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Preparation method of N,N-diethyl hydroxylamine

A technology of diethylhydroxylamine and triethylamine, which is applied in the N field, can solve the problems of white oil carry-over, low production efficiency, and affecting product quality, and achieve the effects of reducing accumulation, improving production efficiency, and avoiding the use of white oil

Active Publication Date: 2021-02-19
JINING KENDRAY CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are following defects in the cracking process of triethylamine oxide: (1) white oil is used as the cracking medium, and some white oil will be brought into the product during the cracking process, which will affect the product quality; (2) it needs to be replaced regularly Deteriorated white oil, so as not to affect further use; (3) The reaction is a batch process, and the production efficiency is low

Method used

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  • Preparation method of N,N-diethyl hydroxylamine
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  • Preparation method of N,N-diethyl hydroxylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Mix triethylamine, 27.5% hydrogen peroxide and sodium bicarbonate in a ratio of 1:1.2:0.05, and react at 135°C with a stirring speed of 90rpm to prepare triethylamine oxide, and obtain triethylamine oxide The quality score is 82%.

Embodiment 2

[0022] The specification of the tubular reactor used in the test is Φ8*1*1000mm, and the reaction pressure is 1atm. The reactor was heated to an internal temperature of 100°C with jacketed heat-conducting oil, and triethylamine oxide with a mass fraction of 82% was fed in at a rate of 5.74 g / min by a convection pump, and the reaction time was 60 s. After stabilizing the reaction system for 10 min, samples were taken for analysis.

Embodiment 3

[0024] The specification of the tubular reactor used in the test is Φ8*1*1000mm, and the reaction pressure is 1.5atm. The reactor was heated to an internal temperature of 200°C with jacketed heat transfer oil, and triethylamine oxide with a mass fraction of 82% was fed in at a rate of 34.5 g / min by a convection pump, and the reaction time was 360 s. After stabilizing the reaction system for 10 min, samples were taken for analysis.

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Abstract

The invention discloses a preparation method of N,N-diethyl hydroxylamine. The preparation method comprises the following steps: reacting following raw materials: triethylamine, a catalyst and hydrogen peroxide with a mass percentage of 27.5% to prepare triethylamine oxide; continuously injecting the obtained triethylamine oxide into a tubular reactor, and reacting at the temperature of 100-200 DEG C under a pressure of 1-2 atm to obtain N,N-diethyl hydroxylamine. The tubular reactor is used as a reaction medium for triethylamine oxide cracking, so that the use of white oil is avoided, the clarity of the product is improved, and the production efficiency of the product is improved.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, and more specifically relates to a preparation method of N,N-diethylhydroxylamine. Background technique [0002] N, N-diethylhydroxylamine is mainly used as a polymerization inhibitor in the production and storage of conjugated olefins such as styrene, divinylbenzene, butadiene, isoprene and acrylonitrile, and other monomers containing active bonds. . As a polymerization inhibitor, N, N-diethylhydroxylamine has good polymerization inhibition effect, and the polymerization inhibition efficiency is not affected by temperature changes. It not only has high polymerization inhibition efficiency in liquid phase, but also has good polymerization inhibition efficiency in gas phase. polymerization inhibition performance. [0003] There are many synthetic methods of N,N-diethylhydroxylamine. From the perspective of industrialization such as synthetic cost, raw material price, yield, and product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C239/10B01J19/00B01J3/04
CPCC07C239/10B01J19/00B01J3/042C07B63/04C07C7/20C07C253/32C07C15/46C07C15/44C07C11/16C07C11/18C07C255/08
Inventor 陈军民宋芬陈语桐张平华毕德元
Owner JINING KENDRAY CHEM TECH CO LTD
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