JP6795810B2 - Air filter manufacturing method - Google Patents
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Description
本発明は、空気中に含まれる有害物質を除去するためのエアフィルターの製造方法に関する。 The present invention relates to a method for manufacturing an air filter for removing harmful substances contained in air.
東日本大震災における原子力発電所の事故の影響で、大量の放射性セシウムが拡散した。しかし、水に溶解した放射性セシウムを水から除去するための放射性セシウム吸着繊維は、ほとんど知られていなかった。なお、特許文献１には、金属イオン吸着性の変性アクリロニトリルポリマーが開示されているが、セシウムは対象となっていない。また、特許文献２には、セシウムを吸着することができるとの記載があるが、実際にセシウムを吸着したデータはない。また、ゼオライト粉末は放射性セシウムを吸着することが知られているが、ゼオライト粉末の回収は極めて困難であり、また、ゼオライトは一旦吸着した放射性セシウムを放出する性質があるため、放射性セシウムの回収には向いていなかった。 Due to the impact of the nuclear power plant accident caused by the Great East Japan Earthquake, a large amount of radioactive cesium was diffused. However, little is known about radioactive cesium-adsorbing fibers for removing radioactive cesium dissolved in water from water. Although Patent Document 1 discloses a modified acrylonitrile polymer that adsorbs metal ions, it does not cover cesium. Further, although Patent Document 2 describes that cesium can be adsorbed, there is no data that actually adsorbs cesium. Zeolite powder is known to adsorb radioactive cesium, but it is extremely difficult to recover the zeolite powder, and since zeolite has the property of releasing the once adsorbed radioactive cesium, it can be used to recover radioactive cesium. Was not suitable.
このような背景から、本発明者らは、水に溶解した放射性セシウムを効率的に吸着、回収することのできる、放射性セシウム吸着繊維及びその製造方法を提案した（特許文献３）。 Against this background, the present inventors have proposed a radioactive cesium-adsorbing fiber capable of efficiently adsorbing and recovering radioactive cesium dissolved in water and a method for producing the same (Patent Document 3).
ところで、放射性セシウムは、ミスト（霧状の水）に溶解した状態で空気中に含まれる場合がある。したがって、特に、原発事故の際の避難場所の建物内部へ空気を取り入れる際は、このような空気中に含まれる放射性セシウムを除去する必要がある。 By the way, radioactive cesium may be contained in the air in a state of being dissolved in mist (mist-like water). Therefore, it is necessary to remove radioactive cesium contained in such air, especially when air is taken into the building of the evacuation site in the event of a nuclear accident.
そこで、本発明は、ミスト（霧状の水）に溶解した状態で空気中に含まれる放射性セシウムを除去することができる、エアフィルターの製造方法を提供することを目的とする。 Therefore, an object of the present invention is to provide a method for manufacturing an air filter capable of removing radioactive cesium contained in air in a state of being dissolved in mist (mist-like water).
本発明者らは鋭意検討した結果、Ｎ−メチルピロリドン（ＮＭＰ）にポリスルホンを溶解するとともにゼオライトを分散させ、これを水中にシリンジを用いて押し出すことにより得られた、ゼオライトを担持した多孔質のポリスルホンを、所定の温度で加熱しながら加圧することでペレット化したものをエアフィルターとして用いた場合に、空気中に含まれる放射性セシウムを除去することができ、さらに、空気中に含まれるアンモニアをも除去することができることを見出し、本発明に想到した。 As a result of diligent studies, the present inventors have obtained a porous structure carrying zeolite, which is obtained by dissolving polysulfone in N-methylpyrrolidone (NMP) and dispersing zeolite in water and extruding it into water using a syringe. When polysulfone pelletized by pressurizing while heating at a predetermined temperature is used as an air filter, radioactive cesium contained in the air can be removed, and ammonia contained in the air can be removed. We found that it can also be removed, and came up with the present invention.
すなわち、本発明のエアフィルターの製造方法は、ゼオライト粒子が分散したポリスルホンの溶液を調製する溶液調製工程と、この溶液を水中に押し出してゼオライト粒子を担持したポリスルホンの繊維を成形する繊維成形工程と、この繊維を加熱しながら加圧してペレット化するペレット化工程とを備えたことを特徴とする。 That is, the method for producing an air filter of the present invention includes a solution preparation step of preparing a solution of polysulfone in which zeolite particles are dispersed, and a fiber molding step of extruding this solution into water to form polysulfone fibers carrying zeolite particles. It is characterized by comprising a pelletization step of pressurizing and pelletizing the fibers while heating them.
