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Method for preparation of trimesic acid by catalytic oxidation of Anderson type heteropoly acid

A technology of trimesic acid and catalytic oxidation, which is applied in the field of catalytic chemistry, can solve the problems of cumbersome reaction process and post-treatment, and produce a large amount of three wastes, and achieve the effects of simple operation, reduction of three wastes, and cost reduction

Inactive Publication Date: 2018-09-04
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] When the above synthesis of pyromellitic acid is prepared from pyromellitic dianhydride or phthalic acid diester, the reaction process and post-treatment are cumbersome, and a large amount of waste is required, which brings pressure on environmental protection and life.

Method used

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  • Method for preparation of trimesic acid by catalytic oxidation of Anderson type heteropoly acid
  • Method for preparation of trimesic acid by catalytic oxidation of Anderson type heteropoly acid
  • Method for preparation of trimesic acid by catalytic oxidation of Anderson type heteropoly acid

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Experimental program
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Effect test

Embodiment 1

[0040] 1.2020g (0.01mol) of mesitylene, 0.1201g (0.0001mol) of [NH 4 ] 3 [FeMo 6 o 18 (OH) 6 ]·7H 2 O polyoxometalates, 0.0106g (0.0001mol) of sodium carbonate, and 3ml of solvent acetonitrile are put into a dry reaction test tube, and after the temperature is raised to 100°C, they are reacted in air, and the pressure (gauge pressure) is 1.0MPa After insulated reaction for 12 hours, the reaction was stopped, and the reaction system was extracted 3 times with ethyl acetate. The obtained product was decompressed to remove the solvent, separated by column chromatography to obtain trimesic acid, and the obtained product was subjected to LC-MS to obtain 2.0383 g of the product. The yield is 97%. figure 1 Is [NH in embodiment 1 4 ] 3 [FeMo 6 o 18 (OH) 6 ]·7H 2 Schematic representation of the structure of the O polyoxometallate. figure 2 Is [NH in embodiment 1 4 ] 3 [FeMo 6 o 18 (OH) 6 ]·7H 2 Infrared spectra of O polyoxometalates.

Embodiment 2

[0042] 1.2020g (0.01mol) of mesitylene, 0.1201g (0.0001mol) of [NH 4 ] 3 [FeMo 6 o 18 (OH) 6 ]·7H 2 The sodium carbonate of O polyoxometalate, 0.0106g (0.0001mol), and the solvent acetonitrile of 5ml drop into in the hydrothermal reaction kettle of liner polytetrafluoroethylene, note, check whether there is damage to equipment before use, pour into water Add solvent and raw materials into the thermal reactor container, stir and dissolve, blow nitrogen into the container for a period of time, make the system in an inert atmosphere, tighten the lid of the hydrothermal reactor in use, then add catalyst, place it in an oven, and heat up to After 100°C, connect the oxygen tank to make the pressure (gauge pressure) about 1.0MPa, keep the temperature for 12 hours, and then stop the reaction. After the kettle body was naturally cooled to room temperature, the lid of the kettle was opened, and the reaction system was extracted 3 times with ethyl acetate. The obtained product was d...

Embodiment 3

[0044] 1.2020g (0.01mol) of mesitylene, 0.1186g (0.0001mol) of [NH 4 ] 4 [NiMo 6 o 18 (OH) 6 ]·5H 2 O polyoxometalate catalyst, 0.0106g (0.0001mol) of sodium carbonate, 30wt% hydrogen peroxide of 0.03mol and solvent acetonitrile of 12ml drop into dry and clean pressure-resistant tube, after being heated up to 100 ℃, in Pressure (gauge pressure) is after insulation reaction 12h under 1.0MPa, stop reaction, with ethyl acetate, reaction system is extracted 3 times, the product obtained decompresses and removes solvent, column chromatography separates and obtains trimesic acid, and the obtained product LC-MS was carried out to obtain 2.0383g of the product with a yield of 97%. figure 1 Is [NH in embodiment 1 4 ] 4 [NiMo 6 o 18 (OH) 6 ]·5H 2 Schematic representation of the structure of the O polyoxometallate. figure 2 Is [NH in embodiment 3 4 ] 4 [NiMo 6 o 18 (OH) 6 ]·5H 2 Infrared spectra of O polyoxometalates.

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Abstract

The invention discloses a method for preparation of trimesic acid by catalytic oxidation of Anderson type heteropoly acid. The method comprises the steps of: 1) subjecting mesitylene to oxidation reaction in a solvent under the action of a catalyst, an oxidant and an additive; wherein the catalyst is Anderson type heteropoly acid, and the oxidant is air, oxygen or hydrogen peroxide; 2) at the endof the oxidation reaction, filtering out the catalyst, then adding an extraction solvent and water, and conducting extraction repeatedly to obtain an organic phase and an aqueous phase; and 3) carrying out drying, filtering, concentration and purification treatment on the organic phase in order, thus obtaining trimesic acid. The preparation method provided by the invention has the advantages of simplicity, high yield, green and efficient reaction, mild reaction conditions, and environmental friendliness, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry, relates to the catalytic field of polyoxometalates, and in particular relates to a method for preparing trimesic acid by catalytic oxidation of Anderson type heteropolyacids. Background technique [0002] Catalysis is the most promising and practical research direction in the application of polyoxometalates (also known as polyacids or polyoxometalates, or POMs for short). Polyoxometallates combine the excellent properties of acid-base catalysts, redox catalysts, and metal oxide nanocatalysts, and are considered to be green multifunctional catalysts with wide applications. As early as the beginning of the 20th century, people began to study the catalytic performance of polyacids. So far, eight polyacid catalytic industrialization projects have been successfully developed. [0003] Trimesic acid, molecular weight: 210.1400, white to slightly yellow crystalline powder. Solubility: eas...

Claims

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Application Information

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IPC IPC(8): C07C51/265C07C51/285C07C63/307
CPCC07C51/265C07C51/285C07C63/307
Inventor 余焓张梦齐
Owner SHANGHAI INST OF TECH