CN102259954A - Waste acid recycling process and matching device thereof - Google Patents
Waste acid recycling process and matching device thereof Download PDFInfo
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- CN102259954A CN102259954A CN 201110215697 CN201110215697A CN102259954A CN 102259954 A CN102259954 A CN 102259954A CN 201110215697 CN201110215697 CN 201110215697 CN 201110215697 A CN201110215697 A CN 201110215697A CN 102259954 A CN102259954 A CN 102259954A
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- spent acid
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Abstract
The invention relates to a waste acid recycling process and a matching device thereof, belonging to the technical field of water treatment. The waste acid recycling process comprises the following steps of: carrying out pre-treatment on waste acid by virtue of ultrafiltration membrane air flotation; vertically mounting an ultrafiltration membrane assembly, and then feeding the waste acid from the lower part of the ultrafiltration membrane assembly by utilizing a gas-liquid hybrid power device to carry out ultrafiltration membrane air flotation purification treatment; and recycling the waste acid by adopting air flotation dialysis after the pre-treatment, thus having the advantages of low energy consumption, strong operability, good effluent quality, small waste acid recycling volume, high concentration and the like. The matching device comprises a waste acid tank and a pre-treatment ultrafiltration membrane assembly which is vertically arranged, wherein the pre-treatment ultrafiltration membrane assembly is connected with a penetrating fluid discharge pipe, the lower part of the pre-treatment ultrafiltration membrane assembly is connected with a feeding pipe, the upper part of the pre-treatment ultrafiltration membrane assembly is connected with a concentrated solution discharge pipe, the other end of the feeding pipe of the pre-treatment ultrafiltration membrane assembly is communicated with the waste acid tank, and the feeding pipe is provided with the gas-liquid hybrid power device. The device has a compact structure, is stable in operation and simple in management and is applicable to recycling of multiple waste acids.
Description
Technical field
The invention belongs to water-treatment technology field, be specifically related to a kind of spent acid reclaim technology and with the device of this process matching.
Background technology
The steel members blank electroplating surface, the spraying last as all will through overpickling with remove the surface oxide compound, produce a large amount of spent pickle liquors simultaneously.The workpiece kind is different with processing request, and the requirement of pickle solution also is not quite similar, and wherein cleans the most common with hydrochloric acid.Hydrochloric acid cleans in the waste liquid and mainly contains Fe
2+, H
+And Cl
-Ion exists a certain amount of greasy dirt and suspended substances such as silica flour, carbon element in addition.Just do not handle directly discharging if these spent pickle liquors do not add, not only waste resource, also can bring serious environmental to pollute.
At the Iron And Steel Industry spent pickle liquor, present processing mode mainly contains crystallisation by cooling method, evaporative crystallization method, torch firing decomposition method, ion exchange method, solvent extration, neutralisation, dialysis etc.But problems such as investment of these processing mode ubiquities and running cost height, treatment effect are undesirable, wherein methods such as crystallisation by cooling method, evaporative crystallization method, torch firing decomposition method also have defectives such as energy consumption height, maintenance of the equipment difficulty, also can produce large quantity of exhaust gas and waste residue simultaneously; Ion exchange method and dialysis operation stability are poor, and recovered acid is not thorough; Solvent extration and neutralisation need consume a large amount of chemical reagent, bring secondary pollution easily.
As seen, traditional spent acid processing mode can not satisfy the policy requirements of country's " recycling economy ", and market presses for the novel spent acid treatment technology that investment is little, the rate of recovery is high, the recovered acid volume is little, working cost is low.
Summary of the invention
Purpose of the present invention aims to provide a kind of spent acid and reclaims technology, and the device with this process matching also is provided simultaneously.
Based on above-mentioned purpose, the present invention has taked following technical scheme: a kind of spent acid reclaims technology, comprise and utilize ultra-filtration membrane air supporting that spent acid is carried out pretreated step: hyperfiltration membrane assembly vertically is installed, is utilized the gas-liquid mixed power set that spent acid is infeeded from the hyperfiltration membrane assembly bottom to carry out the ultra-filtration membrane air-float purification then and handle.
Utilize the gas-liquid mixed power set that pretreated spent acid is infeeded dialyzer, carry out the air supporting dialysis.
Raffinate after the dialysis (residue wastewater) is carried out aeration, precipitation and solid-liquid separation successively, and liquid phase (waste water) enters the aftertreatment hyperfiltration membrane assembly and carries out the processing of ultra-filtration membrane air-float purification once more under the promotion of gas-liquid mixed power set.
