CN101157507B - Method for treating fluoric containing drainage - Google Patents
Method for treating fluoric containing drainage Download PDFInfo
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- CN101157507B CN101157507B CN2007101535723A CN200710153572A CN101157507B CN 101157507 B CN101157507 B CN 101157507B CN 2007101535723 A CN2007101535723 A CN 2007101535723A CN 200710153572 A CN200710153572 A CN 200710153572A CN 101157507 B CN101157507 B CN 101157507B
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- fluoride
- calcium
- reactive tank
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- water
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5209—Regulation methods for flocculation or precipitation
-
- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/583—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing fluoride or fluorine 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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention provides a treatment method for fluoride-containing wasterwater, which can inhibit precipitation of fine calcium fluoride to get stable treated water and produce sludge with low miosture content in less procedures. The treatment method includes: a reaction procedure of adding calcium compound into the fluoride-containing wasterwater to produce insoluble with calcium fluoride, a separation procedure of performing solid-liquid separation between the sludge with calcium fluoride insoluble and separation water, a sludge return procedure of returning the separated sludge used as returning sludge to the reaction procedure. In the reaction procedure, calcium compound, the equivalent of which is less than the equivalent of the fluoride compound ions, is added to the reaction groove of the first section by using two series connected reaction grooves, to ensure that the density of the calcium ions residues is more than 1 milligram per litre and less than 5 milligram per litre, and the density of the fluoride compound ions residues is less than 80 milligram per litre; calcuim compound, the equivalent of which is more than the equivalent of the fluoride compound residues in the reaction groove of the first section, is added to the reaction groove of the second section, to ensure that the density of the fluoride ions is less than 15 milligram per litre.
Description
Technical field
The present invention relates in fluoride waste, add calcium cpds such as calcium chloride and calcium hydroxide, make fluorine become insoluble Calcium Fluoride (Fluorspan) (CaF
2) and carry out the method for solid-liquid separation.The present invention be more particularly directed to make calcium cpd to act on fluorine in the waste water effectively, obtain the treating water of fine water, and generate the treatment process of the fluoride waste of the low mud of water ratio.
Background technology
As the fluorinated water that contains fluoride ion, have in making semiconductor device from the fluoride waste of silicon wafer manufacturing process discharge, pickling waste waters, the waste water that the aluminium surface treatment produces, the waste water that the fluoric acid manufacturing produces, the waste water that the fertilizer manufacturing produces, the waste water of waste incineration generation etc. from the discharge of stainless-steel sheet manufacturing process.General two sections following processing, the multistage of adopting handled, and these fluoride wastes are handled.
That is: employing has the treatment process of following operation: add calcium hydroxide at first section in fluoride waste, pH is adjusted to 10～11 first reaction process; With add the excessive calcium hydroxide that is equivalent to 120～250mg/L calcium ion to this reaction solution, and with hydrochloric acid neutral second reaction process (for example, referring to Patent Document 1).Because the reaction of calcium hydroxide and fluoric acid is very slow under alkaline condition, so pH is maintained acidity or neutrality, and adds that to be equivalent to fluorion be 0.3～0.5 normal calcium hydroxide, separate the insolubles that generates, supernatant water is carried out same processing (for example, referring to Patent Document 2) repeatedly.
Patent documentation 1: TOHKEMY 2004-283759 (claims, Fig. 1)
Patent documentation 2: No. the 3378362nd, Japanese Patent (claims, the 13rd section)
Adopt calcium hydroxide as making the undissolved reagent of fluorine, when double as is adjusted to 10～11 pH adjustment agent with pH, then add the above calcium hydroxide of fluorion equivalent sometimes, fine Calcium Fluoride (Fluorspan) is separated out, this Calcium Fluoride (Fluorspan) leak in the treating water, produces treating water water quality problem of unstable.In addition, if in order to obtain the treating water of fine water, flocculation agent such as use polymkeric substance carry out coagulative precipitation to the fine Calcium Fluoride (Fluorspan) that generates and handle the problem that the water ratio that then produces the mud that generates uprises, the amount of waste increases.In addition, adopting interpolation is 0.3～0.5 normal calcium hydroxide with respect to fluorion, when separating the method for the insolubles that is generated, must add operation and separation circuit repeatedly at least 3 times.And to reduce fluorine concentration in the treating water to 15mg/L, then must carry out repeatedly 4～5 times.
