CN105461138A - Method for recycling sulfuric acid and hydrochloric acid from smelting wastewater and realizing fluorine open circuit - Google Patents
Method for recycling sulfuric acid and hydrochloric acid from smelting wastewater and realizing fluorine open circuit Download PDFInfo
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- CN105461138A CN105461138A CN201510995647.7A CN201510995647A CN105461138A CN 105461138 A CN105461138 A CN 105461138A CN 201510995647 A CN201510995647 A CN 201510995647A CN 105461138 A CN105461138 A CN 105461138A
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- film evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C01B17/88—Concentration of sulfuric acid
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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
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/08—Thin film evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention relates to a method for recycling sulfuric acid and hydrochloric acid from smelting wastewater and realizing a fluorine open circuit. The method comprises the following steps: (1) filtering suspended solids in wastewater by virtue of a micro-filtration membrane; (2) primarily evaporating and concentrating wastewater, condensing 70%-90% of water for reuse, and enabling 10%-30% of raffinate to enter a falling film evaporation device; and (3) separating hydrochloric acid and hydrofluoric acid by virtue of an improved falling film evaporation device, processing secondary steam by virtue of defluorination liquid, so as to obtain diluted hydrochloric acid, and simultaneously collecting concentrated sulfuric acid at the bottom of the improved falling film evaporation device. The method provided by the invention has the advantages that concentrated sulfuric acid and hydrochloric acid are completely separated, the fluorine open circuit is realized by virtue of hydrofluoric acid, the reduction of residues and the resource recovery are realized, and the like.
Description
Technical field
The present invention relates to chemical industry environmental protection field, particularly relate in a kind of smelting wastewater synchronously reclaim hydrochloric acid, sulfuric acid and realize fluorine open circuit method.Present method be applicable to process in flue gas during smelting the acid water produced, the zinc electrolyte produced in zinc hydrometallurgy and other easily produce the field of high fluorine, chloride wastewater.
Background technology
In the art production process of a lot of smelting industry, a lot of waste water containing high fluorine, chlorine can be produced.In hydrometallurgy zinc process, the leach liquor of zinc sulfate is also containing a large amount of fluorine, chlorine.The existence of fluorine, chlorine can affect carrying out smoothly of electrolytic zinc process, so seem very important to the process of zinc electrolyte.Fluorine, chlorine are controlled within limits, can avoid occurring positive plate corrosion and equipment corrosion.Flue gas during smelting washs with acid usually, and in the process of rinsing, the fluorine in flue gas, chlorine enter in the acid solution of circulation, and this kind of spent acid solution contains various heavy, have the fluorine of higher concentration, chlorine simultaneously.
At present, in the high fluorine of process, chlorine water, following methods is mainly contained: alkali liquid washing method, ion exchange method, extraction process.Ion-exchange-resin process utilizes some ion in resins exchange water or group, thus realize the object to this ion remaval, and after ion exchange process reaches the upper limit, resolved by resin, these resins can be reused.Resin, except fluorine, research that also to have had scholar to do in chlorine relevant, can have good effect at some low concentration wastewaters, but easily be polluted for the waste water of high density.Extraction process removes fluorine, chlorine, and fluorine, chlorine are retained in extraction raffinate body.Investigator is had fluorine, chlorine to be stayed in aqueous phase, but because fluorine, chlorine ion concentration are low and make to be unfavorable for reclaiming.
In the prior art, process smelting wastewater that is fluorine-containing, chlorine, usually with alkali lye neutralization, generally do not consider the reuse of acid, cause the huge waste of acid.In addition, usually need a large amount of alkali directly with fluorine, chloride wastewater, the quantity of slag produced after process is larger.
Summary of the invention
The invention solves in prior art to fluorine in smelting wastewater, chlorine treatment process exist except fluorine, the inefficient problem of chlorine.
A kind of method of reclaim(ed) sulfuric acid and hydrochloric acid and fluorine open circuit from smelting wastewater: adopt membrane filtration to be removed by suspended substance the smelting wastewater containing high fluorine chlorine, enter primary evaporator, control temperature and pressure make the water of 70-90% steam reuse, and the raffinate of 10-30% enters improvement type falling film evaporation device, obtain high-concentration sulfuric acid bottom improvement type falling film evaporation device after treatment; The secondary steam obtained, through the process of defluorinate liquid, obtains not fluorine-containing hydrochloric acid;
Described improvement type falling film evaporation device is increase air blast interface bottom general falling film evaporation device, the continuous air blast of gas blower by connecting during falling film evaporation; Blast rate is 500 ~ 2000Nm
3/ h, the temperature of falling film evaporation is 110-120 DEG C, and the bottom of improvement type falling film evaporation device is provided with pipeline sulfuric acid being circulated to top, and pipeline is provided with recycle pump, and the process of falling film evaporation is constantly circulated.