The penetrating fluid (clear water) of discharging from the aftertreatment hyperfiltration membrane assembly returns dialyzer and does and receive liquid and use, and concentrated solution (air water mixed solution) returns precipitate phase and does circular treatment.
The concentrated solution of discharging from the pre-treatment hyperfiltration membrane assembly (gas acid mixed solution) imports circular treatment in the untreated spent acid.
Described spent acid reclaims the corollary apparatus of technology, comprise spent acid groove and the vertical pre-treatment hyperfiltration membrane assembly of installing, be connected with the penetrating fluid vent pipe on the pre-treatment hyperfiltration membrane assembly, and the bottom is connected with feed-pipe, top is connected with the concentrated solution vent pipe, the other end of pre-treatment hyperfiltration membrane assembly feed-pipe is communicated with the spent acid groove, and this feed-pipe is provided with the gas-liquid mixed power set.
The other end of described pre-treatment hyperfiltration membrane assembly concentrated solution vent pipe inserts in the spent acid groove.
Described device also comprises buffer memory groove and dialyzer, and the other end of pre-treatment hyperfiltration membrane assembly penetrating fluid vent pipe inserts in the buffer memory groove, and the buffer memory groove is communicated with the opening for feed of dialyzer by pipeline, and this connecting pipe is provided with the gas-liquid mixed power set.
The raffinate outlet of described dialyzer links to each other with aeration tank, settling tank, solid-liquid separator and aftertreatment hyperfiltration membrane assembly successively, and the water outlet of solid-liquid separator is communicated with the feed-pipe of aftertreatment hyperfiltration membrane assembly, and this feed-pipe is provided with the gas-liquid mixed power set; The concentrated solution vent pipe of aftertreatment hyperfiltration membrane assembly returns settling tank and inserts wherein.
The other end of the penetrating fluid vent pipe of aftertreatment hyperfiltration membrane assembly links to each other with the reception liquid of dialyzer inlet.
Spent acid of the present invention reclaims the air supporting of technology utilization ultra-filtration membrane spent acid is carried out pre-treatment, can guarantee that hyperfiltration membrane assembly is long-term, effectively remove colloid in the spent acid in the steady running, suspended substances such as greasy dirt and a large amount of silica flour, carbon element: spent acid carries a large amount of microbubbles and enters hyperfiltration membrane assembly, suspended substances such as the greasy dirt in the spent acid, colloid and silica flour, carbon element stick on the microbubble and taken out of membrane module by microbubble behind membrane sepn, have effectively prevented the pollution on film surface; Simultaneously, microbubble purges the film surface constantly, has also played the effect on lasting purification membrane surface.Membrane process is introduced in air supporting, thoroughly overcome the defective that membrane module easily stopped up and cleaned difficulty, kept that membrane separation technique is efficient, energy-saving and environmental protection, facility compact, process are simple, be easy to advantage such as control, for the later stage recovering waste acid has been paved road.
Utilize the ultra-filtration membrane air-float purification to handle spent acid is carried out pre-treatment, ferrous ion in the spent acid can be converted into ferric ion, no matter later stage is to adopt dialysis or adopt traditional heating roasting method to reclaim spent acid, can improve the working efficiency of the clearance and the equipment of iron ion.
Shandong sodium method now has in the world comparatively widely and uses as the representative in the roasting method.The Shandong roughly flow process of sodium method now is: spent acid at the preconcentrator internal heating, is concentrated the back with being pumped into the stoving oven top, make it be vaporific and spray in the stove; Atomizing spent acid decomposes in stove generates hydrogen chloride gas and powdery ferric oxide; Ferric oxide is discharged from furnace bottom; Hydrogenchloride reaches preconcentrator from furnace roof through double-cyclone dust collector with combustion gases, and the gas after double-cyclone dust collector, preconcentrator purify postcooling enters the bottom, absorption tower from preconcentrator; Hydrogen chloride in gas is absorbed by the washing water from the cat head ejection, forms regenerating acid at the bottom of tower, and the tail gas of cat head is taken away through chimney by blower fan and discharged.
Though Shandong sodium method principle now is simple, but its road in the popularization of China is not smooth, investment is big, energy consumption is high, maintenance of the equipment is difficult except that having, easily produce in the operational process the shortcoming such as waste gas waste residue, and shower nozzle should stop up in the torch firing process, the treatment effect instability also is the important factor that influences its popularization.In the actual production, spent acid is not the ideal system of a stable homogeneous, except that chlorion, iron ion, also has a large amount of other impurity in the system, such as silica flour, carbon element etc.If spent acid is not carried out suitable pre-treatment, will certainly the frequent jams shower nozzle during torch firing, influence organic efficiency and effect.If adopt ultra-filtration membrane air supporting in advance spent acid to be carried out pre-treatment, not only can remove the easily stifled impurity in the spent acid in time, effectively, help Shandong carrying out smoothly of sodium method now.
