WO2017017833A1 - Procédé de traitement d'eaux usées contenant du fluor et dispositif à cet effet - Google Patents

Procédé de traitement d'eaux usées contenant du fluor et dispositif à cet effet Download PDF

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Publication number
WO2017017833A1
WO2017017833A1 PCT/JP2015/071613 JP2015071613W WO2017017833A1 WO 2017017833 A1 WO2017017833 A1 WO 2017017833A1 JP 2015071613 W JP2015071613 W JP 2015071613W WO 2017017833 A1 WO2017017833 A1 WO 2017017833A1
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WIPO (PCT)
Prior art keywords
fluorine
added
calcium
containing wastewater
aluminum
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PCT/JP2015/071613
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English (en)
Japanese (ja)
Inventor
祐司 和田
則子 志村
寛子 河村
とみ子 斎藤
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Ｎｅｃファシリティーズ株式会社
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Priority to JP2017530559A priority Critical patent/JP6508747B2/ja
Priority to PCT/JP2015/071613 priority patent/WO2017017833A1/fr
Priority to TW105123702A priority patent/TWI651275B/zh
Publication of WO2017017833A1 publication Critical patent/WO2017017833A1/fr

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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
    • C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56—Macromolecular compounds
    • 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

Definitions

  • the present invention relates to a processing method and a processing apparatus which are widely used as a processing method for fluorine-containing wastewater and which separates solid and liquid by converting calcium into calcium fluoride by adding calcium.
  • Fluorine is a substance used in large quantities in the industry, and fluorine-containing wastewater is generated from, for example, semiconductor manufacturing plants, liquid crystal manufacturing plants, metal surface treatment plants, stainless steel manufacturing plants, ceramics manufacturing plants, and the like. It is a substance harmful to the human body, and the Water Pollution Control Law requires that it be treated to 8 mg / L or less, which is the drainage standard, when discharged into land water.
  • a method for treating fluorine-containing wastewater there is known a method (referred to as a calcium method) in which a calcium compound is added to fluorine-containing wastewater, and fluorine is converted into hardly soluble calcium fluoride fine particles and then solid-liquid separation is performed.
  • a calcium method there is a problem that about 10 to 20 mg / L of fluorine that has not been completely converted to calcium fluoride remains dissolved and flows out into the treated water. Therefore, in order to comply with wastewater standards, it is necessary to install advanced treatment equipment after the calcium method. Examples of advanced treatment methods include the aluminum method in which an aluminum salt is added and then solid-liquid separation, or phosphoric acid.
  • a fluoroapatite method in which a compound is added and then solid-liquid separated is known.
  • the aluminum method uses the property that dissolved fluorine is taken into the insoluble precipitates of aluminum hydroxide (Al (OH) 3 ) produced by the reaction between aluminum ions and alkali by adsorption or coprecipitation. It is.
  • Al hydroxide Al (OH) 3
  • sulfate bands generator name for aluminum sulfate
  • PAC polyaluminum chloride
  • PAC has characteristics such as a greater turbidity effect, that is, a suspended substance (SS) trapping effect than a sulfate band, and excellent agglomeration performance even at low water temperatures.
  • SS suspended substance
  • the aluminum method is widely adopted as an advanced treatment method because the aluminum salt is inexpensive and the fluorine concentration is surely lowered as the amount of aluminum added is increased.
  • the fluoroapatite method requires at least three times the amount of removed fluorine (about 5 times the mass) of phosphorus from its chemical formula, but in fact, calcium phosphate other than fluoroapatite is simultaneously produced, It is necessary to add much more phosphorus.
  • the price of a phosphoric acid compound is about 10 times that of an aluminum salt, and the running cost is very high, so the fluoroapatite method is rarely used as an advanced treatment method.
  • the aluminum salt used in the calcium method hardly contributes to insolubilization of dissolved fluorine, like the aluminum salt used in the aluminum method.
  • Patent Document 3 a method of adding a phosphoric acid compound after adding calcium and before solid-liquid separation is disclosed.
  • the method described in Patent Document 3 has a feature that it can treat a relatively high concentration fluorine-containing wastewater to several mg / L or less in a single stage treatment.
  • the treatment effect by fluoroapatite is not sufficient, and it is necessary to add about several hundred mg / L of phosphoric acid compound as phosphorus, which increases the running cost. was there.
