JP6515593B2 - Method of treating metal-containing sludge - Google Patents
Method of treating metal-containing sludge Download PDFInfo
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- JP6515593B2 JP6515593B2 JP2015043285A JP2015043285A JP6515593B2 JP 6515593 B2 JP6515593 B2 JP 6515593B2 JP 2015043285 A JP2015043285 A JP 2015043285A JP 2015043285 A JP2015043285 A JP 2015043285A JP 6515593 B2 JP6515593 B2 JP 6515593B2
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- 239000010802 sludge Substances 0.000 title claims description 78
- 229910052751 metal Inorganic materials 0.000 title claims description 52
- 239000002184 metal Substances 0.000 title claims description 52
- 238000000034 method Methods 0.000 title claims description 25
- 229920006317 cationic polymer Polymers 0.000 claims description 36
- 229920006318 anionic polymer Polymers 0.000 claims description 17
- 150000003839 salts Chemical group 0.000 claims description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 229910052719 titanium Inorganic materials 0.000 claims description 16
- 239000010936 titanium Substances 0.000 claims description 16
- 239000000701 coagulant Substances 0.000 claims description 15
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 10
- 229910052791 calcium Inorganic materials 0.000 claims description 10
- 239000011575 calcium Substances 0.000 claims description 10
- -1 dialkylaminoalkyl methacrylate alkyl chloride Chemical class 0.000 claims description 10
- 229910052749 magnesium Inorganic materials 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 claims description 10
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 7
- 208000005156 Dehydration Diseases 0.000 claims description 4
- BHDFTVNXJDZMQK-UHFFFAOYSA-N chloromethane;2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical group ClC.CN(C)CCOC(=O)C(C)=C BHDFTVNXJDZMQK-UHFFFAOYSA-N 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 238000003672 processing method Methods 0.000 claims description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N acrylic acid methyl ester Natural products COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 24
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 12
- 239000000920 calcium hydroxide Substances 0.000 description 12
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 12
- 229920000642 polymer Polymers 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 10
- 239000000178 monomer Substances 0.000 description 10
- 239000000706 filtrate Substances 0.000 description 8
- 230000002776 aggregation Effects 0.000 description 7
- 238000004220 aggregation Methods 0.000 description 7
- 239000003513 alkali Substances 0.000 description 7
- 238000010979 pH adjustment Methods 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 7
- 125000000129 anionic group Chemical group 0.000 description 5
- 239000010865 sewage Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- WQHCGPGATAYRLN-UHFFFAOYSA-N chloromethane;2-(dimethylamino)ethyl prop-2-enoate Chemical group ClC.CN(C)CCOC(=O)C=C WQHCGPGATAYRLN-UHFFFAOYSA-N 0.000 description 4
- 244000144992 flock Species 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 1
- 125000005250 alkyl acrylate group Chemical group 0.000 description 1
- 125000001930 alkyl chloride group Chemical group 0.000 description 1
- 150000001805 chlorine compounds Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 125000004663 dialkyl amino group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 229940088644 n,n-dimethylacrylamide Drugs 0.000 description 1
- YLGYACDQVQQZSW-UHFFFAOYSA-N n,n-dimethylprop-2-enamide Chemical compound CN(C)C(=O)C=C YLGYACDQVQQZSW-UHFFFAOYSA-N 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000004056 waste incineration Methods 0.000 description 1
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Treatment Of Sludge (AREA)
Description
本発明は金属含有汚泥の処理方法に関し、特に、チタン、マグネシウム及びカルシウムを含む金属含有汚泥にアルカリを添加し、ついで高分子凝集剤を添加する金属含有汚泥の処理方法に関する。 The present invention relates to a method for treating metal-containing sludge, and more particularly to a method for treating metal-containing sludge in which an alkali is added to a metal-containing sludge containing titanium, magnesium and calcium and then a polymer flocculant is added.
金属含有汚泥は、鉱山廃水、化学工場廃水、製錬所廃水、製鉄所廃水、メッキ工場廃水、塗料系廃水、ゴミ焼却場廃水等の処理過程より生じる。 Metal-containing sludge is produced from the treatment process of mine wastewater, chemical factory wastewater, smelter wastewater, steel mill wastewater, plating factory wastewater, paint wastewater, waste incineration wastewater and the like.
従来、重金属を含め、金属を含有する汚泥や水の処理方法としては、カチオン系高分子凝集剤を添加し、続いてアニオン系又はノニオン系の高分子凝集剤を添加する方法（特許文献１）、アルカリ凝集沈殿を行った後に、高分子凝集剤で処理を行う方法（特許文献２、３）が提案されている。 Conventionally, as a method of treating sludge or water containing metal, including heavy metals, a method of adding a cationic polymer flocculant and subsequently adding an anionic or nonionic polymer flocculant (Patent Document 1) The method (patent document 2, 3) which processes with a polymer coagulant | flocculant is proposed, after performing alkaline aggregation precipitation.
しかしながら、前記特許文献１〜３の方法は、いずれもフロック形成後、機械脱水に耐え得る十分に強固なフロックを形成させることができなかった。そのため、単位時間当たりの汚泥の処理量を大きくすることができず、脱水後のケーキ含水率も十分に低下させることができないという問題があった。 However, any of the methods of Patent Documents 1 to 3 described above can not form a sufficiently strong floc that can withstand mechanical dewatering after floc formation. Therefore, the amount of sludge treated per unit time can not be increased, and there is a problem that the moisture content of the cake after dehydration can not be sufficiently reduced.