The smelting wastewater of fluorine-containing chlorine comprises: the leach liquor of zinc sulfate in hydrometallurgy zinc process, or the waste water that flue gas during smelting obtains after overpickling; In the smelting wastewater of fluorine-containing chlorine, main component is sulfuric acid, chlorion and fluorion.
The reduced pressure that described primary evaporator reclaims controls at-0.85--0.95Mpa.
Described primary evaporator temperature controls at 65-75 DEG C.
After the process of improvement type falling film evaporation device, the mass content of the high-concentration sulfuric acid finally obtained is 70-85%.
Described defluorinate liquid is one or more in ground silica, water glass and boric acid.
Device used is lining teflon material.
The invention provides the method that fluorine in wastewater chlorine removes, by membrane filtration pretreated waste water, enter vapo(u)rization system, under the effect of negative pressure, water is steamed in a large number.Remaining raffinate enters improvement type falling film evaporation device, and bottom of device collects the vitriol oil, opens gas blower, and by the efficient air blast of air blast interface, accelerate secondary steam effusion, hydrogen fluoride defluorinate liquid absorbs, and the liquid after absorption is not fluorine-containing hydrochloric acid.
Method provided by the invention, effectively can realize the vitriol oil, the recovery of hydrochloric acid and the open circuit of fluorine, and technique is simple, be easy to control.The ion concentration range that this technology adapts to is larger, go for that process acidity is 0.5-5mol/L, the content of fluorion is 1-10g/L, the ion content of chlorine is the waste water of 1-20g/L, improve and used limestone vegetation in the past, avoid producing a large amount of gypsum offscums, save wastewater treatment expense.Waste water resource obtains reuse, and comprehensive cyclic utilization rate can reach 80-90%.
Accompanying drawing explanation
Fig. 1 is present invention process schema.
Fig. 2 is for improving falling film evaporation device figure, and wherein 1 is raffinate entrance after primary evaporator, and 2 is steam inlet, and 3 is condensation-water drain, and 4 is air blast interface, and 5 is gas blower, and 6 is vitriol oil outlet, and 7 is recycle pump, and 8 is secondary steam outlet.
Embodiment
The technical problem solved to make invention, technical scheme are clearly understood, accompanying drawings and embodiment are described in further detail the present invention.Embodiment described herein in order to explain the present invention, but is not intended to limit the present invention.The invention provides a kind of method that reclaim(ed) sulfuric acid, hydrochloric acid and fluorine are opened a way from smelting wastewater, waste water adopts membrane filtration to be removed by suspended substance in advance as shown in Figure 1, enter primary evaporator system, control temperature and pressure make most of water steam, and remaining raffinate enters improvement type falling film evaporation system, system bottom obtains the vitriol oil, and secondary steam first uses the process of defluorinate liquid, obtains not fluorine-containing hydrochloric acid.Embodiment 1 and embodiment 2 all adopt the technology of the present invention, and embodiment 3 adopts traditional falling film evaporation technology as a comparison case.
Embodiment 1
Certain zinc electrolyte taken from by sample, the acidity 2.0mol/L of waste water, chloride ion content is 3.1g/L, content of fluoride ion is 1.1g/L, enters primary evaporator system, passes through steam heating, the reduced pressure of primary evaporator controls at-0.85Mpa, primary evaporator temperature controls, at 65 DEG C, to distill out the water of 72%, reuse.When the massfraction of sulfuric acid in vinasse arrives about 30%, raffinate after distillation is pumped into improvement type falling film evaporation device, because this bottom of device has additional air blast interface, air blast interface is arranged at more than sulfuric acid liquid level, by the efficient air blast of gas blower connected, the temperature of improvement type falling film evaporation device is 110 DEG C, and blast rate is 1200Nm
3/ h, the bottom of improvement type falling film evaporation device is provided with pipeline sulfuric acid being circulated to top simultaneously, and pipeline is provided with recycle pump, and utilize recycle pump to carry out repeatedly circulated sprinkling, secondary steam absorbs through water glass, obtains not fluorine-containing hydrochloric acid.The massfraction of the vitriol oil of improvement type falling film evaporation device bottom collection finally can reach 75%, this method is utilized to be 98.6% by the fluorine extrusion rate in waste water, chlorine extrusion rate is 98.3%, and the crystallisate of separating out at the bottom of tank is cooled to 20 DEG C, and filtering separation can obtain the crystal salt containing arsenic.