  • Patent Document 4 can treat semiconductor factory wastewater containing 400 mg / L of fluorine up to 2.9 mg / L, there is a problem that the effect is not sufficient if the type of wastewater is different, as will be described later. .
  • the object of the present invention is to provide an advanced treatment sufficiently lower than the wastewater standard of 8 mg / L even with fluorine-containing wastewater containing a wide variety of coexisting substances at a high concentration by a simple device having only one solid-liquid separation device. It is an object of the present invention to provide a method for treating fluorine-containing wastewater, which can obtain water quality and can minimize the addition amount of a phosphoric acid compound that greatly affects running cost.
  • the inventors have earnestly studied the calcium method for fluorine-containing wastewater, and as a result, have obtained the following new knowledge.
  • a chemical containing a phosphate compound is added, and then an aluminum salt having a basicity of 20 to 80% is added.
  • the present inventors have found that even a wastewater containing various coexisting substances can be treated to a fluorine concentration that is surely lower than the wastewater standard of 8 mg / L, and the present invention has been completed.
  • the present invention has been made on the basis of the above knowledge, and the fluorine-containing wastewater treatment method according to the present invention adds calcium to the fluorine-containing wastewater to solidify the fluorine in the wastewater as a calcium fluoride insolubilized product.
  • the method for treating fluorine-containing wastewater to be liquid-separated calcium is added to the wastewater, a chemical containing a phosphoric acid compound is added without separating insoluble precipitates formed, and aluminum having a basicity of 20 to 80% is then added. It is characterized by adding salt.
  • the pH after addition of the phosphoric acid compound is preferably 4 to 9, and the pH after addition of the aluminum salt is preferably 5.5 to 8.
  • the phosphoric acid compound is preferably added in an amount of 1 to 5 times the amount of dissolved fluorine after adding calcium in the wastewater as phosphorus
  • the aluminum salt is the phosphoric acid compound to be added
  • it is preferably added in the range of 0.2 to 3.0 by mass ratio of P / Al.
  • the solid-liquid separated sludge does not have a crystalline fluoroapatite peak in X-ray diffraction.
  • the fluorine-containing wastewater treatment apparatus includes a reaction tank A that causes a calcium compound to act on fluorine-containing wastewater, a reaction tank B that causes a phosphoric acid compound to act on a treatment liquid from the reaction tank A, and the reaction.
  • the fluorine concentration can be reliably processed to 8 mg / L or less.
  • FIG. 1 is an apparatus and process explanatory diagram showing an embodiment of the present invention.
  • the fluorine-containing wastewater treatment apparatus in this embodiment includes a reaction tank A10, a reaction tank B20, a reaction tank C30, a coagulation tank 40, and a precipitation tank 50.
  • Fluorine-containing waste water 1 is introduced into the reaction tank A10, and calcium 2 and, if necessary, a pH adjusting agent 3 such as sulfuric acid, hydrochloric acid, caustic soda, slaked lime, and the like are added and mixed.
  • a pH adjusting agent 3 such as sulfuric acid, hydrochloric acid, caustic soda, slaked lime, and the like are added and mixed.
  • fine particles of calcium fluoride are generated.
  • the chemical 4 containing a phosphoric acid compound is added to the treated water from the reaction tank A10 in the reaction tank B20 and mixed with stirring.
  • the calcium 2 added in the reaction tank A10 surplus calcium that did not react with fluorine reacts with fluorine and phosphoric acid to produce fluoroapatite.
  • the dissolved fluorine concentration does not decrease so much by the re-dissolution of calcium fluoride.
  • the phosphoric acid compound used here may be any compound that can react with calcium and fluorine in the liquid to form fluoroapatite, and examples thereof include phosphoric acid and phosphate.
  • phosphoric acid and phosphate In addition to substances containing phosphate ions, phosphorous acid or hypophosphorous acid and its salts, such as low-oxidized phosphorus, are added, and an oxidizing agent is added to generate phosphate ions in the reaction vessel B20. You may let them.
  • the amount of the phosphoric acid compound to be added here depends greatly on the concentration of dissolved fluorine that did not react with calcium in the reaction tank A10. If the dissolved fluorine concentration is 10 to 20 mg / L, fluorine can be processed to about 4 mg / L, which is significantly lower than 8 mg / L, by adding 1 to 2 times the mass of phosphorus. If 2 to 5 times the mass of phosphorus is added, it can be processed to about 1 mg / L.
  • the pH in the reaction vessel B20 is desirably adjusted to a range suitable for the production of fluoroapatite, and specifically, it is desirably 4 to 9.