Summary of the invention
Find by the present invention, in order to obtain stable treated water with less operation, and the low mud of generation water ratio, if remove fluorion at first roughly, even then add the above calcium cpd of equivalent of residual fluoride ion, also can suppress to generate fine Calcium Fluoride (Fluorspan), to such an extent as to solve above-mentioned prior art problems.That is: a first aspect of the present invention relates to the treatment process of fluoride waste, it is characterized in that, comprising: add calcium cpd in fluoride waste, generate the reaction process of the insolubles that contains Calcium Fluoride (Fluorspan);
The mud and the dried up separation circuit that carries out solid-liquid separation of branch that will contain the Calcium Fluoride (Fluorspan) insolubles of generation; With
The above-mentioned mud that separation is obtained is back to the mud reflow process of above-mentioned reaction process as returned sluge, wherein,
In above-mentioned reaction process, use placed in-line 2 sections reactive tanks, in first section reactive tank, add normal calcium cpd less than fluoride ion, making residual calcium ion is below the above 50mg/L of 1mg/L, making residual fluoride ion is below the 80mg/L; In second section reactive tank, add first section reactive tank the calcium cpd more than the equivalent of residual fluoride ion, make fluoride ion concentration less than 15mg/L.
In addition, a second aspect of the present invention relates in first aspect, the pH of first section reactive tank is adjusted to the treatment process of 3～6 fluoride waste.
The invention effect
Add the normal calcium cpd less than fluoride ion in first section reactive tank, making residual calcium ion is below the above 50mg/L of 1mg/L, therefore can suppress the generation of fine Calcium Fluoride (Fluorspan), removes fluorine roughly.In addition, excessively add the calcium cpd more than the equivalent of residual fluoride ion to second section reactive tank, fluoride ion is not dissolved, therefore can suppress the generation of fine Calcium Fluoride (Fluorspan).Make the treating water water conditioning, and the growth of Calcium Fluoride (Fluorspan) particle is increased, thus, generate the low mud of water ratio.In addition, the pH of first section reactive tank is adjusted at 3～6 o'clock, also can even the addition of calcified material is few.
Description of drawings
Fig. 1 is the system diagram of the embodiment of the treatment process of expression fluoride waste of the present invention.
Fig. 2 is the graphic representation of the solubleness of expression Calcium Fluoride (Fluorspan).Among the figure, the longitudinal axis is represented calcium concn, and transverse axis is represented fluoride ion concentration, and dotted line is a solubility curve, and solid line was a solubility curve, and long and short dash line is the equivalent line of calcium ion and fluoride ion.
Embodiment
Below, with reference to Fig. 1, embodiment is described.
Fig. 1 is the sketch chart of treatment scheme of the present invention.Wherein, 1 is that former water flows into pipeline, and 2 is first reactive tank, and 3 is second reactive tank, and 4 is collection surface, and 5 is settling bath, and 6 is the mud return line road, and 7 for calcium adds pipe arrangement, and 8 are pH adjustment agent injection pipe arrangement.
Former water as fluoride waste flows into pipeline 1 inflow first reactive tank from former water, at this, adds the normal calcium cpd less than fluoride ion.In addition, inject pH and adjust agent, pH is adjusted to 3～11, preferably be adjusted to 3～6.Make the reaction of calcium ion and fluoride ion, separate out Calcium Fluoride (Fluorspan).If pH is less than 3, then the solubleness of Calcium Fluoride (Fluorspan) increases, and fluoride ion concentration can not reduce.And if pH then significantly separates out lime carbonate greater than 11, produce the problem of incrustation scale (scale).PH is 3～6 o'clock, makes the fluoride ion reaction with less calcium addition, separates out Calcium Fluoride (Fluorspan).At this moment, following returned sluge becomes nuclear, and Calcium Fluoride (Fluorspan) is separated out on its surface, has therefore suppressed the generation of fine Calcium Fluoride (Fluorspan), and the growth of Calcium Fluoride (Fluorspan) particle is increased.
