CN105461138B - A kind of method that sulfuric acid and hydrochloric acid and fluorine open circuit are reclaimed from smelting wastewater - Google Patents
A kind of method that sulfuric acid and hydrochloric acid and fluorine open circuit are reclaimed from smelting wastewater Download PDFInfo
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- CN105461138B CN105461138B CN201510995647.7A CN201510995647A CN105461138B CN 105461138 B CN105461138 B CN 105461138B CN 201510995647 A CN201510995647 A CN 201510995647A CN 105461138 B CN105461138 B CN 105461138B
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- fluorine
- falling film
- film evaporation
- sulfuric acid
- evaporation device
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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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The present invention relates to a kind of method that sulfuric acid and hydrochloric acid and fluorine open circuit are reclaimed from smelting wastewater, comprise the following steps：(1) micro-filtrate membrane filtration removes the suspension in waste water；(2) primary evaporator concentration waste water, the Water circulation of condensation 70 90%；Remaining 10 30% raffinate enters improvement type falling film evaporation device；(3) defluorinate liquid is passed through using improvement type falling film evaporation device separation hydrochloric acid and hydrofluoric acid, caused indirect steam, obtains watery hydrochloric acid, while in the improvement type falling film evaporation device bottom collection concentrated sulfuric acid.Method provided by the invention has realizes and is kept completely separate that fluorine is opened a way with hydrofluoric acid by the concentrated sulfuric acid, hydrochloric acid simultaneously, realizes the advantages that quantity of slag minimizing is with resource reclaim.
Description
Technical field
The present invention relates to chemical industry environmental protection field, more particularly to synchronously reclaiming hydrochloric acid, sulfuric acid and real in a kind of smelting wastewater
The method of existing fluorine open circuit.This method caused zinc electricity in caused acid water, zinc hydrometallurgy processing flue gas during smelting
Solution liquid and other be also easy to produce the field of high fluorine, chloride wastewater.
Background technology
In the art production process of many smelting industries, the much waste water containing high fluorine, chlorine can be produced.Hydrometallurgy zinc mistake
Cheng Zhong, the leachate of zinc sulfate is also containing substantial amounts of fluorine, chlorine.The presence of fluorine, chlorine can influence being smoothed out for electrolytic zinc process, institute
Seem particularly significant with the processing to zinc electrolyte.By fluorine, chlorine control within limits, positive plate corruption can be avoided the occurrence of
Erosion and equipment corrosion.Flue gas during smelting is generally washed with acid, and during flushing, fluorine, chlorine in flue gas, which enter, to follow
In the acid solution of ring, this kind of acid pickle contains various heavy, while has the fluorine of higher concentration, chlorine.
At present, in terms of high fluorine, chlorine water is handled, mainly there are following methods:Alkali liquid washing method, ion-exchange, extraction.
Ion-exchange-resin process is to utilize some ions or group in resins exchange water, so as to realize the purpose to the ion remaval,
After ion exchange process reaches the upper limit, parsed by resin, these resins may be reused.Resin is in terms of fluorine removal, chlorine
Some scholars have done the research of correlation, can play the role of in some low concentration wastewaters it is good, but for the waste water of high concentration
It is easily contaminated.Extraction removing fluorine, chlorine, extraction raffinate body is retained in by fluorine, chlorine.There is researcher to stay in fluorine, chlorine in aqueous phase,
But due to fluorine, chlorine ion concentration is low and to be unfavorable for reclaiming.
In the prior art, fluorine-containing, chlorine smelting wastewater is handled, is generally neutralized with alkali lye, does not consider the reuse of acid typically,
Cause the huge waste of acid.In addition, directly neutralizing fluorine, chloride wastewater usually requires substantial amounts of alkali, after processing the caused quantity of slag compared with
Greatly.
The content of the invention
The present invention solves low to fluorine removal, chlorine efficiency existing for fluorine in smelting wastewater, chlorine handling process in the prior art
Problem.
A kind of method that sulfuric acid and hydrochloric acid and fluorine open circuit are reclaimed from smelting wastewater：Smelting wastewater containing high-fluorine chlorine is adopted
Suspension is removed with membrane filtration, into primary evaporator, control temperature and pressure make it that 70-90% water steams reuse, and 10-
30% raffinate enters improvement type falling film evaporation device, and improvement type falling film evaporation device bottom obtains high concentration sulphur after treatment
Acid；The indirect steam of acquisition is handled through defluorinate liquid, obtains not fluorine-containing hydrochloric acid；
Described improvement type falling film evaporation device increases air blast interface, falling film evaporation for general falling film evaporation device bottom
When pass through the continuous air blast of air blower of connection；Blast rate is 500~2000Nm3/ h, the temperature of falling film evaporation is 110-120
DEG C, the bottom of improvement type falling film evaporation device is provided with the pipeline that sulfuric acid is recycled to top, and circulating pump is provided with pipeline so that
The process of falling film evaporation constantly circulates.
