JP2006290636A - Titanium hydroxide or titanium dioxide - Google Patents
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- JP2006290636A JP2006290636A JP2005109255A JP2005109255A JP2006290636A JP 2006290636 A JP2006290636 A JP 2006290636A JP 2005109255 A JP2005109255 A JP 2005109255A JP 2005109255 A JP2005109255 A JP 2005109255A JP 2006290636 A JP2006290636 A JP 2006290636A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 71
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 title claims abstract description 52
- 239000002537 cosmetic Substances 0.000 claims description 13
- 239000003973 paint Substances 0.000 claims description 8
- 239000011941 photocatalyst Substances 0.000 claims description 6
- 239000011342 resin composition Substances 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 238000010304 firing Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 7
- 238000000635 electron micrograph Methods 0.000 description 6
- 239000000976 ink Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 238000004438 BET method Methods 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
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Abstract
Description
本発明は、水酸化チタン又は二酸化チタンに関する。 The present invention relates to titanium hydroxide or titanium dioxide.
二酸化チタンは、古くから白色顔料として汎用的に使用されており、化粧料、塗料、プラスチック組成物等の着色剤として使用の他、触媒担体、トナーの外添剤として使用されてきた。近年では、二酸化チタン等が有する光触媒性能を利用した用途も広がりを見せつつある。このような用途としては、各種工業塗料等を挙げることができる。 Titanium dioxide has been widely used as a white pigment for a long time, and has been used as a colorant for cosmetics, paints, plastic compositions, etc., and as an external additive for catalyst carriers and toners. In recent years, applications utilizing the photocatalytic performance of titanium dioxide and the like are also expanding. Examples of such applications include various industrial paints.
これらのチタン系化合物の機能を向上させたりこれまでにない新たな機能を付与したりするために、粒子形状や粒子サイズを種々に変化させる試みが行われている。例えば、粒子径が１０〜１００ｎｍという超微粒子酸化チタンが有する紫外線吸収能を利用したサンスクリーン剤等が知られている。また、リング状の形状を有するアナタース型酸化チタンも公知である（特許文献１参照）。このようなリング状のアナタース型酸化チタンは触媒、光触媒、光電変換材料等の各種担体としての使用が期待されている。 In order to improve the functions of these titanium-based compounds or to add new functions that have never been made, attempts have been made to change the particle shape and particle size in various ways. For example, a sunscreen agent that utilizes the ultraviolet absorbing ability of ultrafine titanium oxide having a particle size of 10 to 100 nm is known. Anatase-type titanium oxide having a ring shape is also known (see Patent Document 1). Such ring-shaped anatase-type titanium oxide is expected to be used as various carriers for catalysts, photocatalysts, photoelectric conversion materials and the like.
このように、特殊な形状を有するチタン系化合物は、その形状に基づいて特殊な機能を発現することが期待されるものであり、これまでにない新たな粒子形状を有する水酸化チタンや酸化チタンが望まれている。
本発明は、上記現状に鑑み、棒状中空状（長径方向に通孔を有する棒状）というこれまでにない特殊な形状を有する水酸化チタン又は二酸化チタンを提供することを目的とするものである。 In view of the above situation, an object of the present invention is to provide titanium hydroxide or titanium dioxide having an unprecedented special shape of a rod-like hollow shape (a rod shape having a through hole in the major axis direction).
本発明は、長径方向に通孔を有する棒状であることを特徴とする水酸化チタン又は二酸化チタンである。
上記水酸化チタン又は二酸化チタンは、長径（ａ）：５≦ａ≦１００μｍ、短径（ｂ）：１≦ｂ≦１０μｍ、中空径（ｃ）：０．５≦ｃ≦８μｍ、アスペクト比（ａ）／（ｂ）：２≦（ａ）／（ｂ）≦５０、中空比（ｂ）／（ｃ）：１．５≦（ｂ）／（ｃ）≦１０を満たすものであることが好ましい。
上記水酸化チタン又は二酸化チタンは、比表面積が０．２〜４００ｍ２／ｇであることが好ましい。
The present invention is a titanium hydroxide or titanium dioxide characterized by a rod shape having through holes in the major axis direction.