According to the inventor's etc. research as can be known: if flow into the fluoride ion concentration of reactive tank and reactive tank residual calcium ion concn be positioned at solubility curve shown in dotted lines in Figure 2 (the theoretical dissolution degree of Calcium Fluoride (Fluorspan) amass [Ca
2+] [F
-]
2=4.9 * 10
-11Mol
3/ l
3) with the zone of crossing the solubility curve clamping shown in the solid line, the generation of then fine Calcium Fluoride (Fluorspan) is suppressed, and separates out Calcium Fluoride (Fluorspan) on the nuclear surface simultaneously, the Calcium Fluoride (Fluorspan) particle is grown up and is increased.In addition, if above-mentioned concentration is the high density that was higher than solubility curve, then generate fine Calcium Fluoride (Fluorspan).When handling fluoride ion and make its concentration less than 15mg/L, must there be the above calcium ion of equivalent of fluoride ion, be preferably than equivalent and Duo the calcium ion of 200～300mg/L.Therefore, according to Fig. 2 as can be known, must at first reduce concentration of fluoride, be below the 80mg/L.
The addition of calcium cpd is determined by following: the fluoride ion concentration that makes first reactive tank is below the 80mg/L, and makes the concentration of residual calcium ion become lower concentration.In other words, even interpolation is less than the normal calcium cpd of fluoride ion, also residual to a certain degree calcium ion in first reactive tank.That is, making residual calcium ion is below the above 50mg/L of 1mg/L.If calcium ion less than 1mg/L, is then worried to remove fluorine roughly; And if calcium ion is greater than 50mg/L, the generation of the Calcium Fluoride (Fluorspan) of then worrying to suppress fine.
Secondly, the reaction solution of first reactive tank 2 that fluorine is removed does not roughly carry out solid-liquid separation, and makes it flow into second reactive tank 3.In this groove, excessively add calcium cpd to more than the equivalent of fluoride ion, residual fluoride ion is not dissolved.At this moment, adjust pH, consider the discharging for the treatment of water, preferably pH is adjusted between 5.8～8.6.
Preferably the reaction solution with second reactive tank 3 imports collection surface 4.When because of setting the reasons such as addition of the calcium cpd be added into first reactive tank 2 or second reactive tank 3 mistakenly, and when causing the generation of the Calcium Fluoride (Fluorspan) that can not suppress fine, perhaps be further to improve treating water water quality, can in collection surface 4, add polymer coagulant (not shown).
Then, make condensed or without reaction solution solid-liquid separation in settling bath 5 of agglomeration process, the insolubles slurry that makes fluorinated calcium is back to first reactive tank 2 as returned sluge from mud return line road 6, becomes the nuclear of separating out Calcium Fluoride (Fluorspan) after calcium and fluoride ion react.The mud quantity of reflux is about 0.01～10 times of raw water flow, is generally 0.05～0.5 times of raw water flow, when the fluoride concn of former water is high, takes into account dilution, is preferably 0.1～10 times.Branch is dried up to be discharged from from treating water escape route 9 as treating water.
As calcified material,, can enumerate calcium chloride and calcium hydroxide as long as the compound of the calcium ion that can dissociate is just passable.Adjust agent as pH, can enumerate acid such as alkali such as sodium hydroxide, potassium hydroxide, calcium hydroxide, hydrochloric acid, sulfuric acid.
Embodiment
[embodiment 1]
According to treatment scheme shown in Figure 1, fluoride waste is handled.
Raw water quality is as described below.
PH:3.4, F:131mg/L, PO
4 3--P:1mg/L, SO
4 2-: 21.3mg/L, SiO
2: 39mg/L, total organic matter (TOC): 3.3mg/L.
The capacity of first reactive tank 2, second reactive tank 3 and collection surface 4 is respectively 1L, and the capacity of settling bath 5 is 15L.The flow of above-mentioned former water is 4L/Hr, and sludge back flow quantity is 0.1L/Hr.Use calcium chloride as calcium cpd, in first reactive tank 2 and second reactive tank 3, add respectively.Adjust about pH, use the sodium hydroxide of 0.1N, the pH of first reactive tank 2 and second reactive tank is adjusted to 5 ± 0.5.In collection surface 4, do not add polymer coagulant, just it is used as hold up tank.In addition, when handling beginning, the median size of adding as kind of crystalline substance to first reactive tank 2 is the Calcium Fluoride (Fluorspan) of 5 μ m.Filter first and second reactive tank interior reaction solution and treating water with membrane filter (membrane filter) (aperture 0.45 μ m), carry out the analysis of filtrate.The results are shown in the table 1.Table 1 has also been represented the addition of calcium chloride.In addition, utilize separating centrifuge,, slough the water in the precipitating sludge, measure water ratio, and be illustrated in the table 1 with 2000G.