Dialysis is another spent acid recovery method comparatively commonly used.Dialyzer externally has four interfaces usually, be opening for feed, reception liquid inlet, dialyzate outlet and raffinate outlet: spent acid and reception liquid (clear water, the general tap water that uses) respectively after opening for feed, acceptable solution inlet enter dialyzer in two side flow of dialyzer, under the promotion of concentration difference, Cl-in the waste acid water passes dialyzer and enters in the acceptable solution, in order to keep electric neutrality, Cl-can carry equimolar positively charged ion and enter acceptable solution together in migration simultaneously.Because Fe in the spent acid
2+Travelling speed in the film inner duct is more than H
+Little, macroscopical result of formation is: HCl is moved to and is formed recovered acid in the acceptable solution, and the pH value of spent acid one side (residue wastewater) constantly raises, and is trapped in the Fe in the spent acid
2+Along with gradating, the rising of pH value is Fe
3+But in the practice, also contain a large amount of greasy dirts and particulate matter such as silica flour, carbon element in the spent acid, if directly with the spent acid feeding dialyzer of such composition complexity, have more than is needed dialyzer that how long will make stops up, and makes whole spent acid treatment system paralysis.This has become the major obstacles that hinders existing dialysis industry popularization.Before entering dialyzer, spent acid utilize ultra-filtration membrane air supporting that spent acid is carried out pre-treatment, can play the effect of the following aspects: 1) remove greasy dirt and other particulate matter in the spent acid, as silica flour, carbon element, bacterium etc., improved the influent quality of back segment dialyzer, for dialyzer continues, steady operation provides guarantee; Simultaneously, compare with ultrafiltration, ultra-filtration membrane air supporting can guarantee membrane module operation steady in a long-term, can not influence the working efficiency of whole waste acid recovery system because of pre-treatment.Dissolve in a large amount of air in the spent acid when 2) the ultra-filtration membrane air-float purification is handled, be equivalent to spent acid has been carried out the aeration processing, can impel the Fe in the spent acid
2+Be converted into Fe
3+, hydrated radius improves, and separates with HCl easier being trapped of dialysis stage, even is converted into Fe (OH)
3From spent acid, separate out.3) spent acid is played certain inspissated, helped to improve the concentration of dialysis recovered acid.
The present invention adopts dialysis to come recovered acid, and has also added air supporting in the dialysis stage after utilizing the ultra-filtration membrane air-float purification that spent acid is carried out pre-treatment, and this more helps Fe
2+To Fe
3+Transform.In addition, air supporting can prevent that equally pollutent from the dialyzer surface attachment, keep clean the dialyzer surface, has guaranteed the operation stability of dialyzer.Dialysis constantly reduces the acid in the residue wastewater, and the pH value raises; When pH value reaches 3 when above, just have lot of F e (OH)
3Separate out.And among the present invention, the pH value of residue wastewater can reach about 6, near neutral, has reduced the alkali number that adds in later stage significantly.And the concentration of recovered acid reaches as high as 17%, and volume is also very little, can directly return to be made into pickle solution in the complex acid groove and to recycle.
Further residue wastewater is carried out aeration after the dialysis, impel Fe
2+Be converted into Fe
3+, residue wastewater finally is converted into the yellow mud water that is dispersed with a large amount of ironic hydroxides.For making Fe
2+Oxidation to carry out ground more thorough, can in the aeration tank, add small amounts of sodium hydroxide and regulate pH value to 7-8.Behind the aeration residue wastewater squeezed in the settling tank and precipitate, be oxidizing reaction and Fe (OH)
3Crystalline is grown, is separated out the competent time that provides.Thereafter through solid-liquid separation, isolated body refuse composition nearly all is Fe (OH)
3, purity can reach 99%, is fed in the market and can increases extra income for enterprise as byproduct.After the solid-liquid separation, also can contain a spot of Fe (OH) in the liquid phase
3, utilize ultra-filtration membrane air supporting once more it to be carried out purifying treatment, water outlet (penetrating fluid) is qualified discharge directly, or uses as the reception liquid of dialyzer, and concentrated solution (air water mixed solution) then returns makes circular treatment in the settling tank.
