JP4541042B2 - Powdered activated carbon for water treatment and method for producing the same - Google Patents
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本発明は、水溶性カルシウム化合物を含む活性炭に、そのカルシウムと反応するに必要な量のリン酸または硫酸を加えることにより、活性炭中に含まれる水溶性カルシウム化合物を水に難溶性の化合物として活性炭に固定し、活性炭により水を処理した場合、難溶性カルシウム化合物の装置内での析出による装置の詰まりを抑えた水処理用活性炭吸着剤に関する。 The present invention relates to activated carbon containing water-soluble calcium compound contained in activated carbon as a compound hardly soluble in water by adding phosphoric acid or sulfuric acid in an amount necessary for reacting with calcium to activated carbon containing water-soluble calcium compound. It is related with the activated carbon adsorbent for water treatment which suppressed clogging of the apparatus by precipitation in the apparatus of a poorly soluble calcium compound when water was processed with activated carbon.
水道原水の浄化に粉末活性炭を使うことはよく知られている。粉末活性炭は、乾燥した状態では発塵が著しいため、湿潤した状態で使用されることが多い。しかしながら、活性炭を湿潤させると、黴の発生の恐れがあるため、活性炭に銀化合物を添着して黴の発生を抑制するといった措置を講ずる必要があった（特許文献１）。
ところが、近年の粉体輸送機器の進歩により、作業時に発塵することなく活性炭を水でスラリー状にして、所定の濃度で水道原水に活性炭を添加することが広く行われるようになった。この方法により、輸送コストが低減でき、細菌類、黴の発生の恐れもなくなった。
しかし活性炭には、天然素材に由来する、または製造工程で用いるアルカリ土類金属化合物に由来する水溶性カルシウム化合物が含まれている。この水溶性カルシウム化合物が上述のスラリー化工程の際に溶出して、カルシウムイオンが処理水中の硫酸イオンと反応し、難熔性の硫酸カルシウムとなって析出する。その析出物が凝集、集積してスラリー輸送装置の目詰まりを起こすことがある。この場合、装置の解体、清掃が必要になり、浄水工程の著しい支障となる。
また、活性炭中の水溶性金属化合物により、粉末活性炭は一般にアルカリ性を呈するが、場合によっては処理後の水が日本水道協会規格 ＪＷＷＡ Ｋ１１３「水道用粉末活性炭」の規格であるｐＨ４〜１１の範囲を逸脱することがある。
したがって、活性炭に含まれる水溶性カルシウム化合物の溶出量を低減し、且つ処理後の水のｐＨ値を規格内のものにする水処理用粉末活性炭の開発が強く求められていた。
However, due to recent advances in powder transportation equipment, it has become widely practiced to add activated carbon to tap water at a predetermined concentration by making activated carbon a slurry with water without generating dust during operation. By this method, transportation costs can be reduced, and there is no risk of generation of bacteria and sputum.
However, activated carbon contains water-soluble calcium compounds derived from natural materials or derived from alkaline earth metal compounds used in the production process. This water-soluble calcium compound is eluted during the above-mentioned slurrying step, and calcium ions react with sulfate ions in the treated water to precipitate as hardly soluble calcium sulfate. The precipitate may aggregate and accumulate, causing clogging of the slurry transport device. In this case, it is necessary to dismantle and clean the device, which significantly hinders the water purification process.
In addition, the activated carbon powder generally exhibits alkalinity due to the water-soluble metal compound in the activated carbon, but in some cases, the treated water has a pH range of 4 to 11 which is the standard of the Japan Water Works Association Standard JWWA K113 “powder activated carbon for water supply”. May deviate.
Accordingly, there has been a strong demand for the development of powdered activated carbon for water treatment that reduces the elution amount of the water-soluble calcium compound contained in the activated carbon and keeps the pH value of the treated water within the standard.
本発明の課題は、活性炭で水を処理した場合、活性炭からのカルシウムイオンの溶出量が抑制され、処理後の水のｐＨが規格内のものとなるように工夫された粉末活性炭を提供することにある。 An object of the present invention is to provide powdered activated carbon that has been devised so that when water is treated with activated carbon, the elution amount of calcium ions from the activated carbon is suppressed, and the pH of the treated water is within the standard. It is in.
