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Preparation method and application of O-benzyl hydroxylamine resin

A technology of benzyl hydroxylamine resin and benzyl hydroxylamine, which is applied in the field of preparation of O-benzyl hydroxylamine resin, can solve problems such as cross contamination, and achieve the effects of cost saving, low energy consumption and simple method

Active Publication Date: 2020-11-10
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above chemical methods need to add other reagents, and may cause cross-contamination, while removing acetaldehyde, other new impurities will also be brought in

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A kind of preparation method of O-benzyl hydroxylamine resin, comprises the steps:

[0032] One, the preparation of O-benzyl acetohydroxylamine resin:

[0033] (1) Add 150g (1.7mol) of ethyl acetate, 50g of water (50mL) and 65g (0.94mol) of hydroxylamine hydrochloride in the 1000mL round bottom flask equipped with condenser, thermometer and stirrer, and Stir and mix evenly at ℃ to obtain a mixed solution; then add dichloromethane to the mixed solution and extract 3 times to obtain acetaminophen dichloromethane solution A (the amount of dichloromethane each time is 120 mL);

[0034] (2) get chloromethylated macroporous styrene-divinylbenzene copolymer 0.7mol and the dichloromethane of 500mL and mix in beaker and carry out swelling 4 hours, after swelling, solid-liquid separation obtains swollen resin B (methyl chloride The content of benzyl chloride in the base macroporous styrene-divinylbenzene copolymer is 12wt%-15wt%);

[0035] (3) Mix and stir the above-mentioned a...

Embodiment 2

[0045] A kind of preparation method of O-benzyl hydroxylamine resin, comprises the steps:

[0046] One, the preparation of O-benzyl acetohydroxylamine resin:

[0047] (1) Add 230g (2.3mol) of ethyl acetate, 50g of water (50mL) and 70g (1.01mol) of hydroxylamine hydrochloride in the 1000mL round bottom flask equipped with condenser, thermometer and stirrer, and at 20 Stir and mix evenly at ℃ to obtain a mixed solution; then add dichloromethane to the mixed solution and extract 3 times to obtain acetaminophen dichloromethane solution A (the amount of dichloromethane each time is 130 mL);

[0048] (2) Get chloromethylated macroporous styrene-divinylbenzene copolymer 0.7mol and the dichloromethane of 300mL and mix in beaker and carry out swelling 3 hours, after swelling, solid-liquid separation obtains swollen resin B (methyl chloride The content of benzyl chloride in the base macroporous styrene-divinylbenzene copolymer is 12wt%-15wt%);

[0049] (3) Mix and stir the above-mention...

Embodiment 3

[0059] A kind of preparation method of O-benzyl hydroxylamine resin, comprises the steps:

[0060] One, the preparation of O-benzyl acetohydroxylamine resin:

[0061] (1) Add 180g (2.07mol) of ethyl acetate, 50g of water (50mL) and 75g (1.08mol) of hydroxylamine hydrochloride in the 1000mL round bottom flask equipped with condenser, thermometer and stirrer, and Stir and mix evenly at ℃ to obtain a mixed solution; then add dichloromethane to the mixed solution and extract 3 times to obtain acetaminophen dichloromethane solution A (the amount of dichloromethane each time is 120 mL);

[0062] (2) Get chloromethylated macroporous styrene-divinylbenzene copolymer 0.7mol and the dichloromethane of 400mL and mix in beaker and carry out swelling 5 hours, after swelling, solid-liquid separation obtains swelled resin B (methyl chloride The content of benzyl chloride in the base macroporous styrene-divinylbenzene copolymer is 12wt%-15wt%);

[0063] (3) Mix and stir the above-mentioned ...

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PUM

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Abstract

The invention discloses a preparation method and application of an O-benzyl hydroxylamine resin. The preparation method of an O-benzyl acetyl hydroxylamine resin comprises the following steps: (1) mixing and stirring ethyl acetate, water and hydroxylamine hydrochloride, and then extracting to obtain a solution A; (2) adding a chloromethylated macroporous styrene-divinyl benzene copolymer into dichloromethane, swelling, and filtering to obtain a resin B; and (3) mixing the solution A and the resin B, adding alkali liquor, and filtering to obtain an O-benzyl acetyl hydroxylamine resin. The preparation method of the O-benzyl hydroxylamine resin comprises the following steps: (1) adding the O-benzyl acetyl hydroxylamine resin into hydrochloric acid, carrying out a reaction, and filtering to obtain an O-benzyl hydroxylamine hydrochloride resin; and (2) adding alkali liquor into the O-benzyl hydroxylamine hydrochloride resin to adjust the pH value, filtering, and washing the filtrate to obtain the O-benzyl hydroxylamine resin. According to the invention, the O-benzyl hydroxylamine resin is used for preparing the aldehyde-free ethanol, so that the energy consumption is low, and cross contamination is avoided; and the O-benzyl hydroxylamine resin disclosed by the invention can be recycled and repeatedly used for preparing aldehyde-free ethanol.

Description

technical field [0001] The invention relates to a preparation method and application of O-benzyl hydroxylamine resin. Background technique [0002] In addition to the daily use of ethanol, aldehyde-free ethanol is mainly used in the fields of medicine (pharmacopoeia) and standard samples. [0003] Traditional formaldehyde-free ethanol preparation methods are mainly divided into physical methods and chemical methods: (1) Physical method (distillation) The preparation process is: the dilute ethanol solution enters the middle part of the light component removal tower, and water is added to the top of the tower to wash the dilute ethanol vapor , acetaldehyde and other low boiling point substances flowing out of the top of the tower, after the ethanol aqueous solution at the bottom of the tower is drawn out, part of it is vaporized and returned to the light component tower, and the other part is sent to the rectification tower. The qualified ethanol is drawn from the upper side o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F8/00C08F8/32C08F8/24C08F212/08C08F212/36C07C29/88C07C31/08
CPCC08F8/00C08F8/32C08F8/24C08F212/08C07C29/88C08F212/36C07C31/08
Inventor 郭建国夏晓涵吕文华吴孝兰
Owner SINOPHARM CHEM REAGENT
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