本発明の目的は、金属含有汚泥の脱水処理において、凝集フロックの強度を高めて機械脱水に耐え得る十分に強固なフロックを形成させることで汚泥の脱水効率を向上し、ケーキ含水率の低下が達成できる金属含有汚泥の脱水方法を提供することにある。 The object of the present invention is to increase the strength of flocculated floc to form a sufficiently strong floc that can withstand mechanical dewatering in the dewatering treatment of metal-containing sludge, thereby improving the dewatering efficiency of the sludge and reducing the moisture content of the cake. It is an object of the present invention to provide a method for dewatering metal-containing sludge that can be achieved.
上記課題を解決するため鋭意検討した結果、金属含有汚泥、特にチタン、マグネシウム及びカルシウムを含む金属含有汚泥に、アルカリでｐＨ調整した後、特定の高分子凝集剤を添加することが有効であることを見出し、本発明を完成するに至った。 As a result of earnestly examining in order to solve the above problems, it is effective to add a specific polymer flocculant to the metal-containing sludge, particularly metal-containing sludge containing titanium, magnesium and calcium after pH adjustment with alkali The present invention has been completed.
すなわち、本発明は、金属含有汚泥をｐＨ１０〜１３となるよう調整した後、まず、ノニオン性構造単位を５〜１０質量％、ジアルキルアミノアルキルメタクリレート塩化アルキル4級塩構造単位を５〜２０質量％、ジアルキルアミノアルキルアクリレート塩化アルキル4級塩構造単位を７０〜９０質量％有するカチオン性高分子凝集剤を添加し、ついでアニオン性高分子凝集剤を添加して脱水処理を行う金属含有汚泥の処理方法に存する。 That is, according to the present invention, after adjusting the metal-containing sludge to have a pH of 10 to 13, first, 5 to 10% by mass of nonionic structural units and 5 to 20% by mass of dialkylaminoalkyl methacrylate alkyl chloride salt structural units A method for treating metal-containing sludge, comprising adding a cationic polymer flocculant having 70 to 90% by mass of a dialkylaminoalkyl acrylate alkyl chloride quaternary salt structural unit and then adding an anionic polymer flocculant To be.
また、本発明は、前記金属含有汚泥がチタンを含む金属含有汚泥である前記の金属含有汚泥の処理方法に存する。 The present invention also resides in the method for treating metal-containing sludge, wherein the metal-containing sludge is a metal-containing sludge containing titanium.
また、本発明は、前記金属含有汚泥中のチタン濃度が０．０１〜１質量％である前記の金属含有汚泥の処理方法に存する。 Moreover, this invention exists in the processing method of the said metal containing sludge whose titanium concentration in the said metal containing sludge is 0.01-1 mass%.
更に、本発明は、前記カチオン性高分子凝集剤中のノニオン性構造単位がアクリルアミド構造単位、ジアルキルアミノアルキルメタクリレート塩化アルキル4級塩構造単位がジメチルアミノエチルメタクリレート塩化メチル4級塩構造単位、ジアルキルアミノアルキルアクリレート塩化アルキル4級塩構造単位がジメチルアミノエチルアクリレート塩化メチル4級塩構造単位である前記の金属含有汚泥の処理方法に存する。 Furthermore, according to the present invention, the nonionic structural unit in the cationic polymer flocculant is an acrylamide structural unit, the alkylaminoalkyl methacrylate alkyl chloride quaternary salt structural unit is a dimethylaminoethyl methacrylate methyl chloride quaternary salt structural unit, a dialkylamino The present invention relates to the method for treating metal-containing sludge, wherein the alkyl acrylate quaternary alkyl chloride structural unit is a dimethylaminoethyl acrylate methyl chloride quaternary structural unit.
本発明の金属含有汚泥の処理方法によれば、金属含有汚泥の脱水処理において、凝集フロックの強度を高めて機械脱水に耐え得る十分に強固なフロックを形成させることで汚泥の脱水効率を向上し、ケーキ含水率の低下が達成できる金属含有汚泥の脱水方法を提供することができる。 According to the method for treating metal-containing sludge of the present invention, in the dewatering treatment of metal-containing sludge, the dewatering efficiency of the sludge is improved by increasing the strength of the flocculated floc to form a sufficiently strong floc that can withstand mechanical dewatering. It is possible to provide a method for dewatering metal-containing sludge which can achieve a reduction in the moisture content of the cake.
以下に本発明を詳細に説明する。
尚、以下「ｐｐｍ」は特に断りのない限り質量基準とする。本発明の金属含有汚泥の処理方法は、チタン、マグネシウム及びカルシウムを含む金属含有汚泥をｐＨ１０以上に調整することにより金属を水酸化物として析出させる。ここに、まず、カチオン性高分子凝集剤を添加して懸濁粒子を吸着してフロックを形成すると同時に汚泥全体を正に荷電させる。ついでアニオン性高分子凝集剤を添加することで、正に荷電した汚泥を荷電中和することにより凝集作用を高めてフロックの巨大化・高密度化を促進させることができるので、後工程の機械脱水に十分耐え得る強度を持ち合わせたフロックを形成することができる。そのため、汚泥の処理量の向上、かつ、ケーキの脱水効果の向上を期待することができる。
The present invention will be described in detail below.
