CN106379869A - Technology for extracting sulfuric acid in waste acid liquor from corrosion of electrode foils - Google Patents
Technology for extracting sulfuric acid in waste acid liquor from corrosion of electrode foils Download PDFInfo
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- CN106379869A CN106379869A CN201610778885.7A CN201610778885A CN106379869A CN 106379869 A CN106379869 A CN 106379869A CN 201610778885 A CN201610778885 A CN 201610778885A CN 106379869 A CN106379869 A CN 106379869A
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- Prior art keywords
- acid
- waste
- sulfuric acid
- liquid
- electrode foil
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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
-
- 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
- C01B17/88—Concentration of sulfuric acid
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses a technology for extracting sulfuric acid in waste acid liquor from corrosion of electrode foils. According to the invention, waste iron slag is added in waste acid liquor for an oxidation treatment, heavy metal in sulfuric acid can be removed and cleaned, purification is convenient, waste iron slag can be comprehensively processed; the whole technology has the advantages of high recovery rate and no pollution, and is the novel and environmentally friendly technology for extracting waste acid liquor from corrosion of electrode foils.
Description
Technical field
The present invention relates to technical field of resource recovery, in more particularly, to a kind of electrode foil corrosion waste acid liquid, extract the work of sulfuric acid
Skill.
Background technology
At present, there is more spent acid output, wherein in the corrosion chambering process that electrode foil produces：Sulfuric acid is 28%, Al3+For
0.8%, hydrochloric acid and nitric acid are 1%, and density is 1140 kg/m3, normal temperature, colourless.Electrode foil corrodes the recovery processing technique of Waste Sulfuric Acid
For：Spent acid ion exchange resin adds lime and adjusts pH precipitation discharge.Although this technique passes through resin energy absorbed portion
Sulfuric acid, but after rinsing through water the concentration of sulfuric acid less than 20%, the sulfuric acid concentration that needs less than etching process, and aluminium ion therein
Concentration over-standard, not only wants enriching sulfuric acid during reuse, it is also contemplated that the impact to etching process for the aluminium ion concentration, cause partially recycled
Acid is unable to reuse；On the other hand add lime precipitation operation and produce substantial amounts of gypsum solid waste, must deliver in Solid Waste Treatment
The heart is processed, and costly, still needs to daily discharge substantial amounts of waste water, the wasting of resources simultaneously.
Patent CN 102079512A discloses the work reclaiming sulfuric acid and sulfate from the spent acid of method for producing gtitanium dioxide with sulphuric acid
Skill, by using three condensations of three evaporations, not utilizing to the heat energy evaporating steam every time, energy consumption is big；Use barrier film press filtration
Machine is filtered, due to aluminum sulfate colloid formed in pressure-filtering process densification filter layer, affect the rate of filtration, and be difficult into
Row continuous operation, and do not reclaim out other material in discarded material yet.
Content of the invention
The technical problem being existed based on background technology, the present invention proposes extraction sulfuric acid in a kind of electrode foil corrosion waste acid liquid
Technique.
The technique extracting sulfuric acid in a kind of electrode foil corrosion waste acid liquid, comprises the following steps：
A, will Waste iron slag add acid pickle in carry out pulp, pump into ore pulp storagetank after Waste iron slag is completely dispersed and is pulped；
B, pump into ore pulp from ore pulp storagetank to autoclave with peristaltic pump, use peristaltic pump from spent acid storagetank to high pressure simultaneously
Reactor pumps into acid pickle, is passed through oxygen in reactor, reacts 1-2 hour, generates and is precipitated as leached mud；
After C, filtration, leached mud is reclaimed, leachate is derived from autoclave simultaneously；
D, leachate importing evaporimeter is carried out heating evaporation, and control into flow quantity and delivery flow, so that sulfuric acid content is reached
After 75-80%, export from the evaporimeter other end and discharge, control the temperature of waste liquid to be 120-125 DEG C；
E, condensation-crystallization：Waste liquid after cooling enters crystallisation by cooling groove, condensation-crystallization 2-3 hour at 25-30 DEG C；
F, centrifugation：After the completion of crystallization, pump into centrifugal separator and finished product sulfuric acid is centrifugally separating to obtain concentrated vitriol and sulfuric acid
Salt mixture, the concentrated vitriol of gained enters in finished product acid storage tank, for electrode foil electroetching production line complex acid.
Preferably, in described step A, the addition of described acid pickle is 3-5 times of ferrous sulfate waste residue addition.
Preferably, described autoclave pressure is 1.2-1.5MPa, and temperature is 130-140 DEG C.
Preferably, the mass ratio of ore pulp and acid pickle is 1：（5-8）.
Leached mud in described step C is used for reclaiming further sulfate.
This programme is beneficial in that compared to traditional scheme：Sulfuric acid is extracted in the electrode foil corrosion waste acid liquid of the present invention
Technique, not only the heavy metal in sulfuric acid can be removed clean, be easy to purify further, and Waste iron slag can also obtain comprehensive
Conjunction is processed；Whole technique, the rate of recovery is high, pollution-free, is that a kind of electrode foil corrosion waste acid liquid of novel environment friendly recycles technique.
