CN107043092A - A kind of energy-saving metallurgical recovery treatment method of waste acid and device - Google Patents
A kind of energy-saving metallurgical recovery treatment method of waste acid and device Download PDFInfo
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- CN107043092A CN107043092A CN201710218719.6A CN201710218719A CN107043092A CN 107043092 A CN107043092 A CN 107043092A CN 201710218719 A CN201710218719 A CN 201710218719A CN 107043092 A CN107043092 A CN 107043092A
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- acid
- sulfuric acid
- sour water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
- C01B17/901—Recovery from spent acids containing metallic ions, e.g. hydrolysis acids, pickling acids
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention discloses one kind energy-saving metallurgical recovery treatment method of waste acid and device.Methods described is that the ferrous sulfate salt crystal of precipitation is collected, and the high-concentration sulfuric acid after processing is collected into sulfuric acid storage tank, carries out production reuse successively through precipitation, the separation of low temperature sour water, crystallization, separation of solid and liquid by metallurgical spent acid.The present invention is separated the sulfate and sulfuric acid in spent acid using the physical method of low-temperature evaporation and cooling two-way simultaneous, without any chemical agent in spent acid processing procedure, so that the moisture evaporation in spent acid is reduced, ferrous sulfate supersaturation in spent acid is separated out in the form of crystal, the ferrous sulfate of precipitation can be sold, sulfuric acid can add water or acid adding after any allotment concentration, it is back to workshop, spent acid is all recycled after separation, with certain economy return, reduce processing cost, realize spent acid processing no pollution, zero-emission, it is complete to reclaim, the purpose of complete utilization, suitable for popularization and application.
Description
Technical field
The invention belongs to method for treating industrial waste acid, particularly a kind of energy-saving metallurgical recovery treatment method of waste acid and dress
Put, it can realize the purpose of full recovery, complete utilization, no pollution and zero-emission.
Background technology
During nature mineral extraction, sulfuric acid, such as hydrometallurgy, seamless steel tube production, aluminium anodes need to be largely used
Oxidation, Treatment of Metal Surface, oil alkylation etc..These industries can produce a large amount of spent acid in industrial production.
It is domestic at present main using adding alkalization to learn neutralisation, while used device, also need largely to use alkali；Liquid after neutralization
Body saliferous is exceeded, could be discharged after need to continuing with；And period can produce substantial amounts of poisonous waste residue.Also have using at evaporation
Spent acid is managed, but technique is complex, and it is larger to consume energy.
Therefore, in face of economic fast-developing and environmentally friendly, recycling economy consciousness reinforcement, needing one kind badly can effectively locate
Manage and recycle spent acid, energy, the process of simple possible can be saved again.
The content of the invention
In view of the shortcomings of the prior art, the present invention proposes a kind of energy-saving metallurgical recovery treatment method of waste acid and device,
It is the metallurgical Waste Sulfuric Acid processing method of energy-saving full recovery, complete utilization, no pollution, zero-emission, and low-temperature evaporation is carried out to spent acid
With cooling two-way simultaneous technique so that the moisture evaporation in spent acid is reduced, the ferrous sulfate supersaturation in spent acid is with the shape of crystal
Formula is separated out, and the ferrous sulfate of precipitation can sell, the remaining slightly higher dilute sulfuric acid of concentration can add water or acid adding after any allotment concentration, reuse
In workshop.
Described a kind of energy-saving metallurgical recovery treatment method of waste acid, it is characterised in that comprise the following steps：Metallurgical spent acid
Collect into spent acid pond, the acid solution being sent to by spent acid pond after sedimentation basin precipitation, precipitation enters sour water separator and carries out low temperature sour water
Separation, the sulfuric acid content after separation into spent acid reaches more than 50%, into crystallization kettle cooling, reduces remaining sulfate in spent acid
Content, is cooled to after 4 DEG C to spent acid temperature and enters solid-liquid separator progress separation of solid and liquid, and the ferrous sulfate salt crystal of precipitation is received
Collection, the high-concentration sulfuric acid after processing is collected into sulfuric acid storage tank, carries out production reuse, liberated heat is collected when crystallization kettle is crystallized
Thermal source needed for being separated as low temperature sour water, the heat source medium after the cooling that exchanged heat through sour water separator and the high concentration after processing
Sulfuric acid realizes the recycling of energy as the low-temperature receiver required for crystallization kettle.