In the following, "ppm" is based on mass unless otherwise noted. In the method of treating metal-containing sludge of the present invention, a metal is precipitated as a hydroxide by adjusting the metal-containing sludge containing titanium, magnesium and calcium to a pH of 10 or more. Here, first, a cationic polymer flocculant is added to adsorb suspended particles to form flocs and at the same time the entire sludge is positively charged. Next, by adding an anionic polymer flocculant, the flocculation action can be enhanced by positively neutralizing the positively charged sludge to promote flocculation and densification; It is possible to form a floc having strength sufficient to withstand dehydration. Therefore, the improvement of the amount of sludge treatment and the improvement of the dewatering effect of the cake can be expected.
前記金属含有汚泥のｐＨ調整は、汚泥にアルカリを添加して行うことができる。前記アルカリとしては、水酸化ナトリウム、水酸化カリウム等のアルカリ金属水酸化物、水酸化カルシウム、水酸化マグネシウムなどのアルカリ土類金属水酸化物などを挙げることができる。中でも汚泥中の金属の析出のし易さより、前記ｐＨ調整用のアルカリとしては、水酸化カルシウムが好ましい。 The pH adjustment of the metal-containing sludge can be performed by adding alkali to the sludge. Examples of the alkali include alkali metal hydroxides such as sodium hydroxide and potassium hydroxide, and alkaline earth metal hydroxides such as calcium hydroxide and magnesium hydroxide. Above all, calcium hydroxide is preferable as the alkali for pH adjustment from the ease of metal deposition in the sludge.
チタン、マグネシウム及びカルシウムを含む金属含有汚泥に水酸化カルシウムを添加して、ｐＨを調整し、金属水酸化物を析出させる。ｐＨ調整後のｐＨは１０以上が好ましく、１０．５以上がより好ましい。また、１３以下が好ましく、１２．０以下がより好ましい。ｐＨ１０未満では汚泥中の金属を十分に捕集できず、ｐＨ１３をこえると後工程で使用するカチオン性高分子凝集剤がエステル系化合物である場合にはエステル基が加水分解を引き起こしてしまい、十分な強度を持つフロックを形成することができなくなる。 Calcium hydroxide is added to metal-containing sludge containing titanium, magnesium and calcium to adjust pH and precipitate metal hydroxide. The pH after pH adjustment is preferably 10 or more, and more preferably 10.5 or more. Moreover, 13 or less is preferable and 12.0 or less is more preferable. If the pH is less than 10, the metal in the sludge can not be collected sufficiently, and if the pH exceeds 13, the ester group causes hydrolysis when the cationic polymer flocculant used in the subsequent step is an ester compound, which is sufficient. It is impossible to form flocks with high strength.
金属含有汚泥としては、チタンを０．０１〜１質量％含み、更にマグネシウム及びカルシウムが含まれていれば、その他の成分の種類や濃度については特に限定されないが、前記金属含有汚泥中の固形物（以下ＴＳと記す）の濃度は通常１．０％以上が好ましく、２．０％以上がより好ましい。また、６．０％以下が好ましく、５．０％以下がより好ましい。前記範囲内であれば、前記金属含有汚泥をｐＨ調整して析出した金属を凝集フロックに巻き込みながら凝集フロックを形成できるので、前記汚泥中の金属と固形物を効率的に除去することができる。 The metal-containing sludge contains 0.01 to 1% by mass of titanium, and further contains magnesium and calcium, and the types and concentrations of the other components are not particularly limited. In general, the concentration of (hereinafter referred to as TS) is preferably 1.0% or more, and more preferably 2.0% or more. Moreover, 6.0% or less is preferable and 5.0% or less is more preferable. If it is within the above-mentioned range, it is possible to form flocculated flocs while adjusting the pH of the metal-containing sludge and winding the deposited metal into flocculated flocs, so that the metals and solids in the sludge can be efficiently removed.
高分子凝集剤は水溶液にして汚泥と混合する。水溶液の濃度は、通常０．０１質量％以上が好ましく、０．０５質量％以上がより好ましい。また、２質量％以下が好ましく、０．５質量％以下がより好ましい。前記範囲内であれば、高分子凝集剤を効率よく前記汚泥に添加することができる。 The polymeric flocculant is in aqueous solution and mixed with the sludge. 0.01 mass% or more is preferable normally, and, as for the density | concentration of aqueous solution, 0.05 mass% or more is more preferable. Moreover, 2 mass% or less is preferable, and 0.5 mass% or less is more preferable. If it is in the said range, a polymer flocculant can be efficiently added to the said sludge.
前記高分子凝集剤の汚泥への添加量は、汚泥のＴＳに対し、通常０．０１質量％以上が好ましく、０．０５質量％以上がより好ましい。また、５質量％以下が好ましく、４質量％以下がより好ましい。前記範囲内であれば、析出した金属を凝集フロックに巻き込みながら凝集フロックを形成できるので、前記汚泥中の金属と固形物を効率的に除去することができる。 0.01 mass% or more is preferable normally with respect to TS of sludge, and, as for the addition amount to the sludge of the said polymer flocculent, 0.05 mass% or more is more preferable. Moreover, 5 mass% or less is preferable, and 4 mass% or less is more preferable. If it is in the said range, since it can form aggregation floc, winding up the deposited metal in aggregation floc, the metal and solid substance in the said sludge can be removed efficiently.
