CN104831298B - A kind of method and device of spray roasting regeneration stainless steel nitration mixture acid-washing waste acid - Google Patents
A kind of method and device of spray roasting regeneration stainless steel nitration mixture acid-washing waste acid Download PDFInfo
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- CN104831298B CN104831298B CN201510195327.3A CN201510195327A CN104831298B CN 104831298 B CN104831298 B CN 104831298B CN 201510195327 A CN201510195327 A CN 201510195327A CN 104831298 B CN104831298 B CN 104831298B
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Abstract
The present invention relates to a kind of acid-washing waste acid method and device of spray roasting regeneration stainless steel nitration mixture, its reaction is made into solid metal iron powder and sour gas using roaster high-temperature oxydation spent acid, again generation regeneration nitration mixture is absorbed through sprinkling, including roaster, scraper, pelletizer, Venturi scrubber, absorption tower, washer, roast furnace top arranges 2 spray guns, and spray gun is lifted by pneumatic means；Roasting furnace bottom is connected with scraper, and the rotated valve of scraper is connected with pelletizer；Roaster is connected with Venturi scrubber, and Venturi scrubber is connected with absorption tower, and absorption tower is connected with washer；Washer is connected through smoke exhaust fan, horizontal type liquid drop separator with denitrification system.Advantage is：Spent acid generates brown iron oxide and regenerated acid, has reclaimed the stainless steel metal ion and free acid closed during pickling with acidifying, regenerated acid return pickling line recycles, and reduces sour consumption by high-temperature roasting, decomposition.
Description
Technical field
It is a kind of using spraying roasting the invention belongs to metallurgy industry stainless steel nitration mixture acid-washing waste acid regeneration field, especially design
Burning method regenerates the method and device of stainless steel nitration mixture acid-washing waste acid.
Background technology
Stainless steel will pass through pickling process, pickle generally use nitric acid and hydrofluoric acid mixed preparing before cold rolling processing,
Caused spent acid is typically handled in medium-sized and small enterprises using neutralisation after pickling, although some Parameter adjustables give up to discharge standard
Free acid and metal oxide in acid can not all reclaim, and waste of resource, using quick lime neutralisation treatment, sludge quantity is big, some
Harmful element can also drain therewith, environment be caused seriously to pollute, in medium-sized and small enterprises, neutralisation is used till today.Adjusted according to market
Look into, to meet that medium-sized and small enterprises seek the urgent demand of spent acid New Method for Processing.
The content of the invention
For overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of spray roasting regeneration stainless steel nitration mixture acid
The method and device of spent acid is washed, using spray roasting, the pyrolytic metal oxide in roaster, evaporates in spent acid and dissociates
Nitric acid and hydrofluoric acid, obtain the spherical particle of metal oxide and recycling nitration mixture.