Embodiment 2
Certain smeltery washing flue gas waste water taken from by sample, the acidity 2.8mol/L of waste water, chloride ion content is 15g/L, and content of fluoride ion is 5g/L, enters primary evaporator system, heated by the afterheat steam of smeltery, the reduced pressure of primary evaporator controls at-0.95Mpa, and primary evaporator temperature controls, at 75 DEG C, to distill out the water of 70%, this part water fluorine, cl content are lower, reuse.When the massfraction of sulfuric acid in vinasse arrives about 30%, raffinate is pumped into improvement type falling film evaporation device, because this bottom of device has additional air blast interface, air blast interface is arranged at more than sulfuric acid liquid level, by the efficient air blast of gas blower connected, the temperature of improvement type falling film evaporation device is 120 DEG C, and blast rate is 1500Nm
3/ h, the bottom of improvement type falling film evaporation device is provided with pipeline sulfuric acid being circulated to top simultaneously, and pipeline is provided with recycle pump, utilizes recycle pump to carry out repeatedly circulated sprinkling, the mixed solution of secondary steam boric acid and potassium hydroxide absorbs, and obtains dilute hydrochloric acid.The massfraction of the vitriol oil obtained bottom improvement type falling film evaporation device finally can reach 80%, this method is utilized to be 99.7% by the fluorine extrusion rate in waste water, chlorine extrusion rate is 99.3%, and the crystallisate of separating out at the bottom of tank is cooled to 20 DEG C, and filtering separation can obtain the crystal salt containing arsenic.
Embodiment 3
Certain smeltery washing flue gas waste water taken from by sample, the acidity 2.8mol/L of waste water, and chloride ion content is 15g/L, content of fluoride ion is 5g/L, enters primary evaporator system, is heated by the afterheat steam of smeltery, distill out the water of 70%, this part water fluorine, cl content are lower, reuse.When the massfraction of sulfuric acid in vinasse arrives about 30%, raffinate is pumped into traditional falling film evaporation system, and the mixed solution of secondary steam boric acid and potassium hydroxide absorbs, and obtains dilute hydrochloric acid.The massfraction of the vitriol oil obtained bottom traditional falling film evaporation system can reach 50%, this method is utilized to be 70.2% by the fluorine extrusion rate in waste water, chlorine extrusion rate is 68.6%, and the crystallisate of separating out at the bottom of tank is cooled to 20 DEG C, and filtering separation can obtain the crystal salt containing arsenic.
Claims (8)
1. the method for reclaim(ed) sulfuric acid and hydrochloric acid and fluorine open circuit from a smelting wastewater, it is characterized in that: adopt membrane filtration to be removed by suspended substance the smelting wastewater containing high fluorine chlorine, enter primary evaporator, control temperature and pressure make the water of 70-90% steam reuse, and the raffinate of 10-30% enters improvement type falling film evaporation device, obtain high-concentration sulfuric acid bottom improvement type falling film evaporation device after treatment; The secondary steam obtained, through the process of defluorinate liquid, obtains not fluorine-containing hydrochloric acid;
Described improvement type falling film evaporation device is increase air blast interface bottom general falling film evaporation device, the continuous air blast of gas blower by connecting during falling film evaporation; Blast rate is 500 ~ 2000Nm
3/ h, the temperature of falling film evaporation is 110-120 DEG C, and the bottom of improvement type falling film evaporation device is provided with pipeline sulfuric acid being circulated to top, and pipeline is provided with recycle pump, and the process of falling film evaporation is constantly circulated.
2. method according to claim 1, is characterized in that, the smelting wastewater of fluorine-containing chlorine comprises: the leach liquor of zinc sulfate in hydrometallurgy zinc process, or the waste water that flue gas during smelting obtains after overpickling; In the smelting wastewater of fluorine-containing chlorine, main component is sulfuric acid, chlorion and fluorion.