  • the aluminum salt 5 having a basicity of 20 to 80% is added.
  • the basicity is a numerical value representing the alkali content of an aluminum salt. If PAC, that is, Al 2 (OH) n Cl 6-n is taken as an example, the basicity is calculated by n / 6 ⁇ 100 (%).
  • the Commercial PAC basicity around 50%, i.e. OH - is but those contained 1.5 moles before and after Al is typically different basicity are also sold.
  • the basicity of sulfuric acid band and aluminum chloride is 0%.
  • a predetermined amount of alkali such as NaOH is added to an aluminum salt having a basicity of 0%, or an acid such as HCl is added to a PAC having a high basicity.
  • alkali such as NaOH
  • HCl an acid such as HCl
  • the addition amount of the aluminum salt 5 is determined by the required fluorine concentration and phosphorus concentration of the treated water, and is preferably 0.2 to 3.0 in terms of P / Al mass ratio (P / Al ratio), preferably 0.5 to 1. 0 is more preferable.
  • P / Al ratio P / Al mass ratio
  • the P / Al ratio is small, the amount of phosphorus outflow to the treated water decreases, but the fluorine treatment performance decreases.
  • the P / Al ratio is increased, the fluorine treatment performance is improved, but the amount of phosphorus outflow to the treated water increases and the amount of expensive phosphorus used increases.
  • reaction vessel C30 once generated fluoroapatite disappears. Since aluminum reacts with phosphoric acid to produce amorphous aluminum phosphate (AlPO 4 ), it is considered that the aluminum ion dissolves when the phosphate ions in the fluoroapatite are extracted. Further, if aluminum is added in an amount equivalent to or more than that for forming aluminum phosphate, almost all of the fluoroapatite disappears, and a part of the aluminum also forms aluminum hydroxide.
  • AlPO 4 amorphous aluminum phosphate
  • the present inventors surprisingly processed fluorine in the reaction tank C30.
  • the reaction was found to proceed rapidly. That is, aluminum phosphate that originally has no fluorine capturing ability, and aluminum hydroxide that should hardly contribute to insolubilization of fluorine by interaction with calcium fluoride, after passing through the steps of reaction tank A10 and reaction tank B20, It was found that the processing ability of fluorine was expressed specifically.
  • the sulfuric acid band and PAC originally have almost no difference in the fluorine trapping ability of the aluminum hydroxide to be produced
  • the aluminum to be added is surprisingly provided after the steps of the reaction tank A10 and the reaction tank B20.
  • the inventors have found that the basicity of the salt is greatly influenced, and that the higher basicity is not necessarily better, and that there is an effective range, and the present invention has been completed.
  • the pH in the reaction vessel C30 is desirably adjusted to a range suitable for the production of aluminum phosphate and aluminum hydroxide, and specifically, it is desirably pH 5.5 to 8.
  • the polymer flocculant 6 is added in the agglomeration tank 40, and the insoluble precipitate is agglomerated and the particles become coarse.
  • the liquid mixture from the flocculation tank 40 is allowed to stand in the precipitation tank 50, so that it is separated into the supernatant water 7 and the sludge 8, and the supernatant water 7 becomes the treated water 9.
  • the sludge 8 is pulled out from the bottom of the sedimentation tank 50 and is reduced in volume by performing a dehydration process or the like as necessary.
  • a membrane treatment apparatus can be used instead of the aggregation tank 40 and the precipitation tank 50.
  • Comparative Example 2 (Comparative Example 2) Compared to Comparative Example 1, except that 50 mg / L of sulfate band or PAC as aluminum was added as aluminum salt and stirred for 30 minutes while maintaining pH 6.5 ⁇ 0.5 with NaOH. The same operation as Example 1 was performed and the fluorine concentration of treated water was measured.
  • Comparative Example 3 The same operation as Comparative Example 1 except that 40 mg / L of phosphoric acid as phosphorus was added immediately before the filtration in Comparative Example 1 and the mixture was stirred for 30 minutes while maintaining the pH at 6.5 ⁇ 0.5 with NaOH. And the treated water fluorine concentration was measured. Moreover, the X-ray-diffraction measurement of the insoluble precipitate obtained by filtration was performed.
  • Comparative Example 4 Comparative Example 3 except that 50 mg / L of an aluminum salt sulfate band as an aluminum salt was added at the stage immediately before filtration in Comparative Example 3 and stirring was performed for 30 minutes while maintaining the pH at 6.5 ⁇ 0.5 with NaOH. The same operation was performed, and the fluorine concentration of the treated water was measured.
