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Method for synthesizing N-isopropylhydroxyla

A technology of isopropylhydroxylamine and propylhydroxylamine salt, applied in the direction of organic chemistry and the like, can solve the problems of complex process, low yield of N-isopropylhydroxylamine, etc., and achieves abundant raw material sources, mild reaction conditions and low production cost. Effect

Active Publication Date: 2013-04-10
JINING KENDRAY CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The invention provides a method for preparing N-isopropylhydroxylamine, which solves the problems of low yield and complicated process of synthesizing N-isopropylhydroxylamine by traditional methods

Method used

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  • Method for synthesizing N-isopropylhydroxyla
  • Method for synthesizing N-isopropylhydroxyla

Examples

Experimental program
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Embodiment 1

[0025] In a 1000L reactor, add 200Kg of diisopropylamine and 200g of Mn (Salen) catalyst, raise the temperature to 60°C, slowly add 500Kg of 30% aqueous hydrogen peroxide solution dropwise, and complete the dropwise addition in 3 hours. Keep warm for 1h. Then add 214L mass percent concentration and be 37% hydrochloric acid solution, hydrolyze under acidic condition, concentrate, cooling crystallization makes 201Kg isopropyl hydroxylamine hydrochloride; Add 600L methyl tert-butyl Ether and 170Kg concentration are 50% sodium hydroxide aqueous solution, separate and obtain 119Kg of 99% isopropyl hydroxylamine, and yield is 88% (calculated as diisopropylamine).

Embodiment 2

[0027] In a 1000L reactor, add 200Kg of diisopropylamine and 300g of Mn(Salen-Ph) catalyst, raise the temperature to 60°C, slowly add 600Kg of 25% aqueous hydrogen peroxide solution dropwise, dropwise after 4 hours, dropwise Complete and continue to insulate for 1 hour, then add 230L of hydrochloric acid solution with a mass percentage concentration of 37%, hydrolyze, concentrate, and cool to crystallize under acidic conditions to obtain 185Kg isopropyl hydroxylamine hydrochloride; add 600L of isopropyl hydroxylamine hydrochloride Tetrahydrofuran and 150Kg concentration are 50% aqueous sodium hydroxide solution, separate and obtain 89Kg of 99% isopropyl hydroxylamine, and the yield is 67% (calculated as diisopropylamine).

Embodiment 3

[0029] In a 1000L reactor, add 200Kg of diisopropylamine and 800g of Fe(Salen) catalyst, raise the temperature to 60°C, slowly add 300Kg of 50% aqueous hydrogen peroxide dropwise, and complete the dropwise addition in 2.5 hours. Insulate for 1h, then add 236L of 37% hydrochloric acid solution in mass percentage concentration, hydrolyze under acidic conditions, concentrate, cool and crystallize to obtain 195Kg isopropyl hydroxylamine hydrochloride; add 635L water and 145Kg concentration is 50% sodium hydroxide aqueous solution, separates and obtains 840Kg of 15.6% isopropyl hydroxylamine, and yield is 86% (calculated as diisopropylamine).

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Abstract

The invention discloses a method for preparing N-isopropylhydroxyla. The method comprises the following steps of: under the action of a catalyst, mixing diisopropylamine and aqueous solution of hydrogen peroxide for reacting; after reacting, performing acidolysis, concentration and cooling crystallization on the reaction liquid to prepare the solid isopropylhydroxylamine salt; and re-dissolving the solid isopropylhydroxylamine salt and adding alkali for neutralizing to obtain the N-isopropylhydroxyla. The catalyst selected in the invention can be dissolved in a reactant system, so that the effect of catalytic reaction is excellent, and the catalyst can be directly added into the reactant; and in the production process, a stirred tank reactor or a pipeline-type reactor can be used.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for synthesizing N-isopropylhydroxylamine. Background technique [0002] The molecular formula of N-isopropyl hydroxylamine is (CH 3 ) 2 CHNH(OH), abbreviated as IPHA, is a secondary alkyl hydroxylamine derivative and is a medium-strength organic reducing agent. With its excellent physical and chemical properties, it is widely used as a polymerization inhibitor and terminal polymerization inhibitor for olefin monomers. Although the traditional N, N-diethylhydroxyl (DEHA) and its derivatives have high inhibition efficiency for conjugated olefins and vinyl monomers not only in the liquid phase, but also in the gas phase performance. As a polymerization inhibitor, it has the advantages of high efficiency, non-toxicity, high solubility, easy removal from monomers and convenient use. In addition to the above-mentioned advantages of N,N-diethylhydroxylamine, N-i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C239/10
Inventor 陈培根谭军宋芬吴墨西杨义文张平华朱正颖陈军民
Owner JINING KENDRAY CHEM TECH CO LTD
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