The titanium hydroxide or titanium dioxide has a major axis (a): 5 ≦ a ≦ 100 μm, a minor axis (b): 1 ≦ b ≦ 10 μm, a hollow diameter (c): 0.5 ≦ c ≦ 8 μm, an aspect ratio (a ) / (B): 2 ≦ (a) / (b) ≦ 50 and hollow ratio (b) / (c): 1.5 ≦ (b) / (c) ≦ 10 are preferably satisfied.
The titanium hydroxide or titanium dioxide preferably has a specific surface area of 0.2 to 400 m 2 / g.
本発明は、上記水酸化チタン又は二酸化チタンを含有することを特徴とする化粧料でもある。
本発明は、上記水酸化チタン又は二酸化チタンを含有することを特徴とする光触媒でもある。
本発明は、上記水酸化チタン又は二酸化チタンを含有することを特徴とする塗料でもある。
本発明は、上記水酸化チタン又は二酸化チタンを含有することを特徴とするインキでもある。
本発明は、上記水酸化チタン又は二酸化チタンを含有することを特徴とする樹脂組成物でもある。
以下に本発明を詳細に説明する。
This invention is also cosmetics characterized by containing the said titanium hydroxide or titanium dioxide.
This invention is also a photocatalyst characterized by containing the said titanium hydroxide or titanium dioxide.
The present invention is also a coating material containing the above-mentioned titanium hydroxide or titanium dioxide.
The present invention is also an ink characterized by containing the above-mentioned titanium hydroxide or titanium dioxide.
This invention is also the resin composition characterized by containing the said titanium hydroxide or titanium dioxide.
The present invention is described in detail below.
本発明の長径方向に通孔を有する棒状である水酸化チタン又は二酸化チタンとは、円柱又は角柱状等の棒状形状を有し、その長軸方向に両端が開口した通孔を有するという形状を有する水酸化チタン又は二酸化チタンである。ただし、本発明の水酸化チタン又は二酸化チタンは、このような形状を有するものと、両端が閉じられており、かつ、長軸方向に空洞を持つものとからなる混合物であってもよい。このような形状を有する水酸化チタン又は二酸化チタンの例を図１及び図２の電子顕微鏡写真に示した。図１及び図２に示されている水酸化チタン又は二酸化チタンは、長径方向に通孔を有する棒状のものと、両端が閉じられており、かつ、長軸方向に空洞を持つものとからなる混合物であることが写真から判断することができる。 The rod-like titanium hydroxide or titanium dioxide having a through hole in the major axis direction of the present invention has a rod-like shape such as a cylinder or a prismatic shape, and has a shape having through-holes opened at both ends in the major axis direction. It has titanium hydroxide or titanium dioxide. However, the titanium hydroxide or titanium dioxide of the present invention may be a mixture composed of such a shape and one having both ends closed and having a cavity in the major axis direction. Examples of titanium hydroxide or titanium dioxide having such a shape are shown in the electron micrographs of FIGS. The titanium hydroxide or titanium dioxide shown in FIGS. 1 and 2 is composed of a rod-shaped one having a through hole in the major axis direction and one having both ends closed and having a cavity in the major axis direction. It can be judged from the photograph that it is a mixture.
本発明の水酸化チタン又は二酸化チタンは、上述したような特殊な形状を有するものであることから、特殊な性質を有することが期待され、この性質に基づく種々の用途が期待される。 Since the titanium hydroxide or titanium dioxide of the present invention has a special shape as described above, it is expected to have a special property, and various uses based on this property are expected.
