CN114853242B - Method for recycling acidic wastewater - Google Patents

Method for recycling acidic wastewater Download PDF

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Publication number
CN114853242B
CN114853242B CN202210495752.4A CN202210495752A CN114853242B CN 114853242 B CN114853242 B CN 114853242B CN 202210495752 A CN202210495752 A CN 202210495752A CN 114853242 B CN114853242 B CN 114853242B
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acid
fluorine
chlorine
water
wastewater
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CN114853242A (en
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姜子燕
叶新军
彭国华
黄海丽
杨会
侯海明
潘从强
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Jinchuan Group Nickel Cobalt Co ltd
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Jinchuan Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/10Treatment of water, waste water, or sewage by heating by distillation or evaporation by direct contact with a particulate solid or with a fluid, as a heat transfer medium
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/16Treatment of water, waste water, or sewage by heating by distillation or evaporation using waste heat from other processes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/20Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/58Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C02F1/62Heavy metal compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/02Temperature
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/03Pressure
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00General aspects of water treatment
    • C02F2301/08Multistage treatments, e.g. repetition of the same process step under different conditions
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00Specific treatment goals
    • C02F2303/14Maintenance of water treatment installations
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)
  • Physical Water Treatments (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention relates to a method for recycling acid wastewater, which relates to the technical field of wastewater recycling and comprises the steps of carrying out filter pressing and desliming on acid wastewater, recycling part of the acid wastewater after the filter pressing and desliming, and feeding the other part of the acid wastewater into an adiabatic evaporation tower to realize concentration and emission reduction of acid water, wherein the concentrated acid water is subjected to sulfuration and impurity removal, three-effect downstream evaporation and concentration, fluorine-chlorine stripping and fluorine-chlorine analysis tower, and the acid water after analysis is filtered by a filter press or enters a mixed acid tank to be mixed with 98% sulfuric acid produced by a sulfuric acid system to be configured into 93% -93.5% sulfuric acid, and then the acid water is sold or directly used for supplementing water in a dry absorption process of an acid making system to reduce the consumption of new water.

Description

Method for recycling acidic wastewater
Technical Field
The invention relates to the technical field of wastewater recycling, in particular to a method for recycling acidic wastewater.
Background
The method is characterized in that metal sulfide associated with ores in the smelting process is often mixed in high-temperature dust-containing multicomponent flue gas in the form of sulfur dioxide and sulfur trioxide, the high-temperature dust-containing multicomponent flue gas enters a matched acid making system, sulfuric acid products are produced through a purifying, cooling, dedusting and demisting process, a drying water process and a double-conversion and double-absorption process, a dynamic wave wet washing process is often adopted for flue gas purification, a large amount of harmful substances such as mineral dust, halogen elements and the like enter a liquid phase from a gas phase in a double-membrane contact process, and are continuously enriched in circulating dilute acid, acidity, solid content, heavy metals and the like are gradually increased, and in order to ensure a spray washing effect, the circulating dilute acid is required to be subjected to open-circuit treatment, so that a certain amount of acid wastewater is produced, and the problems of high treatment cost, large wastewater discharge, difficult recovery of valuable metals and water resources and the like exist in the conventional dilute acid process produced in the smelting process at home and abroad.
Disclosure of Invention
The invention aims at: in order to solve the technical problems in the background technology, the invention provides a method for recycling acidic wastewater.
