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Refining method of 4-(4-formylphenoxy)benzaldehyde

The technology of a formylphenoxy group and a refining method is applied in the refining field of 4-benzaldehyde, can solve the problems that the purity is difficult to reach more than 99.5%, cannot meet the purity of electronic-grade products, etc., and achieves easy recycling, low production cost, The effect of improving quality

Active Publication Date: 2019-02-12
HEBEI HAILI FRAGRANCES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, a small amount of synthetic raw materials generally remain in 4-(4-formylphenoxy)benzaldehyde prepared by conventional reactions, and 4-(4-formylphenoxy)benzaldehyde is also Self-polymerization may occur or aldol condensation reaction occurs with recrystallization solvent, thereby causing the purity (HPLC) of 4-(4-formylphenoxy)benzaldehyde crude product to be difficult to reach more than 99.5%; In addition, 4-(4 -Formylphenoxy) benzaldehyde crude product also has a small amount of inorganic catalyst residues, and a small amount of metal ions introduced in the raw material, so that the single metal ion in the 4-(4-formylphenoxy) benzaldehyde crude product The concentration is generally above 10ppm, which is far from meeting the requirements of electronic grade products for purity (greater than 99.5%) and metal ion concentration (single metal ion is less than 1ppm)

Method used

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  • Refining method of 4-(4-formylphenoxy)benzaldehyde
  • Refining method of 4-(4-formylphenoxy)benzaldehyde

Examples

Experimental program
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Effect test

Embodiment 1

[0047] A kind of refining method of 4-(4-formylphenoxy)benzaldehyde:

[0048]Step 1. Add 6kg of crude product 4-(4-formylphenoxy)benzaldehyde and 30kg of dichloromethane to a 50L glass reactor equipped with heating mantle, mechanical stirring and reflux condenser, stir to dissolve, then add 0.5wt % sodium hydroxide solution 9Kg, stirred and reacted at 10°C for 30min, stood still for 1h, separated the liquid, transferred the oil layer to a 100L glass reactor, washed with 30kg pure water until neutral, stood still to separate the liquid, and collected the oil phase;

[0049] Step 2. Transfer the obtained oil phase into a 50L glass reactor, add 24mg of potassium carbonate, control the vacuum at -0.099MPa, and the temperature is 50°C, and evaporate the dichloromethane solvent to dryness to obtain a concentrate;

[0050] Step 3: Add 36kg of methanol to the concentrate, heat up to 55°C and stir to dissolve, transfer to a 100L crystallization kettle, keep the temperature at 55°C, add...

Embodiment 2

[0052] A kind of refining method of 4-(4-formylphenoxy)benzaldehyde:

[0053] Step 1. Add 6kg of crude product 4-(4-formylphenoxy)benzaldehyde and 12kg of chloroform to a 50L glass reactor equipped with heating mantle, mechanical stirring and reflux condenser, stir to dissolve, then add 0.2wt % sodium hydroxide solution 3.4Kg, react with stirring at 15°C for 1h, let stand for 1h, separate the liquid, transfer the oil layer to a 100L glass reactor, wash with 30kg of pure water until neutral, let stand to separate the liquid, and collect the oil phase ;

[0054] Step 2. Transfer the obtained oil phase into a 50L glass reaction kettle, add 12mg of sodium carbonate, control the vacuum to -0.08MPa, and the temperature is 30°C, and evaporate the chloroform solvent to dryness to obtain a concentrate;

[0055] Step 3: Add 18kg of ethanol to the concentrate, heat up to 50°C and stir to dissolve, transfer to a 100L crystallization kettle, keep the temperature at 50°C, add 14.4kg of pur...

Embodiment 3

[0057] A kind of refining method of 4-(4-formylphenoxy)benzaldehyde:

[0058] Step 1. Add 6kg of crude product 4-(4-formylphenoxy)benzaldehyde and 24kg of dichloroethane to a 50L glass reactor equipped with heating mantle, mechanical stirring and reflux condenser, stir to dissolve, then add 1wt % sodium hydroxide solution 7.9Kg, stirred and reacted at 30°C for 30min, stood still for 1h, separated the liquid, transferred the oil layer to a 100L glass reactor, washed with 30kg pure water until neutral, stood still to separate the liquid, and collected the oil phase ;

[0059] Step 2. Transfer the obtained oil phase into a 50L glass reaction kettle, add 36mg of sodium hydroxide, control the vacuum at -0.09MPa, the temperature is 40°C, and evaporate the dichloroethane solvent to dryness to obtain a concentrate;

[0060] Step 3: Add 30kg of isopropanol to the concentrate, raise the temperature to 60°C and stir to dissolve, transfer to a 100L crystallization kettle, keep the temper...

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Abstract

The invention relates to the technical field of chemical synthesis and specifically discloses a refining method of 4-(4-formylphenoxy)benzaldehyde. The refining method comprises the following steps: treating a chloralkane solution of a crude product of 4-(4-formylphenoxy)benzaldehyde by using dilute aqueous alkali; washing with purified water to remove residual alkali liquor; standing for liquid separation; adding a stabilizer into the oil phase, and performing reduced-pressure concentration to remove chloralkane; adding an alcohol solvent, and stirring and heating for dissolution; adding purified water, and stirring and cooling for crystallization; filtering, washing and drying to obtain a refined product of 4-(4-formylphenoxy)benzaldehyde. According to the method disclosed by the invention, the purity of the prepared product of 4-(4-formylphenoxy)benzaldehyde can reach 99.9% or more, the yield can reach 96% or more, single metal ion concentration is less than or equal to 0.5 ppm, andthe requirement of the electronic-grade product standard on purity and metal ion concentration can be met; therefore, the product of 4-(4-formylphenoxy)benzaldehyde has a broad application prospect.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for refining 4-(4-formylphenoxy)benzaldehyde. Background technique [0002] 4-(4-formylphenoxy)benzaldehyde, the structural formula is: [0003] [0004] Engineering materials prepared from it are widely used in various fields such as electronics, solar energy, photovoltaic power generation, aviation, and aerospace. Among them, 4-(4-formylphenoxy)benzaldehyde used in the field of electronic technology requires the characteristics of high purity (99.9% content) and low single metal ion concentration (content≤0.5ppm). [0005] At present, a small amount of synthetic raw materials generally remain in 4-(4-formylphenoxy)benzaldehyde prepared by conventional reactions, and 4-(4-formylphenoxy)benzaldehyde is also Self-polymerization may occur or aldol condensation reaction occurs with recrystallization solvent, thereby causing the purity (HPLC) of 4-(4-formylph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/575C07C45/80C07C45/86C07C45/81
CPCC07C45/80C07C45/81C07C45/86C07C47/575
Inventor 张云堂李文革邵帅时红粉
Owner HEBEI HAILI FRAGRANCES CO LTD
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