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Preparation method of acetoxime

A technology of acetone oxime and acetone, applied in the field of preparation of acetone oxime, can solve the problems of long reaction time and low yield

Pending Publication Date: 2021-04-20
ZHEJIANG JINHUA NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] There are long reaction times and low yield in the process and technology for preparing acetone oxime in the above inventions and prior art

Method used

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  • Preparation method of acetoxime
  • Preparation method of acetoxime

Examples

Experimental program
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Effect test

Embodiment 1

[0039] A kind of preparation method of acetone oxime, its operation step is:

[0040] Step 1, oximation reaction, 58kg acetone, 21kg ammonia gas, 0.05kg catalyst and 920kg mass percentage concentration are 18% hydroxylamine sulfate solution to add in the mixer, then enter in the oximation reactor after cooling through the cooler, control Temperature 40°C, cyclic reaction for 60 minutes, the reaction liquid in the oximation reactor overflows to the oximation separator for stratification, the upper layer is the acetone oxime organic phase, and the lower layer is the ammonium sulfate mother liquor;

[0041] Step 2, stripping and separation, the ammonium sulfate mother liquor from the oximation separator enters the stripping tower for stripping, and recovers organic substances such as acetone oxime in the ammonium sulfate mother liquor, and the organic phase at the top of the tower is pumped to the oximation reactor circulation pump Imported recycling, the stripping temperature is...

Embodiment 2

[0054] A kind of preparation method of acetone oxime, its operation step is:

[0055] Step 1, oximation reaction, 64kg acetone, 27kg ammonia gas, 1.4kg catalyst and 1400kg mass percent concentration are 22% hydroxylamine sulfate solution and add in the mixer, then enter in the oximation reactor after cooling through the cooler, control Temperature at 50°C, cyclic reaction for 120 minutes, the reaction liquid in the oximation reactor overflows to the oximation separator for stratification, the upper layer is the acetone oxime organic phase, and the lower layer is the ammonium sulfate mother liquor;

[0056] Step 2, stripping and separation, the ammonium sulfate mother liquor from the oximation separator enters the stripping tower for stripping, and recovers organic substances such as acetone oxime in the ammonium sulfate mother liquor, and the organic phase at the top of the tower is pumped to the oximation reactor circulation pump Imported recycling, the stripping temperature ...

Embodiment 3

[0069] A kind of preparation method of acetone oxime, its operation step is:

[0070] Step 1, oximation reaction, 72kg of acetone, 32kg of ammonia, 3kg of catalyst and 1800kg of hydroxylamine sulfate solution with a mass percentage concentration of 24% are added to the mixer, and then enter the oximation reactor after being cooled by a cooler, and the temperature is controlled 60°C, cyclic reaction for 180 minutes, the reaction liquid in the oximation reactor overflows to the oximation separator for stratification, the upper layer is the organic phase of acetone oxime, and the lower layer is the mother liquor of ammonium sulfate;

[0071] Step 2, stripping and separation, the ammonium sulfate mother liquor from the oximation separator enters the stripping tower for stripping, and recovers organic substances such as acetone oxime in the ammonium sulfate mother liquor, and the organic phase at the top of the tower is pumped to the oximation reactor circulation pump Imported recy...

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Abstract

The invention relates to the field of chemical engineering, and provides a preparation method of acetoxime, which comprises the following steps: oximation reaction, steam stripping separation, preliminary purification, distillation purification and the like. The method for preparing acetoxime has the advantages of accessible raw materials, short investment period, obvious economic benefit, no three-waste pollution, simple production technique, favorable market conditions and the like, and can greatly shorten the reaction time, shorten the engineering period, save the energy consumption and lower the production cost by using the titanium-silicon modified kaolin catalyst.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of acetone oxime. Background technique [0002] Oxime is an important class of organic chemical reagents and an important raw material for the preparation of amines by hydrogenation. There are many ways to synthesize oxime, and hydroxylamine and ketoxime are generally used, which is simple and practical. [0003] CN109593046A relates to a preparation method of acetone oxime. The preparation method of acetone oxime of the present invention comprises the following steps: 1) dissolving acetone in an organic solvent to prepare an acetone solution, then adding TS-1 molecular sieve catalyst and ammonia water to the acetone solution to obtain a pre-reaction solution; 2) Heat the pre-reaction liquid to 40-80°C, add hydrogen peroxide solution, react at 40-80°C and pressure 0-1.0MPa for 3-10h, then filter, rectify, and extract with extractant to obtain extract, and ...

Claims

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Application Information

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IPC IPC(8): C07C249/08C07C249/14C07C251/38B01J31/02B01J29/89
Inventor 段仲刚周强徐碧涛张军良江煜
Owner ZHEJIANG JINHUA NEW MATERIALS
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