JP4972584B2 - Recovery method of phosphorus extract - Google Patents
Recovery method of phosphorus extract Download PDFInfo
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- JP4972584B2 JP4972584B2 JP2008052861A JP2008052861A JP4972584B2 JP 4972584 B2 JP4972584 B2 JP 4972584B2 JP 2008052861 A JP2008052861 A JP 2008052861A JP 2008052861 A JP2008052861 A JP 2008052861A JP 4972584 B2 JP4972584 B2 JP 4972584B2
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- 239000011574 phosphorus Substances 0.000 title claims description 121
- 229910052698 phosphorus Inorganic materials 0.000 title claims description 121
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims description 119
- 238000011084 recovery Methods 0.000 title claims description 38
- 238000000034 method Methods 0.000 title claims description 36
- 239000007788 liquid Substances 0.000 claims description 67
- 239000004744 fabric Substances 0.000 claims description 42
- 238000000926 separation method Methods 0.000 claims description 40
- 238000001914 filtration Methods 0.000 claims description 29
- 239000010802 sludge Substances 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 13
- 239000012670 alkaline solution Substances 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000003929 acidic solution Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- -1 polypropylene Polymers 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 229920002978 Vinylon Polymers 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000126 substance Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000010801 sewage sludge Substances 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000005273 aeration Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- DJFBJKSMACBYBD-UHFFFAOYSA-N phosphane;hydrate Chemical compound O.P DJFBJKSMACBYBD-UHFFFAOYSA-N 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Processing Of Solid Wastes (AREA)
- Filtering Materials (AREA)
- Filtration Of Liquid (AREA)
Description
本発明は、リンが溶解した溶液と不溶性成分との混合液から不溶性成分を除去してリン抽出液を回収するリン抽出液の回収方法に関する。 The present invention relates to a method for recovering a phosphorus extract that recovers a phosphorus extract by removing an insoluble component from a mixed solution of a solution in which phosphorus is dissolved and an insoluble component.
近年、リン資源の枯渇が懸念されリン回収技術が注目されている。下水や下水汚泥はリンを含むため、各種のリン回収技術が開発、実用化されている。なかでも、下水汚泥等のようなリン含有汚泥の焼却灰からリンを回収する技術は、リン資源の回収と焼却灰の有効利用の観点から有望視されている。 In recent years, phosphorus recovery technology has attracted attention due to concerns over depletion of phosphorus resources. Since sewage and sewage sludge contain phosphorus, various phosphorus recovery technologies have been developed and put to practical use. Among them, the technology for recovering phosphorus from incineration ash of phosphorus-containing sludge such as sewage sludge is promising from the viewpoint of recovery of phosphorus resources and effective use of incineration ash.
焼却灰からリンを回収するには、焼却灰中のリンを薬剤で抽出する必要があり、抽出方法としては、硫酸、塩酸、硝酸等の強酸性溶液を用いて抽出する方法（例えば、下記特許文献１〜５）や、苛性ソーダ水溶液等のような強アルカリ性溶液を用いて抽出する方法（例えば、下記特許文献６〜８）が知られている。強酸性溶液や強アルカリ性溶液を用いることで、リンを含有する汚泥の焼却灰から、効率よくリンを抽出することができる。 In order to recover phosphorus from the incineration ash, it is necessary to extract the phosphorus in the incineration ash with a chemical. As an extraction method, a method using a strongly acidic solution such as sulfuric acid, hydrochloric acid, nitric acid (for example, the following patent) Documents 1 to 5) and methods of extraction using a strong alkaline solution such as an aqueous caustic soda solution (for example, Patent Documents 6 to 8 below) are known. By using a strong acidic solution or a strong alkaline solution, phosphorus can be efficiently extracted from the incineration ash of sludge containing phosphorus.
そして、焼却灰中のリンを薬剤中に抽出した後、焼却灰と薬剤とを含む混合液を固液分離して焼却灰などの不溶性分を除去し、回収したリン抽出液に、消石灰（水酸化カルシウム）など加えてリン化合物として析出させるようにして、焼却灰からリンを回収している。
リンを含有する汚泥の焼却灰から、リンを高純度でかつ効率よく回収するには、焼却灰中のリンを溶出させたリン抽出液と焼却灰などの不溶性成分とを含む混合液を固液分離して、不溶性成分の混入の少ない清澄なリン抽出液を効率的に回収する必要がある。固液分離する方法としては、例えば、遠心分離、ろ過による方法がある。 To recover phosphorus with high purity and efficiency from incineration ash of phosphorus-containing sludge, a mixed liquid containing phosphorus extract that elutes phosphorus in incineration ash and insoluble components such as incineration ash is solid-liquid. It is necessary to separate and efficiently recover a clear phosphorus extract with little insoluble components. As a method for solid-liquid separation, for example, there are methods by centrifugation and filtration.