本発明は、水酸化カルシウム、炭酸カルシウム、塩化カルシウムなどの水溶性カルシウム化合物を含む活性炭に、そのカルシウムと反応するに必要な量の高濃度リン酸または硫酸を加えることにより、カルシウムをリン酸カルシウムや硫酸カルシウムといった水に難溶性の化合物として活性炭に固定し、活性炭を水と接触させた場合カルシウムイオンの溶出を抑制し、且つ水分含量を抑制した結果、粉末として取り扱う場合も発塵せず、取り扱いも容易な水処理用粉末活性炭を得ることが可能であることを知り、その知見を基に更に研究を重ねて本発明を完成した。
すなわち、本発明は、
（１）水溶性カルシウム化合物を含む活性炭に、そのカルシウムと反応するに必要な量の濃度６０〜１００％のリン酸または硫酸を、リン酸（H 3 PO 4 ）又は硫酸(H 2 SO 4 )として乾燥活性炭に対し０．５〜４重量％混合することにより得られた水道水処理用粉末活性炭。
（２）日本水道協会規格ＪＷＷＡ Ｋ１１３によって測定する乾燥減量が５％以下である（１）記載の水道水処理用粉末活性炭。
（３）粉末活性炭の９０重量％以上が０．１ｍｍ目開きのふるいを通過するものである（１）又は（２）に記載の水道水処理用粉末活性炭。
The present invention adds calcium to calcium phosphate or sulfuric acid by adding high-concentration phosphoric acid or sulfuric acid in an amount necessary to react with calcium to activated carbon containing a water-soluble calcium compound such as calcium hydroxide, calcium carbonate, or calcium chloride. When calcium is fixed to activated carbon as a water-insoluble compound such as calcium, and activated carbon is contacted with water, calcium ion elution is suppressed and the water content is suppressed. Knowing that it is possible to obtain powdered activated carbon for easy water treatment, the present invention was completed by further research based on the knowledge.
That is, the present invention
(1) Activated carbon containing a water-soluble calcium compound is mixed with phosphoric acid or sulfuric acid having a concentration of 60 to 100% required to react with the calcium, phosphoric acid (H 3 PO 4 ) or sulfuric acid (H 2 SO 4 ). Powdered activated carbon for treating tap water obtained by mixing 0.5 to 4% by weight with respect to dry activated carbon.
(2) Japan Water Works Association loss on drying measured by standard JWWA K113 is below 5% or less (1) tap water treatment powdered activated carbon according.
(3) The powdered activated carbon for treating tap water according to (1) or (2) , wherein 90% by weight or more of the powdered activated carbon passes through a sieve having an opening of 0.1 mm.
本発明方法で使用される活性炭の原料は、やし殻、石炭、コークス、木粉、おが屑、天然繊維（例、麻、綿等）、合成繊維（例、レーヨン、ポリエステル等）、合成樹脂（例、ポリアクリロニトリル、フェノール樹脂、ポリ塩化ビニリデン、ポリカーボネート、ポリビニルアルコールなど一般的に用いられるものであればいずれでも良い。特に木粉、おが屑、やし殻、もみ殻、パームやし殻、キャンドルナッツ殻、木炭等の木質系原料が好ましく、木粉、おが屑がさらに好ましい。
活性炭の賦活方法も特に限定されないが、たとえば「活性炭工業」、重化学工業通信社（１９７４）、ｐ．２３〜ｐ．３７に記載の、水蒸気、酸素、炭酸ガスなどの活性ガスでの賦活炭や、リン酸、塩化亜鉛などを用いた薬品賦活炭などハロゲンガスで賦活した以外の活性炭が用いられる。これらのなかでも、水蒸気賦活、酸素賦活、炭酸ガス賦活等のガス賦活法が好ましく、水蒸気賦活法が特に好ましい。
用いられる活性炭のＢＥＴ比表面積は、５００〜２０００ｍ２／ｇが好ましく、さらに好ましくは、７００〜１８００ｍ２／ｇである。上記賦活法により製造された活性炭のなかから、このＢＥＴ比表面積を有するものを選択する。
粉末活性炭は、通常その９０重量％が目開き０．１ｍｍ、好ましくは０．０７５ｍｍの試験用ふるいを通過する粒度まで粉砕して使用するのが好ましい。
The raw materials of activated carbon used in the method of the present invention are palm husk, coal, coke, wood flour, sawdust, natural fibers (eg, hemp, cotton, etc.), synthetic fibers (eg, rayon, polyester, etc.), synthetic resins ( Any of the commonly used materials such as polyacrylonitrile, phenol resin, polyvinylidene chloride, polycarbonate, polyvinyl alcohol, etc. Especially wood flour, sawdust, coconut shell, rice husk, palm coconut shell, candle nut Woody materials such as shells and charcoal are preferred, and wood flour and sawdust are more preferred.