To achieve the above object, the present invention is achieved through the following technical solutions：
A kind of method of spray roasting regeneration stainless steel nitration mixture acid-washing waste acid, makes it using roaster high-temperature oxydation spent acid
Solid metal iron powder and sour gas are reacted into, then generation regeneration nitration mixture is absorbed through sprinkling, specifically includes following steps：
1) 55 DEG C~65 DEG C of the waste mixed acid that pickling line comes is sent into waste acid pot storage, is sent spent acid by filter by spent acid pump
To Venturi scrubber bottom, then circulated and sprayed on Venturi scrubber top by venturi circulating pump, to cool down from roaster
Furnace gas out；Meanwhile part free acid volatilizees, a part of gelled acid is delivered to roaster by branch pipe and is fed in cyclic process
Pump；Sprayed again by spray gun into stove, the spent acid of the atomisation 590-600 DEG C of high temperature in stove issues biochemical reaction, generates
Fe2O3And a small amount of NiO, Cr2O3、TiO2Powder, mix and fallen in stove with iron powder, then pelletizer is promoted through scraper, add water to make
Into 5~25mm of diameter bead；
2) go out Venturi scrubber enters absorption tower bottom containing sour furnace gas, and the liquid that washer is taken out by absorber feed pump exists
Top is sprayed, when the gas of absorption tower bottom rises through filler in tower, liquid that the nitration mixture gas in gas is sprayed by top
Body absorbs, and generation regeneration nitration mixture, is discharged from absorption tower bottom, then send Venturi scrubbing by a nitration mixture part is regenerated by regenerated acid pump
Device sprays, and another part send regenerated acid tank to store after cooler is cooled to 40-50 DEG C；The furnace gas for going out absorption tower enters washer,
The liquid of absorber feed pump outlet stool sprinkling washer is arranged at washer top, washs furnace gas, while constantly mended to washer
The washings of pickling line are filled, the furnace gas after washing enters smoke exhaust fan, and denitrification system is then entered after liquid drop separator；
3) after denitrification system is by bottled liquefied ammonia decompression gasification, quantitatively input in furnace gas pipeline, furnace gas is heated to
Reacted after 290-310 DEG C with ammonia, the NOx in furnace gas resolves into harmless N by honeycomb catalyst device2And vapor, through not
The steel stack that becomes rusty is discharged.
Described venturi circulating pump spray pressure is 0.25-0.35Mpa；
Spray roasting regenerates the device of stainless steel nitration mixture acid-washing waste acid, including roaster, scraper, pelletizer, Wen Qiu
In washer, absorption tower, washer, roaster be divided into up and down two parts form, 3 main burners of upper part arranged tangential, bottom
1 secondary burner is put in distribution, and the bottom of top and the bottom is flat-bottom structure, and upper lower bottom part has uniformly put 1 rotation scraper, for making
Brown iron oxide is loose and scrapes roaster by brown iron oxide is mandatory；Roast furnace top arranges 2 spray guns, and spray gun is by pneumatically filling
Put lifting；Roasting furnace bottom is connected with scraper, and the rotated valve of scraper is connected with pelletizer；Roaster and Venturi scrubber
It is connected, Venturi scrubber is connected with absorption tower, and absorption tower is connected with washer；Washer is through smoke exhaust fan, horizontal type drop
Separator is connected with denitrification system.
Described rotary valve ensures negative pressure in stove to discharge brown iron oxide.
For described roasting furnace body all using stainless steel making, inside does not set refractory material, and outside uses insulation material
Insulation.
Described absorption tower is made by the compound PVDF materials of fiberglass, and inside is provided with the ladder ring packing of PVDF materials, is used
In absorbing the acid gas of decomposition and evaporation in roaster, the equipment of Venturi scrubber two, regeneration nitration mixture is become, regeneration nitration mixture enters
It is standby to enter regenerated acid tank.
Venturi circulating pump circulation acid solution, to cool down, wash furnace gas, evaporation are provided with described Venturi scrubber
Spent acid in inspissator.
Described washer, which is provided with, circulates pump circulation sprinkling washings, contains sour tail gas after washing absorption tower, in furnace gas
Acid gas further absorb.
Compared with prior art, the beneficial effects of the invention are as follows：
The suitable medium-sized and small enterprises of the present invention, meet national requirements for environmental protection after processed by the invention, nitration mixture acid-washing waste acid is renewable,
The metal oxide of recovery can be used for the raw material of metal smelt, and also can return to pickling line after the nitration mixture of regeneration is formulated reuses,
Production cost is reduced, is turned harm into good, is turned waste into wealth.The rate of recovery of metal ion is 98% or so；The rate of recovery of FH acid exists
95% or so；HNO3The rate of recovery 50% or so, its reason is mainly that nitric acid is unstable when temperature is high, pressure is low, easily point
Solve as NO2And H2O。
Spent acid is generated brown iron oxide and regenerated acid, reclaimed stainless with acidifying conjunction during pickling by high-temperature roasting, decomposition
Steel metal ion and free acid, as byproduct export trade, pickling line circulation is returned after the allotment of major product regenerated acid to be made brown iron oxide
With, make pickling, regeneration form closed cycle, reduce sour consumption.After nitride almost all resolves into harmless nitrogen in tail gas
Waste gas is discharged into air by chimney, amount of nitrides in waste gas：＜ 300mg/m3, meet GB28665-2012 national standards.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention.