しかしながら、遠心分離による方法では、遠心分離機は設備コストが高いという問題があった。また、遠心分離機の作動には、回転エネルギーを要するので、運転コストがかかるという問題があった。さらには、遠心分離では、固形分回収率が低く、回収された抽出液中に、数百ｍｇ／Ｌ程度の焼却灰が混入するため、最終製品として得られるリン化合物の商品価値が損なわれる問題があった。 However, in the method using centrifugation, the centrifuge has a problem that the equipment cost is high. Moreover, since the rotational energy is required for the operation of the centrifuge, there is a problem that the operation cost is high. Furthermore, in the centrifugal separation, the solid content recovery rate is low, and the incinerated ash of about several hundred mg / L is mixed in the recovered extract, so that the commercial value of the phosphorus compound obtained as the final product is impaired. was there.
また、ろ過による固液分離方法では、固液分離を効率的に行うことが困難で、工業的なリン回収工程には適用しにくかった。 In addition, the solid-liquid separation method by filtration is difficult to perform solid-liquid separation efficiently, and is difficult to apply to an industrial phosphorus recovery process.
また、上記特許文献８には、フィルタープレスによるろ布を用いたろ過が開示されている。しかしながら、フィルタープレスは、バッチ操作の運転となるため、目的とするリン抽出液を得るために長時間を要する結果、設備が大きくなり設備コストが高くなるという問題があった。また、ろ布が目詰まりし易く、高圧水での頻繁な洗浄を必要とし維持管理が面倒で運転コストも高くなる問題があった。すなわち、フィルタープレスは固形分の汚泥を得ることを目的とした固液分離装置であることから、液体であるリン抽出液を得ることを目的とした操作には不適であり、リン抽出液を得るには効率が悪く、処理に時間を要し、高コストとなる問題があった。 Moreover, the said patent document 8 discloses the filtration using the filter cloth by a filter press. However, since the filter press is operated as a batch operation, it takes a long time to obtain the target phosphorus extract, resulting in a problem that the equipment becomes large and the equipment cost becomes high. Further, there is a problem that the filter cloth is easily clogged, requires frequent washing with high-pressure water, is troublesome to maintain, and increases the operation cost. That is, since the filter press is a solid-liquid separator intended to obtain a solid sludge, it is not suitable for an operation intended to obtain a liquid phosphorus extract, and a phosphorus extract is obtained. However, there is a problem that the efficiency is low, the processing takes time, and the cost is high.
また、強酸性溶液や強アルカリ性溶液を用いて、焼却灰からリンの抽出を行った場合、化学的な腐食や材料劣化がきわめて生じ易い条件であるため、リン抽出液と、リン抽出後の焼却灰を含む不溶性成分とを分離する技術の開発はこれまで充分になされていないのが現状であった。 In addition, when phosphorus is extracted from incineration ash using a strong acid solution or a strong alkaline solution, chemical corrosion and material deterioration are extremely likely to occur. Therefore, the phosphorus extract and incineration after phosphorus extraction At present, the technology for separating insoluble components including ash has not been sufficiently developed.
したがって、本発明の目的は、リンを含有する汚泥の焼却灰から、低コストで、効率よく、清澄なリン抽出液を回収するリン抽出液の回収方法を提供することである。 Accordingly, an object of the present invention is to provide a method for recovering a phosphorus extract that efficiently recovers a clear phosphorus extract at low cost from incinerated ash of sludge containing phosphorus.
上記目的を達成するため、本発明のリン抽出液の回収方法は、リンを含有する汚泥の焼却灰に、強酸性溶液又は強アルカリ性溶液を加えてリンを溶解させるリン溶解工程と、リンが溶解した溶液と不溶性成分との混合液から不溶性成分を除去してリン抽出液を回収する固液分離工程と、を含むリン抽出液の回収方法であって、前記固液分離工程は、吸引ポンプを作動させて前記混合液をろ布を備えたろ過板の一次側に通水させ、該ろ布の一次側表面に前記混合液中の不溶性成分による層を形成させたのち、前記吸引ポンプを停止し、サイフォン効果によりろ過処理を行い、前記ろ過板の二次側からリン抽出液を回収することを特徴とする。 In order to achieve the above object, the method for recovering a phosphorus extract of the present invention includes a phosphorus dissolution step in which a strong acidic solution or a strong alkaline solution is added to the incinerated ash of sludge containing phosphorus to dissolve phosphorus, And a solid-liquid separation step of recovering the phosphorus extract by removing the insoluble component from the mixed solution of the solution and the insoluble component, wherein the solid-liquid separation step includes a suction pump. Operate and let the mixed solution pass through the primary side of the filter plate equipped with a filter cloth , and after forming a layer of insoluble components in the mixed solution on the primary side surface of the filter cloth , stop the suction pump Then, a filtration process is performed by a siphon effect , and a phosphorus extract is recovered from the secondary side of the filter plate.
