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Method for producing high-purity liquid sulfur trioxide for electronic grade sulfuric acid

A liquid sulfur trioxide, production method technology, applied in the field of electronic chemicals, can solve the problems of raw material purity difference, equipment corrosion, etc.

Active Publication Date: 2022-04-05
湖北兴福电子材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing high-purity liquid sulfur trioxide for electronic grade sulfuric acid with simple and easy control, low production cost and stable product quality, using industrial sulfur trioxide as raw material, from production equipment, production and control methods Innovate to solve the problem of raw material purity difference and impurity separation difficulty, and at the same time solve the problem of equipment corrosion caused by sulfuric acid trioxide environment

Method used

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  • Method for producing high-purity liquid sulfur trioxide for electronic grade sulfuric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Use 99.5% industrial sulfur trioxide with metal ion content (calculated as Fe)>0.05% and sulfur dioxide content>0.4% as raw material, enter the weight removal tower at 35°C, control the liquid level of the weight removal tower at 53%, and reboil The outlet temperature of the device is controlled at 44°C, the best working feed temperature, and the gas outlet temperature at the top of the weight removal tower is controlled at 44°C. The sulfur trioxide in the weight removal tower is azeotropically evaporated by the heater, and the sulfur trioxide is converted into a gaseous state. The liquid form falls back to the bottom of the tower, and at the same time, the liquid in the heavy component is extracted at a volume fraction of 35%, and the rest is heated by the reboiler again and then enters the weight removal tower. The sulfur trioxide at the top of the weight removal tower enters the light removal tower at the dew point temperature. The liquid level in the tower tank of th...

Embodiment 2

[0032]Use 99.4% industrial sulfur trioxide with metal ion content (calculated as Fe) > 0.06%, and sulfur dioxide content > 0.5% as raw material, enter the weight removal tower at 36°C, control the liquid level of the weight removal tower at 63%, and reboil The outlet temperature of the device is controlled at 46°C, and the gas outlet temperature at the top of the weight removal tower is controlled at 45°C. The sulfur trioxide in the weight removal tower is azeotropically evaporated by the heater, and the sulfur trioxide is converted into a gaseous state, and the heavy components fall back to the bottom of the tower in liquid form. At the same time, the liquid in the heavy component is produced with a volume fraction of 36%, and the rest is heated by the reboiler again and then enters the de-weighting tower. The liquid level in the tower tank of the light removal tower is controlled at 65%, the outlet temperature of the heater is controlled at 38°C, and the gas outlet temperatur...

Embodiment 3

[0034] Use industrial sulfur trioxide with 99.3%, metal ion content (calculated as Fe)>0.07%, and sulfur dioxide content>0.5% as raw material, enter the weight removal tower at 36°C, control the liquid level of the weight removal tower at 75%, and reboil The outlet temperature of the device is controlled at 48°C, and the gas outlet temperature at the top of the weight removal tower is controlled at 46°C. The sulfur trioxide in the weight removal tower is azeotropically evaporated by the heater, and the sulfur trioxide is converted into a gaseous state, and the heavy components fall back to the bottom of the tower in liquid form. At the same time, the liquid in the heavy component is extracted at a volume fraction of 45%, and the rest is heated by the reboiler again and then enters the de-weighting tower. The liquid level in the tower tank of the light removal tower is controlled at 76%, the outlet temperature of the heater is controlled at 41°C, and the gas outlet temperature a...

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Abstract

The invention discloses a method for producing high-purity liquid sulfur trioxide for electronic-grade sulfuric acid, which comprises the following steps: pumping sulfur trioxide to a heavy component removal tower, obtaining gaseous sulfur trioxide at a constant boiling point, filtering and cooling the sulfur trioxide in sequence, and extracting; the extracted sulfur trioxide enters the middle part of the light component removal tower in a gaseous state, the gaseous sulfur trioxide is subjected to countercurrent flow heat exchange with liquid sulfur trioxide heated by a tower kettle from the middle part of the light component removal tower through a filler, and the sulfur trioxide gas is condensed into a liquid state and is continuously extracted from an outlet of the light component removal circulating pump. Industrial-grade sulfur trioxide is pumped to the heavy component removal tower for boiling point rectification, sulfur trioxide without fuming sulfuric acid enters the sulfur trioxide light component removal tower in a gaseous form and exchanges heat with liquid sulfur trioxide in a countercurrent manner, sulfur trioxide is condensed into liquid, gaseous sulfur dioxide enters a tail gas system from the tower top, liquid sulfur trioxide after light component removal is extracted from an outlet of a light component removal circulating pump, and the liquid sulfur trioxide is recovered from an outlet of the light component removal circulating pump. The content of sulfur trioxide in the prepared high-purity liquid is 99.999%, the content of sulfur dioxide is lower than 2ppm, and the content of total impurities is controlled within 5mu g / g.

Description

technical field [0001] The invention belongs to the field of electronic chemicals, and in particular relates to a device and a method for producing electronic-grade sulfuric acid using high-purity liquid sulfur trioxide. Background technique [0002] Electronic grade sulfuric acid, also known as ultra-pure sulfuric acid, is an ultra-clean and high-purity reagent. It is the most widely used wet electron chemistry in the industry. It is mainly used for cleaning, photolithography, corrosion of silicon wafers, corrosion and cleaning of printed circuit boards, and can effectively remove impurities, inorganic residues and carbon deposits on the wafer. Electronic grade sulfuric acid has been used for cleaning silicon wafers for over 40 years. It is an indispensable key basic chemical reagent in the semiconductor industry. Its purity directly affects the yield of integrated circuits. [0003] my country's electronic grade chemicals started late, and the technology research and in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/90
CPCY02P20/10
Inventor 郭岚峰杨着贺兆波杜林徐昊刘悦介珂平
Owner 湖北兴福电子材料股份有限公司
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