Described a kind of energy-saving metallurgical recovery treatment method of waste acid, it is characterised in that precipitation uses secondary precipitation.
Described a kind of energy-saving metallurgical recovery treatment method of waste acid, it is characterised in that low temperature sour water is separated in pressurized conditions
Under, the boiling point of water is reduced, water is gone out to steam from spent acid, the temperature in the separation of low temperature sour water is 80-0 DEG C, and pressure is in -0.1MPa
Between -0.046MPa.
Described a kind of energy-saving metallurgical recovery treatment method of waste acid, it is characterised in that sedimentation basin, sour water separator, crystallization
Kettle and sulfuric acid storage tank are equipped with THz wave online detection and control dress device, and sulfuric acid, the sulfuric acid in each equipment in spent acid are monitored in real time
The concentration of salt.
Described a kind of energy-saving metallurgical recovery treatment method of waste acid, it is characterised in that crystallization kettle cooling procedure is using ultrasound
Wave interference optimization crystallization.
A kind of described energy-saving metallurgical recovery treatment method of waste acid, it is characterised in that the sulfate concentration in sulfuric acid storage tank
Less than 0.25%.
Described energy-saving metallurgical waste acidity recovery processing unit, it is characterised in that including be sequentially connected spent acid pond, precipitation
Pond, sour water separator, crystallization kettle and solid-liquid separator, the sour water separator connect the first thermal source pump and condenser；Crystallization kettle
Connect Secondary Heat Source pump, low-temperature receiver pump and refrigeration system, solid-liquid separator connection sulfate storage tank and sulfuric acid storage tank, the first thermal source pump
Secondary Heat Source pump is connected, crystallization liberated heat is reached into sour water separator uses as thermal source, low-temperature receiver pump connection sulfuric acid storage tank, the
The thermal source of one thermal source pump and the low-temperature receiver of condenser carry out heat exchange in sour water separator, and the thermal source of the first thermal source pump becomes low-temperature receiver,
The low-temperature receiver is used with the low temperature sulfuric acid in sulfuric acid storage tank as the low-temperature receiver of crystallization kettle.
Described energy-saving metallurgical waste acidity recovery processing unit, it is characterised in that sedimentation basin includes the first sedimentation basin and second
Sedimentation basin.
Described energy-saving metallurgical waste acidity recovery processing unit, it is characterised in that sedimentation basin, sour water separator, crystallization kettle and
Sulfuric acid storage tank is equipped with THz wave online detection and control dress device, and sulfuric acid in each equipment in spent acid, sulfate are monitored in real time
Concentration.
By using above-mentioned technology, compared with prior art, beneficial effects of the present invention are as follows：
1）The present invention is by the way that the first thermal source pump on sour water separator to be connected to the Secondary Heat Source pump on crystallization kettle, by crystallization kettle
Sulphate crystal liberated heat reaches sour water separator and used as thermal source, while the low-temperature receiver pump connection sulfuric acid on crystallization kettle is stored up
Tank, its thermal source becomes after cooling through sour water separator low-temperature receiver, after separation of solid and liquid low temperature sulfuric acid as crystallization kettle low-temperature receiver
With it is using heat pump techniques recovery waste heat, waste cold and makes full use of, and saves big energy；
2）Crystallization kettle is connected ultrasonic wave by the present invention, is disturbed and crystallized using ultrasonic wave, i.e., using high accuracy purification sulphate crystal
Remaining sulfate 0.25%, meets industry reuse standard in technology, the sulfuric acid after processing；
3）The present invention is divided the sulfate and sulfuric acid in spent acid using the physical method of low-temperature evaporation and cooling two-way simultaneous
From without any chemical agent in spent acid processing procedure so that the moisture evaporation in spent acid is reduced, and the sulfuric acid in spent acid is sub-
Iron supersaturation is separated out in the form of crystal, and the ferrous sulfate of precipitation can sell, sulfuric acid can add water or acid adding after any allotment concentration,
Workshop is back to, i.e., is all recycled spent acid after separation, with certain economy return, handling is reduced
With, realize spent acid processing no pollution, zero-emission, it is complete reclaim, the purpose of complete utilization, suitable for popularization and application.