本発明によれば、ミスト（霧状の水）に溶解した状態で空気中に含まれる放射性セシウムや、空気中に含まれるアンモニアを除去することができる、エアフィルターを製造することができる。 According to the present invention, it is possible to manufacture an air filter capable of removing radioactive cesium contained in air and ammonia contained in air in a state of being dissolved in mist (mist-like water).
本発明のエアフィルターの製造方法は、原料として、ポリスルホン、ゼオライト粒子、ポリスルホンを溶解するための溶媒を用い、ゼオライト粒子が分散したポリスルホンの溶液を調製する溶液調製工程と、この溶液を水中に押し出してゼオライトを担持したポリスルホンの繊維を成型する繊維成形工程と、この繊維を加熱しながら加圧してペレット化するペレット化工程とを備える。本発明のエアフィルターの製造方法により製造されるエアフィルターは、多孔質のゼオライト粒子を担持した多孔質のポリスルホンであり、ポリスルホンに微細孔が形成された構造となっていて通気性が良好であるとともに、ポリスルホン中のゼオライト粒子の分散性が良好であることから、空気中の放射性セシウムを含むミストや、空気中のアンモニアを極めて効率的に吸着することができる。 The method for producing an air filter of the present invention uses a polysulfone, zeolite particles, and a solvent for dissolving polysulfone as raw materials, and prepares a solution of polysulfone in which zeolite particles are dispersed, and extrudes this solution into water. It includes a fiber molding step of molding polysulfone fibers carrying zeolite, and a pelletizing step of pressurizing and pelletizing the fibers while heating them. The air filter produced by the method for producing an air filter of the present invention is a porous polysulfone carrying porous zeolite particles, and has a structure in which micropores are formed in the polysulfone and has good air permeability. At the same time, since the zeolite particles in the polysulfone have good dispersibility, mist containing radioactive cesium in the air and ammonia in the air can be adsorbed extremely efficiently.
はじめに、溶液調製工程では、ゼオライト粒子が分散したポリスルホンの溶液を調製する。ここで、ポリスルホンを溶解するための溶媒としては、極性の高い有機溶媒が用いられ、Ｎ−メチルピロリドン（ＮＭＰ）、蟻酸、ｎ−ブタノール、Ｎ，Ｎ−ジメチルホルムアミド、テトラヒドロフランが好ましい。また、ゼオライト粒子としては、１５０メッシュ以下のものが好ましい。 First, in the solution preparation step, a solution of polysulfone in which zeolite particles are dispersed is prepared. Here, as a solvent for dissolving polysulfone, a highly polar organic solvent is used, and N-methylpyrrolidone (NMP), formic acid, n-butanol, N, N-dimethylformamide, and tetrahydrofuran are preferable. The zeolite particles are preferably 150 mesh or less.
また、溶液調製工程において、ポリスルホンを溶媒に溶解する際には、３０〜１００℃に溶媒を加温することによりポリスルホンの溶解が早くなる。また、溶液中のポリスルホン含有量は、１０〜３０質量％が好ましく、溶液中のゼオライト粒子含有量は、２０〜３０質量％が好ましい。なお、必要に応じて、その他の成分を溶液に添加してもよい。 Further, in the solution preparation step, when the polysulfone is dissolved in the solvent, the dissolution of the polysulfone is accelerated by heating the solvent to 30 to 100 ° C. The polysulfone content in the solution is preferably 10 to 30% by mass, and the zeolite particle content in the solution is preferably 20 to 30% by mass. If necessary, other components may be added to the solution.
つぎに、繊維成形工程では、溶液調製工程において調製した溶液を水中に押し出してゼオライトを担持したポリスルホンの繊維を成形する。 Next, in the fiber molding step, the solution prepared in the solution preparation step is extruded into water to mold polysulfone fibers carrying zeolite.
繊維成形工程において、射出に用いられる水の温度を５０℃程度とすることにより、溶媒の水への溶け出しが早く、繊維が形成されやすい。 By setting the temperature of the water used for injection to about 50 ° C. in the fiber molding step, the solvent dissolves quickly in water and fibers are easily formed.
そして、ペレット化工程では、繊維成形工程において成形した繊維を加熱しながら加圧してペレット化する。ここで、所定の形状に成形するために、金型を用いるのが好ましい。 Then, in the pelletization step, the fibers molded in the fiber molding step are pressurized while being heated to be pelletized. Here, it is preferable to use a mold to form a predetermined shape.
