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A method and device for inert gas-assisted purification of OLED materials or intermediates thereof

An inert gas and intermediate technology, applied in chemical instruments and methods, luminescent materials, organic chemistry, etc., can solve the problems of large surface area, unfavorable acquisition of high-purity OLED intermediates or products, and rapid product precipitation.

Active Publication Date: 2021-11-23
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method often causes the product to precipitate too quickly, forming fine powder crystals with a large surface area, which is easy to adsorb impurities on the surface, which is not conducive to obtaining high-purity OLED intermediates or products.

Method used

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  • A method and device for inert gas-assisted purification of OLED materials or intermediates thereof
  • A method and device for inert gas-assisted purification of OLED materials or intermediates thereof
  • A method and device for inert gas-assisted purification of OLED materials or intermediates thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Purification of small molecule blue light material M1 based on phenanthroimidazole

[0034] Weigh 600mg of the crude product, purchased from Alda New Materials Co., Ltd., dissolve in a mixed solvent of 30ml of dichloromethane and 15ml of methanol, place it in a 50ml vacuum buffer bottle, and connect the air inlet on the left side to the absorber of the sulfur hexafluoride cylinder. The pressure valve is connected in series with the gas flow meter, and the gas outlet on the right side is connected to the oil-sealed gas buffer bottle to prevent sucking back.

[0035] Control the pressure reducing valve and adjust the gas flow rate to v through the gas flow meter 0 =180ml / min ventilation for 30min, and according to v(t)=v 0 *(1+0.25[t / 30]) regulates the gas flow rate, where v(t) is the gas flow rate at t(min), v 0 is the initial flow rate, which is 180ml / min here, and t is the moment, calculated from the start of inflation, and the unit is minute.

[0036] Until the vol...

Embodiment 2

[0040] Purification of small molecule blue light material M2 based on benzyne

[0041] Weigh 500mg of the crude product, purchased from Alda New Materials Co., Ltd., dissolve in a mixed solvent of 15ml of dichloromethane and 20ml of methanol, place it in a 50ml vacuum buffer bottle, and connect the air inlet on the left to the absorber of the sulfur hexafluoride cylinder. The pressure valve is connected in series with the gas flow meter, and the gas outlet on the right side is connected to the oil-sealed gas buffer bottle to prevent sucking back.

[0042] Control the pressure reducing valve and adjust the gas flow rate to v through the gas flow meter 0 =180ml / min ventilation for 0.5h, and according to v(t)=v 0 *(1+0.25[t / 30]) regulates the gas flow rate, where v(t) is the gas flow rate at t(min), v 0 is the initial flow rate, here it is 180ml / min, t is the moment, calculated from the start of inflation, and the unit is minute.

[0043] Until the volume of the solution in th...

Embodiment 3

[0047] Purification of small molecule blue light material M3 based on phenanthroimidazole

[0048]Weigh 800mg of crude product, purchased from Arda New Materials Co., Ltd., dissolve in a mixed solvent of 20ml acetone and 20ml ethanol, place it in a 50ml vacuum buffer bottle, and connect the left air inlet to the pressure reducing valve of the sulfur hexafluoride cylinder The gas flowmeter is connected in series, and the gas outlet on the right is connected to the oil-sealed gas buffer bottle to prevent sucking back.

[0049] Control the pressure reducing valve and adjust the gas flow rate to v through the gas flow meter 0 =270ml / min ventilation for 0.5h, and according to v(t)=v 0 *(1+0.25[t / 30]) regulates the gas flow rate, where v(t) is the gas flow rate at t(min), v 0 is the initial flow rate, here it is 270ml / min, t is the moment, calculated from the start of inflation, and the unit is minute.

[0050] Until the volume of the solution reaches between 20 and 25ml, white c...

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Abstract

The invention belongs to the technical field of organic photoelectric materials, and discloses a method and a device for inert gas-assisted purification of OLED materials or intermediates thereof. The method comprises the following steps: dissolving the crude product to be purified in a solvent, then placing it in a container with an inlet and outlet, feeding inert gas through the inlet, and discharging the gas from the outlet, and when the volume in the container decreases and crystals are precipitated, Continue to feed the inert gas for 0-720min, then stop the gas feeding, keep airtight, stand still, filter with suction, and dry the obtained crystals to obtain the purified OLED material or its intermediate. In the invention, the inert gas sulfur hexafluoride is used as the carrier gas to take away part of the solvent molecules, so that the material is precipitated from the liquid phase, and the grain shape control of the product is realized by controlling the gas flow rate. Sulfur hexafluoride gas has a high density, which can effectively cover the liquid surface and take away solvent molecules.

Description

technical field [0001] The invention belongs to the technical field of organic photoelectric materials, in particular to a method and a device for inert gas-assisted purification of OLED materials or intermediates thereof. Background technique [0002] Organic light-emitting diodes (OLEDs) have attracted extensive attention due to their advantages of flexibility, active light emission, high efficiency, low-voltage drive, and easy fabrication of large-area devices. OLED-related research can be traced back to the 1960s. In 1963, Professor Pope of New York University discovered the electroluminescence phenomenon of organic molecular single crystal anthracene for the first time, and then some single crystal structure materials have electroluminescence properties. However, due to the high driving voltage of the device at that time, it failed to attract widespread attention. It was not until 1987 that Dr. Deng Qingyun and others from Kodak Company of the United States produced OL...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D403/10C07D209/86C07D409/10C09K11/06H01L51/56
CPCC07D403/10C07D209/86C07D409/10C09K11/06C09K2211/1011C09K2211/1029C09K2211/1044C09K2211/1092H10K85/615H10K85/6576H10K85/6572
Inventor 应磊曹镛
Owner CHINA PETROLEUM & CHEM CORP
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