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Method for safely preparing pure N, O-dimethylhydroxyamine hydrochloride

A technology of dimethylhydroxylamine hydrochloride and methoxyamine hydrochloride, applied in organic chemistry and other directions, to achieve the effects of accelerating decomposition speed, improving conversion rate and ensuring safety

Inactive Publication Date: 2015-04-01
YANTAI AODONG CHEM MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

We found in the experiment that there is another phenomenon in the result of acidic hydrolysis of ketoxime ether: the hydrolyzate also contains some non-condensable unknown gas

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for safely producing pure N,O-dimethylhydroxylamine hydrochloride, the steps are as follows:

[0020] (1) Take 106g of dried N,O-dimethylhydroxylamine hydrochloride crude product after drying, dissolve it in 500g of water, and detect methoxyamine 5.4% and N,O-dimethylhydroxylamine 94.5% by sampling gas chromatography The mass percentage calculated by the potentiometric titration method is that methoxyamine hydrochloride accounts for 8%, and N, O-dimethyl hydroxylamine hydrochloride accounts for 92%; the calculated sample contains N, O-dimethyl hydroxylamine hydrochloride About 1.0 mol of salt, about 0.1 mol of methoxyamine hydrochloride; add 146g (1.1mol) of 30wt% NaOH solution under ice-water bath conditions, and release methoxyamine and N,O-dimethylhydroxylamine;

[0021] (2) Add 5.2 g of acetone (0.09 mol) to the solution in step (1), stir for 30 min, then add 154 g (1.2 mol) of 30 wt% hydrochloric acid, stir for 6 h at normal pressure and reflux, and discha...

Embodiment 2

[0025] A method for safely producing pure N,O-dimethylhydroxylamine hydrochloride, the steps are as follows:

[0026] (1) Take 110g of dried crude N,O-dimethylhydroxylamine hydrochloride, dissolve it in 500g of water, and detect methoxyamine 6.1% and N,O-dimethylhydroxylamine 93.7% by gas chromatography The mass percentage calculated by the potentiometric titration method is that methoxyamine hydrochloride accounts for 10%, and N, O-dimethyl hydroxylamine hydrochloride accounts for 90%; the calculated sample contains N, O-dimethyl hydroxylamine hydrochloride About 1 mol of salt, about 0.13 mol of methoxyamine hydrochloride; add 160 g (1.2 mol) of 30 wt% NaOH solution under ice-water bath conditions, and release methoxyamine and N,O-dimethylhydroxylamine;

[0027] (2) Add 10 g of methyl ethyl ketone (0.14 mol) to the solution in step (1), stir for 30 min, then add 173 g (1.35 mol) of 30 wt% hydrochloric acid, stir for 6 h under normal pressure and heat to reflux, and discharge ...

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Abstract

The invention relates to a method for safely preparing N, O-dimethylhydroxyamine hydrochloride. The method comprises the steps: dissolving rough N, O-dimethylhydroxyamine hydrochloride into water; feeding an alkaline substance to neutralize to fractionate out methoxyamine and N, O-dimethyl hydroxylamine; then feeding acetone or butanone; preparing ketoxime ethers through acetone or butanone and methoxyamine; then feeding hydrochloric acid; heating and refluxing at a normal pressure to continuously separate out generated non-condensed unidentified gas; performing the operation of distilling off water to replace the refluxing operation after detecting relatively small chromatographic value of methoxyamine in an aqueous liquid; dissolving a water-distilled solid with methyl alcohol; filtering out a methyl alcohol solution for recrystallizing; concentrating and cooling to separate out a crystal; and then centrifuging and drying to obtain the pure N, O-dimethylhydroxyamine hydrochloride. According to the method, ketoxime ethers can be decomposed under an acidic heating condition, so that methoxyamine and N, O-dimethyl hydroxylamine in the heating state are in forms of hydrochloride instead of a free state, and as a result, the safety in production and purification can be ensured.

Description

technical field [0001] The invention relates to compound purification, in particular to a method for safely preparing pure N,O-dimethylhydroxylamine hydrochloride. Background technique [0002] Industrial production of N,O-dimethylhydroxylamine hydrochloride usually first obtains the crude product of N,O-dimethylhydroxylamine hydrochloride with content≤95% (GC detection, impurity is methoxyamine hydrochloride), which The crude product of this kind of purity adopts the technical route of methanol recrystallization to obtain the finished product still content≤95% (GC). [0003] In the case that the recrystallization process scheme is not feasible, the conventional purification scheme is to first dissolve the crude product in water, add alkaline substances to neutralize, distill the aqueous solution of the mixture of methoxyamine and N,O-dimethylhydroxylamine, and then use The N,O-dimethylhydroxylamine fraction is intercepted by the separation method of the rectification tower...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C239/20
Inventor 张震姜伟
Owner YANTAI AODONG CHEM MATERIAL
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