The activation method of the activated carbon is not particularly limited. For example, “activated carbon industry”, heavy chemical industry communication company (1974), p. 23-p. Activated charcoal other than activated with a halogen gas such as activated charcoal with active gas such as water vapor, oxygen, carbon dioxide, or chemical activated charcoal with phosphoric acid, zinc chloride or the like described in 37 is used. Of these, gas activation methods such as water vapor activation, oxygen activation, and carbon dioxide activation are preferred, and water vapor activation methods are particularly preferred.
BET specific surface area of the activated carbon used is preferably from 500~2000m 2 / g, more preferably 700~1800m 2 / g. From the activated carbon produced by the activation method, one having this BET specific surface area is selected.
It is preferable to use the powdered activated carbon after pulverizing it to a particle size in which 90% by weight passes through a test sieve having an opening of 0.1 mm, preferably 0.075 mm.
活性炭に対するリン酸または硫酸の混合量は、活性炭中の水溶性カルシウム化合物の含有量により異なってくる。
活性炭中の水溶性カルシウム化合物の含有量は、一定重量の活性炭を水で抽出し、水中に溶出したカルシウムイオンの濃度を測定するとにより容易に知ることができる。具体的には、日本水道協会規格ＪＷＷＡ Ｋ１１３のｐＨ値の測定方法における抽出液中のカルシウムイオン濃度を、原子吸光光度計、誘導結合プラズマ発光分光光度計等で測定して求めることができる。
本発明においては、このようにして測定した水中のカルシウムイオンの濃度から必要なリン酸や硫酸の混合量を決めればよい。実用上は、上記ＪＷＷＡ Ｋ１１３の方法に従って活性炭処理した水に含まれるカルシウムイオンが１５ｐｐｍ以下、好ましくは１０ｐｐｍ以下となる量のリン酸や硫酸を用いる。活性炭が従来上水処理用に用いられた粉末活性炭である場合は、乾燥活性炭に対し、H3PO4およびH2SO4として通常０．５〜４重量％、好ましくは１〜３重量％である。
必要以上の大量のリン酸や硫酸を添加すると、製品を水と接触させた際、水のｐＨ値が低くなり過ぎて、「水道用粉末活性炭」の規格から外れてしまうことがあるので、必要量の１０重量％過剰の範囲内、好ましくは５重量％過剰の範囲内に止めるのがよい。
The amount of phosphoric acid or sulfuric acid mixed with activated carbon varies depending on the content of the water-soluble calcium compound in the activated carbon.
The content of the water-soluble calcium compound in the activated carbon can be easily determined by extracting a certain weight of activated carbon with water and measuring the concentration of calcium ions eluted in the water. Specifically, the calcium ion concentration in the extract in the method for measuring the pH value of Japan Water Works Association Standard JWWA K113 can be determined by measuring with an atomic absorption photometer, an inductively coupled plasma emission spectrophotometer, or the like.
