JP2011183352A - Method for producing composite particle of natural zeolite and titanium dioxide - Google Patents
Method for producing composite particle of natural zeolite and titanium dioxide Download PDFInfo
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- JP2011183352A JP2011183352A JP2010053932A JP2010053932A JP2011183352A JP 2011183352 A JP2011183352 A JP 2011183352A JP 2010053932 A JP2010053932 A JP 2010053932A JP 2010053932 A JP2010053932 A JP 2010053932A JP 2011183352 A JP2011183352 A JP 2011183352A
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- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 62
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000010457 zeolite Substances 0.000 title claims abstract description 62
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000011246 composite particle Substances 0.000 title claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 title claims 4
- 239000004408 titanium dioxide Substances 0.000 title abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 239000000725 suspension Substances 0.000 abstract description 2
- 150000001768 cations Chemical class 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 150000002894 organic compounds Chemical class 0.000 abstract 1
- 231100000167 toxic agent Toxicity 0.000 abstract 1
- 239000003440 toxic substance Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 230000001877 deodorizing effect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000019645 odor Nutrition 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- UPZFLZYXYGBAPL-UHFFFAOYSA-N 2-ethyl-2-methyl-1,3-dioxolane Chemical compound CCC1(C)OCCO1 UPZFLZYXYGBAPL-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 229910001579 aluminosilicate mineral Inorganic materials 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010800 human waste Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000008262 pumice Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
Description
本発明は、バインダーを用いないで天然ゼオライト破砕物の表面に二酸化チタン層を形成させた複合粒子に関る。また、この発明は当該複合粒子が吸着能を有する光触媒に関るものである。 The present invention relates to composite particles in which a titanium dioxide layer is formed on the surface of a crushed natural zeolite without using a binder. The present invention also relates to a photocatalyst in which the composite particles have an adsorption ability.
天然ゼオライトはアルミノ珪酸塩系の鉱物であり、イオン交換能、吸着能、分子節能、触媒能など各種の優れた機能を持つ物質である。この優れたゼオライトの特性を活かし、さらに他の機能性材料との複合化を図ることにより高付加価値化することが望まれている。 Natural zeolite is an aluminosilicate mineral and is a substance having various excellent functions such as ion exchange capacity, adsorption capacity, molecular capacity and catalytic capacity. It is desired to increase the added value by taking advantage of the characteristics of this excellent zeolite and further compositing with other functional materials.
天然ゼオライトと光触媒機能を有する酸化チタンを結合して複合化する方法としては、
バインダ−含有溶液中に天然ゼオライト粉砕物と酸化チタン粉末を加えて得られるスラリーを噴霧乾燥によって造粒して複合材を製造する方法が特許文献１に記載されている。
As a method of combining and combining natural zeolite and titanium oxide having a photocatalytic function,
Patent Document 1 discloses a method of producing a composite material by granulating a slurry obtained by adding a pulverized natural zeolite and titanium oxide powder into a binder-containing solution by spray drying.
また、軽石、バーミキュライト、シリカゲル等の粉状物の表面に、ゼオライト系鉱物、酸化チタン、酸化亜鉛、白金等の金属酸化物など、複数種類配合した脱臭・抗菌剤に、アクリル系樹脂、酢酸ビニル系樹脂、エチレン酢酸等およびＰＶＡ溶液、ＣＭＣ溶液、澱粉等の接着補助剤を配合してなる脱臭・抗菌溶液を添着加工する方法が特許文献２に記載されている。 In addition, deodorizing and antibacterial agents, such as zeolitic minerals, titanium oxide, zinc oxide, and metal oxides such as platinum on the surface of powdered materials such as pumice, vermiculite, and silica gel, acrylic resins, vinyl acetate Patent Document 2 describes a method of attaching a deodorizing / antibacterial solution formed by blending a resin-based resin, ethylene acetic acid or the like and an adhesion assistant such as PVA solution, CMC solution, starch or the like.
