CN110092522A - A kind of processing method of the fluorine-containing waste water of nitrose containing ammonia nitrogen - Google Patents
A kind of processing method of the fluorine-containing waste water of nitrose containing ammonia nitrogen Download PDFInfo
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- CN110092522A CN110092522A CN201910489800.7A CN201910489800A CN110092522A CN 110092522 A CN110092522 A CN 110092522A CN 201910489800 A CN201910489800 A CN 201910489800A CN 110092522 A CN110092522 A CN 110092522A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/02—Fluorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/04—Preparation with liquid nitric acid
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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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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
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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
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/03—Pressure
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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)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Agronomy & Crop Science (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a kind of processing methods of fluorine-containing waste water of nitrose containing ammonia nitrogen, and described method includes following steps: (1) concentrated sulfuric acid, high temperature and pressure distillation being added into waste water；(2) nitration mixture distilled out in step (1) is absorbed with potassium hydroxide solution, when faintly acid, is added potassium hydroxide and is neutralized to neutrality, and rear concentration centrifugation obtains the mixed salt of potassium nitrate and potassium fluoride；(3) mixed salt of potassium nitrate and potassium fluoride that step (2) obtains is placed in air, potassium fluoride in mixed salt water suction, potassium fluoride crystal grain becomes larger, with sieve by the mixed salt bulky grain potassium fluoride and little particle potassium nitrate separate；(4) potassium fluoride is dried in vacuo in step (3), obtains anhydrous potassium fluoride；(5) it distills mother liquid obtained middle addition ammonium hydroxide to step (1) to neutralize to obtain ammonium sulfate, condensing crystallizing obtains ammonium sulfate.Present invention process is simple, all linked with one another, low in cost, and resource makes full use of, and in the process without time useless generation.
Description
Technical field
The present invention relates to fluorine-containing nitrogen-containing wastewater processing technology fields, more particularly, to a kind of fluorine-containing nitrose containing ammonia nitrogen
The processing method of waste water.
Background technique
The fluorine-containing nitrose waste water harm containing ammonia nitrogen is huge, and a large amount of ammonia nitrogen and nitrogen oxides will cause the eutrophy of water body
Change, tremendous influence is caused to environment.The processing method of simple fluoride waste is mainly chemical precipitation method, absorption method, cold
Jelly method, ultrafiltration method for removing fluor, electroosmose process low efficiency, and input cost is high, therefore not extensive utilization.The processing side of ammonia nitrogen waste water
Method is mainly blow-off method, biochemical method, chemical precipitation method etc..But for fluorine-containing nitrogen-containing wastewater, these methods may and can not be taken
Good effect is obtained, and relatively fewer for the research of such waste water containing nitric acid.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of processing of fluorine-containing nitrose waste water containing ammonia nitrogen by the application
Method.Present invention process is simple, all linked with one another, low in cost, and resource makes full use of, and in the process without time useless generation.
Technical scheme is as follows:
A kind of processing method of the fluorine-containing waste water of nitrose containing ammonia nitrogen, the treating method comprises following steps:
(1) it is slowly added to the concentrated sulfuric acid into waste water, is distilled under high temperature and pressure after mixing evenly, the water outlet of steam water is slowly or not
When water outlet, mother liquor is added fraction water in step (2) and is diluted, and to guarantee the efficiency of distillation, is referred to by measuring evaporated mother liquor anion
It marks to determine distillation end point, confirms that the anion in mother liquor is sufficiently distilled；
(2) nitration mixture distilled out in step (1) is absorbed with potassium hydroxide solution, when solution to faintly acid, is added a small amount of
Potassium hydroxide is neutralized to neutrality, rear concentration centrifugation, obtains the mixed salt of potassium nitrate and potassium fluoride, and evaporates isolated in the process
Divide water reuse into step (1) for diluting mother liquor；
(3) mixed salt of potassium nitrate and potassium fluoride that step (2) obtains is placed in air, the potassium fluoride in mixed salt is inhaled
Water, potassium fluoride crystal grain become larger, and with sieve by bulky grain and separate small in the mixed salt, wherein bulky grain is fluorination
Potassium, little particle are potassium nitrate, and potassium fluoride enters step (4) processing, and potassium nitrate, which is collected, is used as product；
(4) potassium fluoride is dried in vacuo in step (3), obtains anhydrous potassium fluoride；
(5) after step (1) distillation, ammonium hydroxide is added into mother liquor and neutralizes to obtain ammonium sulfate, condensing crystallizing obtains sulphur
Sour ammonium, and fraction water reuse isolated in concentration process is used to dilute mother liquor into step (1).