  • Example 1 In Comparative Example 4, the same operation as in Comparative Example 4 was carried out except that basic basin 53% PAC was used instead of the sulfuric acid band, and the treated water fluorine concentration was measured. Moreover, the X-ray-diffraction measurement of the insoluble precipitate obtained by filtration was performed. Furthermore, immediately before the addition of phosphoric acid, immediately before the addition of PAC, and after adding PAC and adjusting the pH with NaOH, the liquid after 30 minutes is filtered through 5A filter paper to remove insoluble precipitates and dissolved. The concentrations of fluorine, phosphorous phosphorus and aluminum were measured.
  • Example 5 (Comparative Example 5) In Example 1, phosphoric acid was added simultaneously with the addition of slaked lime, and the same operation as in Example 1 was performed except that the pH was adjusted to 6.5 ⁇ 0.5 with sulfuric acid and stirred for 30 minutes. Was measured.
  • Example 6 (Comparative Example 6)
  • the addition of PAC was performed simultaneously with the addition of phosphoric acid, and the same operation as in Example 1 was performed except that the pH was adjusted to 6.5 ⁇ 0.5 with NaOH and stirred for 30 minutes. Was measured.
  • Example 7 In Example 1, the same operation as in Example 1 was performed except that the addition order of phosphoric acid and PAC was reversed, and the fluorine concentration of treated water was measured.
  • Table 2 shows the treatment conditions of Example 1 and Comparative Examples 1 to 7 and the measurement results of the treated water fluorine concentration. Moreover, the X-ray-diffraction measurement result of the deposit (sludge) of Example 1 and Comparative Example 3 is shown in FIG. Further, Table 3 shows the dissolved fluorine, phosphate phosphorus, and aluminum concentrations measured in each reaction stage in Example 1. According to Table 2, the order of addition of chemicals is important for improving the fluorine treatment performance, and it is effective to add in the order of calcium ⁇ phosphoric acid ⁇ aluminum, and chemicals are added in this order. Even in this case, it can be seen that it is more effective to use PAC than aluminum sulfate as the aluminum salt.
  • Example 1 after the addition of phosphoric acid, dissolved fluorine and a part of phosphoric acid produce fluoroapatite. Then, by addition of PAC, the fluoroapatite disappears and dissolved fluorine. It can be seen that the phosphate ion concentration is greatly reduced. Moreover, since the dissolved Al concentration does not change, it can be said that the total amount of added aluminum is insoluble. Nevertheless, the X-ray diffraction measurement of Example 1 did not have the crystalline fluoroapatite peak as seen in Comparative Example 3, but only the calcium fluoride peak was detected.
  • Example 1 aluminum is added in an amount equal to or greater than the equivalent of aluminum phosphate production, that is, 0.8 with a P / Al (mass ratio) of 0.87 or less. From the above, it can be seen that after the disappearance of fluoroapatite, a mixture of aluminum phosphate, which is an amorphous substance, and aluminum hydroxide is formed, and simultaneously dissolved fluorine is insolubilized.
  • Example 3 In Example 2, the same operation as Example 2 was performed except that disodium hydrogen phosphate was used instead of phosphoric acid, and the treated water fluorine concentration was measured. Even when disodium hydrogenphosphate was added, the pH hardly changed and the pH was in the range of 6.5 ⁇ 0.5 for 30 minutes, so NaOH was not added.
  • the measurement result of the treated water fluorine concentration of Examples 2 and 3 is shown in FIG.
  • the treatment water fluorine concentration tends to decrease as the addition amount of phosphoric acid and PAC increases.
  • Comparative Examples 8 and 9 The treated water fluorine concentration of Comparative Examples 8 and 9 is shown in FIG. From the results of Comparative Example 8, it can be seen that the fluorine treatment effect produced by the aluminum salt producing aluminum hydroxide has almost no difference between sulfate bands and PACs having different basicities. Further, from the results of Comparative Example 9, it can be recognized that aluminum phosphate itself has a very low ability to capture fluorine because the treatment effect of fluorine is greatly reduced when aluminum phosphate coexists.
  • Example 4 The same operation as in Example 1 was performed except that aluminum salts having various basicities were used as the aluminum salt, and the fluorine concentration of the treated water was measured. The results are shown in Table 4 together with the results of Example 1 and Comparative Example 4.
  • FIG. 5 is a graph showing the relationship between basicity and treated water fluorine concentration.
  • Example 5 In Example 1, the same operation as in Example 1 was performed except that the pH after addition of phosphoric acid was set to 3 to 9, and the fluorine concentration in the treated water was measured.
  • Example 6 In Example 1, the same operation as in Example 1 was performed except that the pH after addition of PAC was set to 4.5 to 9, and the treated water fluorine concentration was measured.