Specific embodiment
Embodiment 1
The technique extracting sulfuric acid in a kind of electrode foil corrosion waste acid liquid, comprises the following steps：
A, will Waste iron slag add acid pickle in carry out pulp, pump into ore pulp storagetank after Waste iron slag is completely dispersed and is pulped；
B, pump into ore pulp from ore pulp storagetank to autoclave with peristaltic pump, use peristaltic pump from spent acid storagetank to high pressure simultaneously
Reactor pumps into acid pickle, is passed through oxygen in reactor, reacts 1.5 hours, generates and is precipitated as leached mud；
After C, filtration, leached mud is reclaimed, leachate is derived from autoclave simultaneously；
D, leachate importing evaporimeter is carried out heating evaporation, and control into flow quantity and delivery flow, so that sulfuric acid content is reached
After 77-78%, export from the evaporimeter other end and discharge, control the temperature of waste liquid to be 122 DEG C；
E, condensation-crystallization：Waste liquid after cooling enters crystallisation by cooling groove, condensation-crystallization 2.5 hours at 28 DEG C；
F, centrifugation：After the completion of crystallization, pump into centrifugal separator and finished product sulfuric acid is centrifugally separating to obtain concentrated vitriol and sulfuric acid
Salt mixture, the concentrated vitriol of gained enters in finished product acid storage tank, for electrode foil electroetching production line complex acid.
In described step A, the addition of described acid pickle is 4 times of ferrous sulfate waste residue addition.
Described autoclave pressure is 1.3MPa, and temperature is 135 DEG C.
Ore pulp is 1 ton, 6 tons of acid pickle, and the speed being passed through oxygen is 0.15 ton hour.
Embodiment 2
The technique extracting sulfuric acid in a kind of electrode foil corrosion waste acid liquid, comprises the following steps：
A, will Waste iron slag add acid pickle in carry out pulp, pump into ore pulp storagetank after Waste iron slag is completely dispersed and is pulped；
B, pump into ore pulp from ore pulp storagetank to autoclave with peristaltic pump, use peristaltic pump from spent acid storagetank to high pressure simultaneously
Reactor pumps into acid pickle, is passed through oxygen in reactor, reacts 2 hours, generates and is precipitated as leached mud；
After C, filtration, leached mud is reclaimed, leachate is derived from autoclave simultaneously；
D, leachate importing evaporimeter is carried out heating evaporation, and control into flow quantity and delivery flow, so that sulfuric acid content is reached
After 75-76%, export from the evaporimeter other end and discharge, control the temperature of waste liquid to be 120 DEG C；
E, condensation-crystallization：Waste liquid after cooling enters crystallisation by cooling groove, condensation-crystallization 2 hours at 30 DEG C；
F, centrifugation：After the completion of crystallization, pump into centrifugal separator and finished product sulfuric acid is centrifugally separating to obtain concentrated vitriol and sulfuric acid
Salt mixture, the concentrated vitriol of gained enters in finished product acid storage tank, for electrode foil electroetching production line complex acid.
Preferably, in described step A, the addition of described acid pickle is 5 times of ferrous sulfate waste residue addition.
Preferably, described autoclave pressure is 1.2MPa, and temperature is 140 DEG C.
Ore pulp is 1 ton, 6 tons of acid pickle, and the speed being passed through oxygen is 0.12 ton hour.
Embodiment 3
The technique extracting sulfuric acid in a kind of electrode foil corrosion waste acid liquid, comprises the following steps：
A, will Waste iron slag add acid pickle in carry out pulp, pump into ore pulp storagetank after Waste iron slag is completely dispersed and is pulped；
B, pump into ore pulp from ore pulp storagetank to autoclave with peristaltic pump, use peristaltic pump from spent acid storagetank to high pressure simultaneously
Reactor pumps into acid pickle, is passed through oxygen in reactor, reacts 1 hour, generates and is precipitated as leached mud；
After C, filtration, leached mud is reclaimed, leachate is derived from autoclave simultaneously；
D, leachate importing evaporimeter is carried out heating evaporation, and control into flow quantity and delivery flow, so that sulfuric acid content is reached
After 79-80%, export from the evaporimeter other end and discharge, control the temperature of waste liquid to be 125 DEG C；
E, condensation-crystallization：Waste liquid after cooling enters crystallisation by cooling groove, condensation-crystallization 3 hours at 30 DEG C；
F, centrifugation：After the completion of crystallization, pump into centrifugal separator and finished product sulfuric acid is centrifugally separating to obtain concentrated vitriol and sulfuric acid
Salt mixture, the concentrated vitriol of gained enters in finished product acid storage tank, for electrode foil electroetching production line complex acid.
In described step A, the addition of described acid pickle is 3 times of ferrous sulfate waste residue addition.
Described autoclave pressure is 1.5MPa, and temperature is 130 DEG C.
