CN107739121A - A kind of further treatment technique of fluorine-containing silicon waste water - Google Patents
A kind of further treatment technique of fluorine-containing silicon waste water Download PDFInfo
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- CN107739121A CN107739121A CN201710949501.8A CN201710949501A CN107739121A CN 107739121 A CN107739121 A CN 107739121A CN 201710949501 A CN201710949501 A CN 201710949501A CN 107739121 A CN107739121 A CN 107739121A
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- fluorine
- solution
- medicament
- waste water
- further treatment
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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
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- 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
-
- 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
- C02F2001/007—Processes including a sedimentation step
-
- 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
Abstract
The invention discloses a kind of further treatment technique of fluorine-containing silicon waste water, comprise the following steps：（1）It will carry out being incubated 10 20min after fluorine-containing 90 95 DEG C of water sample heat temperature raising；（2）In above-mentioned solution, medicament 1 is slowly added to, stirring while adding, mixing speed is in 2~3r/s, after adding, 0.5~1h of boiling；（3）In above-mentioned solution, medicament 2 is added, and adjusts pH to 7~9, it is stirring while adding, 2~3h is incubated after adding, mixing speed is in 0.5~1r/s in insulating process；（4）Step（3）After the completion of can carry out the separation of hydrate deposition and solution, filter liquor is water outlet.The present invention utilizes Hydrothermal Synthesiss process, the Element Mineralizations such as fluorine in solution, silicon, phosphorus is formed stable hydrate deposition, and carries out depth fluorine removal by effects such as cladding, ion exchange, absorption, complexings, and filter liquor is water outlet, and qualified discharge can be achieved.
Description
Technical field
The present invention relates to technical field of waste water processing, more particularly to a kind of further treatment technique of fluorine-containing silicon waste water.
Background technology
Oil repellent is too high in water not only results in human body fluorine poisoning, causes fluorosis of bone, den tal fluorosis etc., while can also make plant
Thing is poisoned, and is influenceed agriculture-stock production, is caused serious environmental pollution.Often there is precipitation with processing method for the fluoride waste of routine
Method, absorption method and coagulation sedimentation, the wherein precipitation method are mainly used in industry high-concentration fluoride waste, and absorption rule is used for drinking
It is appropriate for low fluoride waste application coagulation sedimentation with the processing of water.But in actual process, for containing simultaneously
There is the waste water of fluorine and silicon, phosphorus etc., content of fluoride ion tends not to reach after being handled using conventional method《Integrated wastewater discharge mark
It is accurate（GB8978~1996）》Middle I levels discharge standard 10mg/L, and water quality is unstable, under the situation that environmental condition changes, such as by
Hot content of fluoride ion is likely to occur bounce-back rise, the risk of environmental pollution be present.
CN104512973 discloses a kind of processing method of fluoride waste, including：Wastewater pH is adjusted to less than 5, then is carried out
Neutralization precipitation, separation of solid and liquid obtains one-level filtrate after waste water carries out flocculating setting after precipitation；One-level filtrate is carried out with aluminum contained compound
Separation of solid and liquid obtains two level filtrate after coagulating sedimentation；Two level filtrate progress coagulant precipitation is finally obtained into supernatant, it goes out water fluoridation
Below 10mg/L can be reached.This method is suitable for the higher waste water of F-, SO42- and Al3+ concentration.
CN102070267 discloses a kind of method for handling acid phosphorous fluoride waste, including：Hydrogen-oxygen is added into waste water
Change calcium, and it is 12~14 to control reaction pH；Add sulfuric acid after filtering into filtrate again, adjust pH to 9~11, finally use aluminum sulfate
Adjust pH to 6~7；It, which goes out water fluoridation, after precipitation separation can be reduced to below 10mg/L.
All it is the going out after its processing by directly adding containing the direct fluorine removal of the precipitating reagents such as aluminium, calcic in the prior art above
Water fluoridation is also only capable of reaching below 10mg/L, it is difficult to meet below 5mg/L requirement, in its water outlet often also because exist fluorine and
Silicon compound causes water sample to stablize preservation, and after storage a period of time or condition change are heated, the fluorine ion in water sample contains
Amount occurs that bounce-back is gone up, and remote superstate Oil repellent discharge standard, serious fluorine be present and stains risk.
