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Separating production of ketoxime by three-phase amino-oximate reaction

An amidoximation reaction and oximation reaction technology, applied in oxime preparation, organic chemistry and other directions, can solve the problems of complex reaction process, catalyst loss, long process flow, etc., and achieve guaranteed product quality, reduced deactivation speed, prolonged The effect of the operating cycle

Active Publication Date: 2007-04-04
HUBEI JINXIANGNING CHEM ENG TECHENOLOGY CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are two disadvantages in the above-mentioned method for synthesizing cyclohexanone oxime by hydroxylamine salt multistep: (1) reaction process is complicated, and technical process is long; (2) process by-product inorganic ammonium salt releases a large amount of nitrogen oxides and sulfur oxides, Corrosion of equipment and pollution of the environment
[0011] (2) The particle diameter of the original catalyst powder in the reaction solution is mostly 0.1-0.3 μm, and it is difficult to completely separate it by means of hydrocyclone and sedimentation, resulting in loss of catalyst. When membrane separation and other means are used, the separation load is too heavy due to the small size of the particles. In addition, the catalyst is easy to swell under alkaline conditions, resulting in blockage of membrane pores and difficulty in continuous operation.

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  • Separating production of ketoxime by three-phase amino-oximate reaction
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Examples

Experimental program
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Effect test

Embodiment 1

[0041] Example 1: Into a 250ml glass reactor with magnetic stirring, 2.5g of titanium-silicon molecular sieve catalyst, 15.0g of cyclohexanone and 25.0g of cyclohexane were added in advance. After the temperature was raised to 69° C., 20.8 g of 27.5% hydrogen peroxide and 22.9 g of 25% ammonia were added dropwise at a constant speed, and the reaction was carried out at the azeotropic temperature of alkane and water for 2 hours. After the addition, the reaction was extended for 1 hour. Keep the temperature above 60°C and extract the product 3 times with fresh cyclohexane, the amount of cyclohexane used is 25.0g / time, separate the raffinate phase 40.8g for later use, and mix the extraction phase with the light phase of the reaction product to obtain cyclohexanone oxime- Cyclohexane solution. The contents of cyclohexanone and cyclohexanone oxime in the solution were analyzed by gas chromatography, and the calculated reaction results are shown in Table 1.

Embodiment 2

[0042] Example 2: Example 1 was repeated, except that the raffinate phase in Example 1 was not the fresh Ti-Si molecular sieve catalyst added in advance. After the reaction product was extracted, 79.1 g of the raffinate phase was separated, and the water was evaporated by a rotary evaporator at a pressure of 0.01 MPa and a temperature of 50° C. The concentrated weight was 40.1 g. The product was analyzed by gas chromatography, and the reaction results are shown in Table 1.

Embodiment 3～6

[0043] Embodiment 3~6: repeat embodiment 2, be to repeat 10 times, 20 times, 30 times and 40 times of oximation-separation-concentration process respectively, the water weight that evaporates every time is about 35~40g, the recycled content The concentrated raffinate phase of the catalyst was 39-44 g. The product was analyzed by gas chromatography, and the reaction results are shown in Table 1.

[0044] Experiment number

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Abstract

Production of ketoxime by three-phase oximation reacting separation is carried out by taking ketone as raw materials, non-homogeneous catalytic oximation reacting for ketone and hydrogen peroxide and amine to obtain ketoxime under existence of insoluble or micro-soluble solvent, separating phase for oximation reactant, separating out heavy-phase reactant from water and circulation utilizing.

Description

technical field [0001] The invention relates to a method for preparing, separating and preparing ketoxime, further illustrating that ketone is used as a raw material, and ketoxime is prepared, separated and prepared through liquid-liquid-solid three-phase ammoximation. Background technique [0002] Aliphatic ketones or aromatic ketones can be condensed with ammonia derivatives such as hydroxylamine to generate corresponding ketoximes, and then a series of amides can be synthesized by applying Beckmann rearrangement. Among them, the rearrangement of cyclohexanone oxime to caprolactam has important industrial significance. [0003] Caprolactam, scientific name ε-caprolactam, is an important petrochemical product widely used in the manufacture of nylon and engineering plastics. The industrial production methods of caprolactam mainly include cyclohexanone-hydroxylamine method, cyclohexane photonitrosation method and toluene method. Wherein the cyclohexanone-hydroxylamine metho...

Claims

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Application Information

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IPC IPC(8): C07C251/32C07C249/08
Inventor 罗和安吴剑刘国清
Owner HUBEI JINXIANGNING CHEM ENG TECHENOLOGY CO LTD