ペレット化工程において加圧する圧力の範囲は、ペレット化ができる値であればよく、特に限定されるものではないが、例えば、２０〜２００ｋｇｆ／ｃｍ２とすることができる。 The range of the pressure to be pressurized in the pelletizing step is not particularly limited as long as it can be pelletized, but can be, for example, 20 to 200 kgf / cm 2 .
以下、本発明のエアフィルターの製造方法と、本発明のエアフィルターの製造方法により得られたエアフィルターについて具体的に説明する。なお、本発明は以下の実施例に限定されるものではなく、種々の変形実施が可能である。 Hereinafter, the method for manufacturing the air filter of the present invention and the air filter obtained by the method for manufacturing the air filter of the present invention will be specifically described. The present invention is not limited to the following examples, and various modifications can be made.
（１）エアフィルターの製造
原料として、ポリスルホン、ゼオライト粒子、ＮＭＰを用いた。
(1) Production of air filter Polysulfone, zeolite particles, and NMP were used as raw materials.
室温にて、ポリスルホン３０質量％、ゼオライト粒子３０質量％、ＮＭＰ４０質量％となるように原料を混合し、ゼオライト粒子が分散したポリスルホンの溶液を作製した。この溶液をシリンジに入れ、シリンジの先を水中に入れた状態でシリンジの先から溶液を水中に押し出すと、水中に繊維が成形された。得られた繊維は、多孔質のポリスルホン中にゼオライト粒子が取り込まれている構造を有していた。 At room temperature, the raw materials were mixed so as to have 30% by mass of polysulfone, 30% by mass of zeolite particles, and 40% by mass of NMP to prepare a solution of polysulfone in which zeolite particles were dispersed. When this solution was put into a syringe and the solution was extruded into water from the tip of the syringe with the tip of the syringe in water, fibers were formed in the water. The obtained fiber had a structure in which zeolite particles were incorporated into porous polysulfone.
つぎに、内径４０ｍｍのステンレス製の円筒内に上記で作製した繊維を入れ、油圧プレス機を用いて１００ｋｇｆ／ｃｍ２の圧力で加圧してペレット化し、直径４０ｍｍ、厚さ約１０ｍｍのエアフィルターを得た。 Next, the fibers prepared above are placed in a stainless steel cylinder having an inner diameter of 40 mm and pressurized with a pressure of 100 kgf / cm 2 using a hydraulic press to pelletize an air filter having a diameter of 40 mm and a thickness of about 10 mm. Obtained.
（２）放射性セシウムを含むミストの除去試験
製造したエアフィルターを用いて、放射性セシウムを含むミストの除去試験を行った。試験に用いた実験装置概略図を図１に示す。
(2) Removal test of mist containing radioactive cesium A removal test of mist containing radioactive cesium was performed using the manufactured air filter. A schematic diagram of the experimental device used in the test is shown in FIG.
超音波霧化装置を用いて、放射性セシウムを含む検体液を霧化して直径約４μｍのミストを生成させた。このミストを含む気体をドライ真空ポンプにより吸引し、吸着装置に設けられた吸着材（エアフィルター）と接触させた。吸着材を通過した気体を氷水で冷却されたトラップに導き、気体に含まれる水分を凝縮させて検出液として回収した。 Using an ultrasonic atomizer, the sample solution containing radioactive cesium was atomized to generate a mist having a diameter of about 4 μm. The gas containing this mist was sucked by a dry vacuum pump and brought into contact with an adsorbent (air filter) provided in the adsorber. The gas that passed through the adsorbent was guided to a trap cooled with ice water, and the water contained in the gas was condensed and recovered as a detection liquid.
吸着材としては、本実施例のエアフィルターのほか、比較例として、本実施例のエアフィルターと同じサイズ（直径４０ｍｍ、厚さ約１０ｍｍ）に加工した、外気処理用の中性フィルターとして用いられる市販のポリエステルモダアクリル製のフィルター（比較例１）と、業務用及び家庭用エアコンのフィルターとして用いられる市販のウレタン樹脂性のフィルター（比較例２）を用いて、同条件にて試験を実施した。 As the adsorbent, in addition to the air filter of this example, as a comparative example, it is used as a neutral filter for outside air treatment processed to the same size (diameter 40 mm, thickness about 10 mm) as the air filter of this example. The test was carried out under the same conditions using a commercially available polyester mod acrylic filter (Comparative Example 1) and a commercially available urethane resin filter (Comparative Example 2) used as a filter for commercial and household air conditioners. ..
