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Preparation method for compound-type nitrating agent and application thereof in passivation aromatic ring nitration

A nitrating agent and composite technology, which is applied to the preparation of nitro compounds, catalysts for physical/chemical processes, formation/introduction of nitro/nitroso groups, etc., which can solve the problems of expensive catalysts, increased preparation costs, and passivation of aromatic rings. There are few problems such as nitrification research, and the effects of improving nitrification effect, low cost and environmental protection are achieved.

Active Publication Date: 2019-02-22
浙江工业大学上虞研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the catalyst that this method adopts is expensive, makes preparation cost improve
In the prior art, there are many studies on the nitration of active aromatic rings, but less research on the nitration of passivated aromatic rings

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Dissolve sodium nitrate and bismuth nitrate in deionized water to prepare a mixed solution, then add 1-butyl-3-methylimidazolium hexafluorophosphate, stir and mix evenly, and stir at 60-70°C for 30 minutes , cooled to room temperature after stirring treatment, then added silica sol, the prepared mixed material was transferred to the reactor, and reacted at 120°C for 2 hours. After the reaction was completed, it was filtered at room temperature and dried to obtain component A; Among them, the mass concentrations of sodium nitrate and bismuth nitrate are 30% and 8% respectively; the mass ratio of sodium nitrate, 1-butyl-3-methylimidazolium hexafluorophosphate and silica sol is 1:0.013:8;

[0028] (2) Dissolve tetrabutyl titanate in absolute ethanol, then add sodium dodecylbenzenesulfonate solution with a mass concentration of 5%, and stir in a water bath at 50-60°C for 2 hours after the dropwise addition to obtain Titanium glue; wherein, the mass ratio of tetrabutyl t...

Embodiment 2

[0033] (1) Dissolve sodium nitrate and bismuth nitrate in deionized water to prepare a mixed solution, then add 1-butyl-3-methylimidazolium hexafluorophosphate, stir and mix evenly, and stir at 60-70°C for 80 minutes , cooled to room temperature after stirring treatment, then added silica sol, the prepared mixed material was transferred to the reactor, and reacted at 120°C for 7h, after the reaction was completed, filtered and dried at room temperature to obtain component A; among them, the mixed solution Among them, the mass concentrations of sodium nitrate and bismuth nitrate are 50% and 20% respectively; the mass ratio of sodium nitrate, 1-butyl-3-methylimidazolium hexafluorophosphate and silica sol is 1:0.025:10;

[0034] (2) Dissolve tetrabutyl titanate in absolute ethanol, then add sodium dodecylbenzenesulfonate solution with a mass concentration of 15%, and stir in a water bath at 50-60°C for 3 hours after the dropwise addition to obtain Titanium glue; wherein, the mass...

Embodiment 3

[0039](1) Dissolve sodium nitrate and bismuth nitrate in deionized water to prepare a mixed solution, then add 1-butyl-3-methylimidazolium hexafluorophosphate, stir and mix evenly, and stir at 60-70°C for 40 minutes , cooled to room temperature after stirring treatment, then added silica sol, the prepared mixed material was transferred to the reaction kettle, and reacted at 120°C for 3 hours. After the reaction was completed, filtered at room temperature and dried to obtain component A; wherein, the mixed solution Among them, the mass concentrations of sodium nitrate and bismuth nitrate are 35% and 10% respectively; the mass ratio of sodium nitrate, 1-butyl-3-methylimidazolium hexafluorophosphate and silica sol is 1:0.015:8;

[0040] (2) Dissolve tetrabutyl titanate in absolute ethanol, then add a sodium dodecylbenzenesulfonate solution with a mass concentration of 7%, and stir in a water bath at 50-60°C for 2.2 hours after the dropwise addition to obtain Titanium-containing g...

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PUM

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Abstract

The invention discloses a preparation method for a compound-type nitrating agent. The preparation method specifically comprises the following steps: firstly using sodium nitrate and bismuth nitrate asactive components, using 1-butyl-3-methylimidazolium hexafluorophosphate as a modifier, and using silica sol as a carrier, preparing a component A; using tetrabutyl titanate as a titanium source, using sodium dodecyl benzene sulfonate as a modifier, and using yttrium chloride as an active component, preparing a component B, enabling the component A and the component B to be mixed, and preparing the compound-type nitrating agent. The nitrating agent prepared by the method is good in stability, excellent in mechanical property, and good in nitration effect while used for nitration of a passivation aromatic ring, and capable of effectively improving a yield of a nitration product.

Description

Technical field: [0001] The invention relates to the field of organic synthesis, in particular to the preparation of a composite nitrating agent and its application in passivating aromatic ring nitration. Background technique: [0002] Aromatic nitro compounds prepared by the nitration reaction of aromatic compounds are important intermediates and products of organic chemical industry, and are widely used in dyes, medicines, pesticides and explosives. The electrophilic nitration of aromatic rings is an important method for the preparation of such aromatic nitro compounds. However, this type of nitration method is mainly aimed at activated aromatic rings, such as toluene, aniline and phenol and their derivatives, and the nitration reaction of passivated aromatic rings is relatively received less attention. On the one hand, this is because the nitration reaction of passivated aromatic rings is relatively difficult, mainly relying on the nitration of nitric-sulfur mixed acid, ...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/06C07B43/02B01J21/06
CPCC07B43/02C07C201/08B01J21/063C07C205/06
Inventor 王哲许萌吴仁则李大权陈佳莹
Owner 浙江工业大学上虞研究院有限公司
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