CN-224207421-U - Device for producing ultrapure phosphane by differential pressure thermal coupling rectification

CN224207421UCN 224207421 UCN224207421 UCN 224207421UCN-224207421-U

Abstract

The utility model provides a device for producing ultrapure phosphane by differential pressure thermal coupling rectification, wherein the top of a first rectifying tower is provided with a first condensation reflux device, the bottom of the first rectifying tower is provided with a first reboiler, the top of a second rectifying tower is provided with a second condensation reflux device, the bottom of the second rectifying tower is provided with a second reboiler, the top of the first rectifying tower is sequentially connected with the second reboiler, the first condensation reflux device and the second rectifying tower through a conveying pipeline, the top of a third rectifying tower is provided with a third condensation reflux device, the bottom of the third rectifying tower is provided with a third reboiler, and the bottom of the second rectifying tower is connected with the third rectifying tower through a conveying pipeline. The top of the third rectifying tower is provided with a diaphragm compressor, normal temperature filling can be guaranteed by lifting the pressure of a product, and meanwhile, an outlet of the diaphragm compressor is connected with the first reboiler B so as to fully utilize the heat of the gas phase at the top of the third rectifying tower.

Inventors

YE RUI
ZHOU XUN
HE ZHAOBO
GONG HAOLEI
YANG ZHUO

Assignees

湖北兴福电子材料股份有限公司
三峡公共检验检测中心

Dates

Publication Date: 20260508
Application Date: 20250506

Claims (10)

1. The device for producing the ultrapure phosphane by differential pressure thermal coupling rectification is characterized by comprising a heavy removal unit, a light removal unit and a product unit; The weight removing unit comprises a first rectifying tower, a first condensing reflux device is arranged at the top of the first rectifying tower, and a first reboiler is arranged at the bottom of the first rectifying tower; the light component removing unit comprises a second rectifying tower, the top of the second rectifying tower is provided with a second condensation reflux device, and the bottom of the second rectifying tower is provided with a second reboiler; The top of the first rectifying tower is sequentially connected with a second reboiler, a first condensation reflux device and a second rectifying tower through a conveying pipeline; the product unit comprises a third rectifying tower, a third condensing reflux device is arranged at the top of the third rectifying tower, and a third reboiler is arranged at the bottom of the third rectifying tower; the bottom of the second rectifying tower is connected with the third rectifying tower through a conveying pipeline.
2. The apparatus for producing ultrapure phosphane by differential pressure thermal coupling distillation according to claim 1, wherein the first condensate reflux is further connected to an upper portion of the first distillation column.
3. The apparatus for producing ultrapure phosphane by differential pressure thermal coupling rectification of claim 1, wherein the first reboiler comprises a first reboiler A and a first reboiler B.
4. The apparatus for producing ultrapure phosphane by differential pressure thermal coupling rectification as claimed in claim 1, wherein the gas phase outlet of the top of the second rectification column is connected with a third reboiler, the third reboiler is connected with a second condensation reflux device, and the second condensation reflux device is connected with the upper part of the second rectification column.
5. The apparatus for producing ultrapure phosphane by differential pressure thermal coupling rectification as claimed in claim 1, wherein the bottom of the second rectification column is connected with a second reboiler through a conveying pipeline, and the second reboiler is connected with the lower part of the second rectification column.
6. The apparatus for producing ultrapure phosphane by differential pressure thermal coupling rectification as claimed in claim 2, wherein the top of the third rectification column is connected with a diaphragm compressor, the diaphragm compressor is connected with a first reboiler B, and the first reboiler B is connected to a third condensate reflux unit.
7. The apparatus for producing ultrapure phosphane by differential pressure thermal coupling distillation according to claim 6, wherein the third condensate reflux is connected in part to the upper portion of the third distillation column and in part to the product charge cylinder zone.
8. The apparatus for producing ultrapure phosphane by differential pressure thermal coupling rectification as claimed in claim 1, wherein the bottom of the third rectification column is respectively connected with a third reboiler and a byproduct tank via a conveying pipeline, and the third reboiler is connected with the lower part of the third rectification column.
9. The apparatus for producing ultrapure phosphane by differential pressure thermal coupling distillation as recited in claim 1, wherein the bottom of the first distillation column is connected to the byproduct tank via a transfer line.
10. The apparatus for producing ultrapure phosphane by differential pressure thermal coupling rectification as recited in claim 8, wherein the byproduct tank is connected with a byproduct filling steel cylinder, and a liquid nitrogen cylinder is arranged outside the filling steel cylinder.