本発明のリン抽出液の回収方法によれば、リン抽出液とリン抽出後の焼却灰とを含む混合液を、ろ布を備えたろ過板の一次側に通水させて、該ろ布の一次側表面に混合液中の不溶性成分による層を形成させた状態でろ過処理を行う。ろ布の一次側表面に形成させた不溶性成分による層は、フィルターとして機能するので、ろ過板の二次側から回収するリン抽出液は、焼却灰などの不溶性成分の混入が少なく、極めて清澄なリン抽出液を効率よく回収することができる。 According to the method for recovering a phosphorus extract of the present invention, a mixed liquid containing a phosphorus extract and incinerated ash after phosphorus extraction is passed through the primary side of a filter plate provided with a filter cloth, Filtration is performed in a state where a layer of insoluble components in the mixed liquid is formed on the primary side surface. Since the layer of insoluble components formed on the primary surface of the filter cloth functions as a filter, the phosphorus extract recovered from the secondary side of the filter plate is very clear and contains little insoluble components such as incineration ash. The phosphorus extract can be efficiently recovered.
本発明のリン抽出液の回収方法では、前記ろ過板として、支持材の両面をろ布で囲み、該ろ布の全周を閉じて袋状となし、少なくとも一端にリン抽出液回収管が接続されているろ過板を用いることが好ましい。 In the method for recovering a phosphorus extract of the present invention, as the filter plate, both sides of a support material are surrounded by a filter cloth, the entire periphery of the filter cloth is closed to form a bag, and a phosphorus extract recovery pipe is connected to at least one end. It is preferable to use a filter plate.
本発明のリン抽出液の回収方法では、前記ろ布として、ポリプロピレン、塩化ビニリデン、ビニロンから選ばれた一種以上の材質で構成されたものを用いることが好ましい。これらの材質からなるろ布は、耐薬品性に優れるので、ろ過処理時にろ布が劣化し難く、ろ布の交換頻度を抑えることができる。 In the method for recovering a phosphorus extract of the present invention, it is preferable to use a filter made of at least one material selected from polypropylene, vinylidene chloride, and vinylon as the filter cloth. Since the filter cloth made of these materials is excellent in chemical resistance, the filter cloth is hardly deteriorated during the filtration treatment, and the frequency of replacement of the filter cloth can be suppressed.
本発明のリン抽出液の回収方法では、前記固液分離工程において、ろ過処理を開始する前に、前記混合液を攪拌することが好ましい。混合液中の不溶性成分は沈降し易いので、混合液中の不溶性成分の濃度が低い場合、ろ布の一次側表面に溶液中の不溶性成分による層を形成する際に時間を要することがあるが、ろ過処理を開始する前に、混合液を攪拌することで、不溶性成分の沈降を防止できる。このため、ろ布の一次側表面に溶液中の不溶性成分による層を短時間で形成でき、効率よくリン抽出液を回収できる。 In the method for recovering a phosphorus extract of the present invention, in the solid-liquid separation step, it is preferable to stir the mixed solution before starting the filtration treatment. Since insoluble components in the mixed solution easily settle, when the concentration of insoluble components in the mixed solution is low, it may take time to form a layer of insoluble components in the solution on the primary surface of the filter cloth. The insoluble component can be prevented from settling by stirring the mixed solution before starting the filtration treatment. For this reason, the layer by the insoluble component in a solution can be formed in a short time on the primary surface of a filter cloth, and a phosphorus extract can be efficiently recovered.
本発明によれば、リン抽出液とリン抽出後の焼却灰とを含む混合液を、ろ布を備えたろ過板の一次側に通水させて、該ろ布の一次側表面に混合液中の不溶性成分による層を形成させた状態でろ過処理を行うので、ろ布の一次側表面に形成させた不溶性成分による層がフィルターとして機能し、ろ過板の二次側から、焼却灰などの不溶性成分の混入が少ない、極めて清澄なリン抽出液を効率よく回収することができる。 According to the present invention, the mixed solution containing the phosphorus extract and the incinerated ash after the phosphorus extraction is passed through the primary side of the filter plate provided with the filter cloth, and the mixed solution is added to the primary surface of the filter cloth. Because the filtration process is performed in a state where a layer of insoluble components is formed, the layer of insoluble components formed on the primary side surface of the filter cloth functions as a filter, and insoluble ash and other insolubles from the secondary side of the filter plate. An extremely clear phosphorus extract containing little components can be efficiently recovered.
本発明のリン抽出液の回収方法は、リンを含有する汚泥の焼却灰に強酸性溶液又は強アルカリ性溶液を加えてリンを溶解させるリン溶解工程と、リンが溶解した溶液と不溶性成分との混合液から不溶性成分を除去してリン抽出液を回収する固液分離工程と、を含む工程からなる。まず、図面を用いて、本発明のリン抽出液の回収方法の固液分離工程で用いるリン抽出液の回収装置について説明する。 The method for recovering the phosphorus extract of the present invention includes a phosphorus dissolution step in which a strong acidic solution or a strong alkaline solution is added to the incinerated ash of sludge containing phosphorus to dissolve phosphorus, and a mixture of a solution in which phosphorus is dissolved and an insoluble component And a solid-liquid separation step of recovering the phosphorus extract by removing insoluble components from the solution. First, a phosphorus extract recovery apparatus used in the solid-liquid separation step of the phosphorus extract recovery method of the present invention will be described with reference to the drawings.