Fig. 2 is regenerated acid tank field process chart.
Fig. 3 is roaster combustion system process chart.
In figure：1- roaster 2- Venturi scrubber 3- waste acid pot 4- spent acid pump 5- filter 6- venturi
Circulating pump 7- roaster feed pump 8- spray gun 9- scraper 10- pelletizer 11- rotary valve 12- absorption tower 13-
Regenerated acid pump 14- cooler 15- regenerated acid tank 16- washer 17- absorber feed pump 18- smoke exhaust fans 19-
The main 223- masters of burner two of the liquid drop separator 20- denitrification system 21- chimney main 222- of burner one of 22- pair burners 221-
The 23- sack filling machine 24- gelled acid filters of burner three.
Embodiment
The present invention is described in detail with reference to Figure of description, it should be noted that the implementation of the present invention is unlimited
In following embodiment.
See Fig. 1-Fig. 3, the method that spray roasting regenerates stainless steel nitration mixture acid-washing waste acid, using the high-temperature oxydation of roaster 1
Spent acid makes its reaction into solid metal iron powder and sour gas, then absorbs generation regeneration nitration mixture through sprinkling, specifically includes following step
Suddenly：
1) 55 DEG C~65 DEG C of the waste mixed acid that pickling line comes is sent into waste acid pot 3 and stored, and spent acid is passed through into filter by spent acid pump 4
5 are sent to the bottom of Venturi scrubber 2, then are circulated and sprayed on the top of Venturi scrubber 2 by venturi circulating pump 6, and venturi follows
The spray pressure of ring pump 6 is 0.25-0.35Mpa (most preferably 0.3Mpa)；To cool down the furnace gas come out from roaster 1, furnace gas is by 380
DEG C drop to 95 DEG C；Meanwhile part free acid volatilizees, a part of gelled acid is delivered to roaster by branch pipe and is fed in cyclic process
Pump 7；Sprayed again by spray gun 8 into stove, the spent acid of the atomisation 590-600 DEG C of high temperature in stove issues biochemical reaction, raw
Into Fe2O3And a small amount of NiO, Cr2O3、TiO2Powder, mix and fallen in stove with iron powder, then pelletizer 10 is promoted through scraper 9, add
Water causes 5~25mm of diameter bead (most preferably diameter 20mm), enters after sack filling machine 23 is packed and takes out；
2) go out Venturi scrubber 2 enters the bottom of absorption tower 12 containing sour furnace gas, and washer 16 is taken out by absorber feed pump 17
Liquid top spray, when the gas of the bottom of absorption tower 12 rises through filler in tower, on the nitration mixture gas in gas
The liquid absorption of portion's sprinkling, generation regeneration nitration mixture, is discharged from the bottom of absorption tower 12, then will regenerate nitration mixture one by regenerated acid pump 13
Dispensing Venturi scrubber 2 sprays, and another part send regenerated acid tank 15 to store (cooling after cooler 14 is cooled to 40-50 DEG C
It is optimal to 45 DEG C)；The furnace gas for going out absorption tower 12 enters washer 16, and the spray of the outlet stool of absorber feed pump 17 is arranged at the top of washer 16
The liquid of washer 16 is spilt, washs furnace gas, while the washings of pickling line, the furnace gas after washing are constantly supplemented to washer 16
Into smoke exhaust fan 18, denitrification system 20 is then entered after liquid drop separator 19；
3) after denitrification system 20 is by bottled liquefied ammonia decompression gasification, quantitatively input in furnace gas pipeline, furnace gas is heated to
Reacted after 290-310 DEG C with ammonia, the NOx in furnace gas resolves into harmless N by honeycomb catalyst device2And vapor, through not
Rust steel stack 21 is discharged.