Ore pulp is 1 ton, 8 tons of acid pickle, and the speed being passed through oxygen is 0.2 ton hour.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (4)
1. extract the technique of sulfuric acid in a kind of electrode foil corrosion waste acid liquid it is characterised in that comprising the following steps：
A, will Waste iron slag add acid pickle in carry out pulp, pump into ore pulp storagetank after Waste iron slag is completely dispersed and is pulped；
B, pump into ore pulp from ore pulp storagetank to autoclave with peristaltic pump, use peristaltic pump from spent acid storagetank to high pressure simultaneously
Reactor pumps into acid pickle, is passed through oxygen in reactor, reacts 1-2 hour, generates and is precipitated as leached mud；
After C, filtration, leached mud is reclaimed, leachate is derived from autoclave simultaneously；
D, leachate importing evaporimeter is carried out heating evaporation, and control into flow quantity and delivery flow, so that sulfuric acid content is reached
After 75-80%, export from the evaporimeter other end and discharge, control the temperature of waste liquid to be 120-125 DEG C；
E, condensation-crystallization：Waste liquid after cooling enters crystallisation by cooling groove, condensation-crystallization 2-3 hour at 25-30 DEG C；
F, centrifugation：After the completion of crystallization, pump into centrifugal separator and finished product sulfuric acid is centrifugally separating to obtain concentrated vitriol and sulfuric acid
Salt mixture, the concentrated vitriol of gained enters in finished product acid storage tank, for electrode foil electroetching production line complex acid.
2. extract the technique of sulfuric acid in electrode foil corrosion waste acid liquid as claimed in claim 1 it is characterised in that described step
In A, the addition of described acid pickle is 3-5 times of ferrous sulfate waste residue addition.
3. extract the technique of sulfuric acid in electrode foil corrosion waste acid liquid as claimed in claim 1 it is characterised in that described high pressure
Reactor pressure is 1.2-1.5MPa, and temperature is 130-140 DEG C.
4. extract the technique of sulfuric acid in electrode foil corrosion waste acid liquid as claimed in claim 1 it is characterised in that ore pulp and spent acid
The mass ratio of liquid is 1：（5-8）.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610778885.7A CN106379869A (en) | 2016-08-31 | 2016-08-31 | Technology for extracting sulfuric acid in waste acid liquor from corrosion of electrode foils |
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| CN201610778885.7A CN106379869A (en) | 2016-08-31 | 2016-08-31 | Technology for extracting sulfuric acid in waste acid liquor from corrosion of electrode foils |
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| CN106379869A true CN106379869A (en) | 2017-02-08 |
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| CN201610778885.7A Pending CN106379869A (en) | 2016-08-31 | 2016-08-31 | Technology for extracting sulfuric acid in waste acid liquor from corrosion of electrode foils |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108033472A (en) * | 2017-12-29 | 2018-05-15 | 南通森莹化工科技有限公司 | A kind of electrode foil produces spent acid Zero-discharge treating process |
| CN108862348A (en) * | 2018-08-14 | 2018-11-23 | 徐晨 | A kind of recoverying and utilizing method of electrode foil corrosion Waste Sulfuric Acid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103882431A (en) * | 2012-12-19 | 2014-06-25 | 温州大学 | Zero emission recovery treatment method and system for corrosion waste acid in aluminum foil industry |
| CN103935966A (en) * | 2014-04-09 | 2014-07-23 | 南通职业大学 | Recycling process of waste sulfuric acid from corrosion of electrode foil |
| CN104071853A (en) * | 2014-07-17 | 2014-10-01 | 广西平果锋华科技有限公司 | Method utilizing waste sulfuric acid and ferrous sulfate to produce polymeric ferric sulfate through oxygen pressurizing |
| CN104355336A (en) * | 2014-10-17 | 2015-02-18 | 陕西华陆化工环保有限公司 | Method of utilizing ferrous sulfate waste residue to prepare polymeric ferric sulfate |
-
2016
- 2016-08-31 CN CN201610778885.7A patent/CN106379869A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103882431A (en) * | 2012-12-19 | 2014-06-25 | 温州大学 | Zero emission recovery treatment method and system for corrosion waste acid in aluminum foil industry |
| CN103935966A (en) * | 2014-04-09 | 2014-07-23 | 南通职业大学 | Recycling process of waste sulfuric acid from corrosion of electrode foil |
| CN104071853A (en) * | 2014-07-17 | 2014-10-01 | 广西平果锋华科技有限公司 | Method utilizing waste sulfuric acid and ferrous sulfate to produce polymeric ferric sulfate through oxygen pressurizing |
| CN104355336A (en) * | 2014-10-17 | 2015-02-18 | 陕西华陆化工环保有限公司 | Method of utilizing ferrous sulfate waste residue to prepare polymeric ferric sulfate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108033472A (en) * | 2017-12-29 | 2018-05-15 | 南通森莹化工科技有限公司 | A kind of electrode foil produces spent acid Zero-discharge treating process |
| CN108862348A (en) * | 2018-08-14 | 2018-11-23 | 徐晨 | A kind of recoverying and utilizing method of electrode foil corrosion Waste Sulfuric Acid |
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