[comparative example 1]
In embodiment 1, do not add calcium chloride to second reactive tank, only add and compare excessive calcium chloride with the fluoride ion equivalent to first reactive tank, in addition, handle similarly to Example 1.The water quality for the treatment of water is illustrated in the table 1.
[comparative example 2]
In comparative example 1, in collection surface 4, add polymer coagulant Network リ Off ロ ッ Network (Kurita Water Industries Ltd's registered trademark) PA331 (partial hydrolystate of polyacrylamide) with 3mg/L, in addition, handle equally with comparative example 1.The water quality for the treatment of water is illustrated in the table 1.In addition, utilize separating centrifuge,, slough the water in the precipitating sludge, measure water ratio, and be illustrated in the table 1 with 2000G.
Table 1
| Experiment No. | |
Comparative example 1 | Comparative example 2 | |
| First reactive tank | Calcium cpd addition (mgCa/L) | 90 | 340 | 340 |
| F ionic concn (mgF/L) | 64 | 15 | 15 | |
| Calcium concn (mgCa/L) | 8 | 195 | 195 | |
| Second reactive tank | Calcium cpd addition (mgCa/L) | 250 | 0 | 0 |
| F ionic concn (mgF/L) | 15 | - | - | |
| Calcium concn (mgCa/L) | 195 | - | - | |
| Treating water | F ionic concn (mgF/L) | 13 | 13 | 13 |
| Total F concentration (mgF/L) | 13 | 40 | 13 | |
| Turbidity (NTU) | ＜1 | 23 | ＜1 | |
| Generate mud (after the centrifuge dehydration) | Water ratio (%) | 8 | - | 42 |
| Sludge quantity (weight in wet base: g/d) | 26 | - | 42 |
Learn from table 1: comparative example 1, because the reaction of the calcium of the fluorine of high density and high density generates fine Calcium Fluoride (Fluorspan) particle, because leak to the treating water side, total fluorine for the treatment of water is dense, does not obtain good treating water again.In comparative example 2, because remove, so obtain good treating water with the fine Calcium Fluoride (Fluorspan) particle of polymer coagulant cohesion and with its precipitation.But, be difficult for control except that moisture, so the mud generation increases owing to condensed the mud of subparticle.In embodiment 1, even the calcium total addition level is identical,, generate so suppressed fine Calcium Fluoride (Fluorspan) particulate because in first reactive tank, remove fluorine roughly, Calcium Fluoride (Fluorspan) is separated out on kind of a brilliant surface, obtain good water quality treatment thus.
Claims (2)
1. the treatment process of a fluoride waste is characterized in that, comprising:
In fluoride waste, add calcium cpd, generate the reaction process of the insolubles that contains Calcium Fluoride (Fluorspan);
The mud and the dried up separation circuit that carries out solid-liquid separation of branch that will contain the Calcium Fluoride (Fluorspan) insolubles of generation; With
The described mud that separation is obtained is back to the mud reflow process of described reaction process as returned sluge, wherein,
In described reaction process, use placed in-line 2 sections reactive tanks, in first section reactive tank, add normal calcium cpd less than fluoride ion, making residual calcium ion is below the above 50mg/L of 1mg/L, making residual fluoride ion is below the 80mg/L; In second section reactive tank, add first section reactive tank the calcium cpd more than the equivalent of residual fluoride ion, make fluoride ion concentration less than 15mg/L.