Whole technical process, which can adopt, computerizeds control, bunch grade adjustment, the monitoring of whole process picture, makes important parameter control essence
Standard, ensure product quality, save manpower and labor intensity.
Spray roasting regenerate stainless steel nitration mixture acid-washing waste acid device, including roaster 1, scraper 9, pelletizer 10,
Venturi scrubber 2, absorption tower 12, washer 16, the bottom of roaster 1 are connected with scraper 9, the rotated valve 11 of scraper 9 with
Pelletizer 10 connects；Roaster 1 is connected with Venturi scrubber 2, and Venturi scrubber 2 is connected with absorption tower 12, absorption tower
12 are connected with washer 16；Washer 16 is connected through smoke exhaust fan 18, horizontal type liquid drop separator 19 with denitrification system 20.
Wherein, roaster 1 is made using nickeliferous ＞ 25% nickelic stainless steel, using gas fuel combustion flue gas as heat
Source, pyrolytic spray into the spent acid in stove and metal oxide, evaporation spent acid the nitric acid and hydrofluoric acid to dissociate, produce graininess
Metal oxide, mainly there is following reaction：FeF3→Fe2O3+HF↑H2O (liquid) → H2O (vapour)
HF (liquid) → HF (gas) ↑
HNO3(liquid) → HNO3(gas) ↑
MeFx→MeO↓+HF↑
Me(NO3)y→MeO↓+HNO3↑
Roaster 1 is divided into two parts up and down and formed.The main burner 221-223 of upper part arranged tangential 3, lower part arrangement 1
Platform pair burner 22.The bottom of top and the bottom uses flat-bottom structure, and upper lower bottom part all arranges 1 rotation scraper 9, for making oxygen
It is loose and scrape roaster 1 by brown iron oxide is mandatory to change iron powder, avoids bottom from accumulating brown iron oxide.Reacting furnace top layout
2 spray guns 8,1 is standby with 1, is used alternatingly.Spray gun 8 is lifted using pneumatic means.Whole body of heater is interior all using stainless steel making
Portion does not have refractory material, lining acid resisting material is not had in stove, its advantage is short construction period, and maintenance capacity is few.Using guarantor outside body of heater
Adiabator is incubated.Rotary valve 11 is configured with outside roaster 1, brown iron oxide can be discharged and ensure that negative pressure in stove.It is further provided with
Brown iron oxide pelletizer 10, brown iron oxide is made into spherolite, a diameter of 5~25mm, spherical iron powder packs export trade.
Venturi scrubber 2, made by stainless steel, PVDF materials, if venturi circulating pump 6 circulates acid solution, cooling, washing
Furnace gas, spent acid in evaporation concentrator.
The absorption tower 12 (3mm is thick optimal) of the compound PVDF materials of fiberglass, making its performance, both high temperature resistant is rotten by force, saves and throws again
Money, inside set the ladder ring packing of PVDF materials, decompose and steam in 2 liang of roaster 1, Venturi scrubber equipment for absorbing
The acid gas of hair, become regeneration nitration mixture.It is standby into regeneration nitration mixture basin.
Stainless steel and the washer of PVDF materials 16, washer 16 set circulation pump circulation sprinkling washings, washing absorption tower
Contain sour tail gas after 12, the acid gas in furnace gas is further absorbed.
Inner flue gas of the stove is extracted out using smoke exhaust fan 18, and overcomes venturi and the resistance on absorption tower 12, negative pressure is in before machine,
Can acid gas is excessive in anti-locking system, while furnace gas is delivered into next procedure.