The smelting wastewater of fluorine-containing chlorine includes：The leachate of zinc sulfate during hydrometallurgy zinc, or flue gas during smelting pass through
The waste water obtained after pickling；Main component is sulfuric acid, chlorion and fluorine ion in the smelting wastewater of fluorine-containing chlorine.
The reduced pressure of described primary evaporator recovery is controlled in -0.85--0.95Mpa.
Described primary evaporator temperature control is at 65-75 DEG C.
After the processing of improvement type falling film evaporation device, the mass content of the high-concentration sulfuric acid finally given is 70-85%.
Described defluorinate liquid is the one or more in Cab-O-sil, waterglass and boric acid.
Device used is lining teflon material.
The method that the present invention provides the removing of fluorine in wastewater chlorine, by membrane filtration pretreated waste water, into vapo(u)rization system, negative
In the presence of pressure, water is largely steamed.Remaining raffinate enters improvement type falling film evaporation device, and bottom of device collects the concentrated sulfuric acid,
Air blower is opened, by the efficient air blast of air blast interface, accelerates indirect steam effusion, hydrogen fluoride is absorbed with defluorinate liquid, after absorption
Liquid is not fluorine-containing hydrochloric acid.
Method provided by the invention, the open circuit of the concentrated sulfuric acid, the recovery of hydrochloric acid and fluorine can be effectively realized, technique is simple, is easy to
Control.The ion concentration range that this technology adapts to is larger, and it is 0.5-5mol/L, the content of fluorine ion to go for handling acidity
The waste water that ion concentration for 1-10g/L, chlorine is 1-20g/L, is improved and was neutralized in the past using lime, avoids producing substantial amounts of stone
Cream waste residue, save wastewater treatment expense.Waste water resource obtains reuse, and comprehensive cyclic utilization rate is up to 80-90%.
Brief description of the drawings
Fig. 1 is present invention process flow chart.
Fig. 2 is improves falling film evaporation device figure, wherein 1 is raffinate entrance after primary evaporator, 2 be steam inlet, and 3 be condensation
Water out, 4 be air blast interface, and 5 be air blower, and 6 be that the concentrated sulfuric acid exports, and 7 be circulating pump, and 8 be that indirect steam exports.
Embodiment
In order that the solved technical problem of invention, technical scheme are more clearly understood, it is described with reference to the drawings and embodiment
The present invention is described in further detail.Embodiment described herein is not to explain the present invention, but not
For limiting the present invention.The invention provides a kind of method that sulfuric acid, hydrochloric acid and fluorine open circuit are reclaimed from smelting wastewater, such as Fig. 1
Shown waste water is in advance removed suspension using membrane filtration, and into primary evaporator system, control temperature causes major part with pressure
Water steams, and remaining raffinate enters improvement type falling film evaporation system, and system bottom obtains the concentrated sulfuric acid, and indirect steam first uses defluorinate
Liquid processing, obtains not fluorine-containing hydrochloric acid.Embodiment 1 uses the technology of the present invention with embodiment 2, and embodiment 3 is as a comparison case
Using traditional falling film evaporation technology.
Embodiment 1
Sample is derived from certain zinc electrolyte, the acidity 2.0mol/L of waste water, chloride ion content 3.1g/L, and content of fluoride ion is
1.1g/L, into primary evaporator system, heated by steam, the reduced pressure control of primary evaporator is steamed in -0.85Mpa, primary
Temperature control is sent out at 65 DEG C, distills out 72% water, reuse.When in vinasse sulfuric acid mass fraction reach 30% or so,
Raffinate after distillation is pumped into improvement type falling film evaporation device, because the bottom of device has additional air blast interface, air blast interface is set
It is placed in more than sulfuric acid liquid level, by the efficient air blast of the air blower of connection, the temperature of improvement type falling film evaporation device is 110 DEG C, drum
Airspeed is 1200Nm3/ h, while the bottom of improvement type falling film evaporation device is provided with the pipeline that sulfuric acid is recycled to top, pipeline
On be provided with circulating pump, carry out multiple circulated sprinkling using circulating pump, indirect steam obtains not fluorine-containing by sodium metasilicate absorption
Hydrochloric acid.The mass fraction of the concentrated sulfuric acid of improvement type falling film evaporation device bottom collection may finally reach 75%, can using this method
So that by the fluorine extrusion rate in waste water, as 98.6%, chlorine extrusion rate is 98.3%, the crystal that tank bottom separates out is cooled to 20 DEG C, filtering
Separation can obtain the crystal salt containing arsenic.