Description

Device for producing ultrapure phosphane by differential pressure thermal coupling rectification Technical Field The utility model relates to the technical field of purification and detection of electronic grade special gas, in particular to a device for producing ultrapure phosphane by differential pressure thermal coupling rectification. Background Electronic grade phosphine, which is an indispensable key electron gas in the semiconductor process, has extremely high technical threshold and takes the leading position in similar products. It plays an important role in the core processes of ion implantation, doping, etc. Phosphine is a key raw material for chemical vapor deposition of GaAs and InAIP in the LED industry, particularly during epitaxial growth of GaAs-based LEDs. In addition, it is also considered a core N-type dopant source in semiconductor device fabrication. Furthermore, phosphine is widely used in various fields such as chemical vapor deposition of polysilicon, epitaxial growth of GaP materials, ion implantation process, MOCVD process, and preparation of phosphorosilicate glass passivation film. The influence of the electronic-grade phosphine is not limited to the process, and plays a role in various high-tech fields such as chips, integrated circuits, liquid crystal displays, photovoltaics, aerospace, national defense and the like, so that the irreplaceable important position of the electronic-grade phosphine is highlighted. Differential pressure thermal coupling rectification is a thermal coupling rectification process, which enables the temperature of the top of a conventional rectifying tower to be higher than the temperature of the bottom of a depressurization rectifying tower by selecting proper operating pressure. Therefore, the steam at the top of the conventional rectifying tower can be used as a heat source of the depressurization rectifying tower, and the process realizes the heat coupling between part or all of the condensers at the top of the conventional rectifying tower and the load of the reboiler at the bottom of the depressurization rectifying tower, so that the heat loss is reduced. CN 214287448U discloses a phosphine gas purifying device, which is used for purifying byproduct phosphine gas in the sodium hypophosphite production process, but the device is difficult to purify to obtain electronic grade phosphine. CN 117339340A discloses an electronic grade phosphine purification system and method, and the rectification towers are not subjected to heat integration, so that excessive steam is consumed at the bottom of the tower, excessive electric quantity is consumed at the top of the tower, and the operation cost is high. Disclosure of Invention The utility model aims to provide a device for producing ultrapure phosphane by differential pressure thermal coupling rectification, which aims to solve the problems of high energy consumption and high operation cost of a phosphine purification system in the prior art. In order to solve the technical problems, the invention provides a method for producing ultrapure phosphane by differential pressure thermal coupling rectification, which comprises a heavy removal unit, a light removal unit and a product unit, wherein the heavy removal unit comprises a first rectification tower, the top of the first rectification tower is provided with a first condensation reflux device, the bottom of the first rectification tower is provided with a first reboiler, the light removal unit comprises a second rectification tower, the top of the second rectification tower is provided with a second condensation reflux device, the bottom of the second rectification tower is provided with a second reboiler, the top of the first rectification tower is connected with the middle part of the second rectification tower through a conveying pipeline, the product unit comprises a third rectification tower, the top of the third rectification tower is provided with a third condensation reflux device, the bottom of the third rectification tower is provided with a third reboiler, and the bottom of the second rectification tower is connected with the third rectification tower through a conveying pipeline. Further, the high-temperature gas phase at the top of the first rectifying tower firstly enters the second reboiler to serve as a heat source, then enters the first condensation reflux device, one part of the gas phase is used as reflux of the first rectifying tower after being cooled by the heat conducting oil, and the other part of the gas phase is used as feed of the second rectifying tower, so that the heat of the gas phase at the top of the tower is fully utilized, and the steam consumption of the second reboiler and the heat conducting oil consumption of the first condensation reflux device are saved. Further, the high-temperature gas phase at the top of the second rectifying tower firstly enters the third reboiler to serve as a heat source, then enters the secon