そして、試験前の検体液の放射性セシウム濃度と、試験後の検出液の放射性セシウム濃度を測定し、計算式｛（試験前検体液放射性セシウム濃度−試験後検出液放射性セシウム濃度）／試験前検体液放射性セシウム濃度｝×１００により、放射性セシウムの除去率を求めた。 Then, the radioactive cesium concentration of the sample solution before the test and the radioactive cesium concentration of the detection solution after the test are measured, and the calculation formula {(pre-test sample solution radioactive cesium concentration-post-test detection solution radioactive cesium concentration) / pre-test sample The removal rate of radioactive cesium was determined by the liquid radioactive cesium concentration} × 100.
その結果を下表に示す。比較例１、２ではほとんど放射性セシウムを除去できなかったが、実施例では、約９０％の放射性セシウムを除去することができた。 The results are shown in the table below. In Comparative Examples 1 and 2, almost no radioactive cesium could be removed, but in Examples, about 90% of the radioactive cesium could be removed.
（３）アンモニアの除去試験
製造したエアフィルターを用いて、アンモニアの除去試験を行った。試験に用いた実験装置概略図を図２に示す。
(3) Ammonia removal test An ammonia removal test was conducted using the manufactured air filter. A schematic diagram of the experimental apparatus used in the test is shown in FIG.
アンモニア検知機を備えた約７８Ｌの密閉容器中にアンモニアの気体発生源を収容し、アンモニアを発生させた。アンモニアの初期濃度は、４９．４ｐｐｍであった。このアンモニアを含む気体をドライ真空ポンプにより６Ｌ／分の吸引速度で吸引し、吸着カラム（断面積約９．６ｃｍ２、長さ約３８ｃｍ、容積約３６５ｃｍ３）に充填した吸着材（エアフィルター）（充填量１０２ｇ、充填密度約２７９ｇ／Ｌ）と面速度約１０４ｃｍ／秒で接触させた。また、気体は密閉容器と吸着カラムの間を循環させた。 A gas source of ammonia was housed in a closed container of about 78 L equipped with an ammonia detector to generate ammonia. The initial concentration of ammonia was 49.4 ppm. This gas containing ammonia is sucked by a dry vacuum pump at a suction rate of 6 L / min, and the adsorbent (air filter) is filled in an adsorption column (cross-sectional area about 9.6 cm 2 , length about 38 cm, volume about 365 cm 3 ). It was brought into contact with (filling amount 102 g, filling density about 279 g / L) at a surface speed of about 104 cm / sec. The gas was also circulated between the closed container and the adsorption column.
そして、密閉容器に設けたアンモニア検知機により、アンモニア濃度を測定した。 Then, the ammonia concentration was measured by an ammonia detector provided in a closed container.
その結果を図３〜５に示す。本実施例の吸着材（エアフィルター）は、アンモニアを除去することができた。 The results are shown in FIGS. 3 to 5. Ammonia could be removed from the adsorbent (air filter) of this example.
この結果をもとに、一般公衆トイレ（１０ｍ×５ｍ×３ｍ）の想定空間１５０ｍ３において、アンモニア除去率のシミュレーションを行った。吸着材（エアフィルター）は、断面積０．２５ｍ２、長さ２．５ｃｍ、体積６２５０ｃｍ２、重量６．２５ｋｍ（比重を１とする）と想定した。また、面速度は、公衆トイレ内の水が飛び散らない速度の２．５ｍ／秒とし、それに合わせて通気速度は０．６２５ｍ３／秒（３７５００Ｌ／分）とした。 Based on this result, a simulation of the ammonia removal rate was performed in an assumed space of 150 m 3 of a general public toilet (10 m × 5 m × 3 m). The adsorbent (air filter) was assumed to have a cross-sectional area of 0.25 m 2 , a length of 2.5 cm, a volume of 6250 cm 2 , and a weight of 6.25 km (specific gravity is 1). The surface speed was 2.5 m / sec, which is the speed at which water in the public toilet does not scatter, and the ventilation speed was 0.625 m 3 / sec (37500 L / min).
アンモニアの初期濃度を５０ｐｐｍとして計算したところ、図６に示すように数分でアンモニアの８０％以上を除去することができるという結果が得られ、本発明のエアフィルターが公衆トイレのアンモニア除去に使用可能であることが確認された。 When the initial concentration of ammonia was calculated as 50 ppm, it was found that 80% or more of ammonia could be removed in a few minutes as shown in FIG. 6, and the air filter of the present invention was used for removing ammonia in public toilets. It was confirmed that it was possible.
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