Embodiment 2
Sample is derived from certain smeltery washing flue gas waste water, the acidity 2.8mol/L of waste water, chloride ion content 15g/L, fluorine
Ion concentration is 5g/L, into primary evaporator system, is heated by the afterheat steam of smeltery, the reduced pressure control of primary evaporator
System is in -0.95Mpa, and primary evaporator temperature control distills out 70% water at 75 DEG C, and this part water fluorine, chlorinity are relatively low, returns
With.When the mass fraction arrival 30% or so of sulfuric acid in vinasse, raffinate is pumped into improvement type falling film evaporation device, due to this
Bottom of device has additional air blast interface, and air blast interface is arranged at more than sulfuric acid liquid level, by the efficient air blast of the air blower of connection, changes
The temperature for entering formula falling film evaporation device is 120 DEG C, blast rate 1500Nm3/ h, while the bottom of improvement type falling film evaporation device
Portion is provided with the pipeline that sulfuric acid is recycled to top, is provided with circulating pump on pipeline, and multiple circulated sprinkling is carried out using circulating pump, and two
The mixed liquor of secondary steam boric acid and potassium hydroxide absorbs, and obtains watery hydrochloric acid.Improvement type falling film evaporation device bottom obtains dense
The mass fraction of sulfuric acid may finally reach 80%, can be 99.7% by the fluorine extrusion rate in waste water using this method, chlorine abjection
Rate is 99.3%, and the crystal that tank bottom separates out is cooled to 20 DEG C, and the crystal salt containing arsenic can be obtained by being separated by filtration.
Embodiment 3
Sample is derived from certain smeltery washing flue gas waste water, the acidity 2.8mol/L of waste water, chloride ion content 15g/L, fluorine
Ion concentration is 5g/L, into primary evaporator system, is heated by the afterheat steam of smeltery, distills out 70% water, this portion
Divide water fluorine, chlorinity relatively low, reuse.When the mass fraction arrival 30% or so of sulfuric acid in vinasse, raffinate is pumped into tradition
Falling film evaporation system, the mixed liquor of indirect steam boric acid and potassium hydroxide absorbs, and obtains watery hydrochloric acid.Traditional falling film evaporation
The mass fraction for the concentrated sulfuric acid that system bottom obtains can reach 50%, can be by the fluorine extrusion rate in waste water using this method
70.2%, chlorine extrusion rate is 68.6%, and the crystal that tank bottom separates out is cooled to 20 DEG C, and the crystallization containing arsenic can be obtained by being separated by filtration
Salt.
Claims (8)
- A kind of 1. method that sulfuric acid and hydrochloric acid and fluorine open circuit are reclaimed from smelting wastewater, it is characterised in that：High-fluorine chlorine will be contained Smelting wastewater is removed suspension using membrane filtration, and into primary evaporator, control temperature causes 70-90% water to steam with pressure Reuse, and 10-30% raffinate enters improvement type falling film evaporation device, improvement type falling film evaporation device bottom obtains after treatment To high-concentration sulfuric acid；The indirect steam of acquisition is handled through defluorinate liquid, obtains not fluorine-containing hydrochloric acid；Described improvement type falling film evaporation device increases air blast interface for general falling film evaporation device bottom, leads to during falling film evaporation Cross the continuous air blast of air blower of connection；Blast rate is 500~2000Nm3/ h, the temperature of falling film evaporation is 110-120 DEG C, is changed The bottom for entering formula falling film evaporation device is provided with the pipeline that sulfuric acid is recycled to top, is provided with circulating pump on pipeline so that falling liquid film The process of evaporation constantly circulates.
- 2. according to the method for claim 1, it is characterised in that the smelting wastewater of fluorine-containing chlorine includes：Hydrometallurgy zinc process The leachate of middle zinc sulfate, or the waste water that flue gas during smelting obtains after overpickling；Main component in the smelting wastewater of fluorine-containing chlorine For sulfuric acid, chlorion and fluorine ion.
- 3. according to the method for claim 1, it is characterised in that the control of the reduced pressure of described primary evaporator- 0.85--0.95Mpa。
- 4. the method according to claim 1 or 3, it is characterised in that described primary evaporator temperature control is at 65-75 DEG C.
- 5. according to the method for claim 1, it is characterised in that described indirect steam composition is water, hydrofluoric acid, hydrochloric acid Mixture.
- 6. according to the method for claim 1, it is characterised in that described defluorinate liquid is in Cab-O-sil, waterglass and boric acid One or more.
- 7. according to the method for claim 1, it is characterised in that after the processing of improvement type falling film evaporation device, final The mass content of the high-concentration sulfuric acid arrived is 70-85%.
- 8. according to the method for claim 1, it is characterised in that device used is lining teflon material.
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| 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 |
| CN106564921B (en) * | 2016-11-03 | 2018-01-02 | 中国神华能源股份有限公司 | The method that acid recycles in flyash acidity extraction alumina technology |
| 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 |
| 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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| JP2006348359A (en) * | 2005-06-17 | 2006-12-28 | Kazuhiro Niizawa | Metal recovery method |
| CN103014355B (en) * | 2012-12-13 | 2014-12-24 | 马永涛 | Multi-metal comprehensive recycling process for copper smelting ash |
| CN104445095B (en) * | 2014-12-18 | 2016-05-25 | 中南大学 | A kind of method of smelting dirty acid purification |
| CN105060596A (en) * | 2015-07-23 | 2015-11-18 | 江苏德邦工程有限公司 | Membrane method and falling film evaporation salt-containing wastewater zero emission treatment method, and device thereof |
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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 |
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