JP2017114755A - Zeolite and manufacturing method therefor - Google Patents
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本発明は、疎水性を高めたゼオライト、及びその製造方法に関する。 The present invention relates to a zeolite with improved hydrophobicity and a method for producing the same.
ゼオライトは大表面積を有するアルミノシリケ−ト多孔体であり、水分子や、アルデヒド類、ケトン類をはじめとする低分子量の有機物吸着性能に優れている。ゼオライトの吸着特性はＳｉＯ2／Ａｌ2Ｏ3モル比に依存し、低ＳｉＯ2／Ａｌ2Ｏ3モル比を有するゼオライトは、強い親水性を示すため、エアコンや冷蔵庫等の除湿剤として工業的にも多用されている。一方で高ＳｉＯ2／Ａｌ2Ｏ3モル比を有するゼオライトは、比較的疎水性を示すため、有機溶剤やアルデヒド等の有害有機物除去剤として、ハニカムロータやフィルタ等に用いられている。しかしながら、水の共存下で有機物質を効率的に吸着させるためには、ゼオライトの吸水能力をできる限り低くしなければならない。 Zeolite is an aluminosilicate porous material having a large surface area, and is excellent in the adsorption performance of low molecular weight organic substances such as water molecules, aldehydes and ketones. Adsorption properties of the zeolite depends on the SiO 2 / Al 2 O 3 molar ratio, the zeolite having a low SiO 2 / Al 2 O 3 molar ratio, in order to show a strongly hydrophilic, industrial as dehumidifying agent such as air conditioners and refrigerators Is also frequently used. On the other hand, zeolite having a high SiO 2 / Al 2 O 3 molar ratio is relatively hydrophobic, and is therefore used in honeycomb rotors, filters, and the like as a removal agent for harmful organic substances such as organic solvents and aldehydes. However, in order to efficiently adsorb organic substances in the presence of water, the water absorption capacity of zeolite must be as low as possible.
シリカやゼオライト等の多孔性物質に対する更なる疎水化処理としては、例えば疎水性シリカをトリメチルエトキシシラン［Ｍｅ3−Ｓｉ−ＯＥｔ］（例えば、特許文献１）や、ヘキサメチルジシラザン［Ｍｅ3Ｓｉ−ＮＨ−ＳｉＭｅ3］（例えば、特許文献２）などの有機シリル化剤で処理する方法、あるいはゼオライトにポリビニルアルコールを塗付したのち、不活性ガス流通下で加熱して炭化処理を施す方法（例えば、特許文献３）等の技術が知られている。 As a further hydrophobizing treatment for porous materials such as silica and zeolite, for example, hydrophobic silica is trimethylethoxysilane [Me 3 -Si-OEt] (for example, Patent Document 1) or hexamethyldisilazane [Me 3 Si. A method of treating with an organic silylating agent such as —NH—SiMe 3 ] (for example, Patent Document 2), or a method of applying carbonization treatment by applying polyvinyl alcohol to zeolite and then heating under an inert gas flow ( For example, a technique such as Patent Document 3) is known.
ゼオライトに対する疎水化処理方法として、前述したように種々の技術が開示又は報告されているが、これらの技術においては、試薬が高価であったり、有機溶媒を必要とするために製造工程や残液処理工程が煩雑であったり、表面が有機物で被覆されているために耐熱性に劣るなど、工業的な実用化には依然として課題が多い。
本発明は、簡便な処理によりＭＦＩ型のゼオライトの疎水性を高めたゼオライト及びその製造方法を提供することを課題とする。
As described above, various techniques have been disclosed or reported as hydrophobizing treatment methods for zeolite. However, in these techniques, a reagent is expensive or an organic solvent is required, so that a manufacturing process or residual liquid is used. There are still many problems in industrial practical use such as complicated processing steps and inferior heat resistance because the surface is coated with organic matter.
An object of the present invention is to provide a zeolite in which the hydrophobicity of MFI-type zeolite is increased by a simple treatment and a method for producing the same.