The invention adopts the following technical scheme for realizing the purposes: a method for recycling acidic wastewater, comprising the following steps:
s1, carrying out filter pressing and desliming on acid wastewater, wherein after the acid wastewater is subjected to filter pressing and desliming, one part of the acid wastewater is returned to the system for recycling, the other part of the acid wastewater enters an adiabatic evaporation tower, and the part of the acid wastewater enters the adiabatic evaporation tower adopts a low-temperature flue gas adiabatic evaporation technology, so that a good adiabatic humidifying effect is achieved, concentration and emission reduction of acid water are realized, and the acid sludge is produced by filter pressing and smelted by a heavy tempering system;
concentrating the waste acid concentrated by the adiabatic evaporation tower in the S2S 1 to 41%, then delivering the concentrated waste acid to a vulcanization impurity removal system through a circulating pump, and settling and press-filtering the waste acid by a primary vulcanization reactor, a primary thickener, a secondary vulcanization reactor and a secondary thickener to recycle vulcanized slag, thereby realizing the purification and removal of heavy metal impurities;
s3, evaporating and concentrating the dilute acid vulcanized in the S2 by adopting three-effect concurrent evaporation and concentration;
s4, conveying the waste acid obtained after evaporation and concentration in the S3 to a fluorine-chlorine stripping system, carrying out gas-liquid interaction reaction on hot air and dilute acid in a stripping tower, and improving the acid water temperature so as to reduce the solubility of fluorine-chlorine ions, automatically separating out fluorine-chlorine in a form of hydrogen fluoride and hydrogen chloride molecules in an acidic environment into a gas phase, stripping fluorine and chlorine ions in the waste acid into the gas phase, and finally, entering a tail gas absorption tower, and discharging after further spray washing and absorption;
s5, conveying the acid water after the fluorine and chlorine are blown off in the step S4 to a fluorine and chlorine analysis tower, filtering the analyzed acid water by a filter press or mixing the analyzed acid water with 98% sulfuric acid produced by a sulfuric acid mixing tank and a sulfuric acid system to prepare 93% -93.5% sulfuric acid, and then selling the sulfuric acid or directly using the sulfuric acid to supplement water in a dry absorption process of an acid making system to reduce the consumption of new water.
In order to prevent strong corrosion and easy crystallization in the acid water concentration process, in the step S3, equipment which takes phenolic resin impregnated graphite as a main material is adopted as evaporation equipment.
Further, the heat of the hot air in the step S4 is derived from the heat emitted when the diluted acid and the 98% concentrated acid are mixed in the step S5, and steam is not used, so that the steam consumption can be saved.
Further, the fluorine-chlorine analysis tower in the step S5 adopts a negative pressure vacuum method to control the partial pressure of the sulfuric acid surface at-75 kPa to-80 kPa.
Further, in the mixing process of the acid obtained by filtering the acid water after the analysis in the step S5 by a filter press and 98% sulfuric acid, a large amount of reaction heat can be released, the acid temperature is controlled to be 85-120 ℃, and the fluorine-chlorine analysis efficiency can be improved.
The utility model provides an acid wastewater recycling's system, includes adiabatic vaporization system, vulcanization edulcoration system, triple effect evaporation concentration system, fluorine chlorine stripping system and dilute acid system of mixing, the export of adiabatic vaporization system and the entry intercommunication of vulcanization edulcoration system, the export of vulcanization edulcoration system and the entry intercommunication of triple effect evaporation concentration system, the export of triple effect evaporation concentration system and fluorine chlorine stripping system entry intercommunication, fluorine chlorine stripping system's export and dilute acid system of mixing's entry intercommunication.
