JP5189727B2 - Method for producing metal oxide nanocapsules - Google Patents
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- JP5189727B2 JP5189727B2 JP2005150753A JP2005150753A JP5189727B2 JP 5189727 B2 JP5189727 B2 JP 5189727B2 JP 2005150753 A JP2005150753 A JP 2005150753A JP 2005150753 A JP2005150753 A JP 2005150753A JP 5189727 B2 JP5189727 B2 JP 5189727B2
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- 229910044991 metal oxide Inorganic materials 0.000 title claims description 31
- 150000004706 metal oxides Chemical class 0.000 title claims description 31
- 239000002088 nanocapsule Substances 0.000 title claims description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000003093 cationic surfactant Substances 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 239000012702 metal oxide precursor Substances 0.000 claims description 15
- 239000003945 anionic surfactant Substances 0.000 claims description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- -1 alkane sulfonates Chemical class 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical class OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 claims description 2
- 235000021317 phosphate Nutrition 0.000 claims description 2
- 150000003871 sulfonates Chemical class 0.000 claims description 2
- 239000004711 α-olefin Substances 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims 2
- 150000004703 alkoxides Chemical class 0.000 claims 1
- 230000001678 irradiating effect Effects 0.000 claims 1
- CENHPXAQKISCGD-UHFFFAOYSA-N trioxathietane 4,4-dioxide Chemical compound O=S1(=O)OOO1 CENHPXAQKISCGD-UHFFFAOYSA-N 0.000 claims 1
- 239000000047 product Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- XRWMGCFJVKDVMD-UHFFFAOYSA-M didodecyl(dimethyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCC XRWMGCFJVKDVMD-UHFFFAOYSA-M 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 229940067741 sodium octyl sulfate Drugs 0.000 description 6
- WFRKJMRGXGWHBM-UHFFFAOYSA-M sodium;octyl sulfate Chemical compound [Na+].CCCCCCCCOS([O-])(=O)=O WFRKJMRGXGWHBM-UHFFFAOYSA-M 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000002775 capsule Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 3
- 239000002537 cosmetic Substances 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- SWSFKKWJEHRFFP-UHFFFAOYSA-N dihexadecyl(dimethyl)azanium Chemical class CCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCC SWSFKKWJEHRFFP-UHFFFAOYSA-N 0.000 description 1
- VIXPKJNAOIWFMW-UHFFFAOYSA-M dihexadecyl(dimethyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCC VIXPKJNAOIWFMW-UHFFFAOYSA-M 0.000 description 1
- OGQYPPBGSLZBEG-UHFFFAOYSA-N dimethyl(dioctadecyl)azanium Chemical class CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC OGQYPPBGSLZBEG-UHFFFAOYSA-N 0.000 description 1
- PSLWZOIUBRXAQW-UHFFFAOYSA-M dimethyl(dioctadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC PSLWZOIUBRXAQW-UHFFFAOYSA-M 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000007332 vesicle formation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Oxygen, Ozone, And Oxides In General (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Silicon Compounds (AREA)
Description
本発明は、金属酸化物ナノカプセルの製造方法に関し、更に詳細には、界面活性剤により形成されるベシクルを鋳型とする金属酸化物ナノカプセルの製造方法に関する。 The present invention relates to a method for producing metal oxide nanocapsules, and more particularly to a method for producing metal oxide nanocapsules using a vesicle formed of a surfactant as a template.
近年、界面活性剤が形成する分子集合体を鋳型として用い、メソポーラス金属酸化物を合成する方法が報告された（非特許文献１）。このような、メソポーラス金属酸化物は、高比表面積であり、均一な細孔を有するため、触媒担体、香粧品等、多岐にわたる分野での利用が期待されている。 In recent years, a method for synthesizing mesoporous metal oxides using a molecular assembly formed by a surfactant as a template has been reported (Non-patent Document 1). Such a mesoporous metal oxide has a high specific surface area and uniform pores, so that it is expected to be used in various fields such as a catalyst carrier and cosmetics.
しかしながら、上記の方法で得られたメソポーラス金属酸化物の形状は、鋳型である界面活性剤が形成する分子集合体の形状に依存するため、使用目的によってはその効果を十分に得ることができないという問題もあった。 However, since the shape of the mesoporous metal oxide obtained by the above method depends on the shape of the molecular assembly formed by the surfactant as a template, the effect cannot be sufficiently obtained depending on the purpose of use. There was also a problem.
