CN210764815U - Useless mixed acid recovery processing device of stainless steel pickling - Google Patents
Useless mixed acid recovery processing device of stainless steel pickling Download PDFInfo
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Abstract
The utility model discloses a stainless steel pickling waste mixed acid recovery processing device, which comprises a pretreatment system, an evaporation concentration system and an extraction system which are communicated in sequence according to the processing direction of waste mixed acid; the evaporation concentration system comprises an evaporation heating tank, a primary condenser, a secondary condenser, a vacuum system and a dilute acid recovery device communicated with the secondary condenser, wherein the evaporation heating tank, the primary condenser, the secondary condenser and the vacuum system are sequentially communicated; the extraction system comprises a first extraction device for extracting iron, a second extraction device for extracting nickel and a third extraction device for extracting chromium; the utility model discloses an utilize the useless mixed acid of evaporative concentration system and extraction system to handle the flow, carry out evaporative concentration to useless mixed acid, distill and retrieve nitric acid and hydrofluoric acid in the useless mixed acid. The effect of concentrating and enriching metal ions is achieved in the evaporation process; and extracting corresponding metal ions by using extracting agents respectively. Not only can recycle nitric acid and hydrofluoric acid and concentrate and enrich metal ions, but also can reduce the addition amount of the medicament and the extraction time.
Description
Technical Field
The utility model relates to a sewage treatment technical field especially relates to a useless mixed acid recovery processing device of stainless steel pickling.
Background
In the annealing and pickling production process of stainless steel, HF and HNO are generally used3And carrying out acid pickling by using mixed acid, wherein the main purpose of the acid pickling by using mixed acid is to remove scale, namely an oxide layer, formed on the surface of the steel strip in the hot rolling and annealing processes. Meanwhile, the surface of the stainless steel is passivated by acid cleaning, so that the corrosion resistance of the steel plate is improved. Since HF and HNO3 are expensive, and considering the requirements of environmental protection and sustainable development of resources, it is necessary to perform a regeneration treatment on the mixed acid spent acid solution. The composition of the waste liquid varies depending on the type of steel to be pickled. The waste liquid of the general acid-washing nickel and chromium stainless steel contains HNO3150～160g/L、HF 30～50g/L、Fe3 +30～40g/L、Ni+6～8g/L、Cr3+6-8 g/L. The waste liquid has strong corrosivity and causes great harm to human bodies and environment without treatment. According to the current major technologies all over the world, the recovery technology of mixed acid mainly comprises three technologies, one technology is a free acid recovery process of Canada ECO-TEC company, and the system mainly adopts a simple resin adsorption process technology to remove dissolved metals in acid pickling liquor and returns the purified acid liquor to an acid pickling tank for continuous use. The other is the regeneration technology of the pyrolysis mixed acid of Austria ANDRITZ-RUNTHER company, and the regeneration technology of the pyrolysis mixed acid is realized by leading the free hydrofluoride in the waste acidThe acid, nitric acid and water evaporate at high temperature, changing from liquid to gas. Then hydrofluoric acid and nitric acid steam are absorbed in water in an absorption tower to generate hydrofluoric acid and nitric acid, thereby realizing the recovery of mixed acid waste acid. The third is the mixed acid complete acid regeneration technique of the STEULER company, Germany, which, in terms of technology, first considers the recovery of nitric acid and then the only aqueous solution of crystals of metal fluoride which is fed to the spray roaster. Therefore, the recovery rate of the nitric acid is improved, and the amount of waste acid to be roasted is reduced, so that the consumption of natural gas and liquid ammonia is greatly reduced.
In addition, as a process for treating and recovering valuable substances from waste liquid, there are a reduced pressure evaporation method, a solvent extraction method, an electrodialysis method, an ion exchange method, and the like, and among them, the reduced pressure evaporation method is most commonly used.