The content of the invention
It is an object of the invention to provide a kind of further treatment technique of fluorine-containing silicon waste water, using Hydrothermal Synthesiss process, make
The Element Mineralization such as fluorine, silicon, phosphorus forms stable hyrate precipitation in solution, and by coating, adsorbing, ion exchange, the work such as complexing
With depth fluorine removal is carried out, then carry out precipitation and separated with solution, filter liquor is water outlet, and qualified discharge can be achieved.
A kind of further treatment technique of fluorine-containing silicon waste water according to embodiments of the present invention, comprises the following steps：
（1）It will be incubated after fluorine-containing water sample heat temperature raising；
（2）In step（1）In solution after processing, medicament 1 is slowly added to, stirring while adding, mixing speed adds in 2~3r/s
After complete, 0.5~1h of boiling；
（3）In step（2）In solution after processing, medicament 2 is slowly added to, and adjusts pH to 7~9, it is stirring while adding, after adding
2~3h is incubated, mixing speed is in 0.5~1r/s in insulating process；
（4）In step（3）In solution after processing, after standing cooling, i.e., sediment separate out and solution, filter liquor are
Water.
On the basis of such scheme, the step（1）In, 90-95 DEG C is heated to, soaking time is 10~20min.
On the basis of such scheme, the step（2）In medicament 1 include aluminium salt and trace rare-earth element.Rare earth element
Content be aluminum salt solution 0.01-0.05%, rare earth element is LREE, "dead" pollution, and main rise promotes hydro-thermal
The effect of synthesis, be advantageous to the formation of hyrate structure.
On the basis of such scheme, the dosage of the medicament 1 is 0.1%.On the basis of such scheme, the step（3）
In medicament 2 include aluminium polychloride and polyacrylamide.The solubility product of calcirm-fluoride and fluoro complex can be changed, reduce dissolving
Degree, improve cladding and suction-operated.
On the basis of such scheme, the step（4）In precipitation slag can by backflow return to step（3）In make crystal seed
Recycle.
The chemism of defluorinate in the present invention：
At 90-95 DEG C, the first step：Medicament 1 rapid hydration reaction generation hydrate 1, reaction principle after being added in waste water：
（1）ND·2SiO2·2H2O+6OH-→2NDO2- +2SiO32-+5H2O
（2）2NDO2-+2SiO32-+2H2O+2Na+→Na2O·ND2O3·2SiO2+4OH-
Second step：In the presence of medicament 2, using calcium hydroxide particle as kernel, the reaction generation solubility of hydrate 1 with top layer
Smaller hyrate 2, it is wrapped in the surface of hydrate 1, its reaction principle：
ND·SiO3+3Ca（OH）2+2Al（OH）4-→3CaO·NDO3·xSiO2·（6-2x）H2O+2（1-x）OH-
In addition, other reactions that may occur include the ion exchange and fluorine ion and aluminium of anion and fluorine ion in hyrate
The complex compound such as the complexing of ion, generation AlF3, AlF4-, AlF63-.
Wherein ND is that coagulant and flocculation aid composition, reaction equation are found out in the present invention, medicament 1, the auxiliary agent usage amount of medicament 2
By the element silicon in system（Also the major element such as P, AS is included）Content is determined due in the system step, containing Fe3+, SiO2
Isocolloid material, difficulty in filtration is very big if not adding assistant, and the filter cake ionized impurity separated is more, easily causes pollution.The present invention
Filter cake after technique separation is not present pollution factor, and containing wet low, can be used for other purposes, or fill.
The present invention has an advantageous effect in that compared with prior art：Fluorine-containing silicon waste water is handled using the present invention, added
The aluminum salt solution of rare earth element is with the addition of, Hydrothermal Synthesiss process can be promoted, the Element Mineralizations such as fluorine in solution, silicon, phosphorus is formed surely
Determine aquation precipitation, and by coating, adsorbing, the progress depth defluorinate of ion exchange, complexing, and the addition pair of rare earth element
Its water purification performance has considerable influence, can improve coagulation effect, when its anion is Cl-, SO42-, to aluminium polychloride (PAC)
Tool is significantly improved, and then carries out precipitation separation, and filter liquor is water outlet, and qualified discharge, the filter cake after separation can be achieved
, can be used for other purposes in the absence of pollution factor, and containing wet low, or landfill.Present invention process is simple, and solid waste discharge amount is small, water outlet fluorine energy
It is stable to be down to below 5mg/L, discharged wastewater met the national standard is realized, avoids environmental pollution.