従って、従来のメソポーラス金属酸化物とは異なる新しい形状の金属酸化物の製造法を案出し、これにより得られた生成物の物性を調べ、その利用を図ることが求められている。 Accordingly, it has been demanded to devise a method for producing a metal oxide having a new shape different from that of the conventional mesoporous metal oxide, to investigate the physical properties of the product obtained thereby, and to use the product.
本発明者は、上記課題を解決すべく、鋭意研究を行った結果、ベシクルとして知られている、二つのアルキル基を有する界面活性剤が形成する二分子膜閉鎖小胞体を鋳型として用いることにより、金属酸化物のナノカプセルが容易に得られることを見出し、本発明を完成した。 As a result of diligent research to solve the above-mentioned problems, the present inventor uses a bilayer closed vesicle formed by a surfactant having two alkyl groups, which is known as a vesicle, as a template. The inventors have found that metal oxide nanocapsules can be easily obtained and completed the present invention.
すなわち本発明は、ベシクルの生成能力を備えた二鎖型カチオン界面活性剤およびアニオン界面活性剤を水に対して前記二鎖型カチオン界面活性剤を３０ないし６０ｍＭの濃度および前記アニオン界面活性剤を６ないし１５ｍＭの濃度をもって添加するとともに強度が７５ないし６００Ｗの超音波を照射することにより、前記二鎖型カチオン界面活性剤およびアニオン界面活性剤を水に溶解させて水溶液を生成するとともに前記両界面活性剤によるベシクルを形成し、次に前記水溶液に濃度が０.０１ないし０.５Ｍの金属酸化物前駆体を添加し、次に当該水溶液を、水熱反応に付し、更にこれを焼成して粒子状の金属酸化物ナノカプセルを得ることを特徴とする金属酸化物ナノカプセルの製造方法である。 That is, the present invention provides a double-chain cationic surfactant and an anionic surfactant having a vesicle-producing ability with a concentration of 30 to 60 mM of the double-chain cationic surfactant and anionic surfactant with respect to water. Addition with a concentration of 6 to 15 mM and irradiation with ultrasonic waves having an intensity of 75 to 600 W dissolve the double-chain cationic surfactant and anionic surfactant in water to form an aqueous solution, and both the interfaces A vesicle with an activator is formed, and then a metal oxide precursor having a concentration of 0.01 to 0.5M is added to the aqueous solution, and then the aqueous solution is subjected to a hydrothermal reaction, which is further calcined. Thus, a metal oxide nanocapsule is obtained by obtaining a particulate metal oxide nanocapsule.
本発明方法により、中空構造を有した金属酸化物のナノカプセルが容易に調製できる。そして、この金属酸化物ナノカプセルは、低比重でしかも高比表面積であるという性質を有するので、薬物担体、化粧品基剤、屈折率調整剤等として利用することができるものである。 By the method of the present invention, a metal oxide nanocapsule having a hollow structure can be easily prepared. And since this metal oxide nanocapsule has the property of having a low specific gravity and a high specific surface area, it can be used as a drug carrier, a cosmetic base, a refractive index adjusting agent and the like.
本発明方法は、二鎖型カチオン界面活性剤および金属酸化物前駆体を含有する水溶液を、水熱反応に付した後、これを焼成することにより、金属酸化物ナノカプセルを製造する方法である。 The method of the present invention is a method for producing metal oxide nanocapsules by subjecting an aqueous solution containing a double-chain cationic surfactant and a metal oxide precursor to a hydrothermal reaction and then firing the solution. .
本発明により得られる金属酸化物ナノカプセルとしては、例えば、シリカ、チタニア、アルミナ等の金属酸化物のものが挙げられる。これら金属酸化物の原料となる金属酸化物前駆体としては、それぞれの金属酸化物に対応し、例えば、テトラエチルオルトシリケート、酸化硫酸チタン等を利用することができる。 Examples of the metal oxide nanocapsules obtained by the present invention include metal oxides such as silica, titania, and alumina. As the metal oxide precursors that are the raw materials for these metal oxides, for example, tetraethylorthosilicate, titanium oxide sulfate, and the like can be used.