本発明の水酸化チタン又は二酸化チタンは、これらを厳密に区別する必要はないものである。すなわち、二酸化チタンの一般的な製造方法である沈殿法は、水酸化チタンを製造した後、焼成によって二酸化チタンを製造するものである。本発明の水酸化チタン又は二酸化チタンは、焼成前のほぼ純粋な水酸化チタン、高度に焼成して得られた純度の高い二酸化チタン、焼成の程度が低く、水酸化チタンと二酸化チタンが混在した状態のもののすべてを包含するものである。 The titanium hydroxide or titanium dioxide of the present invention does not need to be strictly distinguished. That is, the precipitation method, which is a general method for producing titanium dioxide, is to produce titanium dioxide by firing after producing titanium hydroxide. Titanium hydroxide or titanium dioxide of the present invention is almost pure titanium hydroxide before firing, high purity titanium dioxide obtained by highly firing, low degree of firing, titanium hydroxide and titanium dioxide mixed Includes everything in the state.
本発明の二酸化チタンは、アナタース型であってもルチル型であってもよい。また、水酸化チタン及び二酸化チタン以外の不純物の含有量は１質量％未満であることが好ましい。 The titanium dioxide of the present invention may be anatase type or rutile type. Moreover, it is preferable that content of impurities other than titanium hydroxide and titanium dioxide is less than 1 mass%.
本発明の水酸化チタン又は二酸化チタンは、長径（ａ）：５≦ａ≦１００μｍ、短径（ｂ）：１≦ｂ≦１０μｍ、中空径（ｃ）：０．５≦ｃ≦８μｍ、アスペクト比（ａ）／（ｂ）：２≦（ａ）／（ｂ）≦５０、中空比（ｂ）／（ｃ）：１．５≦（ｂ）／（ｃ）≦１０の条件を満たす大きさであることが好ましい。 The titanium hydroxide or titanium dioxide of the present invention has a major axis (a): 5 ≦ a ≦ 100 μm, a minor axis (b): 1 ≦ b ≦ 10 μm, a hollow diameter (c): 0.5 ≦ c ≦ 8 μm, and an aspect ratio. (A) / (b): 2 ≦ (a) / (b) ≦ 50, hollow ratio (b) / (c): 1.5 ≦ (b) / (c) ≦ 10 Preferably there is.
上記長径（ａ）を５μｍ以上とすることで、容易に棒状形状をなすことができる点で好ましい。更に、上記長径（ａ）を１００μｍ以下とすることで安定的に棒状を維持することができる点で好ましい。上記短径（ｂ）を１μｍ以上とすることで、棒状形状を維持するのに充分な強度を得ることができる点で好ましく、１０μｍ以下とすることで棒状形状を容易に得ることができる点で好ましい。中空径（ｃ）を０．５μｍ以上とすることで、連続した中空部分を得ることができる点で好ましく、８μｍ以下とすることで、棒状形状を維持するに充分な強度を得ることができる点で好ましい。なお、上記中空径（ｃ）とは、棒状の水酸化チタン又は二酸化チタンの長径方向の通孔の径を意味する。 It is preferable that the major axis (a) is 5 μm or more because a rod-like shape can be easily formed. Furthermore, it is preferable in that the rod shape can be stably maintained by setting the major axis (a) to 100 μm or less. By making the said short axis (b) 1 micrometer or more, it is preferable at the point which can obtain intensity | strength sufficient to maintain a rod-shaped shape, By the point which can obtain a rod-shaped shape easily by setting it as 10 micrometers or less. preferable. The hollow diameter (c) is preferably 0.5 μm or more, so that a continuous hollow portion can be obtained, and by 8 μm or less, sufficient strength can be obtained to maintain the rod shape. Is preferable. In addition, the said hollow diameter (c) means the diameter of the through-hole of the major axis direction of rod-shaped titanium hydroxide or titanium dioxide.
