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Green preparation technology of phthalic dicarboxaldehyde

A technology for the preparation of o-phthalaldehyde, which is applied in the field of green preparation technology of o-phthalaldehyde, can solve the problems of low yield of intermediate products, high product cost, and large environmental pollution, and achieve short reaction time and simple preparation process , the effect of high product purity

Active Publication Date: 2013-09-04
XI'AN PETROLEUM UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0019] The purpose of the present invention is to overcome the defects of low intermediate product yield, difficult separation, high product cost, and large chemical environmental pollution in the prior art, and provide a kind of intermediate product with mild reaction conditions, simple preparation process, short reaction time and easy separation of intermediates. Green preparation process of o-phthalaldehyde with high product purity, no pollution and low energy consumption

Method used

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  • Green preparation technology of phthalic dicarboxaldehyde
  • Green preparation technology of phthalic dicarboxaldehyde
  • Green preparation technology of phthalic dicarboxaldehyde

Examples

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Embodiment 1

[0032] Add 0.10mol of 1,3-dihydroisobenzofuran, 0.20mol of hydrogen peroxide, 0.3g of phosphomolybdenum heteropolyacid and 10g of water into the three-necked flask in sequence, put in an electromagnetic stirrer, install a reflux condenser and After the temperature probe, set the reaction temperature to 30°C, ultrasonic power to 200W, and run for 30 minutes. After the reaction is completed, cool down to room temperature, extract with an equal volume of ethyl acetate for 3 times, combine the extracts, and remove the acetic acid in the extract by distillation. Ethyl ester, to obtain the crude product of phthalaldehyde, mix the crude product of phthalaldehyde with the recrystallization solvent petroleum ether according to the mass ratio of 1:3, stir under reflux for 15min, drop to 10°C, and obtain phthalaldehyde by suction filtration For formaldehyde crystals, the phthalaldehyde crystals were placed in a vacuum drying oven with a vacuum degree of 60 Pa and a temperature of 50°C for...

Embodiment 2

[0034] Add 0.10mol of 1,3-dihydroisobenzofuran, 0.20mol of hydrogen peroxide, 0.3g of phosphomolybdenum heteropolyacid and 10g of water into the three-necked flask in sequence, put in an electromagnetic stirrer, install a reflux condenser and After the temperature probe, set the reaction temperature to 35°C, the ultrasonic power to 250W, and run for 30 minutes. After the reaction is completed, cool down to room temperature, use an equal volume of ethyl acetate to extract 3 times, combine the extracts, and remove the acetic acid in the extracts by distillation. Ethyl ester, to obtain the crude product of phthalaldehyde, mix the crude product of phthalaldehyde with the recrystallization solvent petroleum ether according to the mass ratio of 1:3, stir under reflux for 15min, drop to 10°C, and obtain phthalaldehyde by suction filtration For formaldehyde crystals, the phthalaldehyde crystals were placed in a vacuum drying oven with a vacuum degree of 60 Pa and a temperature of 50 °C...

Embodiment 3

[0036] Add 0.10mol of 1,3-dihydroisobenzofuran, 0.26mol of hydrogen peroxide, 0.5g of phosphomolybdenum heteropolyacid, and 10g of water in sequence in the three-necked flask, put it into an electromagnetic stirrer, and install a reflux condenser and a temperature probe. , set the reaction temperature at 40°C, ultrasonic power at 300W, and run for 40min. After the reaction was completed, cool down to room temperature, extract three times with an equal volume of ethyl acetate, combine the extracts, remove ethyl acetate by distillation, and obtain phthalate The crude product of formaldehyde is recrystallized with petroleum ether for the crude product of o-phthalaldehyde, and is vacuum-dried to obtain the product of o-phthalaldehyde (the specific steps are the same as in Example 1), and the yield is 43%. The petroleum ether is reclaimed by distillation, and the petroleum ether recovered reusable.

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Abstract

The invention discloses a green preparation technology of phthalic dicarboxaldehyde, which takes 1, 3 -phthalan as raw material, hydrogen peroxide as an oxidant and immobilized rare earth metal and polyoxometallate (heteropoly acid) as catalysts, and water as solvent, and under the invigorating effect of ultrasonic field, the phthalic dicarboxaldehyde product is obtained through the processing steps of catalytic oxidation, ligarine recrystallization, suction filtration and the like. Compared with the prior art, the green preparation technology provided by the invention has the advantages as followings: the process reaction conditions are mild, the preparation process is simple, raw materials are easy to access, the reaction time is short, the product purity is high, zero contamination, small energy consumption and green economy are achieved, and the green preparation technology facilitates the popularization and the use of phthalic dicarboxaldehyde in the industries such as chemical engineering, medical and the like.

Description

technical field [0001] The content of the invention belongs to the technical field of fine chemicals, and relates to a green preparation process of o-phthalaldehyde. Background technique [0002] O-phthalaldehyde (O-phthalaldehyde OPA) is a kind of important medicine and chemical industry intermediate, since Alfa found that it has good effect aspect the disinfection aspect being used for medical endoscope in 1994, this field carries out OPA disinfection function After more research, it has been developed into a new type of high-efficiency disinfectant and has been certified by the US FDA, and its value has also risen greatly. In recent years, advanced countries such as the United States, Canada, and Japan have gradually replaced the medical disinfectant glutaraldehyde (glutaraldehyde GTA) with o-phthalaldehyde. [0003] At present, there are four main synthetic routes of o-phthalaldehyde: [0004] (1) o-xylene bromination hydrolysis method [0005] It is produced by bromi...

Claims

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Application Information

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IPC IPC(8): C07C47/52C07C45/59
Inventor 唐璇黄风林成西涛
Owner XI'AN PETROLEUM UNIVERSITY
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