A kind of refining method of 4-(4-formylphenoxy)benzaldehyde

A formylphenoxy and purification method technology, applied in the field of purification of 4-benzaldehyde, can solve the problems of inability to meet the purity of electronic-grade products, the purity is difficult to reach more than 99.5%, etc., and achieves easy recycling, low price, and high production efficiency. low cost effect

Active Publication Date: 2021-04-06
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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  • A kind of refining method of 4-(4-formylphenoxy)benzaldehyde
  • A kind of refining method of 4-(4-formylphenoxy)benzaldehyde

Examples

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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 reactor, 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 pure water,...

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 method for refining 4-(4-formylphenoxy)benzaldehyde. The refining method adopts a dilute alkali solution to process the chlorinated alkane solution of the crude product of 4-(4-formylphenoxy)benzaldehyde, then washes with purified water to remove the residual lye, leaves it to stand for liquid separation, and adds Stabilizer, concentrated under reduced pressure to remove chlorinated alkanes, then added alcohol solvent, stirred and heated to dissolve, added purified water, stirred and cooled to crystallize, filtered, washed, dried to obtain 4-(4-formylphenoxy)benzaldehyde finished product. The purity of the 4-(4-formylphenoxy)benzaldehyde product obtained by the present invention can reach more than 99.9%, the yield can reach more than 96%, and the concentration of a single metal ion≤0.5ppm can meet the requirements of electronic grade product standards. The requirements of purity and metal ion concentration have broad application prospects.

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 Patents(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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