In the present invention, the necessary mixing amount of phosphoric acid and sulfuric acid may be determined from the concentration of calcium ions in the water thus measured. Practically, phosphoric acid or sulfuric acid is used in such an amount that the calcium ion contained in the water treated with activated carbon according to the method of JWWA K113 is 15 ppm or less, preferably 10 ppm or less. When the activated carbon is powdered activated carbon conventionally used for water treatment, it is usually 0.5 to 4% by weight, preferably 1 to 3% by weight as H 3 PO 4 and H 2 SO 4 with respect to the dry activated carbon. is there.
It is necessary to add a large amount of phosphoric acid or sulfuric acid that is more than necessary, because when the product is brought into contact with water, the pH value of the water becomes too low and may deviate from the standard of “powder activated carbon for water supply”. The amount should be kept within an excess of 10% by weight, preferably within an excess of 5% by weight.
リン酸または硫酸の活性炭への混合は、活性炭の混合に用いられる公知の方法を利用することができる。たとえば「化学工学便覧」、丸善（１９９９）、ｐ．８７６〜ｐ．８７８に記載されている水平円筒型、Ｖ型、二重円錐型、揺動回転型、単軸リボン型、複軸パドル型、回転鋤型、二軸遊星かくはん型、円錐スクリュー型、高速かくはん型、回転円盤型、ローラー付回転容器型、かくはん付回転容器型、高速楕円ローター型、気流かくはん型、無かくはん型等の容器に活性炭を入れ、リン酸または硫酸を添加し、混合することができる。
加えるリン酸または硫酸は、混合後の乾燥減量（日本水道協会規格 ＪＷＷＡ Ｋ１１３の方法によって測定する乾燥減量）を、例えば５重量％以下、好ましくは３重量％以下と少なくするのが好ましい。このために、リン酸または硫酸の濃度を通常５０重量％以上（１００％以下）、さらに６０〜１００重量％とするのが好ましく、７０〜９０重量％とするのが最も好ましい。酸の濃度が低いと水の量が多くなるため、活性炭の乾燥減量が好ましい範囲を超えたり、水溶性カルシウム化合物と反応するだけのリン酸および/または硫酸を添加できなくなることがあるので好ましくない。
活性炭とリン酸および／または硫酸の混合は、通常５〜８０℃で行うことができるが、５〜３５℃の常温で行えばよい。混合時間は、活性炭全体が均一になる時間でよく、混合機の形式によって任意に選定することができる。通常は、１０分〜１０時間、さらに好ましくは、３０分〜５時間である。このようにして活性炭にリン酸および／または硫酸を吸着させた後、必要により水洗、乾燥してもよいが、通常その必要はない。
For mixing phosphoric acid or sulfuric acid with activated carbon, a known method used for mixing activated carbon can be used. For example, “Chemical Engineering Handbook”, Maruzen (1999), p. 876-p. 878 horizontal cylinder type, V type, double cone type, swing rotation type, single axis ribbon type, double axis paddle type, rotary saddle type, two axis planetary agitation type, conical screw type, high speed agitation type , Rotating disc type, rotating vessel type with roller, rotating vessel type with stirring, high-speed elliptical rotor type, airflow stirring type, non-stirring type, etc., activated carbon can be added, phosphoric acid or sulfuric acid can be added and mixed .
It is preferable that the phosphoric acid or sulfuric acid to be added reduce the loss on drying after mixing (loss on drying measured by the method of Japan Water Works Association Standard JWWA K113), for example, 5% by weight or less, preferably 3% by weight or less. Therefore, the concentration of phosphoric acid or sulfuric acid is usually 50% by weight or more (100% or less), more preferably 60 to 100% by weight, and most preferably 70 to 90% by weight. If the acid concentration is low, the amount of water increases, which is not preferable because the loss on drying of activated carbon may exceed the preferred range, or phosphoric acid and / or sulfuric acid that only reacts with water-soluble calcium compounds may not be added. .
Mixing of activated carbon and phosphoric acid and / or sulfuric acid can be usually performed at 5 to 80 ° C., but may be performed at room temperature of 5 to 35 ° C. The mixing time may be a time for the entire activated carbon to be uniform, and can be arbitrarily selected depending on the type of the mixer. Usually, it is 10 minutes to 10 hours, more preferably 30 minutes to 5 hours. Thus, after making phosphoric acid and / or sulfuric acid adsorb | suck to activated carbon, you may wash and dry as needed, but it is not necessary normally.