本発明者は、熱的な変性を受けにくいＭＦＩ型のゼオライトにおいて、当該ゼオライトを高温で熱処理することで、ゼオライトの疎水性が高められることを見出した。
すなわち本発明は、下記の〔１〕及び〔２〕に関する。
〔１〕ＳｉＯ2／Ａｌ2Ｏ3モル比１００〜１５００のＭＦＩ型ゼオライトを５００〜９００℃の温度で焼成して得られる、ゼオライト。
〔２〕ＳｉＯ2／Ａｌ2Ｏ3モル比１００〜１５００のＭＦＩ型ゼオライトを５００〜９００℃の温度で焼成する工程を有するゼオライトの製造方法。
The present inventor has found that the hydrophobicity of the zeolite can be increased by heat-treating the zeolite at a high temperature in the MFI type zeolite which is not easily subjected to thermal modification.
That is, the present invention relates to the following [1] and [2].
[1] A zeolite obtained by calcining MFI type zeolite having a SiO 2 / Al 2 O 3 molar ratio of 100 to 1500 at a temperature of 500 to 900 ° C.
[2] A method for producing a zeolite comprising a step of calcining an MFI type zeolite having a SiO 2 / Al 2 O 3 molar ratio of 100 to 1500 at a temperature of 500 to 900 ° C.
本発明によれば、簡便な処理により疎水性を高めたゼオライト及びその製造方法を提供することができる。 According to the present invention, it is possible to provide a zeolite having improved hydrophobicity by a simple treatment and a method for producing the same.
本発明のゼオライトは、ＳｉＯ2／Ａｌ2Ｏ3モル比１００〜１５００のＭＦＩ型ゼオライトを５００〜９００℃の温度で焼成して得られる。このように、簡便な処理により疎水性を高めたゼオライトが得られる。 The zeolite of the present invention can be obtained by calcining MFI type zeolite having a SiO 2 / Al 2 O 3 molar ratio of 100 to 1500 at a temperature of 500 to 900 ° C. Thus, a zeolite with improved hydrophobicity can be obtained by a simple treatment.
本明細書において、上記の工程を経て得られた疎水性が高められたゼオライトを「疎水化ＭＦＩ型ゼオライト」と称する。疎水化ＭＦＩ型ゼオライトは、同一のＳｉＯ2／Ａｌ2Ｏ3モル比のＭＦＩ型ゼオライトにおいて、未処理のＭＦＩ型ゼオライトと比較して、高いｎＣ４／Ｈ2Ｏ吸着選択比を示すＭＦＩ型ゼオライトを意味する。
未処理のＭＦＩ型ゼオライトｎＣ４／Ｈ2Ｏ吸着選択比（Ｓｃ）に対する疎水化ＭＦＩ型ゼオライトのｎＣ４／Ｈ2Ｏ吸着選択比（Ｓｅ）の向上率｛〔（Ｓｅ−Ｓｃ）／Ｓc〕×１００｝（％）は、特に限定されないが、好ましくは１％以上、より好ましくは３％以上、更に好ましくは５％以上、更に好ましくは８％以上、更に好ましくは１２％以上、更に好ましくは１５％以上である。当該向上率｛〔（Ｓｅ−Ｓｃ）／Ｓc〕×１００｝（％）は、その上限は特に限定されないが、例えば、３０％以下である。
ｎＣ４／Ｈ2Ｏ吸着選択比は、実施例に記載の測定方法による。
In the present specification, the zeolite having increased hydrophobicity obtained through the above-described steps is referred to as “hydrophobized MFI type zeolite”. Hydrophobized MFI-type zeolite is an MFI-type zeolite having a high nC4 / H 2 O adsorption selectivity ratio compared with untreated MFI-type zeolite in the same SiO 2 / Al 2 O 3 molar ratio MFI-type zeolite. means.
