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Electronic grade phosphorane purification system and processing method

A processing method and electronic-grade technology, applied in the field of purification systems, can solve the problems of reducing the downstream processing load and affecting the purity of phosphine, and achieve the effect of reducing the gas-liquid contact time and improving the purity

Active Publication Date: 2018-11-16
南京佳华科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is in order to solve that above-mentioned prior art does not go out hydrogen sulfide and carbon dioxide influence follow-up phosphine purity, and organic amines such as MDEA are to H in the process of going out acid gas. 2 S and CO 2 There is a problem of selective absorption, and an electronic grade phosphine purification system integrating absorption, desorption, condensation, compression, adsorption and rectification is provided, based on the fact that the azeotropic temperature of hydrogen sulfide and impurities is close to the product phosphine, while carbon dioxide Based on the principle of low boiling point of difficult-to-separate ethane, all hydrogen sulfide and part of carbon dioxide are selectively absorbed by controlling the number of theoretical plates, and then the unabsorbed carbon dioxide and ethane are azeotropically removed from the top of the rectification tower through rectification. The purification system further purifies the phosphine with a purity of 98%wt to obtain phosphine with the content of all impurities ≤ 100ppb, which not only increases the yield from the existing 85% to over 95%, but also increases the purity from 6N to 7N, thus reducing downstream processing load

Method used

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  • Electronic grade phosphorane purification system and processing method
  • Electronic grade phosphorane purification system and processing method
  • Electronic grade phosphorane purification system and processing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] like figure 1 As shown, a purification system of electronic-grade phosphine includes an absorption tower 1, a condenser 2, a gas-liquid separation tank 3, a desorption tower 4, a desorption tower top condenser 5, a reboiler 6, a heat exchanger 7, Compressor 8, adsorption system, light removal rectification tower 10, light removal rectification tower overhead condenser 11, light removal rectification tower kettle reboiler 12, heavy weight removal rectification tower 13, heavy weight rectification tower Top condenser 14 and reboiler 15 of heavy-removing rectification column tower kettle; Described absorption tower 1 is provided with the lower part air inlet that is used to pass into phosphine raw material, upper absorption liquid inlet, tower bottom liquid outlet, tower top Gas outlet; the top gas outlet of the absorption tower 1 is connected to the condenser 2, the non-condensable gas outlet of the condenser 2 is connected to the air inlet of the compressor 8, and the co...

Embodiment 2

[0056] like figure 1 As shown, a purification system of electronic grade phosphine includes an absorption tower 1, a condenser 2, a compressor 8, an adsorption system, a light removal rectification tower 10, a light removal rectification tower top condenser 11, a light removal rectification tower Distillation column tower kettle reboiler 12, weight-removing rectification tower 13, weight-removing rectification tower overhead condenser 14 and weight-removing rectification tower tower kettle reboiler 15; Described absorption tower 1 is provided with for feeding The lower air inlet of the phosphine raw material, the upper absorption liquid inlet, the liquid outlet at the bottom of the tower, and the gas outlet at the top of the tower; the gas outlet at the top of the absorption tower 1 is connected to the condenser 2, and the non-condensable gas outlet of the condenser 2 It is connected with the air inlet of compressor 8, and the condensate reflux outlet of condenser 2 is connect...

Embodiment 3

[0058] like figure 1 As shown, a purification system of electronic grade phosphine includes an absorption tower 1, a condenser 2, a compressor 8, an adsorption system, a light removal rectification tower 10, a light removal rectification tower top condenser 11, a light removal rectification tower Distillation column tower kettle reboiler 12, weight-removing rectification tower 13, weight-removing rectification tower overhead condenser 14 and weight-removing rectification tower tower kettle reboiler 15; Described absorption tower 1 is provided with for feeding The bottom air inlet and the top gas outlet of the phosphine raw material are filled with zinc oxide or iron oxide in the absorption tower 1; the tower top gas outlet of the absorption tower 1 is connected with the air inlet of the compressor 8; The outlet of the compressor 8 is connected to the inlet of the adsorption system, the adsorption system includes two parallel adsorption towers 9, the adsorption towers 9 are fil...

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PUM

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Abstract

The invention discloses an electronic grade phosphorane purification system. The electronic grade phosphorane purification system comprises an absorbing tower, a compressor, an adsorption system, a light removal rectifying tower, and a heavy removal rectifying tower. The invention also discloses an electronic grade phosphorane processing method. The method comprises the following steps: a phosphorane raw material is introduced in the tower from bottom of the absorbing tower, realizes counter-current contacting with absorption liquid from down to up, and the whole hydrogen sulfide and carbon dioxide accounting for 10-40% of that of total amount are absorbed; gas at the top of the absorbing tower is compressed through a compressor and is introduced to the adsorption system, and passes through an adsorbent layer for absorbed dehydration from up to down; the gas through the absorbed dehydration is introduced to the light removal rectifying tower for rectification, a light component is discharged from the top of the light removal rectifying tower to a condenser at the top of the light removal rectifying tower, a heavy component is introduced to the heavy removal rectifying tower for rectification, the light component is discharged from the top of the tower and is discharged to the condenser at top of the heavy removal rectifying tower, and noncondensable gas at the top of the condenser is a phosphorane finished product. The phosphorane purification system takes amine liquid as absorption liquid, and the purity of the obtained phosphorane is greatly increased, which can achieve 7N.

Description

technical field [0001] The invention relates to a purification system for electronic grade phosphine and a treatment method for phosphine based on the purification system. Background technique [0002] Phosphine (PH 3 ) and arsine (AsH 3 ) are similar in physical properties, both are important N-type doping sources in semiconductor manufacturing, and are also used in ion implantation processes, epitaxial GaP materials, polysilicon chemical vapor deposition, etc., and are extremely important electronic special gases. In addition, they are also widely used in solar cells, food fumigation and other fields. [0003] The synthesis methods of phosphine mainly include chemical method, electrolysis method and microwave method, but no matter which kind of synthesis process will produce unnecessary impurities. At present, the purity of domestically synthesized phosphine after pretreatment is 98-99%, and the impurities contained in it are for N 2 , O 2 , CO, CH 4 , CO 2 、SiH 4 ...

Claims

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Application Information

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IPC IPC(8): C01B25/06
CPCC01B25/06
Inventor 赵怡谢佳华侯文贵
Owner 南京佳华科技股份有限公司
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