Embodiment
For feature, technological means and the concrete function reached of the present invention can be further appreciated that, below with specific implementation
Mode is described in further detail to the present invention.
Embodiment 1：
The present embodiment comprises the following steps：
（1）Water sampling 300g, it is 20mg/L to detect the Oil repellent that dissociates in sample, and fluosilicic acid radical content is 15mg/L, heat temperature raising
To after 90 DEG C, Oil repellent rises to 27.1mg/L, and fluosilicic acid radical content is 8.8mg/L, is incubated 10min；
（2）In step（1）In solution after processing, be slowly added to the solution of medicament 1, it is stirring while adding, mixing speed in 2r/s,
At 90 DEG C, boiling 0.5h；
（3）In step（2）In solution after processing, medicament 2 is slowly added to, adjusts pH to 8, it is stirring while adding, 90 DEG C after adding
Lower insulation 2h, mixing speed is in 0.5r/s in insulating process；
（4）In step（3）In solution after processing, after standing cooling, you can carrying out sediment separate out and solution, sediment can lead to
Cross backflow and return to step（3）In recycled as crystal seed, filter liquor is water outlet, survey solution in dissociate Oil repellent be
4.7mg/l, fluosilicic acid radical content are 2.4mg/l.
Embodiment 2：
The present embodiment comprises the following steps：
（1）Water sampling 800g, the Oil repellent that dissociates in sample is 20mg/l, and fluosilicic acid radical content is 230mg/l, is heated to 90
After DEG C, Oil repellent rises to 127.4mg/L, and fluosilicic acid radical content is 94.3mg/L, is incubated 10min；
（2）In step（1）In solution after processing, the solution of medicament 1 is slowly added to, stirring while adding, mixing speed is in 2~3r/
S, boiling 0.5h；
（3）In step（2）In solution after processing, medicament 2 is slowly added to, adjusts pH to 9, it is stirring while adding, 90 DEG C after adding
3h is incubated, mixing speed is in 0.7r/s in insulating process；
（4）In step（3）In solution after processing, after standing cooling, i.e., sediment separate out and solution, sediment can pass through backflow
Return to step（3）In recycled as crystal seed, filter liquor is water outlet, and it is 4.9mg/l to survey in solution the Oil repellent that dissociates, fluorine
Silicate content is 3.6mg/l.
Embodiment 3：
The present embodiment comprises the following steps：
（1）Water sampling 10000g, the Oil repellent that dissociates in sample is 20mg/l, and fluosilicic acid radical content is 15mg/l, is heated to
After 90 DEG C, Oil repellent rises to 26.8mg/L, and fluosilicic acid radical content is 6.41mg/L, is incubated 10min；
（2）In step（1）In solution after processing, the solution of medicament 1 is slowly added to, stirring while adding, mixing speed adds in 3r/s
95 DEG C are warming up to after complete, boiling 0.5h；
（3）In step（2）In solution after processing, medicament 2 is slowly added to, adjusts pH to 8, it is stirring while adding, 90 DEG C after adding
3h is incubated, mixing speed is in 1r/s in insulating process；
（4）In step（3）In solution after processing, after standing cooling, i.e., sediment separate out and solution, sediment can pass through backflow
Return to step（3）In recycled as crystal seed, filter liquor is water outlet, and it is 4.5mg/l to survey in solution the Oil repellent that dissociates, fluorine
Silicate content is 2.8mg/l.
Embodiment 4：
The present embodiment comprises the following steps：
（1）Water sampling 10000g, the Oil repellent that dissociates in sample is 20mg/l, and fluosilicic acid radical content is 28mg/l, is heated to
After 90 DEG C, Oil repellent rises to 34.2mg/L, and fluosilicic acid radical content is 13.6mg/L, is incubated 10min；
（2）In step（1）In solution after processing, the solution of medicament 1 is slowly added to, stirring while adding, mixing speed adds in 3r/s
95 DEG C are warming up to after complete, boiling 1h；
（3）In step（2）In solution after processing, medicament 2 is slowly added to, adjusts pH to 9, it is stirring while adding, 95 DEG C after adding
3h is incubated, mixing speed is in 1r/s in insulating process；
（4）In step（3）In solution after processing, after standing cooling, i.e., sediment separate out and solution, sediment can pass through backflow
Return to step（3）In recycled as crystal seed, filter liquor is water outlet, and it is 3.9mg/l to survey in solution the Oil repellent that dissociates, fluorine
Silicate content is 2.9mg/l.