また、天然ゼオライトを含む無機系多孔性吸着剤に無機系光分解剤（アナターゼ型酸化チタン）を配合し、ハイブリッド型ミネラル吸着除去材を得る方法（機能性材料の混合法）が特許文献３に記載されている。 Patent Document 3 discloses a method (mixing method of functional materials) in which a hybrid mineral adsorbing and removing material is blended with an inorganic photodecomposition agent (anatase type titanium oxide) in an inorganic porous adsorbent containing natural zeolite. Are listed.
更に、金属の水酸化物及び金属の酸化物の少なくとも一方を主成分とする脱臭成分と、無機材料からなる調湿成分とを混合粉砕法により混合し、焼成することによって成形体を作製し、４０〜１２０℃での乾燥又は９００℃以下での焼成を行う方法が特許文献４に記載されている。 Furthermore, a deodorizing component containing at least one of a metal hydroxide and a metal oxide as a main component and a humidity control component made of an inorganic material are mixed by a mixed pulverization method, and fired to produce a molded body. Patent Document 4 describes a method of drying at 40 to 120 ° C. or baking at 900 ° C. or lower.
この他に天然ゼオライトの表面に酸化チタンをバインダ−を用いて塗布するもの、天然ゼオライト粉末と酸化チタン粉末を混合した造粒物が知られている。 In addition to this, a product obtained by applying titanium oxide to the surface of natural zeolite using a binder, and a granulated product obtained by mixing natural zeolite powder and titanium oxide powder are known.
工場，し尿処理場，ごみ処理場，家畜飼育場などの種々の施設から発生する悪臭物質以外にも日常の生活環境においても悪臭が発生することがある、これらは人間の健康を害する恐れがある例もある、また、有害でなくても人によっては不快感を受けたりストレスを感じたりする場合がある。 In addition to malodorous substances generated from various facilities such as factories, human waste treatment plants, garbage disposal plants, and livestock breeding facilities, odors may be generated in daily living environments, which may harm human health. There are examples, and some people may feel uncomfortable or stressed even if they are not harmful.
悪臭等を除去，低減するために、活性炭やゼオライト等の多孔性物質に悪臭を吸着させて除去する方法か用いられてきたが、一定の量を吸収すると飽和状態になり、それ以上は吸収しなくなることが問題である。 In order to remove and reduce malodor, etc., a method of adsorbing and removing malodor on porous materials such as activated carbon and zeolite has been used. However, when a certain amount is absorbed, it becomes saturated and more than that is absorbed. It is a problem to disappear.
天然ゼオライトと酸化チタンを複合させた粒子で悪臭物質を吸着させて、それを紫外線照射の励起による酸化チタンの光触媒作用によって分解させ、悪臭物質の吸着が飽和状態になることなく、長期期間にわたり悪臭物質を除去、削減させる複合粒子の提供を課題とする。 Malodorous substances are adsorbed with particles made of a composite of natural zeolite and titanium oxide, and decomposed by the photocatalytic action of titanium oxide by excitation with ultraviolet irradiation, and the malodorous substances are not saturated and become malodored over a long period of time. It is an object to provide composite particles that remove and reduce substances.
本発明は、天然ゼオライト粉砕物を酸化チタン懸濁液に付けた後、それを乾燥、焼成して天然ゼオライトの表面に酸化チタン層を形成させた複合粒子で、吸着能、イオン交換能、光触媒機能を有する複合粒子。 The present invention is a composite particle in which a pulverized natural zeolite is applied to a titanium oxide suspension and then dried and fired to form a titanium oxide layer on the surface of the natural zeolite. Composite particles having a function.
本発明は、天然ゼオライト粉砕物、破砕物の表面に光触媒機能を有する酸化チタンをバインダ−を使用することなく、また造粒作業を要せず、焼き付けすることにより高付加価値化を目指したものであり、前記の特許文献等の内容とは全く異なる。 The present invention aims to increase the added value by baking titanium oxide having a photocatalytic function on the surface of pulverized natural zeolite and crushed material without using a binder and without granulating work. And completely different from the contents of the above-mentioned patent documents.