本発明の水処理用粉末活性炭は、活性炭に所定量の濃リン酸または硫酸を添加、混合し、次いで、得られた活性炭を粉砕するか、あるいは予め活性炭を粉砕し、得られた粉末活性炭にリン酸または硫酸を添加、混合し、必要に応じてさらに粉砕、混合することにより製造することができる。しかし、より均一にリン酸および／または硫酸を混合するためにはリン酸または硫酸添加の前に粉砕する方が好ましい。 The powdered activated carbon for water treatment of the present invention is prepared by adding and mixing a predetermined amount of concentrated phosphoric acid or sulfuric acid to the activated carbon, and then pulverizing the obtained activated carbon or previously pulverizing the activated carbon, It can be produced by adding and mixing phosphoric acid or sulfuric acid, and further grinding and mixing as necessary. However, in order to mix phosphoric acid and / or sulfuric acid more uniformly, it is preferable to grind before adding phosphoric acid or sulfuric acid.
活性炭の粉砕は、通常活性炭の粉砕に用いられる設備を使用することができる。たとえば「化学工学便覧」、丸善（１９９９）、ｐ．８４５〜ｐ．８５２にあるエロフォールミル、堅型ローラーミル、ハンマーミル、ブレードミル、ピンミル等の高速回転ミル、ボールミル、ジェットミルなどで粉砕することができる。
粉砕粒度は用途によって異なるが、上水処理用に用いられる場合は、通常０．１ｍｍの目開きのふるいを９０重量％通過する程度のものが好ましく、０．０７５ｍｍの目開きのふるいを９０重量％以上通過する粒度のものがさらに好ましい。
本発明の活性炭は、従来から上水施設などで用いられている装置にそのまま、且つ同一条件で使用することができる。
For the pulverization of the activated carbon, equipment usually used for pulverization of the activated carbon can be used. For example, “Chemical Engineering Handbook”, Maruzen (1999), p. 845-p. It can be pulverized by a high-speed rotary mill such as an erotic fall mill, a rigid roller mill, a hammer mill, a blade mill, or a pin mill, a ball mill, a jet mill, and the like.
The pulverized particle size varies depending on the application, but when used for water treatment, it is usually preferable to pass 90% by weight of a 0.1 mm sieve, and 90% by weight of a 0.075 mm sieve. More preferably, the particle size is at least%.
The activated carbon of the present invention can be used as it is in an apparatus conventionally used in a water supply facility or the like under the same conditions.
本発明の活性炭は、洗浄工程を経由しなくても水と接触させたときのカルシウム溶出量が少なく、処理後の水のｐＨ値上昇、難溶性カルシウム化合物の析出が起き難く、特に上水処理に好適に用いることができる。また、乾燥減量が少なく、微生物の増殖の懸念が少なく、長期にわたって保管した場合の品質の劣化も少ない。 The activated carbon of the present invention has a small amount of calcium elution when it is brought into contact with water without going through a washing step, the pH value of water after treatment is hardly increased, and precipitation of sparingly soluble calcium compounds hardly occurs. Can be suitably used. In addition, there is little loss on drying, there is little concern about the growth of microorganisms, and there is little deterioration in quality when stored for a long time.
以下に実施例、比較例および実験例を挙げて、本発明をさらに具体的に説明する。 Hereinafter, the present invention will be described more specifically with reference to examples, comparative examples, and experimental examples.