Brief description of the drawings
Fig. 1 is structural representation of the invention.
In figure：1- spent acid pond, the sedimentation basins of 21- first, the sedimentation basins of 22- second, 3- sour water separators, 4- crystallization kettles, 5- is solid
Liquid/gas separator, 6- sulfuric acid storage tanks, 7- the first thermal source pumps, 8- condensers, 9- Secondary Heat Source pumps, 10- low-temperature receiver pumps, the storage of 11- sulfate
Tank, 12- ultrasonic waves, 13- THz waves online detection and control dress device.
Embodiment
Below in conjunction with Figure of description and embodiment, the invention will be further described, but protection scope of the present invention is simultaneously
It is not limited only to this：
As shown in figure 1, the present invention energy-saving metallurgical waste acidity recovery processing unit, including be sequentially connected spent acid pond 1, precipitation
Pond, sour water separator 3, crystallization kettle 4 and solid-liquid separator 5, the sour water separator 3 connect the first thermal source pump 7 and condenser 8；
The connection Secondary Heat Source of crystallization kettle 4 pump 9, low-temperature receiver pump 10 and refrigeration system, the connection sulfate of solid-liquid separator 5 storage tank 11 and sulfuric acid storage
Crystallization liberated heat is reached sour water separator 3 and used as thermal source by tank 6, the first thermal source pump 7 connection Secondary Heat Source pump 9, low-temperature receiver
Pump 10 connects sulfuric acid storage tank 6, and the low-temperature receiver of the sulfuric acid of low temperature as crystallization kettle 4 is used, in practical operation of the present invention, and low-temperature receiver pump 10 is also
The first thermal source pump 7 can be connected, because the thermal source of the first thermal source pump 7 comes from Secondary Heat Source pump 9, the thermal source enters sour water separator
3, the water given in sour water heating, sour water heating evaporation in the presence of vacuum is cooled by the dry empty vapour in condenser 8 and forms water progress
Reuse or discharge, heat source temperature reduction become low-temperature receiver, and the low-temperature receiver can also crystallize required low-temperature receiver as crystallization kettle 4.
During just work of the invention, the low-temperature receiver that crystallization kettle 4 needs when crystallizing is provided by refrigeration system, work to certain time
When, refrigeration system is closed, the low temperature that low-temperature receiver is obtained after separation of solid and liquid（4℃）Sulfuric acid provide or by sour water separator 3 through and
The low-temperature receiver that first thermal source pump 7 comes out is provided, and as refrigerating fluid, helps butterfly crystal.In order to improve sedimentation effect, precipitation of the invention
Pond is included at least two, embodiment using two sedimentation basins：First sedimentation basin 21 and the second sedimentation basin 22, in order to improve crystallization
Effect, reduces the sulphates content that grinds in sulfuric acid, and the present invention connects ultrasonic wave 12, interference optimization crystallization, reduction on crystallization kettle 4
Remaining sulphates content in spent acid.
For the ease of monitoring the concentration of sulfuric acid and sulfate in each device in real time, the present invention is in sedimentation basin, sour water separator
3rd, THz wave online detection and control dress device 13 is equipped with crystallization kettle 4 and sulfuric acid storage tank 6, monitored in real time in each equipment in spent acid
Sulfuric acid, the concentration of sulfate.