Generally speaking, spent acid recovery method of the present invention has that working cost is extremely low, energy consumption is low, workable, advantages such as effluent quality good, the spent acid recovery volume is little, concentration height, the dialyzer of using when ultra-filtration membrane of using in pre-treatment and the aftertreatment and recovered acid can both long-time steady operation, for the working efficiency of membrane lifetime and whole recovery system provides guarantee.The more important thing is that this method can reclaim acid, water and iron ion in the spent acid respectively, has realized the recycling of spent acid, thereby has had vast market prospect.Outside the demineralizing acid type iron and steel pickling waste liquid, Application Areas of the present invention can also be extended to industries such as titanium white production, wet type copper smelting, and the kind of recovered acid can comprise H
2SO
4, HCl, HF, HNO
3, CH
3COOH, H
3PO
4Deng, the metal ion that relates to comprises transition metal ion, rare earth ion and magnesium calcium etc.Can also be used to contain the purification separation processing of metal-salt waste water, as the corrosive fluid liquid waste disposal (iron trichloride) of printed-wiring board (PWB).
Description of drawings
Fig. 1 is the schema that spent acid of the present invention reclaims technology;
Fig. 2 is the structural representation of corollary apparatus of the present invention.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
A kind of spent acid reclaims technology, as shown in Figure 1, is by following steps spent acid to be handled after complex acid, pickling:
1) utilize ultra-filtration membrane air supporting that spent acid is carried out pre-treatment: hyperfiltration membrane assembly vertically is installed, utilize the gas-liquid mixed power set that spent acid is infeeded from the hyperfiltration membrane assembly bottom then, utilize the ultra-filtration membrane air-float purification to remove macrobead pollutents such as wherein greasy dirt, silica flour, carbon element; The concentrated solution of discharging from hyperfiltration membrane assembly (gas acid mixed solution) imports circular treatment in the untreated spent acid.
2) air supporting dialysis: utilize the gas-liquid mixed power set that pretreated spent acid is infeeded dialyzer, carry out the air supporting dialysis, dialyzate is recovered acid, and recovered acid returns the recycling of complex acid stage.
3) aftertreatment: raffinate after the dialysis is carried out aeration, precipitation and solid-liquid separation successively, and liquid phase enters the aftertreatment filter membrane component and carries out secondary air supporting ultrafiltration under the promotion of gas-liquid mixed power set; Secondary air supporting ultrafiltration gained penetrating fluid returns dialyzer and does the use of reception liquid, and concentrated solution returns precipitate phase and does circular treatment.
Device with above-mentioned spent acid recovery process matching as shown in Figure 2, comprises spent acid groove 3, pre-treatment hyperfiltration membrane assembly 4, buffer memory groove 5, dialyzer 6, aeration tank 7, settling tank 8, solid-liquid separator 9 and aftertreatment hyperfiltration membrane assembly 10 successively.Two groups of hyperfiltration membrane assemblies 4 and 10 are all vertically installed (it is vertical that the film silk is) and similar: be connected with penetrating fluid vent pipe 4-2,10-2 on it, and the bottom is connected with feed-pipe 4-3,10-3, top is connected with concentrated solution vent pipe 4-1,10-1.Pre-treatment hyperfiltration membrane assembly 4 is communicated with spent acid groove 3 by the feed-pipe 4-3 that is attached thereto, this feed-pipe 4-3 is provided with gas-liquid mixed power set (specifically being combined by fluid pump 12 and compressed air inlet 13 in the present embodiment), and the concentrated solution vent pipe 4-1 that links to each other with pre-treatment hyperfiltration membrane assembly 4 returns spent acid groove 3 and inserts wherein; The other end of the penetrating fluid vent pipe 4-2 of pre-treatment hyperfiltration membrane assembly 4 inserts in the buffer memory groove 5.
The dialyzate outlet 6-3 of dialyzer 6 feeds in the complex acid groove 1 by pipeline, and what complex acid groove 1 downstream connected successively is pickling tank 2 and spent acid groove 3, and fluid pump 12 and valve 11 all have been installed on the connecting tube between complex acid groove 1, pickling tank 2 and the spent acid groove 3.
Solid-liquid separator 9 concrete uses is plate filter in the present embodiment.
Claims (10)
1. a spent acid reclaims technology, it is characterized in that, comprise and utilize ultra-filtration membrane air supporting that spent acid is carried out pretreated step: hyperfiltration membrane assembly vertically is installed, is utilized the gas-liquid mixed power set that spent acid is infeeded from the hyperfiltration membrane assembly bottom to carry out the ultra-filtration membrane air-float purification then and handle.
