Sulfuric acid recovery method and system

A recovery system and recovery method technology, applied in sulfur trioxide/sulfuric acid, chemical instruments and methods, sulfur compounds, etc., can solve the problems of high energy consumption, high production cost, inconvenient disposal of sulfuric acid waste liquid, etc., and reduce energy consumption. , Low production cost, good recycling effect

Pending Publication Date: 2020-11-27
江苏电科环保有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] Aiming at the shortcomings of existing sulfuric acid waste liquid, such as inconvenient treatment, high production cost, high energy consumption, and unsuitability for the treatment and recycling of sulfuric acid waste liquid in the semiconductor industry, the present invention provides a method for recovering sulfuric acid, which can be conveniently used for sulfuric acid waste in the semiconductor industry. Recycling and processing of waste liquid, low production cost, low energy consumption, good recycling effect, for this reason, the present invention also provides a sulfuric acid recovery system

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  • Sulfuric acid recovery method and system

Examples

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Effect test

Embodiment 1

[0036] A rectification tower equipped with a negative pressure device and connected to the inlet of the reboiler circulation loop is used to perform rectification and pre-concentration on the sulfuric acid waste liquid with a mass fraction of sulfuric acid of 50% and a mass fraction of impurities of 2% at 180°C. The impurities are hydrogen peroxide, hydrogen peroxide, and Metal salt (Fe 2 (SO 4 ) 3 、CuSO 4 ) and organic matter (ketones and toluene), the pressure is -10 KPa, hydrogen peroxide reacts with ketone organic matter to achieve partial removal, and obtain a sulfuric acid pre-concentrate with a sulfuric acid mass fraction of 80% and a dilute sulfuric acid fraction of 0.6%; the sulfuric acid mass fraction The 0.6% dilute sulfuric acid distillate is condensed, passed through ammonia water, and then filtered by RO reverse osmosis membrane, and the obtained ammonium sulfate is used for the preparation of agricultural fertilizers.

[0037] The sulfuric acid pre-concentrat...

Embodiment 2

[0040] A rectification tower equipped with a negative pressure device and connected to the inlet of the reboiler circulation loop is used to perform rectification and pre-concentration on the sulfuric acid waste liquid with a mass fraction of sulfuric acid of 60% and a mass fraction of impurities of 2.5% at 190°C. The impurities are hydrogen peroxide, hydrogen peroxide, and Metal salt (Fe 2 (SO 4 ) 3 、CuSO 4 and NiSO 4 ) and ketone organic matter, the pressure is -15 KPa, hydrogen peroxide reacts with ketone organic matter to achieve double removal, and obtain a sulfuric acid pre-concentrate with a sulfuric acid mass fraction of 85% and a dilute sulfuric acid fraction of 0.8%; a sulfuric acid mass fraction of 0.8% After the dilute sulfuric acid fraction is condensed, ammonia water is passed into it, and then RO reverse osmosis membrane is used for filtration, and the obtained ammonium sulfate is used for the preparation of agricultural fertilizer.

[0041] A fractionation ...

Embodiment 3

[0043] A rectification tower equipped with a negative pressure device and connected to the inlet of the reboiler circulation loop is used to perform rectification and pre-concentration on the sulfuric acid waste liquid with a mass fraction of sulfuric acid of 55% and a mass fraction of impurities of 3% at 185°C. The impurities are hydrogen peroxide, hydrogen peroxide, and Metal salt (Fe 2 (SO 4 ) 3 、CuSO 4 、NiSO 4 ) and organic matter (ketones, alcohols), the pressure is -13 KPa, hydrogen peroxide reacts with ketone organic matter to achieve partial removal, and obtain a sulfuric acid pre-concentrate with a sulfuric acid mass fraction of 82% and a dilute sulfuric acid fraction of 0.7%; the mass fraction of sulfuric acid The dilute sulfuric acid fraction with a fraction of 0.7% is condensed and passed into ammonia water, and then filtered through RO reverse osmosis membrane, and the obtained ammonium sulfate is used for the preparation of agricultural fertilizers.

[0044] ...

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Abstract

The invention provides a sulfuric acid recovery method. The method can be conveniently used for recovery treatment of semiconductor industrial sulfuric acid waste liquid and is low in production cost,low in energy consumption and good in recovery utilization effect, and therefore, the invention further provides a sulfuric acid recovery system. High-concentration semiconductor industrial sulfuricacid waste liquid containing sulfuric acid with the mass fraction of 50-60% is treated by utilizing a distillation principle and adopting a rectification and fractionation two-stage process; during rectification, hydrogen peroxide impurities in the sulfuric acid waste liquid can oxidize organic matter impurities to degrade the organic matters, and when the hydrogen peroxide cannot be completely oxidized and degraded, oxidative degradation of the hydrogen peroxide is performed through an oxidation tower to realize double removal of the organic matters and the hydrogen peroxide impurities; during fractionation, due to the fact that the boiling point of metal salt impurities is high, the metal salt impurities are left at the bottom of a heater after being fractionated, the metal salt impurities are removed through deslagging, the mass fraction of recycled concentrated sulfuric acid reaches 92.5%, and the recycled concentrated sulfuric acid is industrial-grade sulfuric acid which can be directly sold.

Description

technical field [0001] The invention relates to the technical field of treatment and recovery of sulfuric acid waste liquid, in particular to the technical field of treatment and recovery of sulfuric acid waste liquid in the semiconductor manufacturing industry, specifically a sulfuric acid recovery method and system. Background technique [0002] Sulfuric acid is an important industrial raw material. A large amount of sulfuric acid waste liquid will be produced in the industrial production process. If it is discharged directly, it will not only affect the ecological environment, but also cause waste of sulfuric acid resources. Therefore, it is necessary to treat the sulfuric acid waste liquid before discharging. Treatment: At present, the methods for treating sulfuric acid waste liquid mainly include neutralization precipitation method, pyrolysis method, etc. The neutralization precipitation method is generally used to treat sulfuric acid waste liquid with relatively low con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/90C01B17/88C05C3/00
CPCC01B17/905C01B17/901C01B17/88C05C3/00
Inventor 刘晓雨朱玲慧刘围郭维林
Owner 江苏电科环保有限公司
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