一方、本発明において使用される二鎖型カチオン界面活性剤としては、従来からベシクルの製造に用いられている界面活性剤を使用することができる。このような、二鎖型カチオン界面活性剤の例としては、例えば、ジヘキサデシルジメチルアンモニウムブロミド、ジオクタデシルジメチルアンモニウムブロミド等のジアルキルジメチルアンモニウム塩や、ポリオキシエチレン付加ジヘキサデシルジメチルアンモニウム塩、ポリオキシエチレン付加ジオクタデシルジメチルアンモニウム塩等のポリオキシエチレン付加ジアルキルジメチルアンモニウム塩が好ましい。このうち、特に、アルキル基の炭素原子数が１２から２０のジアルキルジメチルアンモニウム塩が好ましい。 On the other hand, as the double-chain cationic surfactant used in the present invention, a surfactant conventionally used in the production of vesicles can be used. Examples of such double-chain cationic surfactants include dialkyldimethylammonium salts such as dihexadecyldimethylammonium bromide and dioctadecyldimethylammonium bromide, polyoxyethylene-added dihexadecyldimethylammonium salt, Polyoxyethylene-added dialkyldimethylammonium salts such as oxyethylene-added dioctadecyldimethylammonium salt are preferred. Of these, dialkyldimethylammonium salts having 12 to 20 carbon atoms in the alkyl group are particularly preferable.
本発明方法は、上記した金属酸化物前駆体と二鎖型カチオン界面活性剤を原料として実施できるが、更にアニオン活性剤を使用することが、中空粒子の孔径の制御の点で好ましい。このような目的のために使用することのできるアニオン界面活性剤としては、例えば、アルキル硫酸塩、ポリオキシエチレン付加アルキル硫酸塩、アルカンスルホン酸塩、アルキルリン酸塩、Ｎ−アシルアルキルタウリン酸、α−オレフィンスルホン酸塩、スルホコハク酸塩等が挙げられる。このうち、アルキル基の炭素原子数が８から２０のアルキル硫酸塩が好ましい。 The method of the present invention can be carried out using the metal oxide precursor and the two-chain cationic surfactant as raw materials, but it is preferable to use an anionic surfactant in terms of controlling the pore diameter of the hollow particles. Examples of anionic surfactants that can be used for such purposes include alkyl sulfates, polyoxyethylene-added alkyl sulfates, alkane sulfonates, alkyl phosphates, N-acyl alkyl tauric acids, Examples include α-olefin sulfonates and sulfosuccinates. Of these, alkyl sulfates having 8 to 20 carbon atoms in the alkyl group are preferred.
上記成分、すなわち、金属酸化物前駆体、二鎖型カチオン界面活性剤および必要によりアニオン界面活性剤を含有する水溶液から金属酸化物ナノカプセルを製造するには、次のようにすればよい。 In order to produce a metal oxide nanocapsule from an aqueous solution containing the above-described components, that is, a metal oxide precursor, a double-chain cationic surfactant, and, if necessary, an anionic surfactant, the following may be performed.
まず、二鎖型カチオン界面活性剤および必要によりアニオン界面活性剤を、水に十分溶解させ、ベシクルを形成させる。この二鎖型カチオン界面活性剤等の溶解およびベシクル形成には、例えば、７５ないし６００Ｗ程度の強度の超音波を照射することが好ましい。 First, a double-chain cationic surfactant and, if necessary, an anionic surfactant are sufficiently dissolved in water to form a vesicle. For dissolution and vesicle formation of the double-chain cationic surfactant or the like, it is preferable to irradiate ultrasonic waves having an intensity of about 75 to 600 W, for example.
このベシクル形成に当たっての、二鎖型カチオン界面活性剤は、３０ないし６０ｍＭ程度の濃度で使用することが好ましく、アニオン性界面活性剤は、１５ｍＭ程度の濃度で使用することが好ましい。 In forming the vesicle, the double-chain cationic surfactant is preferably used at a concentration of about 30 to 60 mM, and the anionic surfactant is preferably used at a concentration of about 15 mM.
上記水溶液中に、金属酸化物前駆体を加え、５００ないし１０００ｒｐｍ程度で、１２ないし２４時間程度撹拌する。加える金属酸化物前駆体は、水溶液中での濃度が０.０１ないし０.５Ｍ程度となる濃度であることが好ましい。 A metal oxide precursor is added to the aqueous solution and stirred at about 500 to 1000 rpm for about 12 to 24 hours. The added metal oxide precursor preferably has a concentration of about 0.01 to 0.5 M in the aqueous solution.