The fluorine in wastewater content is 10-15g/L, ammonia-nitrogen content 5-10g/L, nitrate radical content 8-10g/L.
Vapo(u)rizing temperature described in step (1) is 120-130 DEG C, pressure 0.09-0.1MPa；The volume of the concentrated sulfuric acid is dense
Degree is 98%, and the volume for adding the concentrated sulfuric acid is the 15-20% of wastewater volume, and slowly adding the time is 30-50min；The distillation
The volumetric concentration of mother liquid obtained middle sulfuric acid is 60-80% afterwards；The volume for adding fraction water is 1-1.5 times of mother liquor volume；It is described
Anion index are as follows: fluorine ion < 10mg/L and nitrate anion < 10mg/L.
The volumetric concentration of potassium hydroxide solution described in step (2) is 40-50%；The weakly acidic solution pH value is 2-5,
Neutral solution pH value is 6-7；Thickening temperature is 80-90 DEG C, pressure 0.07-0.08MPa.
Relative air humidity≤80% described in step (3), 20-30 DEG C of temperature, standing time 1-2 days；The sieve
Specification is 20-40 mesh.
Vacuum drying temperature described in step (4) is 150-200 DEG C.
Ammonium sulfate pH value described in step (5) is 5-6；In the concentration process: heating temperature is 80-90 DEG C, pressure
Power is 0.07-0.08MPa.
Beneficial effects of the present invention:
In step (1) of the present invention, by sulfuric acid in the boiling point of hydrofluoric acid and nitric acid difference, by the fluorine ion and nitre in waste liquid
Acid ion is separated from system.In CN200910241880.0 patent plus sulfuric acid will condense conduct after hydrofluoric acid and nitric acid separation
Nitration mixture uses, and does not separate fluorine with nitrate anion, and the mixed vapour of hydrogen fluoride and nitric acid is passed through hydrogen by the present invention in step (2)
It aoxidizing potash lye to absorb, obtains potassium nitrate and potassium fluoride, potassium fluoride has very strong water imbibition, and potassium nitrate water imbibition is small, in
When placing in air, after potassium fluoride water suction, crystalline particle becomes larger, and potassium nitrate crystal particle is constant, therefore by suitably sieving
Net can separate potassium fluoride and potassium nitrate, and potassium fluoride drying can be obtained anhydrous potassium fluoride product, the present invention by fluorine with
Nitrate anion is completely separable, there is the difference of essence with patent CN200910241880.0.After sulfuric acid is concentrated, with sulfuric acid in mother liquor
The raising of concentration, due to the water imbibition of the concentrated sulfuric acid, the fraction water distilled out is fewer and fewer, and the fraction water in step (2) is supplemented
Into mother liquor, the acidity of sulfuric acid is reduced, while ensure that distillation efficiency, fluorine, the nitrate anion in mother liquor can be reduced to
10mg/L or less.The waste water contains ammonia, therefore mother liquor selection is neutralized with ammonium hydroxide, be can be used for producing ammonium sulfate crystallization, is avoided money
The waste in source.
Detailed description of the invention
Fig. 1 is process flow chart of the invention
Specific embodiment
With reference to the accompanying drawings and examples, the present invention is specifically described.