3. method according to claim 1, is characterized in that, the reduced pressure of described primary evaporator controls at-0.85--0.95Mpa.
4. the method according to claim 1 or 3, is characterized in that, described primary evaporator temperature controls at 65-75 DEG C.
5. method according to claim 1, is characterized in that, described secondary steam composition is the mixture of water, hydrofluoric acid, hydrochloric acid.
6. method according to claim 1, is characterized in that, described defluorinate liquid is one or more in ground silica, water glass and boric acid.
7. method according to claim 1, is characterized in that, after the process of improvement type falling film evaporation device, the mass content of the high-concentration sulfuric acid finally obtained is 70-85%.
8. method according to claim 1, is characterized in that, device used is lining teflon material.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106564921A (en) * | 2016-11-03 | 2017-04-19 | 中国神华能源股份有限公司 | Method for acid circulation in process of extracting alumina from fly ash through acid process |
| CN107777691A (en) * | 2016-08-31 | 2018-03-09 | 中国科学院过程工程研究所 | The recovery method of fluorine resource in a kind of acidic fluorine-containing waste water |
| CN108675502A (en) * | 2018-06-13 | 2018-10-19 | 武汉飞博乐环保工程有限公司 | A kind of waste acid resource method |
| CN109608011A (en) * | 2018-11-20 | 2019-04-12 | 台州市宏民环保科技有限公司 | A method of plating cupro-nickel mixing sludge resource utilization utilizes |
| CN111888831A (en) * | 2020-06-24 | 2020-11-06 | 刘发业 | Waste sulfuric acid recovery processing device and application thereof |
| CN111994872A (en) * | 2020-09-01 | 2020-11-27 | 江苏康祥实业集团有限公司 | Method for recovering sulfuric acid in benzene sulfonyl chloride production process |
| CN112387096A (en) * | 2020-10-16 | 2021-02-23 | 楚雄滇中有色金属有限责任公司 | Novel method for purifying and recycling arsenic-containing flue gas by using acidic liquid medium |
| CN112408680A (en) * | 2019-11-29 | 2021-02-26 | 中冶长天国际工程有限责任公司 | Method for fine treatment of wastewater containing fluorine and chlorine |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107777691A (en) * | 2016-08-31 | 2018-03-09 | 中国科学院过程工程研究所 | The recovery method of fluorine resource in a kind of acidic fluorine-containing waste water |
| CN107777691B (en) * | 2016-08-31 | 2020-04-03 | 中国科学院过程工程研究所 | Method for recovering fluorine resource in acidic fluorine-containing wastewater |
| CN106564921A (en) * | 2016-11-03 | 2017-04-19 | 中国神华能源股份有限公司 | Method for acid circulation in process of extracting alumina from fly ash through acid process |
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| CN109608011A (en) * | 2018-11-20 | 2019-04-12 | 台州市宏民环保科技有限公司 | A method of plating cupro-nickel mixing sludge resource utilization utilizes |
| CN112408680A (en) * | 2019-11-29 | 2021-02-26 | 中冶长天国际工程有限责任公司 | Method for fine treatment of wastewater containing fluorine and chlorine |
| CN112408680B (en) * | 2019-11-29 | 2022-12-06 | 中冶长天国际工程有限责任公司 | Method for fine treatment of wastewater containing fluorine and chlorine |
| CN111888831A (en) * | 2020-06-24 | 2020-11-06 | 刘发业 | Waste sulfuric acid recovery processing device and application thereof |
| CN111994872A (en) * | 2020-09-01 | 2020-11-27 | 江苏康祥实业集团有限公司 | Method for recovering sulfuric acid in benzene sulfonyl chloride production process |
| CN112387096A (en) * | 2020-10-16 | 2021-02-23 | 楚雄滇中有色金属有限责任公司 | Novel method for purifying and recycling arsenic-containing flue gas by using acidic liquid medium |
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Address after: Yuelu District City, Hunan province 410083 Changsha Lushan Road No. 932 Co-patentee after: Thiessens environmental Limited by Share Ltd Patentee after: CENTRAL SOUTH University Address before: Yuelu District City, Hunan province 410083 Changsha Lushan Road No. 932 Co-patentee before: CHANGSHA SCIENCE ENVIRONMENTAL TECHNOLOGY CO., LTD. Patentee before: CENTRAL SOUTH University |