なお、上記水溶液は、金属酸化物前駆体の添加に先立ち、必要に応じてｐＨを調製することができる。例えば、シリカによるカプセルを調製する場合には、水溶液中に、アルカリ物質を加え、そのｐＨを１０ないし１３程度とすることが好ましく、このために用いるアルカリ物質としては、水酸化ナトリウム、炭酸水素ナトリウム、アンモニア等が挙げられる。 In addition, prior to the addition of the metal oxide precursor, the aqueous solution can be adjusted in pH as necessary. For example, when preparing a capsule made of silica, it is preferable to add an alkaline substance to an aqueous solution to adjust the pH to about 10 to 13. Examples of the alkaline substance used for this purpose include sodium hydroxide and sodium bicarbonate. , Ammonia and the like.
更に、金属酸化物前駆体を加えられた溶液は、水熱反応に付される。この水熱反応は、例えば、８０ないし１３０℃、好ましくは、１２０℃程度の温度条件下、オートクレーブ中で高圧処理することにより行うことができる。 Furthermore, the solution to which the metal oxide precursor has been added is subjected to a hydrothermal reaction. This hydrothermal reaction can be performed, for example, by high-pressure treatment in an autoclave under a temperature condition of about 80 to 130 ° C., preferably about 120 ° C.
水熱反応により生成した反応物は、常法により固液分離および洗浄を行った後、乾燥され、最終的に焼成され、目的とする金属酸化物のナノカプセルを得ることができる。 The reaction product produced by the hydrothermal reaction is subjected to solid-liquid separation and washing by a conventional method, then dried and finally baked to obtain a target metal oxide nanocapsule.
上記焼成は、４００ないし６００℃程度の温度で、１ないし１２時間程度、好ましくは、４ないし８時間程度加熱することにより行われ、これにより、テンプレートとして用いた界面活性剤を除去することができる。 The firing is performed by heating at a temperature of about 400 to 600 ° C. for about 1 to 12 hours, preferably about 4 to 8 hours, whereby the surfactant used as a template can be removed. .
このようにすることにより、例えば、大きさが１００〜２００ｎｍ、膜の厚さが２０〜３０ｎｍで、その比表面積が約２００ｍ２／ｇの中空粒子として金属酸化物のナノカプセルを得ることができる。 By doing so, for example, metal oxide nanocapsules can be obtained as hollow particles having a size of 100 to 200 nm, a film thickness of 20 to 30 nm, and a specific surface area of about 200 m 2 / g. .
以下実施例を挙げ、本発明を更に詳しく説明するが、本発明はこれら実施例に何ら制約されるものではない。 EXAMPLES Hereinafter, although an Example is given and this invention is demonstrated in more detail, this invention is not restrict | limited at all by these Examples.
実 施 例 １
シリカカプセルの調製：
（１）２５ｍｌの超純水に、二鎖型カチオン界面活性剤であるジラウリルジメチルアンモニウムブロマイド（ＤＤＡＢ）およびアニオン界面活性剤であるソディウムオクチルスルフェート（ＳＯＳ）を全濃度で６０ｍＭとなるように添加し（ＤＤＡＢ／ＳＯＳ＝９／１）、４０ｋＨｚの超音波照射下（１５０Ｗ）で溶解させた。
Example 1
Preparation of silica capsules:
(1) To 25 ml of ultrapure water, dilauryldimethylammonium bromide (DDAB), which is a double-chain cationic surfactant, and sodium octyl sulfate (SOS), which is an anionic surfactant, are adjusted to a total concentration of 60 mM. It was added (DDAB / SOS = 9/1) and dissolved under 40 kHz ultrasonic irradiation (150 W).
次いで、これに１０−２Ｎの水酸化ナトリウム溶液（ｐＨ１３）２５ｍｌを撹拌しつつ添加した。更に、この水溶液に、金属酸化物前駆体としてテトラエチルオルソシリケート０.５４６ｇを添加し、激しく撹拌した。２４時間撹拌を行った後、オートクレーブを用い、この溶液を、１２０℃の水熱反応に付した。 Next, 25 ml of a 10 −2 N sodium hydroxide solution (pH 13) was added thereto with stirring. Further, 0.5546 g of tetraethylorthosilicate as a metal oxide precursor was added to this aqueous solution and stirred vigorously. After stirring for 24 hours, this solution was subjected to a hydrothermal reaction at 120 ° C. using an autoclave.