As illustrated, a kind of energy-saving metallurgical recovery treatment method of waste acid of the present invention, comprises the following steps：Metallurgical spent acid
Collect into spent acid pond 1, the acid solution being sent to by spent acid pond 1 after sedimentation basin precipitation, precipitation enters sour water separator 3 and carries out low temperature acid
Water is separated, and the temperature in the separation of low temperature sour water is 80-0 DEG C, and pressure is between -0.1MPa and -0.046MPa, to spent acid after separation
In sulfuric acid content reach more than 50%, cooled down into crystallization kettle 4, in order to improve crystallization effect, the present invention is using ultrasonic wave interference
Remaining sulphates content in optimization crystallization, reduction spent acid, is cooled to after 4 DEG C into solid-liquid separator 5 to spent acid temperature and is consolidated
Liquid is separated, and the ferrous sulfate salt crystal of precipitation is collected, and the high-concentration sulfuric acid after processing is collected into sulfuric acid storage tank 6, sulfuric acid storage tank 6
Middle sulfate concentration is less than 0.25%, and the sulfuric acid can carry out production reuse through dilution or directly, what crystallization kettle 4 was released when crystallizing
Heat collection is as the thermal source needed for the separation of low temperature sour water, and the high-concentration sulfuric acid after processing is as cold required for crystallization kettle 4
Source, realizes the recycling of energy, makes full use of Cooling and Heat Source, saves big energy, sedimentation basin, sour water separator 3, crystallization kettle 4
And sulfuric acid storage tank 6 is equipped with THz wave online detection and control dress device 13, and sulfuric acid, the sulfuric acid in each equipment in spent acid are monitored in real time
The concentration of salt..
Embodiment 1：
Metallurgical spent acid（Sulfuric acid concentration 25%, sulfate concentration 10%）1t is discharged into behind spent acid pond 1, heavy in the first sedimentation basin 21 and second
The acid solution that shallow lake pond 22 is passed through after secondary precipitation, precipitation enters sour water separator 3 and carries out low temperature sour water separation, and separation temperature is 60
DEG C, pressure is that the acid concentration in -0.08MPa, spent acid is significantly lifted, when sulfuric acid content reaches more than 50%,（Separate water outlet
Measure as 0.5t）, cooled down into crystallization kettle 4, cooling procedure is crystallized using the disturbed optimization of ultrasound, remaining sulfate in reduction spent acid
Content, chilling temperature reaches separation of solid and liquid, the errous sulfate crystal 0.0992t commodity sellings of precipitation, the content after processing after 4 DEG C
62.4% high-concentration sulfuric acid 0.4t can produce reuse.
Embodiment 2：
Metallurgical spent acid（Sulfuric acid concentration 23%, sulfate concentration 8%）1t is discharged into behind spent acid pond 1, heavy in the first sedimentation basin 21 and second
The acid solution that shallow lake pond 22 is passed through after secondary precipitation, precipitation enters sour water separator 3 and carries out low temperature sour water separation, and separation temperature is 65
DEG C, pressure is that the acid concentration in -0.072MPa, spent acid is significantly lifted, when sulfuric acid content reaches more than 50%,（Separate water outlet
Measure as 0.54t）, cooled down into crystallization kettle 4, cooling procedure is crystallized using the disturbed optimization of ultrasound, remaining sulfuric acid in reduction spent acid
Salt content, chilling temperature reaches separation of solid and liquid, the errous sulfate crystal 0.0792t commodity sellings of precipitation, content after processing after 4 DEG C
60.4% high-concentration sulfuric acid 0.38t can produce reuse.