The invention has the beneficial effects that: according to the method for recycling the acid wastewater, provided by the invention, the recycling of the acid wastewater is realized through the adiabatic evaporation system, the vulcanization impurity removal system, the triple-effect evaporation concentration system, the fluorine-chlorine stripping system and the dilute acid mixing system, the running cost of the system is effectively reduced, the production amount of the acid wastewater is obviously reduced from the source, the production of dangerous solid wastes is greatly reduced, and the environmental benefit and the social benefit are obvious.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures. Furthermore, the terms "first," "second," and the like, are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
In describing embodiments of the present invention, it should be noted that the directions or positional relationships indicated by the terms "inner", "outer", "upper", etc. are directions or positional relationships based on those shown in the drawings, or those that are conventionally put in place when the inventive product is used, are merely for convenience of description and simplification of description, and are not indicative or implying that the apparatus or element in question must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Example 1
As shown in fig. 1, a method for recycling acidic wastewater comprises the following steps:
s1, carrying out filter pressing and desliming on acid wastewater, wherein after the acid wastewater is subjected to filter pressing and desliming, one part of the acid wastewater is returned to the system for recycling, the other part of the acid wastewater enters an adiabatic evaporation tower, and the part of the acid wastewater enters the adiabatic evaporation tower adopts a low-temperature flue gas adiabatic evaporation technology, so that a good adiabatic humidifying effect is achieved, concentration and emission reduction of acid water are realized, and the acid sludge is produced by filter pressing and smelted by a heavy tempering system;
concentrating the waste acid concentrated by the adiabatic evaporation tower in the S2S 1 to 41%, then delivering the concentrated waste acid to a vulcanization impurity removal system through a circulating pump, and settling and press-filtering the waste acid by a primary vulcanization reactor, a primary thickener, a secondary vulcanization reactor and a secondary thickener to recycle vulcanized slag, thereby realizing the purification and removal of heavy metal impurities;
s3, evaporating and concentrating the dilute acid vulcanized in the S2 by adopting three-effect concurrent evaporation and concentration;
s4, conveying the waste acid obtained after evaporation and concentration in the S3 to a fluorine-chlorine stripping system, carrying out gas-liquid interaction reaction on hot air and dilute acid in a stripping tower, and improving the acid water temperature so as to reduce the solubility of fluorine-chlorine ions, automatically separating out fluorine-chlorine in a form of hydrogen fluoride and hydrogen chloride molecules in an acidic environment into a gas phase, stripping fluorine and chlorine ions in the waste acid into the gas phase, and finally, entering a tail gas absorption tower, and discharging after further spray washing and absorption;
s5, conveying the acid water after the fluorine and chlorine are blown off in the step S4 to a fluorine and chlorine analysis tower, filtering the analyzed acid water by a filter press or mixing the analyzed acid water with 98% sulfuric acid produced by a sulfuric acid mixing tank and a sulfuric acid system to prepare 93% -93.5% sulfuric acid, and then selling the sulfuric acid or directly using the sulfuric acid to supplement water in a dry absorption process of an acid making system to reduce the consumption of new water.
In order to prevent strong corrosion and easy crystallization in the acid water concentration process, in the step S3, equipment which takes phenolic resin impregnated graphite as a main material is adopted as evaporation equipment.
Further, the heat of the hot air in the step S4 is derived from the heat emitted when the diluted acid and the 98% concentrated acid are mixed in the step S5, and steam is not used, so that the steam consumption can be saved.
Further, the fluorine-chlorine analysis tower in the step S5 adopts a negative pressure vacuum method to control the partial pressure of the sulfuric acid surface at-75 kPa to-80 kPa.
Further, in the mixing process of the acid obtained by filtering the acid water after the analysis in the step S5 by a filter press and 98% sulfuric acid, a large amount of reaction heat can be released, the acid temperature is controlled to be 85-120 ℃, and the fluorine-chlorine analysis efficiency can be improved.
The utility model provides an acid wastewater recycling's system, includes adiabatic vaporization system, vulcanization edulcoration system, triple effect evaporation concentration system, fluorine chlorine stripping system and dilute acid system of mixing, the export of adiabatic vaporization system and the entry intercommunication of vulcanization edulcoration system, the export of vulcanization edulcoration system and the entry intercommunication of triple effect evaporation concentration system, the export of triple effect evaporation concentration system and fluorine chlorine stripping system entry intercommunication, fluorine chlorine stripping system's export and dilute acid system of mixing's entry intercommunication.
