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A kind of production method of ultra-clean high-purity sulfuric acid

A production method and technology of sulfuric acid, applied in the direction of sulfur trioxide/sulfuric acid, etc., can solve the problems such as very strict requirements on metal impurity content, particle size content and anion content, and the production process cannot meet the requirements, so as to achieve the effect of convenient cleaning and replacement.

Active Publication Date: 2017-07-28
JIANGYIN RUNMA ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ultra-clean and high-purity sulfuric acid used in the microelectronic chemical industry has very strict requirements on the content of metal impurities, particle size and anion content. It has been raised from the previous ppm limit to the current ppb limit, or even the ppt limit. There are also clear requirements for the dust particles in the dust, and the existing production process can no longer meet the requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of production method of ultra-clean high-purity sulfuric acid, described method step is as follows:

[0031] (1) Impurity removal: inject industrial-grade sulfuric acid into the treatment tank, add impurity removal agent under mechanical stirring, and filter after standing. The impurity remover is KMnO 4 and K 2 S 2 o 8 A mixture of 3:1 by weight, designed to remove difficult-to-remove impurities such as arsenic in sulfuric acid through redox reactions.

[0032] (2) Rectification: Introduce the filtrate in step (1) into the continuous rectification device through negative pressure, and when the liquid level is slightly higher than the heating furnace wire, conduct electric heating for continuous rectification; feed 1.8L each time. The continuous rectification device is made of stainless steel lined with anti-corrosion material.

[0033] (3) Fractional distillation: the middle distillate in step (2) is collected, and the distillate temperature ranges from 332...

Embodiment 2

[0046] A kind of production method of ultra-clean high-purity sulfuric acid, described method step is as follows:

[0047] (1) Impurity removal: inject industrial-grade sulfuric acid into the treatment tank, add impurity removal agent under mechanical stirring, and filter after standing. The impurity remover is KMnO 4 and K 2 S 2 o 8 The mixture, with a weight ratio of 4:1, is designed to remove difficult-to-remove impurities such as arsenic in sulfuric acid through redox reactions.

[0048] (2) Rectification: Introduce the filtrate in step (1) into the continuous rectification device through negative pressure, and when the liquid level is slightly higher than the heating furnace wire, conduct electric heating for continuous rectification; feed 2.0L each time. The continuous rectification device is made of high-purity quartz glass.

[0049] (3) Fractional distillation: the middle distillate in step (2) is collected, and the distillate temperature ranges from 332°C to 342°...

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Abstract

The invention discloses an ultra-clean high-purity sulfuric acid production method. The ultra-clean high-purity sulfuric acid production method comprises the following steps that 1, impurity removal is performed, namely industrial-grade sulfuric acid is injected into a treatment tank, an impurity removal reagent is added under mechanical stirring, and filtration is performed after standing; 2, rectification is performed, namely filtrate obtained through the step 1 is led into a continuous rectification device under negative pressure, and ohmic heating is performed for continuous rectification when the liquid level is slightly higher than heating furnace wires, wherein the feeding amount each time is 1.8-2.0 L; 3, fractionation is performed, namely middle fraction obtained through the step 2 is collected, and the fraction temperature ranges from 332 DEG C to 342 DEG C; 4, ultra-clean filtration is performed, namely the fraction collected in the step 3 is led into an ultra-clean filtration device under negative pressure to perform ultra-clean filtration; 5, ultra-clean split charging is performed, namely the ultra-clean split charging is performed after the product obtained in the step 4 and subjected to quality inspection meets the requirements. By means of the ultra-clean high-purity sulfuric acid production method, the impurities in the sulfuric acid can be efficiently oxidized and removed. In addition, four filter membranes are adopted for efficient interception, and product quality index exceeds the SEMI-C12 standard.

Description

technical field [0001] The invention relates to a production process for producing ultra-clean and high-purity sulfuric acid. Ultra-clean and high-purity sulfuric acid is mainly used as a strong acid cleaning and corrosive agent in industries such as large-scale integrated circuits and semiconductor discrete devices. The invention belongs to the technical field of microelectronic chemical reagents. Background technique [0002] With the rapid development of semiconductor technology, the requirements for ultra-clean and high-purity reagents are getting higher and higher. In the processing of integrated circuits (IC), ultra-clean and high-purity reagents are mainly used for cleaning and etching the surface of chips and silicon wafers. Their purity and cleanliness have a great influence on the yield, electrical performance and reliability of integrated circuits. significant impact. As an important microelectronic chemical, ultra-clean and high-purity sulfuric acid has been w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/90
Inventor 戈烨铭
Owner JIANGYIN RUNMA ELECTRONICS MATERIAL
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