図１は、本発明のリン抽出液の回収方法の固液分離工程で用いるリン抽出液の回収装置の第１の実施形態である。 FIG. 1 is a first embodiment of a phosphorus extract recovery device used in the solid-liquid separation step of the phosphorus extract recovery method of the present invention.
図中の１は、固液分離槽であり、その下方側は汚泥堆積部をなしている。固液分離槽１の上側部には、混合液供給管Ｌ１が設けられている。固液分離槽１の底部には、汚泥給排口（図示しない）が設けられており、この汚泥給排口から、汚泥排出弁Ｖ１が介装された汚泥引き抜き管Ｌ２が伸びている。固液分離槽１の内部には、ろ過板１０が（この実施形態では３個）配置されている。 1 in the figure is a solid-liquid separation tank, and the lower side thereof forms a sludge accumulation part. A mixed liquid supply pipe L <b> 1 is provided on the upper part of the solid-liquid separation tank 1. A sludge supply / exhaust port (not shown) is provided at the bottom of the solid-liquid separation tank 1, and a sludge extraction pipe L2 in which a sludge discharge valve V1 is interposed extends from the sludge supply / discharge port. Inside the solid-liquid separation tank 1, filter plates 10 (three in this embodiment) are arranged.
図２を併せて参照すると、ろ過板１０は、支持材１１の両面をろ布１２で囲み、該ろ布１２の全周を閉じて袋状の形状をなしている。そして、上下方向に沿って、かつ、幅方向に所定間隔で縫い込んだ複数の縫い目１３によって、上下に伸びる通路を幅方向に複数並んで形成した構造をなしている。また、上端には、リン抽出液回収管Ｌ３が伸びて、配管Ｌ４に接続している。 Referring also to FIG. 2, the filter plate 10 has a bag-like shape by surrounding both sides of the support material 11 with a filter cloth 12 and closing the entire periphery of the filter cloth 12. A plurality of stitches 13 sewn along the vertical direction and at a predetermined interval in the width direction form a structure in which a plurality of paths extending in the vertical direction are formed side by side in the width direction. In addition, at the upper end, a phosphorus extract recovery pipe L3 extends and is connected to the pipe L4.
ろ布１２の材質は、耐薬品性に優れたものであれば特に限定はなく、ポリプロピレン、塩化ビニリデン、ビニロン等が好ましく用いられる。また、ろ布１２の厚さは、０．３〜０．５ｍｍが好ましい。また、ろ布１２の通気速度は、１０〜２０ｍｌ／ｃｍ２／ｓｅｃ ａｔ １２５Ｐａが好ましい。 The material of the filter cloth 12 is not particularly limited as long as it is excellent in chemical resistance, and polypropylene, vinylidene chloride, vinylon and the like are preferably used. The thickness of the filter cloth 12 is preferably 0.3 to 0.5 mm. Further, the ventilation rate of the filter cloth 12 is preferably 10 to 20 ml / cm 2 / sec at 125 Pa.
配管Ｌ４は、それぞれのろ過板１０から伸びたリン抽出液回収管Ｌ３が接続している。そして、その下流側端部は、上下に分岐しており、上方に伸びた配管Ｌ５には、通気弁Ｖ２、吸引ポンプＰ１が介装されている。下方に伸びた配管Ｌ６には、排水弁Ｖ３が介装されおり、この配管Ｌ６は、固液分離槽１内の水位よりも下方に伸びている。 The pipe L4 is connected to a phosphorus extract recovery pipe L3 extending from each filter plate 10. And the downstream end is branched up and down, and a vent valve V2 and a suction pump P1 are interposed in the pipe L5 extending upward. A drain valve V3 is interposed in the pipe L6 extending downward, and this pipe L6 extends downward from the water level in the solid-liquid separation tank 1.
次に、上記リン抽出液の回収装置を用いた、本発明のリン抽出液の回収方法を説明する。 Next, the method for recovering the phosphorus extract of the present invention using the phosphorus extract recovery apparatus will be described.
（リン溶解工程）
リンを含有する汚泥の焼却灰に、強酸性溶液又は強アルカリ性溶液を加えてリンを溶解させる。
(Phosphorus dissolution process)
A strong acidic solution or a strong alkaline solution is added to the incineration ash of sludge containing phosphorus to dissolve phosphorus.
強酸性溶液としては、硫酸、塩酸、硝酸、リン酸等が挙げられる。強アルカリ性溶液としては、水酸化ナトリウム、水酸化カリウム等が挙げられる。 Examples of the strongly acidic solution include sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid and the like. Examples of the strong alkaline solution include sodium hydroxide and potassium hydroxide.
