# US 2014/0191422 A1 · Sublimation method for the purification of organic small molecules

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- Number: US 2014/0191422 A1
- Document ID: US20140191422A1
- Status: Published application
- Kind: A1
- Application number: 14/238,825
- Filed: 2012-08-03
- Published: 2014-07-10
- Earliest claimed: 2011-08-13
- Assignees: Beijing Aglaia Technology Development Co., Ltd.; Guangdong Aglaia Optoelectronic Materials Co., Ltd
- Inventors: Lei Dai; Lifei Cai
- Web page: https://patentgrep.com/patent/US20140191422A1

## CPC

- B01D 7/00: Sublimation (B01D8/00 takes precedence; freeze-drying F26)
- B01D 7/02: Crystallisation directly from the vapour phase (into single crystals C30B23/00)
- C07B 63/00: Purification; Separation (separation of optically-active compounds C07B57/00); Stabilisation; Use of additives
- H10K 71/311: {Purifying organic semiconductor materials}
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C07B: GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR (preparation of carboxylic acid esters by telomerisation C07C67/47; telomerisation C08F)
- H10K: ORGANIC ELECTRIC SOLID-STATE DEVICES

## Abstract

Disclosed is an improved sublimation method for the purification of organic small molecules. The new method features that barriers are applied in the collection region of sublimation tube so that the gas flow path is modified to pass through or bypass the barriers from the heating region to the vacuum pump. The arrangement of the barriers can effectively separate the main product from the impurities. The main product is enriched in a collection region, while the volatile impurities are enriched in an impurity region. This method has been proved to improve the quality of sublimed materials substantially according to the purity measurements and OLED performance tests.

## Claims

### Claim 1

A sublimation purification method of organic small molecules, an organic-small-molecule compound to be sublimed being placed in the heating region of a sublimation tube, and a vacuum pump being started, a temperature gradient being built up by stepwise heating, the main product being enriched in a collection region and the volatile impurities being enriched in an impurity region, the new system comprising barriers fastened in the collection region so that gas is capable of passing through or bypassing the barriers from the heating region to a vacuum pump joint.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the barriers may also be fastened in the impurity region.

### Claim 3 (depends on 1)

The method according to claim 1, wherein the barriers may be semicircular plates and crosswise fastened and staggered on the inner wall of the collection region.

### Claim 4 (depends on 1)

The method according to claim 1, wherein the barriers may be a circular plate with a plurality of through holes, the collection region and/or the impurity region being composed of a plurality of hollow circular cylinders aligned and in close contact with the inner wall of the sublimation tube, a circular plate being fastened in each of the circular cylinder, a particular angle being formed between the axial direction of the circular cylinder and the plane of the circular plate, and the circular cylinder and the circular plate forming a space obstruction unit.

### Claim 5 (depends on 4)

The method according to claim 4, wherein the axial direction of the circular cylinder is perpendicular to the plane of the circular plate.

### Claim 6 (depends on 4)

The method according to claim 4, wherein the through holes are uniformly distributed on the circular plate.

### Claim 7 (depends on 2)

The method according to claim 2, wherein the barriers may be semicircular plates and crosswise fastened and staggered on the inner wall of the collection region.

### Claim 8 (depends on 2)

The method according to claim 2, wherein the barriers may be a circular plate with a plurality of through holes, the collection region and/or the impurity region being composed of a plurality of hollow circular cylinders aligned and in close contact with the inner wall of the sublimation tube, a circular plate being fastened in each of the circular cylinder, a particular angle being formed between the axial direction of the circular cylinder and the plane of the circular plate, and the circular cylinder and the circular plate forming a space obstruction unit.