2. the treatment process of fluoride waste as claimed in claim 1 is characterized in that,
The pH of first section reactive tank is adjusted to 3～6.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006257731A JP4650384B2 (en) | 2006-09-22 | 2006-09-22 | Treatment method for fluorine-containing wastewater |
| JP2006-257731 | 2006-09-22 | ||
| JP2006257731 | 2006-09-22 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101157507A CN101157507A (en) | 2008-04-09 |
| CN101157507B true CN101157507B (en) | 2011-07-27 |
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| CN2007101535723A Expired - Fee Related CN101157507B (en) | 2006-09-22 | 2007-09-21 | Method for treating fluoric containing drainage |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP4650384B2 (en) |
| KR (1) | KR101333261B1 (en) |
| CN (1) | CN101157507B (en) |
| TW (1) | TWI422532B (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823799B (en) * | 2009-03-06 | 2012-08-15 | 昆山工研院华科生物高分子材料研究所有限公司 | Method for treating acidic fluorine-containing waste water |
| TW201236983A (en) * | 2011-03-03 | 2012-09-16 | Chiou-Mei Chen | Treatment method for waste water in process of preparing silicon chip |
| CN102225814B (en) * | 2011-04-13 | 2012-11-14 | 黑龙江省牡丹江农垦奥宇石墨深加工有限公司 | Fluorine-containing waste water processing apparatus and processing method thereof |
| CN102350176A (en) * | 2011-09-07 | 2012-02-15 | 四川明晶光电科技有限公司 | Method for treating fluoride waste water and gas |
| KR101382171B1 (en) * | 2012-11-07 | 2014-04-10 | 대림산업 주식회사 | Method for treating wastewater including fluorine component |
| JP5692278B2 (en) * | 2013-04-25 | 2015-04-01 | 栗田工業株式会社 | Method and apparatus for treating fluoride-containing water |
| CN106255666A (en) * | 2014-06-26 | 2016-12-21 | 栗田工业株式会社 | The processing method of fluoride water and processing means |
| KR101559852B1 (en) * | 2014-11-13 | 2015-10-13 | 오에스케이 주식회사 | Treating method for waste water contaning fluoroboric acid produced in etch process |
| JP6728546B2 (en) * | 2015-03-31 | 2020-07-22 | 住友金属鉱山エンジニアリング株式会社 | Wastewater treatment method, wastewater treatment system |
| CN107792832B (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 |
| KR102112112B1 (en) * | 2019-11-19 | 2020-05-18 | 에코매니지먼트코리아홀딩스 주식회사 | Process for recycling wasteacid |
| CN111646591A (en) * | 2020-06-08 | 2020-09-11 | 苏州晟德水处理有限公司 | Treatment method of semiconductor fluorine-containing wastewater |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1765763A (en) * | 2004-10-28 | 2006-05-03 | 力晶半导体股份有限公司 | Method for treating fluorine-containing waste water |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5223851A (en) * | 1975-08-15 | 1977-02-23 | Hitachi Ltd | Drainage disposal process |
| JPS5846355B2 (en) * | 1976-01-09 | 1983-10-15 | 三菱マテリアル株式会社 | Treatment method for fluorine-containing ammonia waste liquid |
| JPS627490A (en) * | 1985-07-05 | 1987-01-14 | Tokuyama Soda Co Ltd | Treatment of waste water |
| TW495487B (en) * | 1999-06-07 | 2002-07-21 | Ind Tech Res Inst | Process for removing fluoride from wastewater |
| JP2001219177A (en) * | 2000-02-10 | 2001-08-14 | Kurita Water Ind Ltd | Method and apparatus for treating fluorine-containing water |
| TW200538402A (en) * | 2004-05-19 | 2005-12-01 | Powerchip Semiconductor Corp | Method of fluoride-contained wastewater treatment |
| JP4524796B2 (en) * | 2004-12-14 | 2010-08-18 | 栗田工業株式会社 | Method and apparatus for treating fluorine-containing wastewater |
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2006
- 2006-09-22 JP JP2006257731A patent/JP4650384B2/en not_active Expired - Fee Related
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2007
- 2007-09-11 TW TW096133811A patent/TWI422532B/en not_active IP Right Cessation
- 2007-09-21 CN CN2007101535723A patent/CN101157507B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1765763A (en) * | 2004-10-28 | 2006-05-03 | 力晶半导体股份有限公司 | Method for treating fluorine-containing waste water |
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| Title |
|---|
| JP特开2001-219177A 2001.08.14 |
| JP特开2005-840A 2005.01.06 |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4650384B2 (en) | 2011-03-16 |
| JP2008073646A (en) | 2008-04-03 |
| KR20080027193A (en) | 2008-03-26 |
| TW200817289A (en) | 2008-04-16 |
| CN101157507A (en) | 2008-04-09 |
| KR101333261B1 (en) | 2013-11-27 |
| TWI422532B (en) | 2014-01-11 |
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