強酸性溶液を用いてリンを溶解させる場合においては、焼却灰に強酸性溶液を加えて、ｐＨ２以下にして処理することが好ましい。また、５０〜７５℃の温度条件下で処理すると、焼却灰からのリン溶出に要する時間を短縮できるので好ましい。 When phosphorus is dissolved using a strong acid solution, it is preferable to add a strong acid solution to the incinerated ash so that the pH is 2 or lower. Moreover, it is preferable to process under a temperature condition of 50 to 75 ° C. because the time required for phosphorus elution from the incinerated ash can be shortened.
強アルカリ性溶液を用いてリンを溶解させる場合においては、焼却灰に強アルカリ性溶液を加えて、ｐＨ１４程度にして処理することが好ましい。５０〜７５℃の温度条件下で処理すると、焼却灰からのリン溶出に要する時間を短縮できるので好ましい。 In the case where phosphorus is dissolved using a strong alkaline solution, it is preferable to add a strong alkaline solution to the incinerated ash so as to have a pH of about 14. It is preferable to perform the treatment under a temperature condition of 50 to 75 ° C. because the time required for phosphorus elution from the incinerated ash can be shortened.
（固液分離工程）
次に、リンが溶解した溶液と不溶性成分との混合液（以下、「混合液」と記す）を、図１に示すリン抽出液回収装置を用いて固液分離し、混合液から不溶性成分を除去してリン抽出液を回収する。
(Solid-liquid separation process)
Next, the mixed solution of the solution in which phosphorus is dissolved and the insoluble component (hereinafter referred to as “mixed solution”) is subjected to solid-liquid separation using the phosphorus extract recovery device shown in FIG. Remove and recover the phosphorus extract.
混合液は、混合液供給管Ｌ１から固液分離槽１内に供給し、ろ過板１０の上方に至るまで供給する。混合液の供給が完了した後、排水弁Ｖ３を閉じた状態で、通気弁Ｖ２を開いて吸引ポンプＰ１を作動させ、ろ液（リン抽出液）を配管Ｌ４，Ｌ６内に充満させる。このようにすると、ろ過板１０のろ布の一次側表面には、混合液中の不溶性成分による層（以下、「プレコート層」と記す）１４が形成される。プレコート層１４の厚さは、運転条件により異なるので特に限定はしないが、十〜数十ｍｍの厚さになるように形成することが好ましい。 The mixed liquid is supplied from the mixed liquid supply pipe L1 into the solid-liquid separation tank 1 and is supplied up to the upper side of the filter plate 10. After the supply of the mixed liquid is completed, with the drain valve V3 closed, the aeration valve V2 is opened to operate the suction pump P1, and the filtrate (phosphorus extract) is filled in the pipes L4 and L6. In this way, a layer (hereinafter referred to as “precoat layer”) 14 of insoluble components in the mixed solution is formed on the primary side surface of the filter cloth of the filter plate 10. The thickness of the precoat layer 14 is not particularly limited because it varies depending on operating conditions, but it is preferably formed so as to have a thickness of 10 to several tens of mm.
そして、配管Ｌ４，Ｌ６内にリン抽出液を充満し、ろ布１２の一次側表面にプレコート層１４を形成したのち、吸引ポンプＰ１を停止して、通気弁Ｖ２を閉じ排水弁Ｖ３を開く。このようにすると、サイフォン効果により、配管Ｌ６の長さに応じた負圧がろ過板１０の内部に作用し、無動力でろ過が行われ、リン抽出液は、配管Ｌ６を通って系外に排水される。 The pipes L4 and L6 are filled with the phosphorus extract and the precoat layer 14 is formed on the primary surface of the filter cloth 12. Then, the suction pump P1 is stopped, the vent valve V2 is closed, and the drain valve V3 is opened. In this way, due to the siphon effect, a negative pressure corresponding to the length of the pipe L6 acts on the inside of the filter plate 10, filtration is performed without power, and the phosphorus extract passes outside the system through the pipe L6. Drained.
ろ布１２の一次側表面には、プレコート層１４が形成されているので、プレコート層１４がフィルターとして機能し、配管Ｌ６からは、極めて清澄なリン抽出液が得られる。そして、ろ過により固液分離槽１内の水位が一定レベルまで低下すると、混合液供給管Ｌ１から混合液が供給されて、ろ過が連続的に行われる。 Since the precoat layer 14 is formed on the primary surface of the filter cloth 12, the precoat layer 14 functions as a filter, and an extremely clear phosphorus extract is obtained from the pipe L6. And if the water level in the solid-liquid separation tank 1 falls to a fixed level by filtration, a liquid mixture will be supplied from the liquid mixture supply pipe L1, and filtration will be performed continuously.