2. spent acid as claimed in claim 1 reclaims technology, it is characterized in that, utilizes the gas-liquid mixed power set that pretreated spent acid is infeeded dialyzer, carries out the air supporting dialysis.
3. spent acid as claimed in claim 2 reclaims technology, it is characterized in that, raffinate after the dialysis is carried out aeration, precipitation and solid-liquid separation successively, and liquid phase enters the aftertreatment hyperfiltration membrane assembly and carries out the processing of ultra-filtration membrane air-float purification once more under the promotion of gas-liquid mixed power set.
4. spent acid as claimed in claim 3 reclaims technology, it is characterized in that, the penetrating fluid of discharging from the aftertreatment hyperfiltration membrane assembly returns dialyzer and does and receive liquid and use, and concentrated solution returns precipitate phase and does circular treatment.
5. reclaim technology as the arbitrary described spent acid of claim 1-4, it is characterized in that the concentrated solution of discharging imports circular treatment in the untreated spent acid from the pre-treatment hyperfiltration membrane assembly.
6. the described spent acid of claim 1 reclaims the corollary apparatus of technology, comprise spent acid groove and the vertical pre-treatment hyperfiltration membrane assembly of installing, be connected with the penetrating fluid vent pipe on the pre-treatment hyperfiltration membrane assembly, and the bottom is connected with feed-pipe, top is connected with the concentrated solution vent pipe, it is characterized in that, the other end of pre-treatment hyperfiltration membrane assembly feed-pipe is communicated with the spent acid groove, and this feed-pipe is provided with the gas-liquid mixed power set.
7. corollary apparatus as claimed in claim 6 is characterized in that, the other end of described pre-treatment hyperfiltration membrane assembly concentrated solution vent pipe inserts in the spent acid groove.
8. as claim 6 or 7 described corollary apparatus, it is characterized in that, described device also comprises buffer memory groove and dialyzer, the other end of pre-treatment hyperfiltration membrane assembly penetrating fluid vent pipe inserts in the buffer memory groove, the buffer memory groove is communicated with the opening for feed of dialyzer by pipeline, and this connecting pipe is provided with the gas-liquid mixed power set.
9. corollary apparatus as claimed in claim 8, it is characterized in that, the raffinate outlet of described dialyzer links to each other with aeration tank, settling tank, solid-liquid separator and aftertreatment hyperfiltration membrane assembly successively, the water outlet of solid-liquid separator is communicated with the feed-pipe of aftertreatment hyperfiltration membrane assembly, and this feed-pipe is provided with the gas-liquid mixed power set; The concentrated solution vent pipe of aftertreatment hyperfiltration membrane assembly returns settling tank and inserts wherein.
10. corollary apparatus as claimed in claim 9 is characterized in that, the other end of the penetrating fluid vent pipe of aftertreatment hyperfiltration membrane assembly links to each other with the reception liquid of dialyzer inlet.
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| CN2011102156970A CN102259954B (en) | 2011-07-29 | 2011-07-29 | Waste acid recycling process and matching device thereof |
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| CN2011102156970A CN102259954B (en) | 2011-07-29 | 2011-07-29 | Waste acid recycling process and matching device thereof |
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Cited By (4)
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| CN103331111A (en) * | 2013-07-17 | 2013-10-02 | 成都工投电子科技有限公司 | Acid supply device system and method |
| CN104925893A (en) * | 2015-06-18 | 2015-09-23 | 广西柳州市龙发金属表面处理技术有限公司 | Acid activating agent |
| CN108285233A (en) * | 2017-01-09 | 2018-07-17 | 北京水木方科技有限公司 | A kind of method of Recovery Purifying titanium white waste liquid |
| CN109231556A (en) * | 2018-10-16 | 2019-01-18 | 合肥工业大学 | The diffusion dialysis processing unit and its processing method of acid/base waste liquid |
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| CN103331111A (en) * | 2013-07-17 | 2013-10-02 | 成都工投电子科技有限公司 | Acid supply device system and method |
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| CN104925893A (en) * | 2015-06-18 | 2015-09-23 | 广西柳州市龙发金属表面处理技术有限公司 | Acid activating agent |
| CN108285233A (en) * | 2017-01-09 | 2018-07-17 | 北京水木方科技有限公司 | A kind of method of Recovery Purifying titanium white waste liquid |
| CN109231556A (en) * | 2018-10-16 | 2019-01-18 | 合肥工业大学 | The diffusion dialysis processing unit and its processing method of acid/base waste liquid |
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| Publication number | Publication date |
|---|---|
| CN102259954B (en) | 2012-07-25 |
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