Method of preparing hydroxylamine salt by using reaction-extractive distillation coupling technology

A technology of extractive distillation and hydroxylamine salt, which is applied in the preparation of hydroxylamine, carboxylate, nitrogen and non-metallic compounds, etc., can solve the problems of low product yield, poor safety, and poor feasibility, and achieves high product yield and reaction safety. , The effect of low material toxicity

Active Publication Date: 2013-09-25
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Therefore, the hydroxylamine salt synthesis industry urgently needs to adopt a new process method to break the limitation of its reaction balance, fundamentally improve the existing process technology level of hyd

Method used

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  • Method of preparing hydroxylamine salt by using reaction-extractive distillation coupling technology
  • Method of preparing hydroxylamine salt by using reaction-extractive distillation coupling technology
  • Method of preparing hydroxylamine salt by using reaction-extractive distillation coupling technology

Examples

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Effect test

Embodiment 1

[0043] (1) Add 7.31kg of acetone oxime and 9.61kg of hydrochloric acid (which contains about 5.95kg of water) into the stirred reactor. The reactants are compatible, and a uniform solution is formed by stirring;

[0044] (2) Add 10L of toluene to the stirred reactor in proportion to make the reaction system an immiscible two-liquid phase system; stir to disperse the extractant phase and the reactant phase and expand the phase boundary between the two phases area;

[0045] (3) Heat the reaction materials to start the reaction, and control the reaction temperature at 50°C. Control the reaction system pressure to 1×10 5 Pa; The acetone generated in the reaction is immediately separated from the aqueous phase into the organic phase, separated by distillation, and recovered by condensation, thus breaking the limitation of the reversible equilibrium reaction and continuously enriching the target product hydroxylamine salt in the aqueous phase. After the reaction, the oil and water...

Embodiment 2

[0047] (1) Add 7.31kg of acetone oxime and 9.61kg of hydrochloric acid (which contains about 5.95kg of water) into the stirred reactor. The reactants are compatible, and a uniform solution is formed by stirring;

[0048] (2) Add 10L of toluene to the stirred reactor in proportion to make the reaction system an immiscible two-liquid phase system; stir to disperse the extractant phase and the reactant phase and expand the phase boundary between the two phases area;

[0049] (3) Heat the reaction materials to start the reaction, and control the reaction temperature at 180°C. Control the reaction system pressure to 1×10 5 Pa; The acetone generated in the reaction is immediately separated from the aqueous phase into the organic phase, separated by distillation, and recovered by condensation, thus breaking the limitation of the reversible equilibrium reaction and continuously enriching the target product hydroxylamine salt in the aqueous phase. After the reaction, the oil and wate...

Embodiment 3

[0051] (1) Add 7.31kg of acetone oxime and 9.61kg of hydrochloric acid (which contains about 5.95kg of water) into the stirred reactor. The reactants are compatible, and a uniform solution is formed by stirring;

[0052] (2) Add 10L of toluene to the stirred reactor in proportion to make the reaction system an immiscible two-liquid phase system; stir to disperse the extractant phase and the reactant phase and expand the phase boundary between the two phases area;

[0053] (3) Heat the reaction materials to start the reaction, and control the reaction temperature at 50°C. Control the reaction system pressure to 1×10 2 Pa; The acetone generated in the reaction is immediately separated from the aqueous phase into the organic phase, separated by distillation, and recovered by condensation, thus breaking the limitation of the reversible equilibrium reaction and continuously enriching the target product hydroxylamine salt in the aqueous phase. After the reaction, the oil and water...

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Abstract

The invention provides a method of preparing hydroxylamine salt by using reaction-extractive distillation coupling technology. The method comprises the steps of performing a hydrolysis reversible equilibrium reaction to acetoxime/butanone oxime; using reaction-extraction-distillation ternary coupling technology; extracting, distilling and separating acetone (or butanone) as one of reaction products continuously to make it leave the reactant, so as to break the limit of the reaction equilibrium to the reversible reaction, thereby the raw material conversion rate is greatly lifted, the target product hydroxylamine salt is constantly generated and collected in water phase, and the yield is high. The yield of hydroxylamine hydrochloride is 98%, and the yield of other hydroxylamine salts is over 90%; at the same time, reaction product acetone or butanone is separated as the synthesis raw material of acetoxime (or butanone oxime), and the cycle utilization technology is realized.

Description

technical field [0001] The present invention specifically relates to a process suitable for the preparation of hydroxylamine salts. More specifically, acetone oxime or butanone oxime is used as a raw material to synthesize hydroxylamine salts through hydrolysis reaction. One of the reaction products, acetone or butanone, is distilled and separated to leave the reactant phase, thereby breaking the restriction of the reaction equilibrium on the reversible reaction, greatly improving the conversion rate of raw materials, and making the target product hydroxylamine salt continuously generated and enriched in the water phase. Set to obtain a high-yield process method. Background technique [0002] Hydroxylamine salt is a chemical product with a wide range of uses, mainly including hydroxylamine hydrochloride, hydroxylamine sulfate, hydroxylamine phosphate, hydroxylamine nitrate, hydroxylamine perchlorate, hydroxylamine oxalate and other varieties. Hydroxylamine hydrochloride is ...

Claims

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Application Information

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IPC IPC(8): C01B21/14C07C55/07C07C51/41
Inventor 严生虎林春昕张跃沈介发刘建武
Owner CHANGZHOU UNIV
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