Example 2
Carrying out filter pressing and desliming on the acid wastewater of the system, wherein the filter pressing generates acid sludge, and the acid sludge is recycled to the smelting system by a tempering method, and part of filter pressing clear liquid is returned to the system for recycling, and the other part of the clear liquid enters an adiabatic evaporation tower to evaporate concentrated acid; the mixture enters an adiabatic evaporation tower to be evaporated and concentrated to a certain acidity, and then is pumped to a vulcanization impurity removal system by a circulating pump, wherein a vulcanizing agent adopts hydrogen sulfide, and the mixture is subjected to sedimentation and pressure filtration by a primary vulcanization reactor, a primary thickener, a secondary vulcanization reactor and a secondary thickener, so that the vulcanized slag is recovered, and the purification and removal of heavy metal impurities are realized; concentrating the vulcanized waste acid through a three-effect evaporation system, and concentrating and separating different components in the mixed liquid according to different boiling points mainly through steam action; conveying the evaporated and concentrated waste acid to a fluorine-chlorine stripping system, carrying out gas-liquid interaction reaction on hot air and dilute acid in a stripping tower, stripping fluorine and chlorine ions in the waste acid into a gas phase, and finally, entering a tail gas absorption tower, and discharging after further spray washing and absorption; and (3) conveying the acid water after the fluorine-chlorine stripping to a fluorine-chlorine analysis tower, further removing fluorine-chlorine by adopting negative pressure vacuum high temperature, filtering the analyzed acid water by a filter press, and then feeding the filtered acid water into an acid mixing tank to prepare 93-93.5% concentrated sulfuric acid to be used as a finished product for sale.
Example 3
Carrying out filter pressing and desliming on the acid wastewater of the system, wherein the filter pressing generates acid sludge, and the acid sludge is recycled to the smelting system by a tempering method, and part of filter pressing clear liquid is returned to the system for recycling, and the other part of the clear liquid enters an adiabatic evaporation tower to evaporate concentrated acid; the mixture enters an adiabatic evaporation tower to be evaporated and concentrated to a certain acidity, and then is pumped to a vulcanization impurity removal system by a circulating pump, wherein a vulcanizing agent adopts hydrogen sulfide, and the mixture is subjected to sedimentation and pressure filtration by a primary vulcanization reactor, a primary thickener, a secondary vulcanization reactor and a secondary thickener, so that the vulcanized slag is recovered, and the purification and removal of heavy metal impurities are realized; concentrating the vulcanized waste acid through a three-effect evaporation system, and concentrating and separating different components in the mixed liquid according to different boiling points mainly through steam action; conveying the evaporated and concentrated waste acid to a fluorine-chlorine stripping system, carrying out gas-liquid interaction reaction on hot air and dilute acid in a stripping tower, stripping fluorine and chlorine ions in the waste acid into a gas phase, and finally, entering a tail gas absorption tower, and discharging after further spray washing and absorption; and (3) conveying the acid water after the fluorine-chlorine stripping to a fluorine-chlorine analysis tower, further removing fluorine-chlorine by adopting negative pressure vacuum high temperature, filtering the analyzed acid water by a filter press, and directly using the acid water for supplementing water in a dry absorption process of an acid making system, thereby reducing the consumption of new water.
It will be appreciated by those skilled in the art that the present invention can be carried out in other embodiments without departing from the spirit or essential characteristics thereof. Accordingly, the above disclosed embodiments are illustrative in all respects, and not exclusive. All changes that come within the scope of the invention or equivalents thereto are intended to be embraced therein.