Using catalysis denitrification system 20, the NO in furnace gas is decomposed with ammoniaX, harmless nitrogen is become, because platinum is urged
Agent is too expensive, can use V2O5Catalyst is made, burning coal gas does thermal source, and main chemical reactions are as follows：
NO2+NO+2NH3→2N2+3H2O
4NO+4NH3+O2→4N2+6H2O
Reaction temperature：300 DEG C~350 DEG C, nitride almost all is resolved into waste gas after harmless nitrogen by chimney 21
It is discharged into air, amount of nitrides in waste gas：＜ 300mg/m3, meet GB28665-2012 national standards.
The top of roaster 1 is provided with protection cap, to protective roast stove 1.
The suitable medium-sized and small enterprises of the present invention, meet national requirements for environmental protection after processed by the invention, nitration mixture acid-washing waste acid is renewable,
The metal oxide of recovery can be used for the raw material of metal smelt, and also can return to pickling line after the nitration mixture of regeneration is formulated reuses,
Production cost is reduced, is turned harm into good, is turned waste into wealth.The rate of recovery of metal ion is 98% or so；The rate of recovery of FH acid exists
95% or so；HNO3The rate of recovery 50% or so, its reason is mainly that nitric acid is unstable when temperature is high, pressure is low, easily point
Solve as NO2And H2O。
Spent acid is generated brown iron oxide and regenerated acid, reclaimed stainless with acidifying conjunction during pickling by high-temperature roasting, decomposition
Steel metal ion and free acid, as byproduct export trade, pickling line circulation is returned after the allotment of major product regenerated acid to be made brown iron oxide
With, make pickling, regeneration form closed cycle, reduce sour consumption.After nitride almost all resolves into harmless nitrogen in tail gas
Waste gas is discharged into air by chimney, amount of nitrides in waste gas：＜ 300mg/m3, meet GB28665-2012 national standards.
Claims (1)
- A kind of 1. method of spray roasting regeneration stainless steel nitration mixture acid-washing waste acid, it is characterised in that using roaster high temperature oxygen Changing spent acid makes its reaction into solid metal iron powder and sour gas, then absorbs generation regeneration nitration mixture through sprinkling, specifically includes following Step：1) 55 DEG C~65 DEG C of the waste mixed acid that pickling line comes is sent into waste acid pot storage, and spent acid is sent into text by filter by spent acid pump Washer bottom in mound, then circulated and sprayed on Venturi scrubber top by venturi circulating pump, come out with cooling from roaster Furnace gas；Meanwhile part free acid volatilizees, a part of gelled acid delivers to roaster feed pump by branch pipe in cyclic process； Sprayed again by spray gun into stove, the spent acid of the atomisation 590-600 DEG C of high temperature in stove issues biochemical reaction, generates Fe2O3 And a small amount of NiO, Cr2O3、TiO2Powder, mix and fallen in stove with iron powder, then pelletizer is promoted through scraper, add water to cause directly 5~25mm of footpath bead；Described venturi circulating pump spray pressure is 0.25-0.35Mpa；2) go out Venturi scrubber enters absorption tower bottom containing sour furnace gas, and the liquid of washer is taken out on top by absorber feed pump Sprinkling, when the gas of absorption tower bottom rises through filler in tower, the liquid that the nitration mixture gas in gas is sprayed by top is inhaled Receive, generation regeneration nitration mixture, discharged from absorption tower bottom, then send Venturi scrubber to spray by a nitration mixture part is regenerated by regenerated acid pump Spill, another part send regenerated acid tank to store after cooler is cooled to 40-50 DEG C；The furnace gas for going out absorption tower enters washer, washing The liquid of absorber feed pump outlet stool sprinkling washer is arranged at device top, washs furnace gas, while constantly to washer supplemental acid The washings of line are washed, the furnace