A reduced pressure evaporation method: the principle is that sulfuric acid is added into waste acid liquor to replace sulfate radicals with nitrate radicals and fluoride ions in the waste liquor to form metal sulfate, the sulfuric acid, nitric acid and hydrofluoric acid are heated and evaporated to generate gaseous nitric acid and hydrofluoric acid under negative pressure by utilizing the difference of the balance temperature of the sulfuric acid, the nitric acid and the hydrofluoric acid, and the regenerated mixed acid is obtained by condensation and is used for acid pickling again. The residual liquid contains metal salt of sulfuric acid and sulfuric acid, the sulfate forms crystal after cooling, and the sulfuric acid liquid with certain concentration can be recycled after solid-liquid separation. The solid metal sulfate sediment can be separately treated, and the metals such as nickel, chromium and the like in the solid metal sulfate sediment can be recovered.
Solvent extraction method: the principle is that sulfuric acid is introduced into waste liquid, the sulfuric acid and metal salts in the waste liquid are subjected to double decomposition reaction, the metal salts in the waste liquid are converted into metal sulfate, nitric acid and hydrofluoric acid are dissociated, tributyl phosphate (TBP) is used as an extracting agent, the nitric acid and the hydrofluoric acid are transferred into the extracting agent, and then the extracting agent is subjected to back extraction by water in a back extraction tower, so that mixed acid of the nitric acid and the hydrofluoric acid is obtained and is used for pickling again. In this way, the recovery rates of nitric acid and hydrofluoric acid were 95% and 65%, respectively.
The spray roasting technology can recover free acid and combined acid, and the metal salt in the regenerated acid is basically zero. The acid recovery rate and the concentration of the recovered acid are high, and the generated ferric oxide powder can be recycled. The spray roasting technology can almost completely recycle metal ions in the waste acid and the acid liquor, can greatly reduce the wastewater discharged to a wastewater treatment station, but the spray roasting method has complex process flow, huge equipment and large investment, and is suitable for large-scale waste acid recovery production; in addition, roasting waste gas is generated in the production process, and the emission after reaching the standard still has certain influence on the environment.
The purification process of the resin exchange waste acid is simple and convenient to operate; compact occupied area, small investment and suitability for small-scale waste acid recovery production. The resin exchange waste acid purification can only recover free acid, and the acid recovery rate and the concentration of the recovered acid are limited by the concentration of the free acid in the waste acid washing liquid; the metal salt can not be recovered, and the deacidified metal salt needs to be discharged to a sewage treatment station for further treatment. A large amount of sludge is produced after the treatment. In addition, even if the nitrate and the hydrofluoride are discharged after reaching the standard after treatment, the nitrogen and the fluorine have large influence on the environment, the difficulty in removing the nitrogen is large, and the treatment process is complex.
Disclosure of Invention
The utility model aims to overcome the defects existing in the prior art and provide a recovery and treatment device for waste mixed acid in stainless steel pickling.
In order to achieve the above purpose, the utility model adopts the following technical scheme: a stainless steel pickling waste mixed acid recovery processing device comprises a pretreatment system, an evaporation concentration system and an extraction system which are sequentially communicated according to the waste mixed acid processing direction;
the evaporation concentration system comprises an evaporation heating tank, a primary condenser, a secondary condenser, a vacuum system and a dilute acid recovery device communicated with the secondary condenser, wherein the evaporation heating tank, the primary condenser, the secondary condenser and the vacuum system are sequentially communicated;
the extraction system comprises a first extraction device for extracting iron, a second extraction device for extracting nickel and a third extraction device for extracting chromium.
The utility model discloses a useless mixed acid recovery processing device filters useless mixed acid earlier through the preliminary treatment, gets rid of particulate matter impurity, handles through evaporative concentration again, evaporates out hydrofluoric acid and nitric acid in the useless mixed acid through the evaporative heating to through the condenser, carry out the condensation with hydrofluoric acid and form with nitric acid and retrieve sour production line and use. And in the evaporation process, metal ions in the waste mixed acid are concentrated and enriched. The near-saturated concentrate contains mainly metal salts and a small amount of nitric acid. And then an extraction method is adopted, the iron ions in the concentrated solution are extracted and separated by an extracting agent, the nickel in the concentrated solution is extracted and separated, the chromium in the concentrated solution is extracted and separated, the metal ions in the concentrated solution are extracted and separated, the residual concentrated solution is a salt solution without metal ions, and evaporation, concentration, crystallization and drying treatment are carried out to form crystallized salt for recycling.
