] At present, cyclohexanone oxime is mainly produced in industry by the oximation method of hydroxylamine salt, such as hydroxylamine phosphate method (HPO), hydroxylamine sulfate method (HSO) and the like. These methods have many intermediate steps, complex processes, use a large amount of corrosive and heavily polluted raw materials, and cause great harm to the environment. [0003] The ammoximation reaction of cyclohexanone, ammonia and hydrogen peroxide using titanium silicon molecular sieve as a catalyst is a new process for preparing cyclohexanone oxime. This ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/14C07C249/04C07C251/44
Inventor 李瑞
Owner 北京凯美信科科技开发有限责任公司
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