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Continuous refinement system and technology of ultra-pure phosphorus oxychloride of 5N grade

A pure phosphorus oxychloride, ultra-high technology, applied in the field of continuous purification system of 5N ultra-high purity phosphorus oxychloride, can solve the problems of high cost, complex process, long continuous purification process route, etc., achieve low cost, The process is simple and easy to operate, and the effect of reducing the probability of production accidents

Active Publication Date: 2015-11-04
JIANGYIN JIANGHUA MICROELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above two purification methods, the addition of complexes is used to remove metal ions in phosphorus oxychloride, which requires strict control of the purity of the added complexing agent raw materials, high cost, and a long and complicated continuous purification process.

Method used

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  • Continuous refinement system and technology of ultra-pure phosphorus oxychloride of 5N grade
  • Continuous refinement system and technology of ultra-pure phosphorus oxychloride of 5N grade

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Such as figure 1 and figure 2 As shown, the continuous purification system of the 5N grade ultra-high purity phosphorus oxychloride of the embodiment comprises a feed storage tank 1, the feed storage tank 1 is communicated with the raw material tundish 2, and the discharge port of the raw material tundish 2 is respectively connected with the refined The feed port of the still 3 is connected with the shell side feed port of the first condenser 4, and the top discharge port of the rectifying still 3 is connected with the tube-side steam feed port of the first condenser 4 through the rectifying tower 5, The shell side discharge port of the first condenser 4 is connected with the feed port of the raw material tundish 2, the tube side condensate discharge port of the first condenser 4 is connected with the finished product collection unit, and the tube side of the first condenser 4 is light The component outlet is connected to the light component processing unit, the heavy...

Embodiment 2

[0039] The difference between Example 2 and Example 1 is that the temperature of the phosphorus oxychloride raw material entering the first condenser as the condensing medium is 60° C.; the operating pressure of the raw material tundish is 0.15 bar.

[0040] The product was detected by ICP-MS, and the content of various metal impurities: Al=10.52ppb, Ag=0.48ppb, As=2.87ppb, Au=0.28ppb, Ba=1.74ppb, Bi=0.25ppb, Ca=13.61ppb, Co= 0.25ppb, Cu=3.34ppb, Fe=7.53ppb, Ga=0.62ppb, Hg=2.82ppb, K=5.2ppb, Li=1.37ppb, Mg=2.47ppb, Mn=1.4ppb, Na=5.95ppb, Ni= =3.68ppb, Nb=1.6ppb, Pb=1.21ppb, Sn=1.1ppb, Sr=0.5ppb, Ti=1.37ppb, Zn=2.17ppb.

Embodiment 3

[0042] The difference between Example 2 and Example 1 is that the temperature of the phosphorus oxychloride raw material entering the first condenser as the condensing medium is 70° C.; the operating pressure of the raw material tundish is 0.2 bar.

[0043] The product was detected by ICP-MS, and the content of various metal impurities: Al=9.53ppb, Ag=0.59ppb, As=3.51ppb, Au=0.6ppb, Ba=1.8ppb, Bi=1.35ppb, Ca=3.85ppb, Co= 0.23ppb, Cu=0.52ppb, Fe=7.41ppb, Ga=0.24ppb, Hg=2.29ppb, K=1.37ppb, Li=3.35ppb, Mg=4.58ppb, Mn=0.57ppb, Na=2.14ppb, Ni= =0.38ppb, Nb=0.74ppb, Pb=2.74ppb, Sn=0.19ppb, Sr=0.1ppb, Ti=0.15ppb, Zn=0.32ppb.

[0044] Considering the heat loss of the material pipeline, the temperature of the raw material tundish needs to be slightly higher than the above-mentioned phosphorus oxychloride feed temperature, the raw material tundish is generally controlled at 70°C, and the product yield is 85%. Phosphorus oxychloride has the highest yield of purified products.

[0045] ...

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Abstract

The invention discloses a continuous refinement system of ultra-pure phosphorus oxychloride of a 5N grade. The continuous refinement system comprises feeding storage tanks, wherein the feeding storage tanks are communicated with a middle raw-material tank; a discharge opening of the middle raw-material tank is connected with a feed opening of a rectification kettle and a shell-side feed opening of a first condenser respectively; a discharge opening in the top end of the rectification kettle is connected with a tube-side steam feed opening of the first condenser through a rectification tower; a shell-side discharge opening of the first condenser is connected with a feed opening of the middle raw-material tank; a tube-side condensate-liquid discharge opening of the first condenser is connected with a finished-product collecting unit; a tube-side light-component discharge opening of the first condenser is connected with a light-component treating unit; a kettle-bottom heavy-component discharge opening of the rectification kettle is connected with a waste-liquid treating unit; a jacket of the raw-material middle tank and a jacket of the rectification kettle are connected with a circular heating unit of heat conducting oil; a vacuum pump for evacuation is arranged in the light-component treating unit. The continuous refinement system is protected by nitrogen. The invention further discloses a continuous refinement technology. The continuous refinement technology is short in engineering, and the purity of obtained products is high.

Description

technical field [0001] The invention relates to the technical field of production of electronic chemicals, in particular to a continuous purification system and process for 5N-grade ultra-high-purity phosphorus oxychloride. Background technique [0002] High-purity phosphorus oxychloride is a dopant for the production of integrated circuits and solar cells, and one of the raw materials for manufacturing optical fiber preforms. Its purity requirement is as high as 4N, that is, the purity is above 99.9999%, especially for large-scale integrated circuits. For phosphorus oxychloride, it is required that the content of individual metal impurities should not exceed 10ppb. [0003] Chinese Patent Publication No. CN101570323 disclosed a "purity of 99.99999% phosphorus oxychloride production method and its device" on November 04, 2009, wherein phosphorus oxychloride was purified by rectification and two-stage quartz sub-boiling distillation Finally, phosphorus oxychloride with a pur...

Claims

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Application Information

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IPC IPC(8): C01B25/10B01D3/14
Inventor 殷福华朱永刚朱龙栾成邵勇赵文虎李英
Owner JIANGYIN JIANGHUA MICROELECTRONICS MATERIAL
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