Preferably, the evaporation concentration system further comprises a feeding circulating pump and a preheater, and the pretreatment storage tank is sequentially communicated with the feeding circulating pump, the primary condenser and the preheater; the waste water is divided into two branches after passing through a preheater, and one branch is communicated with an evaporation heating tank, a first-stage condenser, a second-stage condenser, a vacuum system or a dilute acid recovery device through pipelines in sequence.
Preferably, the other branch is connected to a pretreatment tank.
Preferably, the evaporation heating tank is connected with an evaporation forced circulation pump, one outlet of the evaporation forced circulation pump is connected with the circulation inlet of the evaporation heating tank, and the other outlet of the evaporation forced circulation pump is connected with the concentrated solution tank.
Preferably, the first extraction device comprises a first extraction tank and a first back-extraction tank which are communicated in sequence.
Preferably, the first extraction device comprises a second extraction tank and a second back-extraction tank which are communicated in sequence; the second extraction tank is communicated with the first extraction tank.
Preferably, the first extraction device comprises a third extraction tank and a third back-extraction tank which are communicated in sequence; the third extraction tank is communicated with the second extraction tank.
Preferably, the device further comprises an evaporative crystallization device, wherein the evaporative crystallization device comprises a first evaporative crystallization device for evaporating ferric salt, a second evaporative crystallization device for evaporating nickel salt, a third evaporative crystallization device for evaporating chromium salt and a fourth evaporative crystallization device for evaporating salt solution without metal ions; the first evaporative crystallization device is communicated with the first extraction device, the second evaporative crystallization device is communicated with the second extraction device, and the third evaporative crystallization device and the fourth evaporative crystallization device are communicated with the third extraction tank.
Preferably, the interior of the evaporation heating tank body is sprayed with a teflon layer.
Preferably, the pretreatment system comprises a waste acid mixing tank, a water pump, a filtering device and a pretreatment storage tank which are sequentially communicated through pipelines; the filter device comprises at least one of a wire-wound cartridge filter, a bag filter, and a PP cartridge filter.
Preferably, the interior of the preheater, the primary condenser and the secondary condenser is sprayed with a tetrafluoro coating.
The beneficial effects of the utility model reside in that:
the utility model discloses an utilize the useless mixed acid treatment process of evaporative concentration system and extraction system. And (3) evaporating and concentrating the waste mixed acid by using a reduced pressure evaporation method, and distilling to recover nitric acid and hydrofluoric acid in the waste mixed acid. The effect of concentrating and enriching metal ions is achieved in the evaporation process. And extracting corresponding metal ions by using extracting agents respectively. The method can not only recycle nitric acid and hydrofluoric acid and concentrate and enrich metal ions, but also reduce the addition amount of the medicament and the extraction time, and the tetrafluoro coating can prevent the corrosion of equipment.
Drawings
FIG. 1 is a schematic diagram of the overall flow structure of the present invention;
FIG. 2 is a schematic process flow diagram of the present invention.
Detailed Description
For better illustrating the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Examples
As shown in fig. 1, the recovery processing device for waste mixed acid in stainless steel pickling of the utility model comprises a pretreatment system 1, an evaporation concentration system 2, an extraction system 3 and an evaporation crystallization system 4 which are sequentially communicated;
the pretreatment system 1 is used for primarily filtering waste mixed acid discharged from a stainless steel pickling line to remove particulate impurities; the structure of the pretreatment system 1 can be realized by adopting the prior art, and the pretreatment system 1 of the embodiment comprises a waste acid mixing tank 11, a water pump 12, a device and a pretreatment storage tank 16 which are sequentially communicated through pipelines;
the filtering device provided by the invention has the functions of removing particulate impurities in waste acid and removing iron oxide scales of stainless steel parts in the pickling process.
