Preparation method of ionic liquid type hydroxylamine salt

A technology of ionic liquid and hydroxylamine salt, which is applied in the preparation of sulfonate, organic chemistry, etc., can solve the problem of difficult recovery of inorganic acid, and achieve the effect of rich variety, environmental friendliness and stable quality

Active Publication Date: 2014-01-29
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process route is simple and easy to operate and easy to operate. It not only obtains environmentally friendly ionic liquid hydroxylamine salt products, but also overcomes the shortcomings of environmental pollution and difficulty in recycling inorganic acids during the use of traditional hydroxylamine inorganic salt products.

Method used

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  • Preparation method of ionic liquid type hydroxylamine salt
  • Preparation method of ionic liquid type hydroxylamine salt
  • Preparation method of ionic liquid type hydroxylamine salt

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Refer to the synthesis method reported in the literature (US5266290, 1993): Weigh 41.0g of hydroxylamine sulfate (0.5mol in terms of hydroxylamine) and dissolve it in 100ml of distilled water (5.56mol), and place the above aqueous solution of hydroxylamine sulfate in a low-temperature constant temperature reactor at -5°C 40g of NaOH solution with a mass percentage of 50% was added dropwise under stirring (among them, the alkali was 0.5mol in terms of hydroxide radicals, and the water was 1.11mol); after the addition was complete, the stirring was continued for 0.1h, and the reaction solution was separated by filtration to obtain The filtrate was 100ml, and the filter cake was washed with 40ml of distilled water, and the combined filtrate and lotion were 140ml in total; in the above combined filtrate and lotion, 0.105g of stabilizer ascorbic acid (0.08% by weight) was added, and the pressure was reduced at 52°C Distill (0.098MPa) and distill for 1h. During this process, t...

Embodiment 2

[0032] Weigh 43.0g of hydroxylamine sulfate (0.52mol in terms of hydroxylamine) and dissolve it in 100ml of distilled water (5.56mol), put the above aqueous solution of hydroxylamine sulfate in a low temperature and constant temperature reactor at 0°C, and add dropwise under stirring a mass percentage of 50% 40g of NaOH solution (among them, the alkali is 0.5mol in terms of hydroxide radicals, and water is 1.11mol); after the addition, continue to stir for 0.1h, filter and separate the reaction solution to obtain 110ml of filtrate, wash the filter cake with 25ml of distilled water, combine the filtrate and washing A total of 135ml of liquid solution; in the above combined filtrate and lotion, add 0.202g of stabilizer ascorbic acid (0.15% by weight), and distill under reduced pressure (0.096MPa) at 54°C for 1.5h, during which the distillate Cool with ice water all the time to obtain 97ml of hydroxylamine aqueous solution distillate. The fraction was determined by the potassium ...

Embodiment 3

[0034]Weigh 41.0g of hydroxylamine sulfate (0.5mol in terms of hydroxylamine) and dissolve it in 70ml of distilled water (3.89mol), put the above aqueous solution of hydroxylamine sulfate in a low temperature and constant temperature reactor at 5°C, and add dropwise under stirring with a mass percentage of 50% 40g of NaOH solution (among them, the alkali is 0.5mol in terms of hydroxide radicals, and water is 1.11mol); after the addition, continue to stir for 0.2h, filter and separate the reaction solution to obtain 75ml of filtrate, wash the filter cake with 25ml of distilled water, combine the filtrate and washing A total of 100ml of solution; in the above combined filtrate and lotion, add 0.102g of stabilizer ascorbic acid (0.10% by weight), and distill under reduced pressure (0.095MPa) at 56°C for 2h, during which the distillate is always Cool with ice water to obtain 50ml of hydroxylamine aqueous solution distillate. The fraction was determined by the potassium permanganat...

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Abstract

The invention discloses a preparation method of an ionic liquid type hydroxylamine salt. The preparation method comprises following steps: (1) preparation of a free hydroxylamine salt aqueous solution, wherein the hydroxylamine salt is delivered into a reactor, deionized water is added for dissolving, alkali lye is added dropwise with stirring, and the solution is subjected to neutralization for 0.05 to 1h; after that the reacted solution is subjected to vacuum filtration so as to obtain a filtrate, a stabilizing agent is added into the filtrate, and the mixture is subjected to reduced pressure distillation so as to obtain a cut fraction which is the free hydroxylamine salt aqueous solution; and (2) preparation of the ionic liquid type hydroxylamine salt, wherein an acid ionic liquid is delivered into a reactor, the free hydroxylamine salt aqueous solution obtained in step (1) is added into the ionic liquid, and the mixed solution is stirred for 0.25 to 4h, and then is subjected to rotary evaporation so as to obtain the white solid ionic liquid type hydroxylamine salt. Process cycle is short, post treatment is simple, clean production can be realized, product yield is high, and quality is stable.

Description

technical field [0001] The invention relates to a preparation method of ionic liquid hydroxylamine salt, specifically a new method for directly neutralizing and replacing inorganic acid in hydroxylamine salt in the existing aqueous solution of hydroxylamine salt and obtaining a target product, which belongs to the technical field of fine chemical products . Background technique [0002] Hydroxylamine is a colorless, odorless, deliquescent white flake or needle crystal with the molecular formula NH 2 Oh. Hydroxylamine monomer is extremely unstable, and pure hydroxylamine crystals decompose rapidly when they are bumped or shaken at room temperature (Chemical Abstracts, 2004 (4): 41-43). Therefore, in the process of production and use, hydroxylamine often exists in the form of inorganic acid salt. At present, the main hydroxylamine salts are hydroxylamine sulfate ((NH 2 Oh) 2 ·H 2 SO 4 ), hydroxylamine hydrochloride (NH 2 OH·HCl), hydroxylamine nitrate (NH 2 OH·HNO 3 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/60C07D233/58C07C309/14C07C303/32C07D213/20
CPCC07C303/32C07D213/04C07D233/58C07D233/60C07C309/14
Inventor 王延吉李志会张东升徐元媛金长青王淑芳赵新强
Owner HEBEI UNIV OF TECH
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