前記カチオン性高分子凝集剤のカチオン性モノマー構造単位としてはジメチルアミノエチルアクリレート塩化メチル４級塩構造単位及びジメチルアミノエチルメタクリレート塩化メチル４級塩構造単位であることが好ましい。 The cationic monomer structural unit of the cationic polymer flocculant is preferably a dimethylaminoethyl acrylate methyl chloride quaternary salt structural unit and a dimethylaminoethyl methacrylate methyl chloride quaternary chloride structural unit.
前記カチオン性高分子凝集剤の全モノマー構造単位に対するジメチルアミノエチルアクリレート塩化メチル４級塩構造単位の含有量は７０〜９０質量％、ジメチルアミノエチルメタクリレート塩化メチル４級塩構造単位の含有量は５〜２０質量％であることが好ましい。また、前記カチオン性高分子凝集剤のノニオン性モノマー構造単位としてはアクリルアミド構造単位であることが好ましい。前記カチオン性高分子凝集剤の全モノマー構造単位に対するアクリルアミド構造単位の含有量は５〜１０質量％であることが好ましい。 The content of the dimethylaminoethyl acrylate methyl chloride quaternary salt structural unit is 70 to 90% by mass, and the content of the dimethylaminoethyl methacrylate methyl chloride quaternary salt structural unit is 5 with respect to all the monomer structural units of the cationic polymer flocculant. It is preferable that it is -20 mass%. The nonionic monomer structural unit of the cationic polymer flocculant is preferably an acrylamide structural unit. It is preferable that content of the acrylamide structural unit with respect to all the monomer structural units of the said cationic polymer flocculent is 5-10 mass%.
前記アニオン性高分子凝集剤のノニオン性モノマー構造単位としてはメタクリルアミド構造単位、アクリルアミド構造単位、Ｎ，Ｎ−ジメチルアクリルアミド構造単位等を挙げることができる。凝集性能から、中でもアクリルアミド構造単位が好ましい。前期アニオン性高分子凝集剤のアニオン性モノマー構造単位としてはアクリル酸（塩）構造単位、２−アクリルアミド−２−メチルプロパン−１−スルホン酸（塩）構造単位等を挙げることができる。凝集性能から、中でもアクリル酸（塩）構造単位が好ましい。 As a nonionic monomer structural unit of the said anionic polymeric flocculent, a methacrylamide structural unit, an acrylamide structural unit, a N, N- dimethyl acrylamide structural unit etc. can be mentioned. Among them, acrylamide structural units are preferable in terms of aggregation performance. Examples of the anionic monomer structural unit of the anionic polymer flocculant include acrylic acid (salt) structural unit, 2-acrylamido-2-methylpropane-1-sulfonic acid (salt) structural unit, and the like. Among them, acrylic acid (salt) structural units are preferred in view of aggregation performance.
前記アニオン性高分子凝集剤の全モノマー構造単位に対するアクリル酸（塩）構造単位の含有量は特に限定されないが、２質量％以上が好ましく、１０質量％以上がより好ましく、３０質量％以上が更に好ましい。また、７０質量％以下が好ましく、６０質量％以下がより好ましく、４０質量％以下が更に好ましい。前記範囲内であれば、析出した金属を凝集フロックに巻き込みながら凝集フロックを形成できるので、前記汚泥中の金属と固形物を効率的に除去することができる。 The content of the acrylic acid (salt) structural unit relative to all monomer structural units of the anionic polymer flocculant is not particularly limited, but 2% by mass or more is preferable, 10% by mass or more is more preferable, and 30% by mass or more is more preferable. Moreover, 70 mass% or less is preferable, 60 mass% or less is more preferable, and 40 mass% or less is still more preferable. If it is in the said range, since it can form aggregation floc, winding up the deposited metal in aggregation floc, the metal and solid substance in the said sludge can be removed efficiently.
水酸化カルシウムなどのアルカリを用いてｐＨ１０〜１３となるように調整したチタン、マグネシウム及びカルシウムを含む金属含有汚泥に、まずカチオン性高分子凝集剤を添加し、ついでアニオン性高分子凝集剤を添加して脱水処理を行う際の全高分子凝集剤に対する各高分子凝集剤の添加割合は、カチオン性高分子凝集剤が５５質量％以上となることが好ましく、６０質量％以上となることがより好ましい。また、７０質量％以下となることが好ましく、６５質量％以下となることがより好ましい。カチオン性高分子凝集剤の添加割合が前記範囲内であれば、高分子凝集剤を添加・撹拌する際に、高分子凝集剤が未反応となって残ることが無いため、ケーキの脱水効率が向上する。 A cationic polymer flocculant is first added to a metal-containing sludge containing titanium, magnesium and calcium adjusted to pH 10 to 13 using an alkali such as calcium hydroxide, and then an anionic polymer flocculant is added The addition ratio of each polymer coagulant with respect to the total polymer coagulant at the time of dehydration treatment is preferably 55% by mass or more of the cationic polymer coagulant, and more preferably 60% by mass or more . Moreover, it is preferable that it becomes 70 mass% or less, and it is more preferable that it becomes 65 mass% or less. If the addition ratio of the cationic polymer flocculant falls within the above range, the polymer flocculant does not remain unreacted when added and stirred, so the dewatering efficiency of the cake is improves.