Embodiment 1
Waste water fluorine content 10g/L, ammonia nitrogen 5g/L, nitrate radical content 8g/L.2 tons of waste water are squeezed into evaporation reaction kettle,
98% concentrated sulfuric acid 300L is slowly added into reaction kettle in 30min, after charging, in 120 DEG C, 0.09MPa carries out decompression steaming
It evaporates, after distilling 2h, slowly, condensed water 500L is added in mother liquor residue 500L for fraction water outlet, continues to distill 2h, mother liquor sampling and measuring
Fluorine and nitrate radical content measure F content 8mg/L, nitrate anion 8mg/L.It distills mother liquid obtained plus ammonium hydroxide and neutralizes pH to 5, in 80 DEG C,
0.07MPa is concentrated under reduced pressure, and has in feed liquid and obviously crystallizes out current blowing, crystallization centrifugation, and the purity of the ammonium sulfate crystallization measured is
99.2%.Distillation gained nitration mixture using 40% KOH absorption liquid to pH value be 2 when, add 40% potassium hydroxide adjust pH to
6, in 80 DEG C, 0.07MPa condensing crystallizing, potassium nitrate and potassium fluoride mixed salt are placed in wet environment 1 day after centrifugation, are measured opposite
Humidity measurements are 60%, and temperature is 20 DEG C.Potassium nitrate is separated with the sieve of 20 mesh and potassium fluoride, gained potassium nitrate purity are
98.1%, potassium fluoride is random block at this time, and potassium fluoride is dried in 150 DEG C after separation, obtains anhydrous potassium fluoride, purity is
98.3%.
Embodiment 2
Waste water fluorine content 12.5g/L, ammonia nitrogen 7.5g/L, nitrate radical content 9g/L.2 tons of waste water are squeezed into evaporation reaction kettle
In, 98% concentrated sulfuric acid 350L is slowly added into reaction kettle in 40min, after charging, in 125 DEG C, 0.095MPa is subtracted
Pressure distillation, after distilling 2h, slowly, condensed water 625L is added in mother liquor residue 500L for fraction water outlet, continues to distill 2h, mother liquor sampling
Fluorine and nitrate radical content are measured, F content 5mg/L, nitrate anion 5mg/L are measured.It distills mother liquid obtained plus ammonium hydroxide and neutralizes pH to 5.5,
In 85 DEG C, 0.075MPa is concentrated under reduced pressure, and is had in feed liquid and is obviously crystallized out current blowing, crystallization centrifugation, the ammonium sulfate crystallization measured
Purity be 99.3%.Distillation gained nitration mixture using 45% KOH absorption liquid to pH value be 3.5 when, add 45% hydroxide
Potassium adjusts pH to 6.5, and in 85 DEG C, 0.075MPa condensing crystallizing, potassium nitrate and potassium fluoride mixed salt are placed in wet environment after centrifugation
In 1.5 days, measure relative humidity measurements be 70%, temperature be 25 DEG C.Potassium nitrate and potassium fluoride, institute are separated with the sieve of 30 mesh
Obtaining potassium nitrate purity is 98.3%, and potassium fluoride is random block at this time, and potassium fluoride is dried in 175 DEG C after separation, obtains nothing
Water potassium fluoride, purity 98.5%.
Embodiment 3
Waste water fluorine content 15g/L, ammonia nitrogen 10g/L, nitrate radical content 10g/L.2 tons of waste water are squeezed into evaporation reaction kettle,
98% concentrated sulfuric acid 400L is slowly added into reaction kettle in 50min, after charging, in 130 DEG C, 0.100MPa carries out decompression steaming
It evaporates, after distilling 2h, slowly, condensed water 750L is added in mother liquor residue 500L for fraction water outlet, continues to distill 2h, mother liquor sampling and measuring
Fluorine and nitrate radical content measure F content 3mg/L, nitrate anion 3mg/L.It distills mother liquid obtained plus ammonium hydroxide and neutralizes pH to 6, in 90 DEG C,
0.0780MPa is concentrated under reduced pressure, and has in feed liquid and obviously crystallizes out current blowing, crystallization centrifugation, the purity of the ammonium sulfate crystallization measured
It is 99.5%.Distillation gained nitration mixture using 50% KOH absorption liquid to pH value be 5 when, add 50% potassium hydroxide adjust pH
To 7, in 90 DEG C, 0.080MPa condensing crystallizing, potassium nitrate and potassium fluoride mixed salt are placed in wet environment 2 days after centrifugation, are measured
Relative humidity measurements are 80%, and temperature is 30 DEG C.Potassium nitrate and potassium fluoride, gained potassium nitrate purity are separated with the sieve of 40 mesh
It is 98.2%, potassium fluoride is random block at this time, and potassium fluoride is dried in 200 DEG C after separation, obtains anhydrous potassium fluoride, purity
It is 98.7%.
