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Method of preparing phthalic acid by polyacid catalyzed oxidation

A technology of phthalic acid and o-xylene, applied in the field of catalytic chemistry and daily chemical industry, can solve the problems of precursor reagents, limited application, high toxicity, etc., reduce manufacturing costs and the generation of three wastes, and avoid halogens The use of initiators, ease of control and effects of industrial production

Inactive Publication Date: 2019-06-28
上海繁德生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The disadvantage of the above synthesis method is that the reaction conditions are complicated, the use of highly corrosive, highly toxic, and easily poisonous reagents, and the use of precious metal ruthenium as a catalyst limit its industrial application.

Method used

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  • Method of preparing phthalic acid by polyacid catalyzed oxidation
  • Method of preparing phthalic acid by polyacid catalyzed oxidation
  • Method of preparing phthalic acid by polyacid catalyzed oxidation

Examples

Experimental program
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Effect test

Embodiment example 1

[0048] Add 1.0617g (0.01mol) of o-xylene, 1% (0.0076g) of Fe-Anderson type polyoxometalate, 1% (0.00106g) of sodium carbonate additive, and 5equiv (0.3g) of solvent acetic acid Put it into a dry reaction test tube, raise the temperature to 100° C., place the reaction in air, keep the reaction at a pressure (gauge pressure) of 1.0 MPa for 20 hours, and then stop the reaction. The reaction system was extracted 3 times with ethyl acetate, the solvent was removed from the obtained product under reduced pressure, and phthalic acid was separated by column chromatography to obtain 0.8956 g of the product with a yield of 54%.

Embodiment example 2

[0050] 1.0617g (0.01mol) of o-xylene, 1% (0.076g) of Fe-Anderson type polyoxometalate, 1% (0.00106g) of sodium carbonate additive, and 5equiv (3g) of solvent acetic acid into In the hydrothermal reaction kettle lined with polytetrafluoroethylene, pay attention to check whether the equipment is damaged before use, add solvent and raw materials into the hydrothermal reaction kettle container, stir and dissolve, and blow nitrogen into the container for a period of time to make The system is in an inert atmosphere. Tighten the lid of the medium hydrothermal reaction kettle, then add the catalyst and place it in the oven. After the temperature rises to 100°C, connect the oxygen tank so that the pressure (gauge pressure) is about 1.0MPa, and keep it warm for 12 hours. Stop responding. 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, and the obtained product was decompre...

Embodiment example 3

[0052] The o-xylene of 1.0617g (0.01mol), the Fe-Anderson type polyoxometalate catalyst of 1% (0.0076g), the sodium carbonate additive of 1% (0.00106g), the hydrogen peroxide of 30% of 3equiv and Put 5 equiv (0.3g) of solvent acetic acid into a dry and clean pressure-resistant tube, raise the temperature to 100°C, and keep the pressure (gauge pressure) at 1.0MPa for 12 hours, then stop the reaction, and dilute the reaction system with ethyl acetate. Extracted 3 times, the obtained product was desolventized under reduced pressure, separated by column chromatography to obtain phthalic acid, 1.2937 g of the product was obtained, and the yield was 78%.

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Abstract

The invention relates to a method of preparing phthalic acid by Anderson polyacid catalyzed oxidation. The method comprises the following steps: adding phthalic acid, an Anderson polyacid catalyst, anadditive and a solvent into a reactor; magnetically stirring the components in an oxygen atmosphere to react; and fully stirring the mixture for 12-24 hours at a reaction temperature of 100-220 DEG Cto obtain a needed product. The method avoids a reaction condition of using a high corrosion, high toxic and easily drug manufacturing reagent at a high temperature and a high pressure in a conventional synthesizing method and adopts the Anderson polyacid as a catalyst, so that the method has extremely high reaction activity and the needed reaction is mild in condition and environment-friendly. The method is high in specific selectivity, recycable and suitable for industrial production. Hydrogen peroxide, air or oxygen is taken as an oxidizing agent, so that the manufacturing cost and three wastes are reduced, and the environmental pressure is alleviated. The method also has the characteristics of being easy to control and produce industrially.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry, in particular to the catalysis of polyoxometalates, in particular to a method for preparing phthalic acid from o-xylene catalyzed by a heteropolyacid catalyst, and belongs to the field of daily chemical industry. Background technique [0002] Ortho-xylene is a colorless transparent liquid with an odor similar to toluene, with a boiling point of 144.4°C, a flash point of 30°C, a spontaneous ignition point of 463°C, an explosion limit of 1% to 7%, a melting point (°C): -25, and a boiling point (°C ): 144.4, relative density (water=1): 0.88, relative vapor density (air=1): 3.66, saturated vapor pressure (kPa): 1.33 (32°C), heat of combustion (kJ / mol): -4845.3, critical Temperature (°C): 359, critical pressure (MPa): 3.7, octanol / water partition coefficient: 3.12, flash point (°C): 25 (CC), ignition temperature (°C): 463, upper limit of explosion (%): 7. Lower explosion limit (%): 0.9, S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/285C07C63/16B01J31/18
Inventor 余焓方海斌茹诗韩生邱丰
Owner 上海繁德生物科技有限公司
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