水熱反応の生成物を、吸引濾過により濾別し、得られた粒子を水洗した。次いで、この粒子を、電気炉を用い、１２０℃で６００分間乾燥し、粉状物を得た。 The product of the hydrothermal reaction was separated by suction filtration, and the resulting particles were washed with water. Next, the particles were dried at 120 ° C. for 600 minutes using an electric furnace to obtain a powdery product.
得られた粉状物について、ＸＲＤ測定（ＲＩＧＡＫＵ ＲＩＮＴ−１１００）およびＴＥＭ観察（日立 Ｈ−７６５０）を行い、その構造評価を行った。この結果、ＸＲＤ測定により、（１００）回折ピークの他に、（２００）回折ピークが確認でき、このものは高い規則性のラメラ構造を形成していることが明らかになった。このことは、ＴＥＭによっても確認され、更に個々の粒子がカプセル状になっている可能性も示された（図１）。 About the obtained powdery substance, XRD measurement (RIGAKU RINT-1100) and TEM observation (Hitachi H-7650) were performed, and the structure evaluation was performed. As a result, XRD measurement confirmed (200) diffraction peak in addition to (100) diffraction peak, and it was revealed that this formed a highly ordered lamellar structure. This was confirmed by TEM, and it was also shown that individual particles may be encapsulated (FIG. 1).
（２）上記（１）で得られた水熱反応の生成物を、電気炉を用い、５００℃で６時間焼成した。 (2) The product of the hydrothermal reaction obtained in the above (1) was baked at 500 ° C. for 6 hours using an electric furnace.
得られた焼成物について、上記（１）と同様ＸＲＤ測定およびＴＥＭ観察を行った。この結果、ＸＲＤ測定では、メソ孔に起因するピークは確認されなかったが、ＴＥＭではカプセル構造が観察できた。 The obtained fired product was subjected to XRD measurement and TEM observation as in (1) above. As a result, no peak due to mesopores was observed in the XRD measurement, but the capsule structure could be observed with TEM.
実 施 例 ２
チタニアカプセルの調製：
（１）２５ｍｌの超純水に、二鎖型カチオン界面活性剤であるジラウリルジメチルアンモニウムブロマイド（ＤＤＡＢ）およびアニオン界面活性剤であるソディウムオクチルスルフェート（ＳＯＳ）を全濃度で６０ｍＭとなるように添加し（ＤＤＡＢ／ＳＯＳ＝９：１）、４０ｋＨｚの超音波照射下（１５０Ｗ）で溶解させた。
Example 2
Preparation of titania capsules:
(1) In 25 ml of ultrapure water, dilauryldimethylammonium bromide (DDAB), which is a double-chain cationic surfactant, and sodium octyl sulfate (SOS), which is an anionic surfactant, are adjusted to a total concentration of 60 mM. The solution was added (DDAB / SOS = 9: 1) and dissolved under 40 kHz ultrasonic irradiation (150 W).
次いで、この水溶液に、金属酸化物前駆体として酸化硫酸チタン５０ｍＭを添加し、激しく撹拌した。２４時間撹拌を行った後、オートクレーブを用い、この溶液を、１２０℃の水熱反応に付した。 Next, 50 mM titanium oxide sulfate as a metal oxide precursor was added to this aqueous solution and vigorously stirred. After stirring for 24 hours, this solution was subjected to a hydrothermal reaction at 120 ° C. using an autoclave.
水熱反応の生成物を、吸引濾過により濾別し、得られた粒子を水洗した。次いで、この粒子を、電気炉を用い、１２０℃で６００分間乾燥し、粉状物を得た。以下、実施例１（２）と同様に焼成し、チタニアカプセルを得た。 The product of the hydrothermal reaction was separated by suction filtration, and the resulting particles were washed with water. Next, the particles were dried at 120 ° C. for 600 minutes using an electric furnace to obtain a powdery product. Thereafter, firing was performed in the same manner as in Example 1 (2) to obtain a titania capsule.
本発明方法で得られる金属酸化物ナノカプセルは、低比重でしかも高比表面積であるという性質を有するので、触媒担体、化粧品基剤、屈折率調整剤等として利用することができるものである。 Since the metal oxide nanocapsule obtained by the method of the present invention has a property of low specific gravity and high specific surface area, it can be used as a catalyst carrier, a cosmetic base, a refractive index adjusting agent and the like.
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