Wherein the filtering device comprises at least one of a wire-wound filter element filter 13, a bag filter 14 and a PP filter element filter 15;
in a preferred embodiment, the filtering means comprises a wire-wound cartridge filter 13, a bag filter 14, a PP cartridge filter 15; and the pore sizes adopted by the wire-wound filter element filter 13, the bag filter 14 and the PP filter element filter 15 are different, the pore sizes are sequentially reduced, and the specific pore size is determined according to the actual situation.
The evaporation concentration system 2 comprises a feeding circulating pump 21, a preheater 22, an evaporation heating tank 23, a first-stage condenser 24, a second-stage condenser 25, a vacuum system 26, a concentrated solution tank 27 and a dilute acid recovery device 28. The pretreatment storage tank 16 is sequentially communicated with a feeding circulating pump 21, a primary condenser 24 and a preheater 22, is divided into two branches through a three-way pipe after passing through the preheater 22, valves 20 are respectively arranged on the two branches, and one branch is sequentially communicated with an evaporation heating tank 23, the primary condenser 24, a secondary condenser 25, a vacuum system 26 or a dilute acid recovery device 28 through a pipeline; the other branch is directly returned to the pretreatment tank 16; an evaporation forced circulation pump 231 is connected to the bottom of the evaporation heating tank 23, one outlet of the evaporation forced circulation pump 231 is connected to the circulation inlet of the evaporation heating tank, the other outlet is connected to the concentrated solution tank 27, and valves 20 are installed on the outlets. The evaporation forced circulation pump is arranged for material circulation of the evaporation heating tank and discharging after evaporation is finished.
The waste mixed acid in the pretreatment storage tank 16 is pumped to a first-stage condenser 24 through a feed circulating pump 21, then enters a preheater 22, is divided into two branches through a tee after being discharged from the preheater 22, is adjusted by installing a valve, and directly enters an evaporation heating tank through one branch; the other branch is directly returned to the pretreatment storage tank. Waste mixed acid is continuously pumped into the outside of a tube nest of a primary condenser (a heat exchanger shell pass) through a waste mixed acid feeding circulating pump, the waste mixed acid enters an evaporation heating tank 23 to be evaporated after reaching a boiling point, evaporated secondary steam enters the inside of the tube nest of the primary condenser 23, and the waste mixed acid outside the tube nest of the primary condenser exchanges heat with the evaporated secondary steam and then exchanges heat with raw steam condensate water through a preheater 22 and then enters the evaporation heating tank 23; at this moment, the waste mixed acid is continuously pumped into the outside of the tube nest of the first-stage condenser (the shell pass of the heat exchanger) through the waste mixed acid feeding circulating pump, exchanges heat with the evaporated secondary steam, exchanges heat with the raw steam condensate water through the preheater 22, and then enters the evaporation heating tank 23, so that the material preheating and waste acid supplementation of the evaporation heating tank are formed, and the evaporation concentration is continuously carried out.
Waste acid heated from the evaporation heating tank 23 enters the inside of a first-stage condenser tube array to exchange heat with waste mixed acid outside the tube array, then enters a second-stage condenser 24 to exchange heat with circulating cooling water, is completely condensed to form condensed dilute acid, and the condensed dilute acid enters a dilute acid recovery device 28 to be collected and recycled, while non-condensable gas is extracted through a vacuum system 26 and discharged to a tail gas treatment system. Under the forced circulation of the evaporation forced circulation pump 231, the waste mixed acid is continuously evaporated and concentrated, and the concentrated saturated waste liquid passes through the conversion valve, and the concentrated liquid is discharged to the concentrated liquid tank 27 by the forced circulation pump and then enters the extraction process.
As preferred embodiment, the utility model discloses a jar body of evaporation heating jar adopts the carbon steel material, the internal portion spraying tetrafluoro material layer of jar, and the heating pipe is put to the inside dish of evaporation heating jar, the heating pipe through set establish with jar internal portion, can increase and useless area of contact who mixes the acid to improve heating efficiency, solved the problem that the tetrafluoro coefficient of heat transfer is low, reached energy-conserving efficient purpose. The interior of the tank is common in the art as to how to coil the heating tube, and therefore, will not be described in detail herein.
