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
View PDF3 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Refining method of 4-(4-formylphenoxy)benzaldehyde
  • Refining method of 4-(4-formylphenoxy)benzaldehyde

Examples

Experimental program
Comparison scheme
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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap