Unlock instant, AI-driven research and patent intelligence for your innovation.

Apparatus and process for vacuum sublimation

a vacuum sublimation and vacuum technology, applied in the direction of sublimation, separation processes, disinfection, etc., can solve the problems that the purification of chemicals cannot be realized through distillation process, the purification of chemicals cannot be achieved through distillation process, and the products with extremely high purity cannot be obtained under a strictly controlled operation environment to produce high quality electronic components. , to achieve the effect of high efficiency, high purity products, and appropriate product purity

Inactive Publication Date: 2008-02-21
IND TECH RES INST
View PDF1 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The apparatus achieves high purity products by maintaining precise temperature and vacuum conditions, allowing for efficient sublimation and condensation, and enabling large-scale production of high purity chemicals with improved yield and reduced contamination, meeting the demands of commercial operations.

Problems solved by technology

Some chemicals cannot be purified via distillation process since their melting temperature is higher than their decomposition temperature.
Products with extremely high purity can only be obtained under a strictly controlled operation environment to produce high quality electronic components.
The purification of these chemicals cannot be realized through distillation process since their melting temperature is higher than their decomposition temperature.
Although the earlier approach of promoting sublimation vapor with noble gases could lower the requirements on the vacuum degree of the system, but the residual substances that cannot be sublimated in the sublimation materials have low apparent density so that they are easy to flow with noble gases, which resulting in products that are contaminated by flowing residues.
Otherwise, these materials can not be evaporated.
If the pressure of system were too high, the vapor from the sublimation process would collide with the residual air in the system, causing the sublimated materials to fall back into the evaporation tank and creating partial vaporization-condensation circulation, thus resulting in difficulties with product output.
Recently, with the continuously increasing demand for such high purity chemicals, materials produced by small-scale purification apparatuses can no longer meet the demand because of their quality difference between each product group and limited productivity.
How to obtain high purity sublimated products from mass production is the main challenge of these apparatuses.
This process is usually not applied to the purification of the chemicals with low vapor pressure, such as CuPc, since products are easily contaminated by flowing residues and high vacuum environment cannot be realized.
However, materials are likely to be spattered, thus causing contamination on products during the mixing process, and products thereof are also difficult to collect.
However, such process cannot apply to mass production due to its poor heating efficiency and incapability to reach the required sublimation temperature (500° C.).
This particular heating process is likely to produce uneven temperature on plate surfaces, thus making the purity of products harder to improve.

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
  • Apparatus and process for vacuum sublimation
  • Apparatus and process for vacuum sublimation
  • Apparatus and process for vacuum sublimation

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0050] Place 250 grams of Alq3 in the evaporation region of the vertical sublimation purification apparatus, close the sealing cap of the pipe, extract air until vacuum degree reaches 3.2×10−5 mbar, heat the heating evaporation device and maintain its temperature at 350° C., maintain the temperature of the condensation device at 260° C., maintain the temperature of the vapor channel incubating device at 330° C., maintain the temperature of the product incubating device at 120° C., and turn on the product scratching device at a regular time interval during the condensation process. When sublimation has completed, pressure has dropped to the initial value, and all heating evaporation and incubating devices have been turned down, 170.5 g of products and 79.1 g of residues can be collected after cooling, achieving 68.2% yield after sublimation.

example 2

[0051] Place 200 grams of NPB in the boat shaped material carrier of the vertical sublimation purification apparatus, place the material carrier at the center of the sublimation channel body, twist and tighten the two end pipes until they are sealed, extract air by connecting the end pipe at the air extraction end with the vacuum system until the vacuum degree reaches 4.5×10−6 mbar, raise the temperature of the center in the heating evaporation device and maintain it at 330° C., and maintain the exterior temperature at 220° C. After three hours of sublimation, 147.0 g of products and 52.4 g of residues can be retrieved, achieving 73.5% yield after sublimation.

example 3

[0052] Place 330 grams of CuPc in the boat shaped material carrier of the vertical sublimation purification apparatus, place the material carrier at the center of the sublimation channel body, twist and tighten two end pipes until they are sealed, extract air by connecting the end pipe at the air extraction end with the vacuum system until vacuum degree reaches 9.2×10−6 mbar, raise the temperature of the center in the heating evaporation device and maintain it at 600° C., and maintain the exterior temperature at 500° C. After sublimation, 241.8 g of products and 84.7 g of residues can be retrieved, achieving 73.2% yield after sublimation.

[0053] In summary, the sublimation purification apparatuses and processes of the present invention have clear advantages compared to the well-known ones. It provides convenient operational processes and meets the requirement of mass production with its improved apparatuses. In addition, the apparatus is capable of sustaining appropriate product pur...

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

PropertyMeasurementUnit
temperatureaaaaaaaaaa
vapor pressureaaaaaaaaaa
sublimation temperatureaaaaaaaaaa
Login to View More

Abstract

A vertical and a horizontal vacuum sublimation apparatus with high efficiency and processes thereof are provided, especially for the materials having high melting point and low vapor pressure. The vertical sublimation purification apparatus comprises a sublimation channel body, a material rack, a heating evaporation device, a condensation device, an incubating device and a product scratching device. The horizontal sublimation purification apparatus comprises a sublimation channel body, a material carrier, a heating evaporation device and two end pipes. The apparatuses of the present invention can be applied on high purity chemicals from mass production, and are capable of sublimating and purifying OLED illumination layer materials including ALq3, NPB and CuPc, which have high melting temperature and low vapor pressure.

Description

[0001] This application is a divisional application of pending U.S. application Ser. No. 10 / 660,715 filed Sep. 12, 2003.BACKGROUND OF THE INVENTION [0002] 1. Field of the Invention [0003] The present invention provides a vertical and a horizontal vacuum sublimation apparatuses with high efficiency and processes thereof, which can be applied on high purity chemicals from mass production. [0004] 2. Description of Related Art [0005] With the development of IT and electrical industries, the requirements for the quality of electronic components are continuously rising. The purity of the chemicals used in electronic components is the main quality-affecting factor. Some chemicals cannot be purified via distillation process since their melting temperature is higher than their decomposition temperature. Sublimation purification is one of the processes for obtaining high purity chemicals. It can be applied to chemicals with high melting temperature and sublimation characteristics. It is based...

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(United States)
IPC IPC(8): B01B1/00B01D7/00
CPCB01D7/00
Inventor JANG, SHYUE-MINGYANG, SHENGLIOU, BANG-ICHEN, JUN-YIJEAN, LONG-SHUENN
Owner IND TECH RES INST