カチオン性高分子凝集剤とアニオン性高分子凝集剤を前記金属含有汚泥に添加する場合には、カチオン性高分子凝集剤を添加してからアニオン性高分子凝集剤を添加するまでの時間は特に限定されないが、通常、カチオン性高分子凝集剤を添加するとフロックが形成され、次いで、アニオン性高分子凝集剤を添加すると前記フロックが更に強固で大きいフロックとなる。 When a cationic polymer coagulant and an anionic polymer coagulant are added to the metal-containing sludge, the time from the addition of the cationic polymer coagulant to the addition of the anionic polymer coagulant is particularly Generally, but not limited to, the addition of a cationic polymeric flocculant results in the formation of floc, and the addition of an anionic polymeric flocculant results in a stronger and larger floc of said floc.
フロックを形成した後は、脱水機を用いてフロックを脱水し、脱水ケーキを得ることができる。脱水機の形式としては、例えば、フィルタープレス型脱水機、スクリュープレス型脱水機、圧入式スクリュープレス型脱水機、真空型脱水機、ベルトプレス型脱水機、遠心型脱水機、多重円板型脱水機などが挙げられる。中でも、汚泥の脱水効率が高いことから、フィルタープレス型脱水機、ベルトプレス型脱水機が好ましい。 After the floc is formed, the floc can be dewatered using a dehydrator to obtain a dewatered cake. As a form of a dehydrator, for example, filter press dehydrator, screw press dehydrator, press-in screw press dehydrator, vacuum dehydrator, belt press dehydrator, centrifugal dehydrator, multiple disc dewatering Machine etc. Among them, a filter press type dehydrator and a belt press type dehydrator are preferable because sludge dewatering efficiency is high.
以下、実施例及び比較例を示して本発明を詳細に説明するが、本発明はその要旨を超えない限り以下の記載によって限定されるものではない。なお、本実施例および比較例における「％」は特に断りのない限り「質量％」を示す。 Hereinafter, the present invention will be described in detail by showing Examples and Comparative Examples, but the present invention is not limited by the following description as long as the gist thereof is not exceeded. In addition, "%" in a present Example and a comparative example shows "mass%" unless there is particular notice.
実施例及び比較例に使用した高分子凝集剤を表１に示す。表中の数値は、各高分子凝集剤中のカチオン性モノマー構造単位、アニオン性モノマー構造単位、ノニオン性モノマー構造単位の含有率を質量％で示したものである。 The polymer flocculants used in Examples and Comparative Examples are shown in Table 1. The numerical values in the table indicate the content of the cationic monomer structural unit, the anionic monomer structural unit, and the nonionic monomer structural unit in each polymer coagulant in mass%.
ＡＡｍ：アクリルアミド
ＤＭＥ：ジメチルアミノエチルアクリレート塩化メチル４級塩
ＤＭＣ：ジメチルアミノエチルメタアクリレート塩化メチル４級塩
ＡＡ：アクリル酸（塩）
AAm: Acrylamide DME: Dimethylaminoethyl acrylate methyl chloride quaternary salt DMC: Dimethylaminoethyl methacrylate Acrylate methyl chloride quaternary salt AA: Acrylic acid (salt)
（実施例１）
チタン、マグネシウム及びカルシウムを含む塗料系金属含有汚泥に水酸化カルシウムを添加してｐＨ１０．７に調整した。ｐＨ調整後の汚泥のＴＳは、財団法人日本下水道協会編「下水試験方法上巻１９９７年度版」ｐ１１６に従い測定したところ、３．７８％であった。また、ｐＨ調整後の汚泥のチタン含有量はＪＩＳ Ｈ １６３２−１：２０１４に記載のＩＣＰ発光分光分析法で測定したところ０．０３質量％であった。前記汚泥３００ｍＬを５００ｍＬビーカーに取り、カチオン性高分子凝集剤Ａ（水溶液濃度０．３質量％）を１５ｍＬ（汚泥への添加率１５０ｐｐｍ）添加し、スパチュラを用いて２００ｒｐｍで３０秒撹拌した。ついでアニオン性高分子凝集剤Ｅ（水溶液濃度０．１質量％）を３０ｍＬ（汚泥への添加率１００ｐｐｍ）添加し、スパチュラを用いて２００ｒｐｍで３０秒撹拌してフロックを形成した。目視により平均フロック径を測定することでフロック径とした。５０メッシュのナイロン製の濾布でフロックが形成した汚泥を濾過し、濾液の濁度を目視で評価した。濾液の濁度は以下の基準で判断した。
Example 1
Calcium hydroxide was added to the paint-based metal-containing sludge containing titanium, magnesium and calcium to adjust to pH 10.7. The pH-adjusted sludge TS was 3.78% as measured according to Japan Sewage Association, Japan, Sewage Test Method Upper Volume 1997 edition, p 116, edited by the Japan Sewage Association. Moreover, when titanium content of the sludge after pH adjustment was measured by the ICP emission-spectroscopic-analysis method of JIS H1632-1: 2014, it was 0.03 mass%. 300 mL of the sludge was taken in a 500 mL beaker, 15 mL (addition rate to sludge: 150 ppm) of a cationic polymer flocculant A (aqueous solution concentration 0.3 mass%) was added, and stirred for 30 seconds at 200 rpm using a spatula. Then, 30 mL (addition rate to sludge: 100 ppm) of an anionic polymer flocculant E (aqueous solution concentration: 0.1 mass%) was added, and the mixture was stirred at 200 rpm for 30 seconds using a spatula to form a floc. The average floc diameter was measured visually to obtain a floc diameter. The sludge formed with flocs was filtered with a 50 mesh nylon filter cloth, and the turbidity of the filtrate was visually evaluated. The turbidity of the filtrate was judged based on the following criteria.