Further, the utility model discloses an inside all spraying of pipeline that evaporation heating jar and one-level air conditioner are connected has the tetrafluoro coating, and shell and tube structure among the preheater 22 and one-level condenser 24, the second grade condenser 25 adoption prior art, and preheater 22 and one-level condenser 24, second grade condenser 25 casing adopt carbon steel material, inside spraying tetrafluoro coating. The strong corrosivity of mixed acid is solved by tetrafluoro coating equipment through the spraying and adopting the tetrafluoro coating, the problem of low tetrafluoro heat transfer coefficient is solved by adopting the combination of a coil pipe and a tube nest, and the effects of energy conservation and high efficiency are achieved through heat transfer area compensation and heat recovery.
The extraction system 3 comprises a first extraction device for extracting iron, a second extraction device for extracting nickel and a third extraction device for extracting chromium, wherein the first extraction device comprises a first extraction tank 31 and a first back-extraction tank 32 which are sequentially communicated, and the second extraction device comprises a second extraction tank 33 and a second back-extraction tank 34 which are sequentially communicated; the third extraction device comprises a third extraction tank 35 and a third back extraction tank 36 which are communicated in sequence;
the evaporative crystallization system 4 comprises a first evaporative crystallization device 41, a second evaporative crystallization device 42, a third evaporative crystallization device 43 and a fourth evaporative crystallization device 44.
Wherein, first extraction tank 31 is arranged in extracting the iron in the concentrate, and first extraction tank 31 is equipped with concentrate entry, raffinate export and contains molysite solution export, and first back extraction tank 32 is including containing molysite solution entry, molysite export and waste liquid export, and the molysite export communicates with first evaporative crystallization device 41. Extracting and separating iron by adding an extracting agent for extracting iron into the first extraction tank 31, enabling concentrated solution to enter the first extraction tank 31 to extract iron salt, enabling mixed solution containing iron to enter the first back-extraction tank 32, extracting iron by back-extraction, obtaining pure iron salt solution by back-extraction, enabling the iron salt solution to enter the first evaporation crystallization device 41 again to obtain pure crystalline iron salt, and enabling the crystalline iron salt to be directly sold as a product. The extracting agent and the extracting method are realized by the prior art, for example, the jarosite method can be adopted: adjusting the pH value of the waste concentrated acid liquor to about 1.5, maintaining the pH value, and adding univalent cations such as NH4+ or Na + at 90-100 ℃, and precipitating the jarosite from the leaching liquor. After the jarosite is precipitated, the concentration of iron in the solution is reduced to 1-3 g/L.
The residual liquid left after the extraction in the first extraction tank 31 enters the second extraction tank 33, the second extraction tank 33 is provided with a residual liquid inlet, a residual liquid outlet and a nickel salt solution outlet, the second back extraction tank 34 comprises a nickel salt solution inlet, a nickel salt outlet and a waste liquid outlet, and the nickel salt outlet is communicated with the second evaporative crystallization device 42. The extraction agent for extracting nickel is added into the second extraction tank 33 to extract and separate nickel, the residual liquid without iron enters the second extraction tank 33 to extract nickel salt, the mixed solution containing nickel enters the second back extraction tank 34, the nickel is extracted through back extraction, the pure nickel salt solution is obtained through back extraction, the nickel salt solution enters the second evaporative crystallization device 42 again to obtain pure crystalline nickel salt, and the crystalline nickel salt can be directly sold as a product. The extraction agent and the extraction method for extracting nickel are realized by adopting the prior art.
The residual liquid left after nickel extraction in the second extraction tank 33 enters a third extraction tank 35, the third extraction tank 35 is provided with a residual liquid inlet, a residual liquid outlet and a chromium salt solution outlet, the third reverse extraction tank 36 comprises a chromium salt solution inlet, a chromium salt outlet and a waste liquid outlet, and the chromium salt outlet is communicated with the third evaporative crystallization device 43. Extracting and separating chromium by adding an extracting agent for extracting chromium into the second extraction tank 33, feeding the nickel-free residual liquid into the second extraction tank 33 to extract chromium salt, feeding the mixed solution containing chromium into the third back-extraction tank 36, extracting chromium by back-extraction, obtaining pure chromium salt solution by back-extraction, feeding the chromium salt solution into the third evaporation and crystallization device 43 to obtain pure crystalline chromium salt, wherein the crystalline chromium salt can be directly sold as a product. The extraction agent and the extraction method for extracting chromium are realized by adopting the prior art.