Claims (7)
1. a kind of processing method of the fluorine-containing waste water of nitrose containing ammonia nitrogen, which is characterized in that the treating method comprises following steps:
(1) it is slowly added to the concentrated sulfuric acid into waste water, is distilled under high temperature and pressure after mixing evenly, the water outlet of steam water is slow or is not discharged
When, mother liquor is added in step (2) fraction water and is diluted, to guarantee the efficiency of distillation, by measurement evaporated mother liquor anion index come
It determines distillation end point, confirms that the anion in mother liquor is sufficiently distilled；
(2) nitration mixture distilled out in step (1) is absorbed with potassium hydroxide solution, when solution to faintly acid, adds a small amount of hydrogen-oxygen
Change potassium and be neutralized to neutrality, rear concentration centrifugation obtains the mixed salt of potassium nitrate and potassium fluoride, and by fraction water isolated in the process
Reuse is into step (1) for diluting mother liquor；
(3) mixed salt of potassium nitrate and potassium fluoride that step (2) obtains is placed in air, the potassium fluoride water suction in mixed salt, fluorine
Change potassium crystal grain to become larger, with sieve by bulky grain and separate small in the mixed salt, wherein bulky grain is potassium fluoride, small
Particle is potassium nitrate, and potassium fluoride enters step (4) processing, and potassium nitrate, which is collected, is used as product；
(4) potassium fluoride is dried in vacuo in step (3), obtains anhydrous potassium fluoride；
(5) after step (1) distillation, ammonium hydroxide being added into mother liquor and neutralizes to obtain ammonium sulfate, condensing crystallizing obtains ammonium sulfate,
And fraction water reuse isolated in concentration process is used to dilute mother liquor into step (1).
2. processing method according to claim 1, which is characterized in that the fluorine in wastewater content is 10-15g/L, ammonia nitrogen
Content is 5-10g/L, nitrate radical content 8-10g/L.
3. processing method according to claim 1, which is characterized in that vapo(u)rizing temperature described in step (1) is 120-130
DEG C, pressure 0.09-0.1MPa；The volumetric concentration of the concentrated sulfuric acid is 98%, and the volume for adding the concentrated sulfuric acid is wastewater volume
15-20%, slowly adding the time is 30-50min；The volumetric concentration of mother liquid obtained middle sulfuric acid is 60-80% after the distillation；It mends
Add the volume of fraction water for 1-1.5 times of mother liquor volume；The anion index are as follows: fluorine ion < 10mg/L and nitrate anion
< 10mg/L.
4. processing method according to claim 1, which is characterized in that the volume of potassium hydroxide solution described in step (2)
Concentration is 40-50%；The weakly acidic solution pH value is 2-5, and neutral solution pH value is 6-7；Thickening temperature is 80-90 DEG C, pressure
Power is 0.07-0.08MPa.
5. processing method according to claim 1, which is characterized in that relative air humidity≤80% described in step (3),
20-30 DEG C of temperature, standing time 1-2 days；The specification of the sieve is 20-40 mesh.
6. processing method according to claim 1, which is characterized in that vacuum drying temperature described in step (4) is 150-
200℃。
7. processing method according to claim 1, which is characterized in that ammonium sulfate pH value described in step (5) is 5-
6；In the concentration process: heating temperature is 80-90 DEG C, pressure 0.07-0.08MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110540332A (en) * | 2019-09-24 | 2019-12-06 | 东海岸环境科技无锡有限公司 | fluorine-containing and chlorine-containing sewage treatment process |
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| CN110540332B (en) * | 2019-09-24 | 2021-09-07 | 东海岸环境科技无锡有限公司 | Fluorine-containing and chlorine-containing sewage treatment process |
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Application publication date: 20190806 |