ろ過処理を継続すると、混合液中の不溶性成分は、ろ過処理中に一部が重力沈降して汚泥堆積部に堆積する。また、プレコート層１４の表面にろ過処理中に不溶性成分が付着して厚みが増し、その一部が剥離して汚泥堆積部に沈降する。そこで、定期的に汚泥排出弁Ｖ１を開き、堆積した汚泥を汚泥引き抜き管Ｌ２から系外に排出する操作を行う。 When the filtration process is continued, a part of the insoluble component in the mixed solution is gravity settled during the filtration process and is deposited in the sludge accumulation part. Further, insoluble components adhere to the surface of the precoat layer 14 during the filtration process, and the thickness increases. A part of the insoluble component peels and settles on the sludge accumulation portion. Therefore, the sludge discharge valve V1 is periodically opened, and the accumulated sludge is discharged from the system through the sludge extraction pipe L2.
なお、焼却灰は、有機物を含まない無機性の粒子からなるものであるので、ろ布１２は目詰まりが生じにくく、ろ過処理中にろ布に付着した不溶性成分は、自重で自然剥離する。剥離した部分には、再度不溶性成分が付着するのでプレコート層が形成される。このため、ろ布１２の洗浄は、装置運転を停止時などのみ行えばよいので、少ない動力で、清澄なリン抽出液を効率よく回収することができる。ろ布１２の洗浄は、例えば、配管Ｌ５から加圧空気や水を供給してろ布の内部に付着した不溶性成分を除去する方法などが挙げられる。 Incinerated ash is made of inorganic particles that do not contain organic matter, and therefore the filter cloth 12 is less likely to be clogged, and insoluble components adhering to the filter cloth during the filtration process naturally peel off due to their own weight. Since the insoluble component adheres again to the peeled portion, a precoat layer is formed. For this reason, the filter cloth 12 can be washed only when the operation of the apparatus is stopped, so that a clear phosphorus extract can be efficiently recovered with a small amount of power. Examples of the cleaning of the filter cloth 12 include a method in which pressurized air or water is supplied from the pipe L5 to remove insoluble components attached to the inside of the filter cloth.
図３に、本発明のリン抽出液の回収方法の固液分離工程で用いるリン抽出液の回収装置の第２の実施形態を示す。 FIG. 3 shows a second embodiment of the phosphorus extract recovery device used in the solid-liquid separation step of the phosphorus extract recovery method of the present invention.
上記第１の実施形態のリン抽出液の回収装置と同一箇所については、同一符号を付してその説明を省略する。 The same parts as those of the phosphorus extract recovery apparatus of the first embodiment are denoted by the same reference numerals, and the description thereof is omitted.
この実施形態では、固液分離槽１内に攪拌装置５が配置されている点で、上記第１の実施形態と相違する。攪拌装置５は、混合液のろ過処理や、汚泥引き抜き管Ｌ２からの汚泥の引き抜きに支障をもたらさないようなものであれは特に限定はなく、例えば、曝気式攪拌装置などが好ましく挙げられる。 This embodiment is different from the first embodiment in that a stirring device 5 is arranged in the solid-liquid separation tank 1. The stirring device 5 is not particularly limited as long as it does not interfere with the filtration treatment of the mixed liquid and the extraction of the sludge from the sludge extraction pipe L2, and an aeration type stirring device, for example, is preferable.
次に、図３に示すリン抽出液の回収装置を用いて混合液を固液分離する方法について説明する。 Next, a method for solid-liquid separation of the mixed solution using the phosphorus extract recovery device shown in FIG. 3 will be described.
混合液を、混合液供給管Ｌ１から固液分離槽１内に供給し、ろ過板の上方に至るまで供給する。この実施形態では、混合液を固液分離槽１内に供給する際、攪拌装置５を作動して、固液分離槽１内の混合液を攪拌する点で上記第１の実施形態と相違する。 The mixed solution is supplied from the mixed solution supply pipe L1 into the solid-liquid separation tank 1 and supplied to the upper side of the filter plate. This embodiment is different from the first embodiment in that when the mixed liquid is supplied into the solid-liquid separation tank 1, the stirring device 5 is operated to stir the mixed liquid in the solid-liquid separation tank 1. .
そして、混合液の供給が完了した後、排水弁Ｖ３を閉じ、通気弁Ｖ２を開いて吸引ポンプＰ１を作動させ、ろ液（リン抽出液）を配管Ｌ４，Ｌ６内に充満させると共に、ろ過板１０のろ布の一次側表面にプレコート層１４を形成させる。 Then, after the supply of the mixed liquid is completed, the drain valve V3 is closed, the vent valve V2 is opened, the suction pump P1 is operated, the filtrate (phosphorus extract) is filled in the pipes L4 and L6, and the filter plate The precoat layer 14 is formed on the primary side surface of ten filter cloths.
配管Ｌ４，Ｌ６内にリン抽出液を充満し、ろ布１２の一次側表面にプレコート層１４を形成したのち、攪拌装置５及び吸引ポンプＰ１を停止し、通気弁Ｖ２を閉じ、排水弁Ｖ３を開き、ろ過処理を行う。 After the pipes L4 and L6 are filled with the phosphorus extract and the precoat layer 14 is formed on the primary surface of the filter cloth 12, the agitator 5 and the suction pump P1 are stopped, the vent valve V2 is closed, and the drain valve V3 is Open and filter.