The residual liquid in the third extraction tank 35 enters the fourth evaporation crystallization device 44, the remaining concentrated liquid is salt solution without metal ions, and evaporation, concentration, crystallization and drying treatment are carried out to form crystallized salt for recycling.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solutions of the present invention can be modified or replaced with equivalents without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A stainless steel pickling waste mixed acid recovery processing device is characterized by comprising a pretreatment system, an evaporation concentration system and an extraction system which are sequentially communicated according to the waste mixed acid processing direction;
the evaporation concentration system comprises an evaporation heating tank, a primary condenser, a secondary condenser, a vacuum system and a dilute acid recovery device communicated with the secondary condenser, wherein the evaporation heating tank, the primary condenser, the secondary condenser and the vacuum system are sequentially communicated;
the extraction system comprises a first extraction device for extracting iron, a second extraction device for extracting nickel and a third extraction device for extracting chromium.
2. The waste mixed acid recovery processing device according to claim 1, wherein the evaporation concentration system further comprises a feed circulation pump and a preheater, and the pretreatment storage tank is sequentially communicated with the feed circulation pump, the primary condenser and the preheater; the waste water is divided into two branches after passing through a preheater, and one branch is communicated with an evaporation heating tank, a first-stage condenser, a second-stage condenser, a vacuum system or a dilute acid recovery device through pipelines in sequence.
3. The waste mixed acid recycling device of claim 2, wherein the other branch is connected with a pretreatment storage tank.
4. The waste mixed acid recycling device of claim 1, wherein the evaporation heating tank is connected with an evaporation forced circulation pump, one outlet of the evaporation forced circulation pump is connected with the circulation inlet of the evaporation heating tank, and the other outlet of the evaporation forced circulation pump is connected with the concentrated solution tank.
5. The waste mixed acid recovery processing device of claim 1, wherein the first extraction device comprises a first extraction tank and a first back-extraction tank which are communicated in sequence.
6. The waste mixed acid recovery processing device of claim 4, wherein the first extraction device comprises a second extraction tank and a second back extraction tank which are communicated in sequence; the second extraction tank is communicated with the first extraction tank.
7. The waste mixed acid recovery processing device of claim 5, wherein the first extraction device comprises a third extraction tank and a third back extraction tank which are communicated in sequence; the third extraction tank is communicated with the second extraction tank.
8. The waste mixed acid recovery processing device according to claim 1, further comprising an evaporative crystallization device, wherein the evaporative crystallization device comprises a first evaporative crystallization device for evaporating iron salt, a second evaporative crystallization device for evaporating nickel salt, a third evaporative crystallization device for evaporating chromium salt and a fourth evaporative crystallization device for evaporating salt solution not containing metal ions; the first evaporative crystallization device is communicated with the first extraction device, the second evaporative crystallization device is communicated with the second extraction device, and the third evaporative crystallization device and the fourth evaporative crystallization device are communicated with the third extraction tank.
9. The waste mixed acid recovery processing device of claim 1, wherein the evaporation heating tank is internally sprayed with a teflon layer, and the preheater, the primary condenser and the secondary condenser are internally sprayed with a teflon coating.
10. The waste mixed acid recovery processing device of claim 1, wherein the pretreatment system comprises a waste mixed acid tank, a water pump, a filtering device and a pretreatment storage tank which are sequentially communicated through a pipeline; the filter device comprises at least one of a wire-wound cartridge filter, a bag filter, and a PP cartridge filter.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110395837A (en) * | 2019-08-01 | 2019-11-01 | 广州市中绿环保有限公司 | A kind of acid-washing stainless steel waste mixed acid recycling and processing device and technique |
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