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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)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

Afin de fournir un procédé de traitement d'eaux usées contenant du fluor qui permet de traiter des eaux usées contenant du fluor qui contiennent une concentration élevée en divers types de matériaux présents conjointement, et en conséquence, d'obtenir une eau traitée de haute qualité d'eau qui descend suffisamment sous la norme d'effluent de 8 mg/L en utilisant un simple dispositif équipé d'un seul séparateur solide-liquide, et également de réduire à un minimum la quantité de composé phosphate ajouté qui influence fortement les coûts d'utilisation, la présente invention concerne un procédé de traitement d'eaux usées contenant du fluor qui implique l'ajout de calcium aux eaux usées contenant du fluor, et la séparation solide-liquide du fluor dans les eaux usées sous forme de matériau insoluble fluorure de calcium, le calcium étant ajouté aux eaux usées, un médicament contenant un composé phosphate y étant ajouté sans séparation du précipité insoluble produit, et un sel d'aluminium possédant une basicité de 20 à 80 % y étant ensuite ajouté.
PCT/JP2015/071613 2015-07-30 2015-07-30 Procédé de traitement d'eaux usées contenant du fluor et dispositif à cet effet WO2017017833A1 (fr)

Priority Applications (3)

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JP2017530559A JP6508747B2 (ja) 2015-07-30 2015-07-30 フッ素含有排水の処理方法とその装置
PCT/JP2015/071613 WO2017017833A1 (fr) 2015-07-30 2015-07-30 Procédé de traitement d'eaux usées contenant du fluor et dispositif à cet effet
TW105123702A TWI651275B (zh) 2015-07-30 2016-07-27 含有氟之排水的處理方法及其裝置

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020218621A1 (fr) 2019-04-26 2020-10-29 ダイキン工業株式会社 Procédé et composition de traitement de l'eau

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS553802A (en) * 1978-06-12 1980-01-11 Kurita Water Ind Ltd Treatment of fluoride ion-containing waste water
JPH10128344A (ja) * 1996-11-06 1998-05-19 Japan Organo Co Ltd フッ素含有排水処理装置及び方法
JP2002177963A (ja) * 2000-12-13 2002-06-25 Yuji Sekine 浄水処理システム及び浄水処理方法
JP2004000962A (ja) * 2002-04-26 2004-01-08 National Institute Of Advanced Industrial & Technology フッ素イオンの除去方法及び除去剤
JP2004122059A (ja) * 2002-10-04 2004-04-22 Kurita Water Ind Ltd フッ素含有水の処理方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1311759A (zh) * 1998-07-17 2001-09-05 日本电气株式会社 含氟废水的处理方法及设备

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS553802A (en) * 1978-06-12 1980-01-11 Kurita Water Ind Ltd Treatment of fluoride ion-containing waste water
JPH10128344A (ja) * 1996-11-06 1998-05-19 Japan Organo Co Ltd フッ素含有排水処理装置及び方法
JP2002177963A (ja) * 2000-12-13 2002-06-25 Yuji Sekine 浄水処理システム及び浄水処理方法
JP2004000962A (ja) * 2002-04-26 2004-01-08 National Institute Of Advanced Industrial & Technology フッ素イオンの除去方法及び除去剤
JP2004122059A (ja) * 2002-10-04 2004-04-22 Kurita Water Ind Ltd フッ素含有水の処理方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020218621A1 (fr) 2019-04-26 2020-10-29 ダイキン工業株式会社 Procédé et composition de traitement de l'eau

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TWI651275B (zh) 2019-02-21
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