Improvement rate of nC4 / H 2 O adsorption selection ratio (S e ) of hydrophobized MFI type zeolite relative to untreated MFI type zeolite nC4 / H 2 O adsorption selection ratio (S c ) {[(S e -S c ) / S c ] × 100} (%) is not particularly limited, but is preferably 1% or more, more preferably 3% or more, still more preferably 5% or more, still more preferably 8% or more, still more preferably 12% or more, More preferably, it is 15% or more. The upper limit of the improvement rate {[(S e −S c ) / S c ] × 100} (%) is not particularly limited, but is, for example, 30% or less.
The nC4 / H 2 O adsorption selection ratio is based on the measurement method described in the examples.
ＭＦＩ型ゼオライトは、国際ゼオライト学会（International Zeolite Association）により付与されている構造コードＭＦＩの幾何構造を有するゼオライトである。
ＭＦＩ型ゼオライトのＳｉＯ2／Ａｌ2Ｏ3モル比は、１００〜１５００であり、より好ましくは２００〜１０００、更に好ましくは２５０〜６００、更に好ましくは３００〜４００である。
ＭＦＩ型ゼオライトの市販品としては、東ソー株式会社製、商品名「HSZ-800」が挙げられる。
The MFI-type zeolite is a zeolite having the geometric structure of the structure code MFI given by the International Zeolite Association.
SiO 2 / Al 2 O 3 molar ratio of MFI-type zeolite is from 100 to 1500, more preferably 200 to 1000, more preferably 250 to 600, more preferably from 300 to 400.
As a commercial product of MFI type zeolite, the product name “HSZ-800” manufactured by Tosoh Corporation may be mentioned.
以下、本発明の疎水化ＭＦＩ型ゼオライトの製造方法について説明する。
本発明のゼオライトの製造方法は、ＳｉＯ2／Ａｌ2Ｏ3モル比１００〜１５００のＭＦＩ型ゼオライトを５００〜９００℃の温度で焼成する工程を有する
焼成の温度は、疎水化ＭＦＩ型ゼオライトの疎水性を高める観点から、５００〜９００℃であり、好ましくは５５０〜８００℃、より好ましくは６００〜７００℃、更に好ましくは６３０〜６８０℃である。
焼成時間は、疎水化ＭＦＩ型ゼオライトの疎水性を高める観点から、好ましくは３０分〜６０分、より好ましくは３５分〜５０分、更に好ましくは３５〜４５分である。
Hereinafter, a method for producing the hydrophobized MFI zeolite of the present invention will be described.
The method for producing a zeolite of the present invention includes a step of calcining MFI type zeolite having a SiO 2 / Al 2 O 3 molar ratio of 100 to 1500 at a temperature of 500 to 900 ° C. The calcining temperature is the hydrophobicity of the hydrophobized MFI type zeolite. From the viewpoint of enhancing the properties, the temperature is 500 to 900 ° C, preferably 550 to 800 ° C, more preferably 600 to 700 ° C, and still more preferably 630 to 680 ° C.
The firing time is preferably 30 minutes to 60 minutes, more preferably 35 minutes to 50 minutes, and even more preferably 35 to 45 minutes, from the viewpoint of increasing the hydrophobicity of the hydrophobized MFI zeolite.
焼成の雰囲気は、窒素、アルゴンなどの不活性ガス雰囲気下であっても、空気中であってもよい。
焼成の雰囲気は、疎水化ＭＦＩ型ゼオライトの疎水性を高める観点から、加湿雰囲気であることが好ましい。
加湿雰囲気としては、例えば、その湿度レベルは１〜３０ｇ／ｍ3である。
加湿雰囲気は、ガスを水中でバブリングしてゼオライトを焼成するオーブンの中に導入すること行うことができる。
The firing atmosphere may be in an inert gas atmosphere such as nitrogen or argon, or in air.
The firing atmosphere is preferably a humidified atmosphere from the viewpoint of increasing the hydrophobicity of the hydrophobized MFI-type zeolite.
As the humidified atmosphere, for example, the humidity level is 1 to 30 g / m 3 .
The humidified atmosphere can be introduced by bubbling a gas in water and introducing it into an oven for firing the zeolite.