以下、本発明の実施形態を図１〜５に基づいて説明する。
酸化チタンゾルをマグネットスタラ−、あるいは超音波発生装置で撹拌、分散させ調製した０．０５ｗｔ％〜１．０ｗｔ％溶液の中に、常温〜１００℃で乾燥した粒径１〜１０ｍｍに破砕した天然ゼオライトを投入して、室温〜１００℃で乾燥させてゼオライトの表面に酸化チタンゾルを均一に沈積させる。
Hereinafter, embodiments of the present invention will be described with reference to FIGS.
Natural zeolite crushed to a particle size of 1 to 10 mm dried at room temperature to 100 ° C. in a 0.05 wt% to 1.0 wt% solution prepared by stirring and dispersing titanium oxide sol with a magnetic stirrer or ultrasonic generator And dried at room temperature to 100 ° C. to uniformly deposit the titanium oxide sol on the surface of the zeolite.
酸化チタンゾルが沈積させた粒径１〜１０ｍｍの天然ゼオライトを電気炉で５００℃〜８００℃で熱処理して酸化チタンをゼオライト表面に焼付け、ゼオライト表面に酸化チタン層を形成させる。 A natural zeolite having a particle diameter of 1 to 10 mm deposited with a titanium oxide sol is heat-treated in an electric furnace at 500 ° C. to 800 ° C., and titanium oxide is baked on the zeolite surface to form a titanium oxide layer on the zeolite surface.
なお、乾燥ゼオライトの代わりに５００℃〜８００℃で予め仮焼したゼオライトを用いて、酸化チタンゾルを沈積させたものを再度５００℃〜８００℃で熱処理してもよい。 In addition, you may heat-process again what made the titanium oxide sol deposit using the zeolite calcined beforehand at 500 to 800 degreeC instead of dry zeolite at 500 to 800 degreeC.
ゼオライトは活性炭と比較して極性ガスを吸着しやすいという特徴がある、さらに天然ゼオライトはブロードな細孔分布を持ち吸着速度の速さと吸着物質の選択幅が広いと云う吸着特性を持つため、悪臭、悪臭物質をよく吸着する。ゼオライト表面に層状で付着している二酸化チタンは、紫外線で励起されゼオライトに吸着された悪臭、悪臭物質を分解させ、吸着と分解が逐次連続するため、ゼオライトは悪臭、悪臭物質によって飽和状態になることはない。 Zeolite is characterized by its ability to adsorb polar gases more easily than activated carbon. Furthermore, natural zeolite has a broad pore distribution and adsorption characteristics such as high adsorption speed and wide selection of adsorbents. Adsorbs bad odor substances well. Titanium dioxide adhering in a layered manner on the zeolite surface decomposes malodorous and malodorous substances adsorbed on the zeolite excited by ultraviolet rays, and the adsorption and decomposition are successively performed. Therefore, the zeolite becomes saturated by the malodorous and malodorous substances. There is nothing.
本発明に用いる天然ゼオライトとしては、島根県内に産するモルディナイトが好ましく表１、図１で示すような特性である。
本発明に用いる酸化チタンとしては、アナタ−ゼ型ゾルが好ましい。 The titanium oxide used in the present invention is preferably an anatase sol.
０．０５ｗｔ％〜１．０ｗｔ％に調製した酸化チタンゾル溶液中に、常温〜１００℃で乾燥した粒径１〜１０ｍｍのゼオライトを酸化チタンゾルの重量１に対して０．５〜２の割合で投入して撹拌した後、溶液中に１０時間以上、室温〜１００℃で静置し乾燥させる。乾燥した試料を電気炉又はガス炉を用いて５００℃〜８００℃の酸化雰囲気中で熱処理して、酸化チタンを焼付け、ゼオライト表面に酸化チタン層を形成させる。 Into a titanium oxide sol solution prepared to 0.05 wt% to 1.0 wt%, zeolite having a particle diameter of 1 to 10 mm dried at room temperature to 100 ° C is added at a ratio of 0.5 to 2 with respect to the weight 1 of the titanium oxide sol. Then, the mixture is allowed to stand in the solution for 10 hours or more at room temperature to 100 ° C. and dried. The dried sample is heat-treated in an oxidizing atmosphere of 500 ° C. to 800 ° C. using an electric furnace or a gas furnace, and titanium oxide is baked to form a titanium oxide layer on the zeolite surface.