市販の水蒸気賦活木質系活性炭（原料活性炭１、目開き０．０７５ｍｍ以下９２％通過、ＢＥＴ比表面積１０２０ｍ２／ｇ）をＪＷＷＡ Ｋ１１３「ｐＨ値」の方法により抽出液を調製した。得られた抽出液を原子分光光度計（日立 Ｚ−８２００）によりカルシウムイオン濃度を測定したところ、２７ｐｐｍであった。
この原料活性炭１の１００重量部に含まれる水溶性カルシウムをリン酸カルシウムに変えるに必要なリン酸（H3PO4）は２．５重量部である。
２ｋｇの原料活性炭１を噴霧用ノズルを設けた単軸リボン型混合機に入れ、１５℃で混合機を運転しながら、濃度８５％のリン酸５９ｇを噴霧した。そのまま１時間混合して活性炭Ｎｏ．１（リン酸含有量２.５重量％、乾燥減量１.３％。）を得た。
A commercially available steam activated wood activated carbon (raw material activated carbon 1, mesh size 0.075 mm or less, 92% passage, BET specific surface area 1020 m 2 / g) was used to prepare an extract by the method of JWWA K113 “pH value”. When the calcium ion concentration of the obtained extract was measured with an atomic spectrophotometer (Hitachi Z-8200), it was 27 ppm.
Phosphoric acid (H 3 PO 4 ) necessary for changing the water-soluble calcium contained in 100 parts by weight of the raw activated carbon 1 to calcium phosphate is 2.5 parts by weight.
2 kg of raw activated carbon 1 was placed in a single-shaft ribbon mixer equipped with a spray nozzle, and 59 g of phosphoric acid having a concentration of 85% was sprayed while operating the mixer at 15 ° C. Mix as it is for 1 hour and use activated carbon no. 1 (phosphoric acid content 2.5% by weight, loss on drying 1.3%) was obtained.
実施例１で用いたと同じ原料活性炭１を２ｋｇ計り取り、噴霧用ノズルを設けた単軸リボン型混合機に入れた。
この原料活性炭１の１００重量部に含まれる水溶性カルシウムを硫酸カルシウムに変えるに必要な硫酸（H2SO4）は２．０重量部である。
混合機を１５℃で運転しながら、濃度９８％の硫酸４１ｇを噴霧し、そのまま１時間混合して活性炭Ｎｏ．２（硫酸含有量２重量％、乾燥減量１.０％。）を得た。
2 kg of the same raw material activated carbon 1 used in Example 1 was weighed and placed in a single-shaft ribbon mixer equipped with a spray nozzle.
The sulfuric acid (H 2 SO 4 ) necessary for changing the water-soluble calcium contained in 100 parts by weight of the raw activated carbon 1 to calcium sulfate is 2.0 parts by weight.
While operating the mixer at 15 ° C., 41 g of sulfuric acid having a concentration of 98% was sprayed and mixed as it was for 1 hour. 2 (sulfuric acid content 2% by weight, loss on drying 1.0%) was obtained.
ヒノキ材おが屑を、４５０℃まで昇温して炭化して素炭を得た。この素炭を流電式電気炉に入れ、８５０℃で１時間水蒸気賦活してＢＥＴ比表面積１０８０ｍ２／ｇの活性炭（原料活性炭２）を得た。この活性炭の粒度は、０．１５０ｍｍ以上が３５％、０．１５０ｍｍ〜０．０７５ｍｍが５７％、０．０７５ｍｍ以下が８％であった。得られた原料活性炭２について、実施例２と同様にして抽出液中のカルシウムイオン濃度を測定したところ、３１ｐｐｍであった。
この原料活性炭２の１００重量部に含まれる水溶性カルシウムをリン酸カルシウムに変えるに必要なリン酸（H3PO4）は２．５重量部である。
原料活性炭２の２ｋｇを計り取り、噴霧用ノズルを設けた単軸リボン型混合機に入れた。混合機を１５℃で運転しながら、８５％リン酸５９ｇを噴霧し、そのまま１時間混合した。その後振動ボールミルを用いて０．０７５ｍｍの目開きのふるいを９５％以上通過するまで粉砕して活性炭Ｎｏ．３（リン酸含有量２.５重量％、乾燥減量1.5％。）を得た。
The cypress sawdust was heated to 450 ° C. and carbonized to obtain raw carbon. This raw carbon was put into a galvanic electric furnace and steam activated at 850 ° C. for 1 hour to obtain activated carbon (raw material activated carbon 2) having a BET specific surface area of 1080 m 2 / g. The particle size of the activated carbon was 35% for 0.150 mm or more, 57% for 0.150 mm to 0.075 mm, and 8% for 0.075 mm or less. About the obtained raw material activated carbon 2, when the calcium ion concentration in an extract was measured like Example 2, it was 31 ppm.