Claims (2)

1. The method for recycling the acid wastewater is characterized by comprising the following steps of:
s1, carrying out filter pressing and desliming on acid wastewater, wherein after the acid wastewater is subjected to filter pressing and desliming, one part of the acid wastewater is returned to the system for recycling, the other part of the acid wastewater enters an adiabatic evaporation tower, and the part of the acid wastewater enters the adiabatic evaporation tower adopts a low-temperature flue gas adiabatic evaporation technology, so that a good adiabatic humidifying effect is achieved, concentration and emission reduction of acid water are realized, and the acid sludge is produced by filter pressing and smelted by a heavy tempering system;
concentrating the waste acid concentrated by the adiabatic evaporation tower in the S2S 1 to 41%, then delivering the concentrated waste acid to a vulcanization impurity removal system through a circulating pump, and settling and press-filtering the waste acid by a primary vulcanization reactor, a primary thickener, a secondary vulcanization reactor and a secondary thickener, recovering vulcanized slag, thereby realizing the purification and removal of heavy metal impurities;
s3, evaporating and concentrating the dilute acid vulcanized in the S2 by adopting three-effect concurrent evaporation and concentration;
in order to prevent strong corrosion and easy crystallization in the acid water concentration process, equipment which takes phenolic resin impregnated graphite as a main material is adopted as evaporation equipment;
s4, conveying the waste acid obtained after evaporation and concentration in the S3 to a fluorine-chlorine stripping system, carrying out gas-liquid interaction reaction on hot air and dilute acid in a stripping tower, and improving the acid water temperature so as to reduce the solubility of fluorine-chlorine ions, automatically separating out fluorine-chlorine in a form of hydrogen fluoride and hydrogen chloride molecules in an acidic environment into a gas phase, stripping fluorine and chlorine ions in the waste acid into the gas phase, and finally, entering a tail gas absorption tower, and discharging after further spray washing and absorption;
the heat of the hot air is derived from the heat emitted when the dilute acid and the 98% concentrated acid in the step S5 are mixed, and steam is not used, so that the steam consumption can be saved;
s5, conveying the acid water after the fluorine and chlorine are blown off in the step S4 to a fluorine and chlorine analysis tower, filtering the analyzed acid water by a filter press or mixing the analyzed acid water with 98% sulfuric acid produced by a sulfuric acid mixing tank and a sulfuric acid system to prepare 93% -93.5% sulfuric acid, and then selling the sulfuric acid or directly using the sulfuric acid to supplement water in a dry absorption process of an acid making system to reduce the consumption of new water;
the fluorine-chlorine analysis tower adopts a negative pressure vacuum method to control the partial pressure of the sulfuric acid surface to be between 75kPa and 80kPa;
the acid obtained by filtering the resolved acid water by a filter press releases a great amount of reaction heat in the mixing process of the acid and 98% sulfuric acid, the acid temperature is controlled to be 85-120 ℃, and the fluorine-chlorine resolving efficiency can be improved.
2. The method for recycling acidic wastewater according to claim 1, comprising an adiabatic evaporation system, a vulcanization impurity removal system, a triple effect evaporation concentration system, a fluorine-chlorine stripping system and a dilute acid mixing system, wherein the outlet of the adiabatic evaporation system is communicated with the inlet of the vulcanization impurity removal system, the outlet of the vulcanization impurity removal system is communicated with the inlet of the triple effect evaporation concentration system, the outlet of the triple effect evaporation concentration system is communicated with the inlet of the fluorine-chlorine stripping system, and the outlet of the fluorine-chlorine stripping system is communicated with the inlet of the dilute acid mixing system.
CN202210495752.4A 2022-05-07 2022-05-07 Method for recycling acidic wastewater Active CN114853242B (en)

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WO2001066500A1 (en) * 2000-03-03 2001-09-13 Illa International L.L.C. Method of producing cumene hydroperoxide, phenol and acetone
CN205699515U (en) * 2016-05-17 2016-11-23 常州泰特环境设备工程有限公司 A kind of dilute sulfuric acid waste liquid 3+1 negative pressure evaporation enrichment facility
CN107445379A (en) * 2017-08-25 2017-12-08 金川集团股份有限公司 A kind of device and method of acid waste water evaporation emission reduction
CN111661972A (en) * 2020-06-29 2020-09-15 株洲冶炼集团科技开发有限责任公司 Process for treating and recycling lead-zinc smelting flue gas washing waste acid

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