０．０５〜１．０ｗｔ％の酸化チタンゾル中で酸化チタンを沈積させたゼオライトを電気炉で６００℃、８００℃の酸化雰囲気中で熱処理した。酸化チタン沈積ゼオライト、６００℃熱処理物（１０℃／ｍｉｎ、１ｈｒ維持）、８００℃（１０℃／ｍｉｎ、１ｈｒ維持）のＸ線回折線図を図１に、濃度の異なる酸化チタンゾル溶液で処理した酸化チタン沈積ゼオライトのＳＥＭ観察結果の電子顕微鏡の写真を図２に、ゼオライト表面に形成されたチタン層のＳＥＭ観察結果の電子顕微鏡の写真を図３に示す。イオン交換容量の変化を示すグラフを図４に示す。なお、８００℃の酸化雰囲気中で熱処理してもゼオライトの結晶の崩壊は認められない。 The zeolite in which titanium oxide was deposited in a 0.05 to 1.0 wt% titanium oxide sol was heat-treated in an oxidizing atmosphere at 600 ° C. and 800 ° C. in an electric furnace. X-ray diffraction diagrams of titanium oxide deposited zeolite, 600 ° C. heat-treated product (10 ° C./min, 1 hr maintenance), 800 ° C. (10 ° C./min, 1 hr maintenance) are treated with titanium oxide sol solutions having different concentrations in FIG. An electron microscope photograph of the SEM observation result of the titanium oxide deposited zeolite is shown in FIG. 2, and an electron microscope photograph of the SEM observation result of the titanium layer formed on the zeolite surface is shown in FIG. A graph showing changes in ion exchange capacity is shown in FIG. In addition, even if heat treatment is performed in an oxidizing atmosphere at 800 ° C., no collapse of the zeolite crystals is observed.
実施例１で得た酸化チタン焼付けゼオライトを用いてＮＯｘの分解試験を行った。
（実験条件）
セルの中に酸化チタン焼付けゼオライトを２５ｇ入れ、そこに１０ｐｐｍのＮＯｘガスを満たし、内部からＵＶランプ（１０Ｗ）を１分間照射して、ＮＯｘガス濃度の変化を測定した、その結果を図５に示す。０．２５ｇのＴｉＯ２がついた仕様はＮＯｘの分解率８９％であった。なお、ＮＯｘガスの分解率は下記の計算式を用いた。
(Experimental conditions)
Twenty-five grams of titanium oxide-baked zeolite was placed in the cell, filled with 10 ppm of NOx gas, irradiated with a UV lamp (10 W) for 1 minute from the inside, and the change in NOx gas concentration was measured. The result is shown in FIG. Show. The specification with 0.25 g of TiO 2 had a NOx decomposition rate of 89%. The following calculation formula was used for the decomposition rate of NOx gas.
本発明は、これまでに発表された酸化チタン・ゼオライト複合粒子に比較して、バインダ−を使用せず、造粒と言う厄介な工程を必要としないため、低コストで簡単に製造でき、また、吸着能、イオン交換能、光触媒機能を十分に発揮できる、室内や車内の脱臭、有害物質の分解、河川水や排水中の有機物や有害生物の分解など、様々な方面で展開が期待出来る。 Since the present invention does not use a binder and does not require a troublesome process of granulation as compared with the previously disclosed titanium oxide / zeolite composite particles, it can be easily manufactured at low cost. It can be expected to develop in various fields, such as deodorization indoors and cars, decomposition of harmful substances, decomposition of organic substances and pests in river water and wastewater, etc., which can fully exhibit adsorption capacity, ion exchange capacity and photocatalytic function.
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| US9290394B2 (en) | 2012-01-26 | 2016-03-22 | Panasonic Intellectual Property Management Co., Ltd. | Method for decomposing organic compound contained in aqueous solution |
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| US9290394B2 (en) | 2012-01-26 | 2016-03-22 | Panasonic Intellectual Property Management Co., Ltd. | Method for decomposing organic compound contained in aqueous solution |
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