Claims (9)
1. a kind of energy-saving metallurgical recovery treatment method of waste acid, it is characterised in that comprise the following steps：Metallurgical spent acid is collected to useless
Sour pond（1）In, by spent acid pond（1）It is sent to the acid solution after sedimentation basin precipitation, precipitation and enters sour water separator（3）Carry out low temperature sour water
Separation, the sulfuric acid content after separation into spent acid reaches more than 50%, into crystallization kettle（4）Remaining sulfuric acid in cooling, reduction spent acid
Salt content, is cooled to after 4 DEG C to spent acid temperature and enters solid-liquid separator（5）Separation of solid and liquid is carried out, the ferrous sulfate of precipitation is brilliant
Body is collected, and the high-concentration sulfuric acid after processing is collected to sulfuric acid storage tank（6）In, carry out production reuse, crystallization kettle（4）Released during crystallization
Heat collection as low temperature sour water separate needed for thermal source, through sour water separator（3）Heat exchange cooling after heat source medium and
High-concentration sulfuric acid after processing is used as crystallization kettle（4）Required low-temperature receiver, realizes the recycling of energy.
2. the energy-saving metallurgical recovery treatment method of waste acid of one kind according to claim 1, it is characterised in that precipitation uses two
Secondary precipitation.
3. the energy-saving metallurgical recovery treatment method of waste acid of one kind according to claim 1, it is characterised in that low temperature sour water point
From under an increased pressure, the boiling point of water is reduced, water is gone out to steam from spent acid, the temperature in the separation of low temperature sour water is 80-0 DEG C, pressure
Power is between -0.1MPa and -0.046MPa.
4. the energy-saving metallurgical recovery treatment method of waste acid of one kind according to claim 1, it is characterised in that sedimentation basin, sour water
Separator（3）, crystallization kettle（4）And sulfuric acid storage tank（6）THz wave online detection and control dress device is equipped with, each equipment is monitored in real time
The concentration of sulfuric acid, sulfate in interior spent acid.
5. the energy-saving metallurgical recovery treatment method of waste acid of one kind according to claim 1, it is characterised in that crystallization kettle（4）It is cold
But process is crystallized using ultrasonic wave interference optimization.
6. the energy-saving metallurgical recovery treatment method of waste acid of one kind according to claim 1, it is characterised in that sulfuric acid storage tank（6）
In sulfate concentration be less than 0.25%.
7. a kind of energy-saving metallurgical waste acidity recovery processing unit according to claim 1, it is characterised in that including connecting successively
The spent acid pond connect（1）, sedimentation basin, sour water separator（3）, crystallization kettle（4）And solid-liquid separator（5）, the sour water separator（3）
Connect the first thermal source pump（7）And condenser（8）；Crystallization kettle（4）Connect Secondary Heat Source pump（9）, low-temperature receiver pump（10）And refrigeration system,
Solid-liquid separator（5）Connect sulfate storage tank（11）And sulfuric acid storage tank（6）, the first thermal source pump（7）Connect Secondary Heat Source pump（9）,
Crystallization liberated heat is reached into sour water separator（3）Used as thermal source, low-temperature receiver pump（10）Connect sulfuric acid storage tank（6）, the first heat
Source pump（7）Thermal source and condenser（8）Low-temperature receiver in sour water separator（3）Carry out heat exchange, the first thermal source pump（7）Thermal source become
Into low-temperature receiver, the low-temperature receiver and sulfuric acid storage tank（6）In low temperature sulfuric acid be used as crystallization kettle（4）Low-temperature receiver use.
8. energy-saving metallurgical waste acidity recovery processing unit according to claim 7, it is characterised in that sedimentation basin includes first
Sedimentation basin（21）With the second sedimentation basin（22）.
9. energy-saving metallurgical waste acidity recovery processing unit according to claim 7, it is characterised in that sedimentation basin, sour water separation
Device（3）, crystallization kettle（4）And sulfuric acid storage tank（6）THz wave online detection and control dress device is equipped with, monitors in each equipment and gives up in real time
The concentration of sulfuric acid, sulfate in acid.
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2017
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