混合液中の不溶性成分は沈降し易いので、混合液の不溶性成分の濃度が低い場合、ろ布の一次側表面に溶液中の不溶性成分によるプレコート層１４を形成する際に時間を要することがあるが、この実施形態では、ろ過処理を開始する前に混合液を攪拌するので、不溶性成分の沈降を防止でき、ろ布の一次側表面にプレコート層１４を短時間で形成でき、ろ過処理開始までに要する時間を短縮でき、リン抽出液の回収効率が向上する。 Since insoluble components in the mixed solution easily settle, when the concentration of the insoluble components in the mixed solution is low, it may take time to form the precoat layer 14 with the insoluble components in the solution on the primary surface of the filter cloth. However, in this embodiment, since the mixed solution is stirred before the filtration process is started, it is possible to prevent sedimentation of insoluble components, the precoat layer 14 can be formed on the primary surface of the filter cloth in a short time, and the filtration process is started. Can be shortened, and the recovery efficiency of the phosphorus extract is improved.
図４に、本発明のリン抽出液の回収方法の固液分離工程で用いるリン抽出液の回収装置の第３の実施形態を示す。 FIG. 4 shows a third embodiment of the phosphorus extract recovery apparatus used in the solid-liquid separation step of the phosphorus extract recovery method of the present invention.
上記第１の実施形態のリン抽出液の回収装置と同一箇所については、同一符号を付してその説明を省略する。 The same parts as those of the phosphorus extract recovery apparatus of the first embodiment are denoted by the same reference numerals, and the description thereof is omitted.
この実施形態では、配管Ｌ４の下流側端部が分岐しているが、配管Ｌ４から分岐して伸びた配管Ｌ７，Ｌ８が、固液分離槽１内の混合液の水位よりも上方に配置されている点で相違する。そして、配管Ｌ７には、通気弁Ｖ２が介装されている。また、配管Ｌ８には、排水弁Ｖ３及び吸引ポンプＰ２が介装されている。 In this embodiment, the downstream end of the pipe L4 is branched, but the pipes L7 and L8 branched and extended from the pipe L4 are disposed above the water level of the mixed liquid in the solid-liquid separation tank 1. Is different. A ventilation valve V2 is interposed in the pipe L7. Further, a drain valve V3 and a suction pump P2 are interposed in the pipe L8.
次に、図４に示すリン抽出液の回収装置を用いて混合液を固液分離する方法について説明する。 Next, a method for solid-liquid separation of the mixed solution using the phosphorus extractor recovery device shown in FIG. 4 will be described.
混合液を、混合液供給管Ｌ１から固液分離槽１内に供給し、ろ過板１０の上方に至るまで供給する。そして、混合液の供給が完了した後、通気弁Ｖ２を閉じ、排水弁Ｖ３を開き、吸引ポンプＰ２を作動してろ過処理を行う。 The mixed solution is supplied from the mixed solution supply pipe L <b> 1 into the solid-liquid separation tank 1 and is supplied up to the upper side of the filter plate 10. Then, after the supply of the mixed liquid is completed, the ventilation valve V2 is closed, the drain valve V3 is opened, and the suction pump P2 is operated to perform the filtration process.
この実施形態では、吸引ポンプＰ２からの吸引によりろ過板１０の内部を負圧にしてろ過処理するので、配管などの設備を簡略化でき、装置全体の小型化がはかれる。なお、プレコート層１４は、ろ過処理開始初期の段階で、混合液中の不溶性成分がろ布１２の一次側表面に付着して形成される。 In this embodiment, since the inside of the filter plate 10 is filtered by suction from the suction pump P2, the equipment such as piping can be simplified, and the entire apparatus can be downsized. The precoat layer 14 is formed by insoluble components in the mixed solution adhering to the primary surface of the filter cloth 12 at the initial stage of the filtration process.
図５に、本発明のリン抽出液の回収方法の固液分離工程で用いるリン抽出液の回収装置の第４の実施形態を示す。 FIG. 5 shows a fourth embodiment of the phosphorus extract recovery apparatus used in the solid-liquid separation step of the phosphorus extract recovery method of the present invention.
この実施形態では、配管Ｌ４の下流側端部から上方に伸びた配管Ｌ５に、通気弁Ｖ２が介装され、配管Ｌ４の下流側端部から下方に伸びた配管Ｌ６に、排水弁Ｖ３及び吸引ポンプＰ２が介装されている点で、上記第１の実施形態と相違する。 In this embodiment, a vent valve V2 is interposed in the pipe L5 extending upward from the downstream end of the pipe L4, and the drain valve V3 and the suction are connected to the pipe L6 extending downward from the downstream end of the pipe L4. The difference from the first embodiment is that a pump P2 is interposed.