The amount of phosphoric acid (H 3 PO 4 ) necessary for changing the water-soluble calcium contained in 100 parts by weight of the starting activated carbon 2 to calcium phosphate is 2.5 parts by weight.
2 kg of raw activated carbon 2 was weighed and placed in a single-shaft ribbon mixer equipped with a spray nozzle. While operating the mixer at 15 ° C., 59 g of 85% phosphoric acid was sprayed and mixed as it was for 1 hour. After that, the mixture was pulverized using a vibrating ball mill until it passed through a sieve with an opening of 0.075 mm to 95% or more, and activated carbon No. 3 (phosphoric acid content 2.5% by weight, loss on drying 1.5%) was obtained.
実施例１で用いたと同じ原料活性炭１の２ｋｇを、噴霧用ノズルを設けた単軸リボン型混合機に入れた。混合機を１５℃で運転しながら、８５％リン酸１９ｇを噴霧し、そのまま１時間混合して活性炭Ｎｏ．４（リン酸含有量０.８重量％、乾燥減量１.１％。）を得た。 2 kg of the same raw material activated carbon 1 used in Example 1 was placed in a single-shaft ribbon mixer equipped with a spray nozzle. While the mixer was operated at 15 ° C., 19 g of 85% phosphoric acid was sprayed and mixed as it was for 1 hour. 4 (phosphoric acid content 0.8% by weight, loss on drying 1.1%) was obtained.
実施例１で用いたと同じ原料活性炭１の２ｋｇを、噴霧用ノズルを設けた単軸リボン型混合機に入れた。混合機を１５℃で運転しながら、９８％硫酸２０ｇを噴霧し、そのまま１時間混合して活性炭Ｎｏ．５（硫酸含有量１重量％、乾燥減量１.０％）を得た。
〔比較例１〕
2 kg of the same raw material activated carbon 1 as used in Example 1 was put in a single-shaft ribbon mixer equipped with a spray nozzle. While the mixer was operated at 15 ° C., 20 g of 98% sulfuric acid was sprayed and mixed as it was for 1 hour. 5 (sulfuric acid content 1% by weight, loss on drying 1.0%) was obtained.
[Comparative Example 1]
実施例１で用いた原料活性炭１をそのまま用いた（活性炭Ｎｏ．６）。
〔比較例２〕
The raw material activated carbon 1 used in Example 1 was used as it was (activated carbon No. 6).
[Comparative Example 2]
実施例１で用いた原料活性炭１を２ｋｇ計りとり、噴霧用ノズルを設けた単軸リボン型混合機に入れた。混合機を１５℃で運転しながら、３５％塩酸１１４ｇを噴霧し、そのまま１時間混合して活性炭Ｎｏ．７（塩酸含有量２重量％）を得た。
〔比較例３〕
2 kg of the activated carbon 1 used in Example 1 was weighed and placed in a single-shaft ribbon mixer equipped with a spray nozzle. While operating the mixer at 15 ° C., 114 g of 35% hydrochloric acid was sprayed and mixed as it was for 1 hour to obtain activated charcoal no. 7 (hydrochloric acid content 2% by weight) was obtained.
[Comparative Example 3]
実施例１で用いた原料活性炭１を２ｋｇ計りとり、噴霧用ノズルを設けた単軸リボン型混合機に入れた。混合機を１５℃で運転しながら、８５％リン酸４．７ｇを噴霧し、そのまま１時間混合して活性炭Ｎｏ．８（リン酸含有量０．２重量％）を得た。
〔比較例４〕
2 kg of the activated carbon 1 used in Example 1 was weighed and placed in a single-shaft ribbon mixer equipped with a spray nozzle. While operating the mixer at 15 ° C., 4.7 g of 85% phosphoric acid was sprayed and mixed as it was for 1 hour to obtain activated carbon No. 8 (phosphoric acid content 0.2% by weight) was obtained.
