Preparation method of ultra-pure sulfuric acid

A sulfuric acid, ultra-pure technology, applied in chemical instruments and methods, sulfur compounds, inorganic chemistry, etc., can solve the problems of high energy consumption, harmful waste gas, inability to effectively remove sulfur dioxide gas, etc. low consumption effect

Active Publication Date: 2016-06-01
JIANGSU DENOIR TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the rectification method consumes a lot of energy and costs, and some impurities are difficult to remove. The waste gas and acid mist produced are harmful to the human body and are not conducive to environmental protection. They are only suitable for small-scale production
The gas absorption method is to purify sulfur trioxide gas, and then absorb it with ultrapure water or wash sulfuric acid to obtain ultra-pure sulfuric acid. This method can effectively avoid the above-mentioned shortcomings of the rectification method, but the existing gas absorption method cannot effectively remove sulfur dioxide. Gas, so that the prepared sulfuric acid contains a certain amount of trace sulfur dioxide impurities, affecting the performance of sulfuric acid

Method used

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  • Preparation method of ultra-pure sulfuric acid
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  • Preparation method of ultra-pure sulfuric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Distillation: Pass the fuming sulfuric acid from the raw material tank 1 into the heat exchanger 2 under the pressure of 0.15 MPa. The heat exchanger 2 is connected with the vaporizer 3, and the water vapor generated in the vaporizer 3 is used as the heating medium. Adjust the flow of water vapor in the vaporizer 3 so that the heating distillation temperature in the heat exchanger 2 is 45°C. Under the action of heat, the sulfur trioxide is partially gasified, and the remaining fuming sulfuric acid is returned to the recovery tank 4, where the trioxide The mass concentration of sulfur is 20%;

[0025] (2) Purification and filtration: the sulfur trioxide gas obtained in step (1) is passed into the separator 5 to remove particulate impurities;

[0026] (3) Separation of sulfur trioxide liquid: the sulfur trioxide gas filtered and removed in step (2) is sequentially passed through a cooler 6 with a temperature of 20-40°C and a condenser 7 with a temperature of 5-15°C fo...

Embodiment 2

[0032] (1) Distillation: Pass the fuming sulfuric acid from the raw material tank 1 into the heat exchanger 2 under the pressure of 0.2 MPa. The heat exchanger 2 is connected with the vaporizer 3, and the water vapor generated in the vaporizer 3 is used as the heating medium. Adjust the flow rate of water vapor in the vaporizer 3 so that the heating distillation temperature in the heat exchanger 2 is 50°C. Under the action of heat, the sulfur trioxide is partially gasified, and the remaining fuming sulfuric acid is refluxed in the recovery tank 4, where the trioxide The mass concentration of sulfur is 20%;

[0033] (2) Purification and filtration: the sulfur trioxide gas obtained in step (1) is passed into the separator 5 to remove particulate impurities;

[0034] (3) Separation of sulfur trioxide liquid: the sulfur trioxide gas filtered and removed in step (2) is first passed into a cooler 6 with a temperature of 20-40°C, and then passed into a condenser 7 with a temperature ...

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Abstract

The invention discloses a preparation method of ultra-pure sulfuric acid. Fuming sulfuric acid is used as a raw material. The preparation method includes following steps: (1), distilling; (2), purifying and filtering; (3), separating sulfur trioxide liquid; (4), second evaporation; (5), multistage absorption; (6), impurity removal through a stripping tower; (7), obtaining a finished product. In the ultra-pure sulfuric acid, concentration of particles greater than or equal to 0.5 um is less than 5 p / ml, concentration of particles greater than or equal to 0.2 um is less than 100 p / ml, content of single metal ions is less than 0.1 ppb, and content of sulfuric dioxide is less than 3 ppm. The preparation method is simple in process and low in energy consumption; the ultra-pure sulfuric acid of ppt grade is obtained through a reasonable purification impurity removal process to obtain sulfur trioxide gaspure and then through multistage absorption and steam stripping, so that content of trace sulfur dioxide impurities in the ultra-pure sulfuric acid is controlled effectively and a foundation is laid for producing new-generation ultra-pure sulfuric acid.

Description

technical field [0001] The invention relates to the technical field of preparation of ultra-pure chemicals, in particular to a method for preparing ultra-pure sulfuric acid with ultra-low sulfur dioxide content. Background technique [0002] Ultra-pure sulfuric acid, also known as high-purity sulfuric acid and electronic-grade sulfuric acid, belongs to ultra-clean and high-purity reagents. It is one of the eight ultra-pure chemical materials commonly used in the semiconductor industry and one of the indispensable key basic chemical reagents in the development of microelectronics technology. The consumption of ultra-pure sulfuric acid ranks first in the IC industry. It is widely used in the assembly and processing of semiconductors and ultra-large-scale integrated circuits. It is mainly used in the diffusion, corrosion, and cleaning of silicon wafers, which can effectively remove impurity particles on the wafers. , inorganic residues and carbon deposits. The purity and clean...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/765
CPCC01B17/7655C01P2006/80
Inventor 阮汝明吴国新徐驰
Owner JIANGSU DENOIR TECH CO LTD
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