−：濾液がほとんど透き通っており、浮遊物はほぼ見られない（ＳＳ量目安：５０ｐｐｍ未満）
＋：濾液に一部濁りが見られ、浮遊物がわずかに存在する（ＳＳ量目安：５０ｐｐｍ以上１００ｐｐｍ未満）
＋＋：濾液に一部濁りが見られ、浮遊物がところどころ存在する。（ＳＳ量目安：１００ｐｐｍ以上２００ｐｐｍ未満）
＋＋＋：濾液に多数の濁りが見られ、浮遊物が全体的に存在する。（ＳＳ量目安：２００ｐｐｍ以上５００ｐｐｍ未満）
＋＋＋＋：濾液全体に多数の濁りが見られ、浮遊物が全体的に存在し、一部粗大な大きさで存在する。（ＳＳ量目安：５００ｐｐｍ以上１０００ｐｐｍ未満）
−: The filtrate is almost clear and almost no suspended matter can be seen (SS amount standard: less than 50 ppm)
+: Partial turbidity is observed in the filtrate, and a slight amount of suspended matter (SS amount standard: 50 ppm or more and less than 100 ppm)
++: A part of turbidity is observed in the filtrate, and suspended matter is present in some places. (SS amount standard: 100 ppm or more and less than 200 ppm)
+ ++: A large amount of turbidity is observed in the filtrate, and suspended matter is totally present. (SS amount standard: 200 ppm or more and less than 500 ppm)
++ ++: A large amount of turbidity is observed throughout the filtrate, and the suspended matter is totally present, and partially present in coarse size. (SS amount standard: 500 ppm or more and less than 1000 ppm)
濾過後、濾布上に残ったフロックを０．１ＭＰａの圧力で１分間プレス脱水して脱水ケーキを得、脱水ケーキの含水率を測定した。含水率の測定は、財団法人日本下水道協会編「下水試験方法上巻１９９７年度版」ｐ２９６〜２９７に従い測定した。 After filtration, the floc remaining on the filter cloth was pressed and dewatered at a pressure of 0.1 MPa for 1 minute to obtain a dewatered cake, and the moisture content of the dewatered cake was measured. The moisture content was measured in accordance with the Japan Sewage Association of Japan, "Sewage test method upper volume 1997 edition" p.
（実施例２）
水酸化カルシウムの添加によるｐＨ調整をｐＨ１２．３にした以外は実施例１と同様にして処理を行った。
(Example 2)
The treatment was performed in the same manner as in Example 1 except that the pH was adjusted to 12.3 by the addition of calcium hydroxide.
（実施例３）
アニオン性高分子凝集剤Ｅの添加量を４５ｍＬ（汚泥への添加率１５０ｐｐｍ）とした以外は実施例１と同様にして処理を行った。
(Example 3)
The treatment was performed in the same manner as in Example 1 except that the addition amount of the anionic polymer coagulant E was 45 mL (addition rate to sludge: 150 ppm).
（比較例１）
水酸化カルシウムの添加によるｐＨ調整をｐＨ９．１にした以外は実施例１と同様にして処理を行った。
(Comparative example 1)
The treatment was performed in the same manner as in Example 1 except that the pH was adjusted to 9.1 by the addition of calcium hydroxide.
（比較例２）
水酸化カルシウムの添加によるｐＨ調整をｐＨ１４．０とした以外は実施例１と同様にして処理を行った。
(Comparative example 2)
The treatment was performed in the same manner as in Example 1 except that the pH was adjusted by adding calcium hydroxide to pH 14.0.
（比較例３）
カチオン性高分子凝集剤Ａをカチオン性高分子凝集剤Ｂにした以外は実施例１と同様にして処理を行った。
(Comparative example 3)
The treatment was performed in the same manner as in Example 1 except that the cationic polymer coagulant A was changed to the cationic polymer coagulant B.
（比較例４）
カチオン性高分子凝集剤Ａを２５ｍＬ（汚泥への添加率２５０ｐｐｍ）添加し、アニオン性高分子凝集剤Ｅを添加しない以外は実施例１と同様にして処理を行った。
(Comparative example 4)
The treatment was performed in the same manner as in Example 1 except that 25 mL of the cationic polymer flocculant A (addition rate to sludge: 250 ppm) was added, and the anionic polymer flocculant E was not added.
（比較例５）
カチオン性高分子凝集剤Ａをカチオン性高分子凝集剤Ｃ（水溶液濃度０．３質量％）にした以外は実施例１と同様にして処理を行った。
(Comparative example 5)
The treatment was performed in the same manner as in Example 1 except that the cationic polymer flocculant A was changed to the cationic polymer flocculant C (aqueous solution concentration 0.3% by mass).