本発明の製造方法により得られる疎水化ＭＦＩ型ゼオライトは、疎水性が高められるため、水分の存在下での有機物の吸着に好ましく用いられ、より具体的には、好ましくは空気中の有機物の吸着に好ましく用いられる。
本発明の疎水化ＭＦＩ型ゼオライトは、より具体的には、脱臭剤等に用いられる。
Hydrophobized MFI-type zeolite obtained by the production method of the present invention is preferably used for the adsorption of organic substances in the presence of moisture, and more specifically, preferably adsorbs organic substances in air, because the hydrophobicity is enhanced. Is preferably used.
More specifically, the hydrophobized MFI type zeolite of the present invention is used as a deodorizing agent or the like.
次に、本発明を実施例により、さらに詳細に説明するが、本発明は、これらの例によってなんら限定されるものではない。
本実施例において、評価は以下の方法で行った。
EXAMPLES Next, although an Example demonstrates this invention further in detail, this invention is not limited at all by these examples.
In this example, evaluation was performed by the following method.
〔吸着容量及びｎＣ４／Ｈ2Ｏ吸着選択比〕
マクベインベーカーバランス法により以下に示す条件により、水蒸気（Ｈ2Ｏ）及びノルマルブタン（ｎＣ４）の吸着試験をそれぞれ別々に行い、ｎＣ４／Ｈ2Ｏ吸着選択比を［ｎＣ４の吸着量（質量％）／Ｈ2Ｏの吸着量（質量％）］から求めた。
・前処理条件：７０３Ｋ、２時間真空排気
・測定条件：２５℃
・Ｈ２Ｏ圧力：３．１ｋＰａ
・ｎＣ４圧力：３３．３ｋＰａ
[Adsorption capacity and nC4 / H 2 O adsorption selection ratio]
The adsorption test of water vapor (H 2 O) and normal butane (nC4) was conducted separately under the conditions shown below by the McBain Baker balance method, and the nC4 / H 2 O adsorption selection ratio was set to [nC4 adsorption amount (mass%). / H 2 O adsorption amount (% by mass)].
・ Pretreatment conditions: 703K, evacuation for 2 hours ・ Measurement conditions: 25 ° C.
・ H 2 O pressure: 3.1 kPa
NC4 pressure: 33.3 kPa
実施例１
ＭＦＩ型ゼオライト（ＳｉＯ2／Ａｌ2Ｏ3モル比＝３３０）を水中でバブリングした空気を導入したオーブン中で、６５０℃で４０分間焼成した。得られたゼオライトの各種物質の吸着容量を評価して、表１に示した。
Example 1
MFI-type zeolite (SiO 2 / Al 2 O 3 molar ratio = 330) was calcined at 650 ° C. for 40 minutes in an oven introduced with air bubbled in water. The adsorption capacity of various substances of the obtained zeolite was evaluated and shown in Table 1.
実施例２
オーブンに対して、水中でバブリングをせずに、空気を導入した以外は実施例１と同様の条件で、ＭＦＩ型ゼオライトを焼成した。得られたゼオライトの各種物質の吸着容量を評価して表１に示した。
Example 2
The MFI-type zeolite was calcined under the same conditions as in Example 1 except that air was introduced into the oven without bubbling in water. The adsorption capacities of various substances in the obtained zeolite were evaluated and shown in Table 1.
実施例３
ＭＦＩ型ゼオライト（ＳｉＯ2／Ａｌ2Ｏ3モル比＝１０００）を水中でバブリングした空気を導入したオーブン中で、６５０℃で４０分間焼成した。得られたゼオライトの各種物質の吸着容量を評価して表１に示した。
Example 3
MFI-type zeolite (SiO 2 / Al 2 O 3 molar ratio = 1000) was calcined at 650 ° C. for 40 minutes in an oven introduced with air bubbled in water. The adsorption capacities of various substances in the obtained zeolite were evaluated and shown in Table 1.