[Comparative Example 4]
実施例１で用いた原料活性炭１を２ｋｇ計りとり、噴霧用ノズルを設けた単軸リボン型混合機に入れた。混合機を１５℃で運転しながら、９８％硫酸４．１ｇを噴霧し、そのまま１時間混合して活性炭Ｎｏ．９（硫酸含有量０．２重量％）を得た。
〔比較例５〕
2 kg of the activated carbon 1 used in Example 1 was weighed and placed in a single-shaft ribbon mixer equipped with a spray nozzle. While operating the mixer at 15 ° C., 4.1 g of 98% sulfuric acid was sprayed and mixed as it was for 1 hour to obtain activated carbon no. 9 (sulfuric acid content 0.2% by weight) was obtained.
[Comparative Example 5]
実施例１で用いた原料活性炭１を２ｋｇ計りとり、噴霧用ノズルを設けた単軸リボン型混合機に入れた。混合機を１５℃で運転しながら、８５％リン酸１１８ｇを噴霧し、そのまま１時間混合して活性炭Ｎｏ．１０（リン酸含有量５重量％）を得た。
〔比較例６〕
2 kg of the activated carbon 1 used in Example 1 was weighed and placed in a single-shaft ribbon mixer equipped with a spray nozzle. While operating the mixer at 15 ° C., 118 g of 85% phosphoric acid was sprayed and mixed as it was for 1 hour to obtain activated carbon no. 10 (phosphoric acid content 5% by weight) was obtained.
[Comparative Example 6]
実施例１で用いた原料活性炭１を２ｋｇ計りとり、噴霧用ノズルを設けた単軸リボン型混合機に入れた。混合機を１５℃で運転しながら、９８％硫酸１０２ｇを噴霧し、そのまま１時間混合して活性炭Ｎｏ．１１（硫酸含有量５重量％）を得た。
〔試験例１〕
2 kg of the activated carbon 1 used in Example 1 was weighed and placed in a single-shaft ribbon mixer equipped with a spray nozzle. While operating the mixer at 15 ° C., 102 g of 98% sulfuric acid was sprayed and mixed as it was for 1 hour to obtain activated carbon No. 11 (5% by weight sulfuric acid content) was obtained.
[Test Example 1]
カルシウム溶出量
試料活性炭をＪＷＷＡ Ｋ１１３「ｐＨ値」の方法に従って調製した試験溶液中のカルシウム濃度を原子分光光度計（日立 Ｚ−８２００）を用いて測定し、カルシウム溶出量とした。
電気伝導率・ｐＨ値
液の電気伝導率及びｐＨ値は、ＪＷＷＡ Ｋ１１３「ｐＨ値」に従い測定した。電気伝導率は、水に含まれる電解質の濃度の指標として測定されるものである。
乾燥減量
ＪＷＷＡ Ｋ１１３「乾燥減量」に従い測定した。
Calcium elution amount The calcium concentration in the test solution prepared by following the method of JWWA K113 “pH value” for the sample activated carbon was measured using an atomic spectrophotometer (Hitachi Z-8200), and the amount of calcium elution was determined.
Electric conductivity and pH value The electric conductivity and pH value of the liquid were measured according to JWWA K113 "pH value". The electric conductivity is measured as an index of the concentration of the electrolyte contained in water.
Loss on drying Measured according to JWWA K113 "Loss on drying".
本発明の水処理用粉末の活性炭は、処理した水のｐＨ値が規格内に収まり、カルシウムの溶出が抑制されているので、難溶性カルシウム化合物の析出による装置の詰まりを抑えることができ、特に上水施設における上水処理に特に好適に用いることができる。
The activated carbon of the powder for water treatment of the present invention has the pH value of the treated water kept within the standard, and the elution of calcium is suppressed, so that clogging of the device due to precipitation of hardly soluble calcium compound can be suppressed. It can be particularly preferably used for water treatment in a water supply facility.
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