（比較例６）
カチオン性高分子凝集剤Ａをカチオン性高分子凝集剤Ｄ（水溶液濃度０．３質量％）にした以外は実施例１と同様にして処理を行った。
(Comparative example 6)
The treatment was performed in the same manner as in Example 1 except that the cationic polymer flocculant A was changed to the cationic polymer flocculant D (aqueous solution concentration 0.3% by mass).
（比較例７）
カチオン性高分子凝集剤Ａを添加せず、アニオン性高分子凝集剤Ｅのみを７５ｍＬ（汚泥への添加率２５０ｐｐｍ）添加した以外は実施例１と同様にして処理を行った。
(Comparative example 7)
The treatment was performed in the same manner as in Example 1 except that the cationic polymer flocculant A was not added, and only 75 mL of the anionic polymer flocculant E (addition rate to sludge: 250 ppm) was added.
実施例および比較例における各試験結果を表２に示す。 The test results in Examples and Comparative Examples are shown in Table 2.
（実施例４）
チタン、マグネシウム及びカルシウムを含む塗料系金属含有汚泥に水酸化カルシウムを添加してｐＨ１１．０に調整した。ｐＨ調整後の汚泥のＴＳは４．０２％であった。また、ｐＨ調整後の汚泥のチタン含有量はＪＩＳ Ｈ １６３２−１：２０１４に記載のＩＣＰ発光分光分析法で測定したところ、０．５質量％であった。前記汚泥３００ｍＬを５００ｍＬビーカーに取り、カチオン性高分子凝集剤Ａ（水溶液濃度０．３質量％）を２５ｍＬ（汚泥への添加率２５０ｐｐｍ）添加し、スパチュラを用いて２００ｒｐｍで３０秒撹拌した。ついでアニオン性高分子凝集剤Ｅ（水溶液濃度０．１質量％）を４５ｍＬ（汚泥への添加率１５０ｐｐｍ）添加し、スパチュラを用いて２００ｒｐｍで３０秒撹拌した。フロック径の測定、濾液の濁度の測定、脱水ケーキの作製及び含水率の測定は実施例１と同様に行った。
(Example 4)
Calcium hydroxide was added to the paint-based metal-containing sludge containing titanium, magnesium and calcium to adjust to pH 11.0. The TS of sludge after pH adjustment was 4.02%. Moreover, it was 0.5 mass% when the titanium content of the sludge after pH adjustment was measured by the ICP emission-spectroscopic-analysis method of JISH1632-1: 2014. 300 mL of the sludge was taken in a 500 mL beaker, 25 mL (addition rate to sludge: 250 ppm) of the cationic polymer flocculant A (aqueous solution concentration 0.3 mass%) was added, and stirred for 30 seconds at 200 rpm using a spatula. Next, 45 mL (addition rate to sludge: 150 ppm) of an anionic polymer flocculant E (aqueous solution concentration: 0.1 mass%) was added, and stirred using a spatula at 200 rpm for 30 seconds. The measurement of the floc diameter, the measurement of the turbidity of the filtrate, the preparation of the dehydrated cake and the measurement of the water content were carried out in the same manner as in Example 1.
（実施例５）
水酸化カルシウムの添加によるｐＨ調整をｐＨ１２．７にした以外は実施例１と同様にして処理を行った。
(Example 5)
Treatment was carried out in the same manner as in Example 1 except that the pH was adjusted to 12.7 by addition of calcium hydroxide.
（実施例６）
アニオン性高分子凝集剤Ｅの添加量を６０ｍＬ（汚泥への添加率２００ｐｐｍ）にした以外は実施例１と同様にして処理を行った。
(Example 6)
The treatment was performed in the same manner as in Example 1 except that the addition amount of the anionic polymer flocculant E was changed to 60 mL (the addition rate to the sludge: 200 ppm).
（比較例８）
水酸化カルシウムの添加によるｐＨ調整をｐＨ８．９にした以外は実施例１と同様にして処理を行った。
(Comparative example 8)
The treatment was carried out in the same manner as in Example 1 except that the pH was adjusted to pH 8.9 by the addition of calcium hydroxide.
（比較例９）
水酸化カルシウムの添加によるｐＨ調整をｐＨ１４．２にした以外は実施例１と同様にして処理を行った。
(Comparative example 9)
The treatment was carried out in the same manner as in Example 1 except that the pH was adjusted to 14.2 by the addition of calcium hydroxide.
（比較例１０）
カチオン性高分子凝集剤Ａをカチオン性高分子凝集剤Ｂにした以外は実施例１と同様にして処理を行った。
(Comparative example 10)
The treatment was performed in the same manner as in Example 1 except that the cationic polymer coagulant A was changed to the cationic polymer coagulant B.
（比較例１１）
カチオン性高分子凝集剤Ａを４０ｍＬ（汚泥への添加率４００ｐｐｍ）添加し、アニオン性高分子凝集剤Ｅを添加しない以外は実施例１と同様にして処理を行った。
(Comparative example 11)
The treatment was performed in the same manner as in Example 1 except that 40 mL of the cationic polymer flocculant A (addition rate to sludge: 400 ppm) was added and the anionic polymer flocculant E was not added.