gas after washing enters smoke exhaust fan, and denitrification system is then entered after liquid drop separator；3) after denitrification system is by bottled liquefied ammonia decompression gasification, quantitatively input in furnace gas pipeline, furnace gas is heated to 290-310 Reacted after DEG C with ammonia, the NOx in furnace gas resolves into harmless N by honeycomb catalyst device2And vapor, through stainless steel smoke Chimney is discharged；Realize the device of the method for spray roasting regeneration stainless steel nitration mixture acid-washing waste acid, including roaster, scraper, make Ball machine, Venturi scrubber, absorption tower, washer, roaster are divided into two parts up and down and formed, 3 masters of upper part arranged tangential Burner, lower part arrange 1 secondary burner, and the bottom of top and the bottom is flat-bottom structure, and upper lower bottom part has uniformly put 1 rotary harrow material Machine, for making brown iron oxide loose and scraping roaster by brown iron oxide is mandatory；Roast furnace top arranges 2 spray guns, spray gun Lifted by pneumatic means；Roasting furnace bottom is connected with scraper, and the rotated valve of scraper is connected with pelletizer；Roaster and text Washer is connected in mound, and Venturi scrubber is connected with absorption tower, and absorption tower is connected with washer；Washer is through Smoke Machine, horizontal type liquid drop separator are connected with denitrification system.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105327903B (en) * | 2015-11-19 | 2018-04-17 | 中冶南方工程技术有限公司 | Spray roasting acid purification system and its cleaning method with sour rifle |
| CN105624715B (en) * | 2016-02-29 | 2017-12-22 | 中冶南方工程技术有限公司 | The acid purification system and its control method of the adaptive complex acid of temperature control |
| CN107574450B (en) * | 2017-10-20 | 2020-07-24 | 鞍山创鑫环保科技股份有限公司 | Stainless steel pickling waste liquid regeneration method and system |
| CN107601605B (en) * | 2017-10-20 | 2023-05-09 | 鞍山创鑫环保科技股份有限公司 | Technology and system for improving yield of regenerated nitric acid from stainless steel pickling waste liquid |
| CN108483398A (en) * | 2018-05-16 | 2018-09-04 | 攀钢集团西昌钢钒有限公司 | A kind of acid regeneration roaster and its acid regeneration process |
| CN109467065B (en) * | 2018-11-30 | 2023-09-19 | 中冶南方工程技术有限公司 | Stainless steel mixed acid waste liquid regenerated acid equipment |
| CN110124463A (en) * | 2019-06-11 | 2019-08-16 | 湖北瑞力源环保科技有限公司 | A kind of exhaust gas purification system and technique for spray roasting hydrochloric acid regenerating device |
| CN112359366B (en) * | 2020-10-10 | 2021-11-23 | 东南大学 | Two-stage roasting regeneration device and method for waste mixed acid |
| CN113774213A (en) * | 2021-08-16 | 2021-12-10 | 中冶南方工程技术有限公司 | Recycling method and system of stainless steel mixed acid pickling sludge |
| CN114314976B (en) * | 2021-11-17 | 2022-09-16 | 江苏新裕泰华环保集团有限公司 | Recovery treatment equipment for treating acidic industrial wastewater and use method thereof |
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| CN204661829U (en) * | 2015-04-22 | 2015-09-23 | 鞍山创新废酸除硅再生工程有限公司 | A kind of device of spray roasting regeneration stainless steel nitration mixture acid-washing waste acid |
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| CN204661829U (en) * | 2015-04-22 | 2015-09-23 | 鞍山创新废酸除硅再生工程有限公司 | A kind of device of spray roasting regeneration stainless steel nitration mixture acid-washing waste acid |
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| 喷雾焙烧工艺在混酸再生中的应用;王瑞红;《科技情报开发与经济》;20101231;第20卷(第36期);第169-171页 * |
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Address after: 114000 6 Yongkang street, Tiexi Economic Development Zone, Anshan, Liaoning. Patentee after: Anshan Chuangxin environmental protection Polytron Technologies Inc Address before: 114000 6 Yongkang street, Tiexi Economic Development Zone, Anshan, Liaoning. Patentee before: Anshan innovation spent acid silica removal reengineer Co., Ltd |
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