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Preparation method of paranitrobenzoic acid
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A technology of p-nitrobenzoic acid and p-nitrotoluene, which is applied in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as hidden dangers of explosion safety, and achieve low production costs and easy separation Effect
Inactive Publication Date: 2009-09-09
EAST CHINA NORMAL UNIV
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Problems solved by technology
In 2006, Professor She Yuanbin from Beijing University of Technology reported on pages 757-761 of Volume 10 of the internationally renowned journal "Organic Process Research & Development" that metalphthalocyanine was used as a catalyst and molecular oxygen was used as an oxidant to prepare p-nitrobenzoic acid. The rate is 90.4%, but a large amount of volatile organic reagentmethanol is used as a solvent in this process, and there is a safety hazard of explosion in a pure oxygen environment
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Embodiment 1
[0018] a), 0.050g cobaltphthalocyanine and 2.0g p-nitrotoluene were dissolved in 10.0g [HMIM]PF 6 ionic liquid, and add 0.58g NaOH to the reactor, stir and mix evenly, and then fill with 0.5Mpa of oxygen.
[0019] b) Place the reaction kettle treated in the previous step at a temperature of 60°C in a constant temperature water bath for constant temperature reaction for 4 hours. After the reaction is completed, let it cool down to room temperature and then pour out the supernatant, and add 0.5mol / L of dilute HCl solution. Until the solution becomes acidic, the product precipitates out. Filter and dry in vacuo to obtain p-nitrobenzoic acid.
[0020] c), taking the catalytic system for repeated use, no obvious reduction in the catalytic activity of the catalyst was found.
Embodiment 2
[0022] a), 0.150g copper phthalocyanine and 6.0g p-nitrotoluene were dissolved in 6.0g [OMIM] BF 6 ionic liquid, and add 5.25gKOH to the reactor, stir and mix evenly, and then fill with 1.0Mpa of oxygen.
[0023] b) Place the reaction kettle treated in the previous step in a constant temperature water bath at 70°C for 8 hours, let it cool down to room temperature, pour out the supernatant, and add 2mol / L of dilute H 2 SO 4 solution until the solution becomes acidic and the product precipitates. Filter and dry in vacuo to obtain p-nitrobenzoic acid.
[0024] c), taking the catalytic system for repeated use, no obvious reduction in the catalytic activity of the catalyst was found.
Embodiment 3
[0026] a), 0.150g cobalt phthalocyanine and 4.0g p-nitrotoluene are dissolved in 8.5g [HMIM] BF 6 ionic liquid, and add 4.0gKOH to the reactor, stir and mix evenly, and then fill with 1.5Mpa of oxygen.
[0027] b) Place the reactor treated in the previous step in a constant temperature water bath of 90°C to react for 6 hours, let it cool down to room temperature, pour out the supernatant, add 3mol / L dilute HCl solution until the solution becomes acidic, The product precipitated out. Filter and dry in vacuo to obtain p-nitrobenzoic acid.
[0028] c), taking the catalytic system for repeated use, no obvious reduction in the catalytic activity of the catalyst was found.
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Abstract
The invention discloses a preparation method of paranitrobenzoic acid. The method comprises the following steps: adding metalphthalocyanine and hydrophobic ionic liquid at a mass ratio of 1:40-200, nitrotroluene and NaOH or KOH at the mass ratio of 1:1-3 to a reaction kettle, and evenly mixing; charging oxygen at the pressure of 0.5-2.5MPa into the reaction kettle, placing the reaction kettle in water bath with the temperature of 60-100 DEG C for thermostatic reaction for 4-12 hours, and cooling to the room temperature; adding deionized water, stirring and keeping standing for layering, and taking supernatant; adding 0.5-3.0mol / L diluted acid solution to the supernatant until the supernatant is acidic, and separating a product out by precipitation; and obtaining the paranitrobenzoic acid after filtrating and vacuum drying. The preparation method has the advantages of low preparation cost, easy separation of a catalytic system from a reaction system, recycled catalyst, and easy separation of the paranitrobenzoic acid from the system without organic solvent.
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