（比較例１２）
カチオン性高分子凝集剤Ａをカチオン性高分子凝集剤Ｃ（水溶液濃度０．３質量％）にした以外は実施例１と同様にして処理を行った。
(Comparative example 12)
The treatment was performed in the same manner as in Example 1 except that the cationic polymer flocculant A was changed to the cationic polymer flocculant C (aqueous solution concentration 0.3% by mass).
（比較例１３）
カチオン性高分子凝集剤Ａをカチオン性高分子凝集剤Ｄ（水溶液濃度０．３質量％）にした以外は実施例１と同様にして処理を行った。
(Comparative example 13)
The treatment was performed in the same manner as in Example 1 except that the cationic polymer flocculant A was changed to the cationic polymer flocculant D (aqueous solution concentration 0.3% by mass).
（比較例１４）
カチオン性高分子凝集剤Ａを添加せず、アニオン性高分子凝集剤Ｅのみを１２０ｍＬ（汚泥への添加率４００ｐｐｍ）添加した以外は実施例１と同様にして処理を行った。
(Comparative example 14)
The treatment was performed in the same manner as in Example 1 except that the cationic polymer flocculant A was not added, and only 120 mL of the anionic polymer flocculant E (addition rate to sludge: 400 ppm) was added.
実施例及び比較例における各試験結果を表３に示す。 The test results in Examples and Comparative Examples are shown in Table 3.
表２及び表３の通り、本発明の処理方法である実施例１〜３及び実施例４〜６は、フロック径が大きくなり、含水率が低下する。これに対し、比較例１、２、８及び９は、ｐＨが１０〜１３を外れるとフロック径が小さく、含水率が高くなることが確認できる。
また、カチオン性高分子凝集剤のみで処理した比較例４及び比較例１１においてはフロックが形成されず、カチオン性高分子凝集剤の組成比を変えたものを使用した比較例３、５、６、１０、１２及び１３、アニオン性高分子凝集剤のみで処理した比較例７及び比較例１４は、フロック径が小さく、含水率は高くなっていることが確認できる。
As shown in Tables 2 and 3, in Examples 1 to 3 and Examples 4 to 6 which are the treatment method of the present invention, the diameter of the floc increases and the water content decreases. On the other hand, in Comparative Examples 1, 2, 8 and 9, it can be confirmed that when the pH is out of 10 to 13, the flock diameter is small and the water content is high.
Moreover, in Comparative Example 4 and Comparative Example 11 in which only the cationic polymer flocculant was treated, no flock was formed, and Comparative Examples 3, 5, 6 using different composition ratios of the cationic polymer flocculant were used. 10, 12 and 13, and Comparative Examples 7 and 14 treated only with the anionic polymer flocculant, it can be confirmed that the flock diameter is small and the water content is high.
本発明によれば、チタン、マグネシウム及びカルシウムを含む金属含有汚泥にアルカリを添加し、ついで高分子凝集剤を添加する金属含有汚泥の処理方法として広く適用できる。
According to the present invention, the method can be widely applied as a method for treating metal-containing sludge in which an alkali is added to a metal-containing sludge containing titanium, magnesium and calcium and then a polymer flocculant is added.
Claims (4)
〜１０質量％、ジアルキルアミノアルキルメタクリレート塩化アルキル４級塩構造単位を
５〜２０質量％、ジアルキルアミノアルキルアクリレート塩化アルキル４級塩構造単位を
７０〜９０質量％有するカチオン性高分子凝集剤を添加し、ついでアニオン性高分子凝集
剤を添加して脱水処理を行う金属含有汚泥の処理方法であって、
前記カチオン性高分子凝集剤中のノニオン性構造単位がアクリルアミド構造単位、
ジアルキルアミノアルキルメタクリレート塩化アルキル４級塩構造単位がジメチルアミノ
エチルメタクリレート塩化メチル４級塩構造単位、
ジアルキルアミノアルキルアクリレート塩化アルキル４級塩構造単位がジメチルアミノエ
チルアクリレート塩化メチル４級塩構造単位、
である金属含有汚泥の処理方法。 After adjusting the metal-containing sludge to have a pH of 10 to 13, first, 5 nonionic structural units
10 to 10% by mass, 5 to 20% by mass of dialkylaminoalkyl methacrylate alkyl chloride quaternary structural unit, 70 to 90% by mass of dialkylaminoalkyl acrylate alkyl chloride quaternary structural unit, and adding a cationic polymer flocculant And a method of treating metal-containing sludge which is then subjected to dehydration treatment by adding an anionic polymer flocculant ,
The nonionic structural unit in the cationic polymer coagulant is an acrylamide structural unit,
Dialkylaminoalkyl methacrylate alkyl chloride quaternary salt structural unit is dimethylamino
Ethyl methacrylate methyl chloride quaternary salt structural unit,
A dialkylaminoalkyl acrylate alkyl chloride quaternary salt structural unit is dimethylamino
Methyl acrylate methyl chloride quaternary salt structural unit,
The method of treating metal-containing sludge .
処理方法。 The method for treating metal-containing sludge according to claim 1, wherein the metal-containing sludge is a metal-containing sludge containing titanium.
記載の金属含有汚泥の処理方法。 The method for treating metal-containing sludge according to claim 1 or 2, wherein the concentration of titanium in the metal-containing sludge is 0.01 to 1% by mass.
１〜３のいずれか一項に記載の金属含有汚泥の処理方法。The processing method of the metal containing sludge as described in any one of 1-3.
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