実施例４
オーブンに対して、水中でバブリングをせずに、空気を導入した以外は実施例３と同様の条件で、ＭＦＩ型ゼオライトを焼成した。得られたゼオライトの各種物質の吸着容量を評価して表１に示した。
Example 4
The MFI zeolite was calcined under the same conditions as in Example 3 except that air was introduced into the oven without bubbling in water. The adsorption capacities of various substances in the obtained zeolite were evaluated and shown in Table 1.
比較例１、２
表１に示すＳｉＯ2／Ａｌ2Ｏ3モル比を有するＭＦＩ型ゼオライトを、加熱処理を行わず、各種物質の吸着容量を評価して、表１に示した。
Comparative Examples 1 and 2
Table 1 shows the MFI-type zeolite having the SiO 2 / Al 2 O 3 molar ratio shown in Table 1 without evaluating the adsorption capacity of various substances.
以上、実施例２と比較例１との対比から、ＭＦＩ型のゼオライトを焼成することで疎水性が高められることが理解できる。これらのnC4/H2O選択比の結果から、当該焼成によって、SiO2/Al2O3比を3倍程度に高めた場合（比較例２参照）と同等の疎水性向上効果が得られると理解できる。
実施例１と比較例１との対比から、ＭＦＩ型のゼオライトを、加湿雰囲気下で焼成することでより顕著に疎水性が高められることが理解できる。これらのnC4/H2O選択比の結果から、当該焼成によって、シリカアルミナ比を3倍程度に高めた場合よりも、優れた疎水性向上効果が得られると理解できる。加湿雰囲気とすることで、水分存在下での焼成となるので、むしろ親水性が高まりそうであるところ、疎水性が高まり、その疎水性向上効果が実施例２に示される非加湿の雰囲気下での焼成で得られる効果よりも、顕著であることは予想外である。
SiO2/Al2O3比を1000にまで高めた場合であっても、実施例３及び４と比較例２との対比から、ゼオライトの疎水性が高められると理解できる。
以上、実施例及び比較例の結果から、ＳｉＯ2／Ａｌ2Ｏ3モル比１００〜１５００のＭＦＩ型ゼオライトを焼成することで疎水性を高めたゼオライトが得られるといえる。
As described above, it can be understood from the comparison between Example 2 and Comparative Example 1 that the hydrophobicity is increased by calcining the MFI-type zeolite. From the results of these nC4 / H 2 O selection ratios, it is possible to obtain the same hydrophobicity improvement effect as that obtained when the SiO 2 / Al 2 O 3 ratio is increased about 3 times by the firing (see Comparative Example 2). Understandable.
From the comparison between Example 1 and Comparative Example 1, it can be understood that the hydrophobicity is remarkably increased by calcining MFI-type zeolite in a humidified atmosphere. From the results of these nC4 / H 2 O selection ratios, it can be understood that the effect of improving the hydrophobicity can be obtained by the firing more than when the silica-alumina ratio is increased about 3 times. Since it becomes firing in the presence of moisture by making the humidified atmosphere, the hydrophobicity is likely to increase rather, the hydrophobicity is increased, and the hydrophobicity improving effect is obtained in the non-humidified atmosphere shown in Example 2. It is unexpected that it is more remarkable than the effect obtained by firing.
Even when the SiO 2 / Al 2 O 3 ratio is increased to 1000, it can be understood from the comparison between Examples 3 and 4 and Comparative Example 2 that the hydrophobicity of the zeolite is increased.
As mentioned above, it can be said from the results of Examples and Comparative Examples that a zeolite having improved hydrophobicity can be obtained by calcining MFI type zeolite having a SiO 2 / Al 2 O 3 molar ratio of 100 to 1500.
本発明の製造方法により得られる疎水化ＭＦＩ型ゼオライトは、疎水性が高められ、水分の存在下での有機物の吸着に好ましく用いられ、より具体的には、脱臭剤等に応用できる。 Hydrophobized MFI-type zeolite obtained by the production method of the present invention has increased hydrophobicity and is preferably used for adsorption of organic substances in the presence of moisture, and more specifically, can be applied to deodorizers and the like.
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