Clean chlorobenzene liquid phase nitration method having superior para-selectivity
A green production and selective technology, applied in the direction of nitro compound preparation, chemical recovery, organic chemistry, etc., can solve the problems of industrial application limitations, accelerated inactivation speed, poor thermal stability, etc., to prevent pollution, separate Ease of use and the effect of a small amount of catalyst
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
Example
[0023] Comparative example 1
[0024] Add 15ml of chlorobenzene into the reaction vessel containing 50ml of carbon tetrachloride solvent, stir and mix at a temperature of 10~15℃, slowly add 25ml of 66.5% (weight) nitric acid dropwise, and add 2gWO after the addition is complete 3 / ZrO 2 Solid super acid catalyst, heated to 60°C and stirred at constant temperature for 6h. After the reaction is over, cool to room temperature, filter to recover the catalyst and separate the organic phase, use 5.0% (weight) NaHCO 3 The aqueous solution and water are washed to near neutrality, the solvent is recovered by distillation and then dried and dehydrated to obtain the product nitrochlorobenzene.
[0025] According to the gas chromatographic analysis result, the mononitrate product yield was 82.9%, and the adjacent ratio was 26:74% (weight).
[0026] It can be seen that under the same conditions, the yield is less than 91.5% without adding acetic anhydride, a water absorbent.
Example
[0027] Comparative example 2
[0028] Add 15ml of chlorobenzene and 20ml of acetic anhydride into the reaction vessel containing 50ml of carbon tetrachloride solvent, stir and mix at a temperature of 10~15℃, slowly add 25ml of 66.5% (weight) nitric acid dropwise, after the addition is complete The temperature was increased to 60°C and the reaction was stirred at a constant temperature for 6 hours. After the reaction is over, cool to room temperature, separate the organic phase, and use 5.0% (weight) NaHCO 3 The aqueous solution and water are washed to near neutrality, the solvent is recovered by distillation and then dried and dehydrated to obtain the product nitrochlorobenzene.
[0029] According to the gas chromatographic analysis result, the yield of mononitrate product was 6%, and the adjacent ratio was 35:65% (weight).
[0030] It can be seen that under other conditions are the same, WO is not used 3 / ZrO 2 The solid super acid catalyst has extremely low yield and cannot be u...
PUM
Abstract
Description
Claims
Application Information
- R&D Engineer
- R&D Manager
- IP Professional
- Industry Leading Data Capabilities
- Powerful AI technology
- Patent DNA Extraction
Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.
© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com