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Pre-purification method before sublimation and purification of OLED (organic light emitting diode) material

A pre-purification, pure water technology, applied in organic chemical methods, chemical instruments and methods, hydrocarbon purification/separation, etc., can solve problems such as low recovery rate, unstable quality, process defects, etc., to improve efficiency and facilitate industrialization Production, the effect of reducing the workload

Active Publication Date: 2015-03-25
YANTAI DERUN LIQUID CRYSTAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to achieve high-purity electronic-grade chemicals that meet the requirements of OLED devices, multiple sublimation purification steps have to be adopted, resulting in low recovery rates and unstable quality.
There are serious design deficiencies or process defects

Method used

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  • Pre-purification method before sublimation and purification of OLED (organic light emitting diode) material
  • Pre-purification method before sublimation and purification of OLED (organic light emitting diode) material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Pre-purification of 9-(2-naphthyl)-10-[4-(1-naphthyl)phenyl]anthracene (NNPA) compound:

[0046] Step a:

[0047] In the there-necked flask, add NNPA crude product 100g, add tetrachloroethane 1500ml, start stirring, and heat; When stirring 2h, when the temperature rose to 105 ° C, the NNPA crude product was all dissolved, and kept this temperature and stirred for 30min.

[0048] Step b:

[0049] When the temperature drops to room temperature, pour the solution into a separatory funnel, add 1000ml of high-purity water, stir and wash for 10 minutes, let stand for 10 minutes, and separate the liquid; then add 1000ml of high-purity water, stir and wash for 10 minutes, stand for 10 minutes, and separate the liquid; repeat this again 7 times; from the 7th time onwards, the resistivity of the washing solution was continuously measured at the level of 8.5 MΩ·cm.

[0050] step c:

[0051] Under the protection of inert gas Ar, the solution obtained in step b was dehydrate...

Embodiment 2

[0055] Pre-purification of N, N-bisnaphthyl-N, N-bisphenyl-1, 1-bisphenyl-1, 1-biphenyl-4, 4-diamine (NPB) compounds:

[0056] The prepurification process is the same as Example 1, except that the NNPA raw material in step a is replaced by NPB, and tetrachloroethane is replaced by dichloromethane, the mass volume ratio of NPB / dichloromethane is 1 / 12, and other steps are similar , will not be repeated.

Embodiment 3

[0058] Pre-refining and purification of 2, 9-dimethyl-4, 7-diphenyl-1, 10-phenyline (BCP) compounds:

[0059] The prepurification process is the same as in Example 1, except that the NNPA raw material in step a is replaced by BCP, tetrachloroethane is replaced by chloroform, and the mass volume ratio of NNPA / tetrachloroethane is replaced by 1 / 15 The mass-volume ratio of BCP / trichloromethane is 1 / 10, and other steps are similar and will not be repeated.

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Abstract

A pre-purification method before sublimation and purification of an OLED material, which is to dissolve the crude OLED material by adding an organic solvent, separate the dissolved solution, then dehydrate the solution, then carry out vacuum distillation, recrystallization, and recrystallization The system is subjected to vacuum filtration, and the obtained filter cake is introduced into a clean room to dry, and a series of processes such as drying and packaging of the filter cake are completed. The present invention starts from the crude product to be sublimated to control the numerous impurities, metal ions, non-metal ions, etc. brought in from the raw material, thereby avoiding the adoption of multiple sublimation purification steps in order to meet the purity requirements of the OLED material during the sublimation process , which greatly improves the recovery rate of products and saves time.

Description

technical field [0001] The present invention relates to a pre-purification method before sublimation and purification of OLED materials, more specifically, before the sublimation and purification of OLED materials, the method of pre-purification is used to reduce the trace ions existing in OLED materials, and by strictly controlling the quality of raw materials, further To improve the efficiency of the subsequent sublimation process and product quality, and reduce waste, it belongs to the technical field of electronic grade compound preparation. Background technique [0002] After Dr. Deng Qingyun published the world's first small molecule, double-layer structure electroluminescent device (Organic light-emitting diode, OLED) in 1987, OLED relied on its unique self-luminescence, wide viewing angle, high contrast, and fast response Features such as speed and thickness of a few millimeters (mm) have become one of the new display technologies that everyone is looking forward to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/84C07C211/58C07C211/55C07D487/22C07D215/30C07D271/107C07F5/06C07C7/00C07C15/28C07D471/04C07D235/18C07F15/00C07B63/00
Inventor 刘鑫勤李强孙伟臧崇琴于青春
Owner YANTAI DERUN LIQUID CRYSTAL MATERIALS
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