Part is not described in detail by the present invention, is the known technology of those skilled in the art.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of further treatment technique of fluorine-containing silicon waste water, it is characterised in that comprise the following steps：
（1）It will be incubated after fluorine-containing water sample heat temperature raising；
（2）In step（1）In solution after processing, medicament 1 is slowly added to, stirring while adding, mixing speed adds in 2~3r/s
0.5~1h of boiling after complete；
（3）In step（2）In solution after processing, medicament 2 is slowly added to, and adjusts pH to 7~9, it is stirring while adding, after adding
2~3h is incubated, mixing speed is in 0.5~1r/s in insulating process；
（4）In step（3）In solution after processing, after standing cooling, sediment separate out and solution, filter liquor are water outlet.
A kind of 2. further treatment technique of fluorine-containing silicon waste water according to claim 1, it is characterised in that the step（1）
In, 90-95 DEG C is heated to, soaking time is 10~20min.
A kind of 3. further treatment technique of fluorine-containing silicon waste water according to claim 1, it is characterised in that the step（2）
In medicament 1 include aluminium salt and trace rare-earth element.
4. the further treatment technique of a kind of fluorine-containing silicon waste water according to claim 3, it is characterised in that the medicament 1
Dosage is controlled 0.1% or so.
A kind of 5. further treatment technique of fluorine-containing silicon waste water according to claim 1, it is characterised in that the step（4）
In medicament 2 include aluminium polychloride and polyacrylamide.
A kind of 6. further treatment technique of fluorine-containing silicon waste water according to claim 1, it is characterised in that the step（4）
In sediment can by backflow return to step（3）In recycled as crystal seed.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423790A (en) * | 2018-04-17 | 2018-08-21 | 湖北省宏源药业科技股份有限公司 | A kind of preparation formula and preparation method thereof except fluorite mineralizer |
| CN108585157A (en) * | 2018-04-23 | 2018-09-28 | 天津大学 | A method of removing coal converts fluorine in wastewater compound |
| CN110885147A (en) * | 2019-12-05 | 2020-03-17 | 南京大学 | Ion exchange defluorination method for efficiently complexing fluorine-containing wastewater |
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| WO2014136651A1 (en) * | 2013-03-04 | 2014-09-12 | 千代田化工建設株式会社 | Silica-containing water treatment apparatus, water treatment system, and method for treating silica-containing water |
| CN104591462A (en) * | 2015-01-15 | 2015-05-06 | 桂林电子科技大学 | Fluoride coprecipitation method for treating strong-acidity high-fluorine wastewater |
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| KR20160122031A (en) * | 2015-04-13 | 2016-10-21 | 최윤진 | Method for preparing sodium fluoride from fluorine-containing waste slurry |
| CN106512936A (en) * | 2016-11-11 | 2017-03-22 | 镇江市高等专科学校 | Hydrothermal method for preparing fluoride removal adsorbent and application thereof |
| CN107399750A (en) * | 2016-05-21 | 2017-11-28 | 上海问鼎环保科技有限公司 | A kind of method and device that liquid and fluoride waste recycling recovery acid solution are thrown using the electricity containing aluminium |
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| EP0255629A1 (en) * | 1986-08-05 | 1988-02-10 | Hoechst Aktiengesellschaft | Method for processing aqueous solutions of fluosilicic acid |
| WO2014136651A1 (en) * | 2013-03-04 | 2014-09-12 | 千代田化工建設株式会社 | Silica-containing water treatment apparatus, water treatment system, and method for treating silica-containing water |
| CN104591462A (en) * | 2015-01-15 | 2015-05-06 | 桂林电子科技大学 | Fluoride coprecipitation method for treating strong-acidity high-fluorine wastewater |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108423790A (en) * | 2018-04-17 | 2018-08-21 | 湖北省宏源药业科技股份有限公司 | A kind of preparation formula and preparation method thereof except fluorite mineralizer |
| CN108585157A (en) * | 2018-04-23 | 2018-09-28 | 天津大学 | A method of removing coal converts fluorine in wastewater compound |
| CN110885147A (en) * | 2019-12-05 | 2020-03-17 | 南京大学 | Ion exchange defluorination method for efficiently complexing fluorine-containing wastewater |
| CN110885147B (en) * | 2019-12-05 | 2021-11-26 | 南京大学 | Ion exchange defluorination method for efficiently complexing fluorine-containing wastewater |
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