次に、図５に示すリン抽出液の回収装置を用いて混合液を固液分離する方法について説明する。 Next, a method for solid-liquid separation of the mixed solution using the phosphorus extractor recovery device shown in FIG. 5 will be described.
混合液を、混合液供給管Ｌ１から固液分離槽１内に供給し、ろ過板１０の上方に至るまで供給する。そして、混合液の供給が完了した後、通気弁Ｖ２を閉じ、排水弁Ｖ３を開き、吸引ポンプＰ２を作動させる。 The mixed solution is supplied from the mixed solution supply pipe L <b> 1 into the solid-liquid separation tank 1 and is supplied up to the upper side of the filter plate 10. Then, after the supply of the mixed liquid is completed, the vent valve V2 is closed, the drain valve V3 is opened, and the suction pump P2 is operated.
この実施形態では、サイフォンで得られる負圧と、吸引ポンプＰ２で得られる負圧とで、ろ過処理を行うことができるので、混合液のろ過速度が向上し、短時間で多量にリン抽出液を回収することができる。なお、プレコート層１４は、ろ過処理開始初期の段階で、混合液中の不溶性成分がろ布１２の一次側表面に付着して形成される。 In this embodiment, since the filtration process can be performed by the negative pressure obtained by the siphon and the negative pressure obtained by the suction pump P2, the filtration speed of the mixed solution is improved, and a large amount of phosphorus extract is obtained in a short time. Can be recovered. The precoat layer 14 is formed by insoluble components in the mixed solution adhering to the primary surface of the filter cloth 12 at the initial stage of the filtration process.
下水汚泥の焼却灰に苛性ソーダを加えて、焼却灰濃度が約８００００ｍｇ／Ｌの混合液を調製し、ｐＨ１４、５０〜６０℃の条件で焼却灰からリン溶解を行った。そして、この混合液を、図１に示すリン抽出液の回収装置を用いて固液分離して、リン抽出液を回収した。ろ過処理は、ろ布１２の一次側に焼却灰による厚さ２０ｍｍの層を形成した状態で、２ｍ３／ｍ２ｈｒのろ過速度でろ過処理を行ったところ、配管Ｌ６から回収できたリン抽出液の焼却灰濃度は１０ｍｇ／Ｌ以下であった。 Caustic soda was added to the incineration ash of sewage sludge to prepare a mixed solution having an incineration ash concentration of about 80,000 mg / L, and phosphorus was dissolved from the incineration ash under the conditions of pH 14, 50-60 ° C. And this liquid mixture was solid-liquid separated using the collection | recovery apparatus of the phosphorus extract shown in FIG. 1, and the phosphorus extract was collect | recovered. The filtration process was carried out at a filtration rate of 2 m 3 / m 2 hr with a 20 mm thick layer of incinerated ash formed on the primary side of the filter cloth 12, and the phosphorus extracted from the pipe L6 was recovered. The incinerated ash concentration of the liquid was 10 mg / L or less.
１：固液分離槽
２：汚泥堆積部
５：攪拌装置
１０：ろ過板
１１：支持材
１２：ろ布
１３：縫い目
１４：プレコート層
Ｌ１〜Ｌ８：配管
Ｐ１，Ｐ２：吸引ポンプ
Ｖ１：汚泥排出弁
Ｖ２：通気弁
Ｖ３：排水弁
1: Solid-liquid separation tank 2: Sludge accumulation unit 5: Stirrer 10: Filter plate 11: Support material 12: Filter cloth 13: Seam 14: Precoat layers L1 to L8: Piping P1, P2: Suction pump V1: Sludge discharge valve V2: Ventilation valve V3: Drain valve
Claims (4)
前記固液分離工程は、吸引ポンプを作動させて前記混合液をろ布を備えたろ過板の一次側に通水させ、該ろ布の一次側表面に前記混合液中の不溶性成分による層を形成させたのち、前記吸引ポンプを停止し、サイフォン効果によりろ過処理を行い、前記ろ過板の二次側からリン抽出液を回収する、
ことを特徴とするリン抽出液の回収方法。 Phosphorus extraction by removing a insoluble component from a phosphorus dissolution process in which phosphorus is dissolved by adding a strong acidic solution or a strong alkaline solution to the incinerated ash of sludge containing phosphorus, and a mixture of the solution in which the phosphorus is dissolved and the insoluble component A solid-liquid separation step of recovering the liquid, and a method of recovering the phosphorus extract,
In the solid-liquid separation step, a suction pump is operated to allow the mixed liquid to pass through a primary side of a filter plate provided with a filter cloth , and a layer of insoluble components in the mixed liquid is formed on the primary side surface of the filter cloth. After forming , stop the suction pump, perform a filtration process by the siphon effect , and recover the phosphorus extract from the secondary side of the filter plate,
A method for recovering a phosphorus extract characterized by the above.
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| KR102524961B1 (en) * | 2018-02-13 | 2023-04-24 | 강원대학교 산학협력단 | Phosphorus recovery method from coagulated disposal sludge |
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