更に、アスペクト比（ａ）／（ｂ）を２以上とすることで棒状形状をなすことができ、５０以下とすることで棒状形状を維持するのに充分な強度を容易に得ることができる点で好ましい。中空比（ｂ）／（ｃ）を１．５以上とすることで、棒状形状を維持するに充分な強度を得ることが容易であり、１０以下とすることで連続した中空部分を容易に得ることができる点で好ましい。また、このようなナノオーダーではないサブミクロンオーダーの大きさの粒子であると、二次凝集を生じることなく一次粒子の状態で取り出すことができるため、特異な形状に基づく性質を容易に得ることができる点でも好ましいものである。 Furthermore, a bar shape can be formed by setting the aspect ratio (a) / (b) to 2 or more, and a strength sufficient to maintain the bar shape can be easily obtained by setting the aspect ratio to 50 or less. Is preferable. By setting the hollow ratio (b) / (c) to 1.5 or more, it is easy to obtain sufficient strength to maintain the rod-like shape, and by setting it to 10 or less, a continuous hollow portion can be easily obtained. It is preferable in that it can be performed. In addition, if the particles are in the order of sub-micron order, not nano order, they can be taken out in the form of primary particles without causing secondary aggregation, so that it is easy to obtain properties based on unique shapes. It is also preferable in that
上記大きさのものを使用することによって、化粧料、触媒、塗料、インキ、樹脂組成物への添加剤として使用した場合のすべり感、着色力、光触媒活性、吸着能等が良好であり、取扱い性も良好である点で好ましい。上記（ａ）〜（ｃ）は、電子顕微鏡写真によって測定することができる。電子顕微鏡によって測定した水酸化チタン又は二酸化チタンの形状を測定することによって、単一の粒子に対する上記（ａ）〜（ｃ）をすべて測定することができる。本明細書において、上記（ａ）〜（ｃ）は、電子顕微鏡測定における視野中の任意の１００個の粒子について、それぞれの（ａ）〜（ｃ）を測定し、これらの平均値を指すものである。上記（ａ）／（ｂ）、（ｂ）／（ｃ）は、このようにして測定した（ａ）〜（ｃ）から算出することにより求めた値である。 By using the above-mentioned size, slippery feeling, coloring power, photocatalytic activity, adsorption ability, etc. are good when used as an additive to cosmetics, catalysts, paints, inks, resin compositions. It is preferable in terms of good properties. Said (a)-(c) can be measured with an electron micrograph. By measuring the shape of titanium hydroxide or titanium dioxide measured with an electron microscope, all of the above (a) to (c) for a single particle can be measured. In the present specification, the above (a) to (c) are obtained by measuring the respective (a) to (c) for any 100 particles in the field of view in the electron microscope measurement, and indicating the average value thereof. It is. The above (a) / (b) and (b) / (c) are values obtained by calculating from (a) to (c) thus measured.
本発明の水酸化チタン又は二酸化チタンは、比表面積が０．２〜４００ｍ２／ｇであることが好ましい。比表面積が０．２ｍ２／ｇ以上であることによって、高い表面積に由来する高い吸着能、光触媒活性能等が期待される。比表面積が４００ｍ２／ｇ以下であることによって、適切な粒子強度と通気性を持つという利点を有するものである。上記比表面積は、ＢＥＴ法によって測定した値である。 The titanium hydroxide or titanium dioxide of the present invention preferably has a specific surface area of 0.2 to 400 m 2 / g. When the specific surface area is 0.2 m 2 / g or more, high adsorption ability, photocatalytic activity ability and the like derived from a high surface area are expected. When the specific surface area is 400 m 2 / g or less, it has an advantage of having appropriate particle strength and air permeability. The specific surface area is a value measured by the BET method.
本発明の水酸化チタン又は二酸化チタンは、特に化粧品分野において使用する場合には、滑り性が良好であることが好ましい。滑り性が良好であると、皮膚に塗布する際になめらかに広がり、広がり、のび及び使用感に優れた化粧品とすることができるためである。本発明の水酸化チタン又は二酸化チタンは、化粧品用途に使用する場合は、ＭＩＵ値０．６以下、ＭＭＤ値０．０４以下であることが好ましい。上記範囲内であることによって、使用感のよい化粧品を得ることができる点で好ましい。 When the titanium hydroxide or titanium dioxide of the present invention is used particularly in the cosmetic field, it is preferable that the slipperiness is good. This is because, when the slipperiness is good, it can be made into a cosmetic product that spreads smoothly, spreads, spreads and feels good when applied to the skin. When used for cosmetic applications, the titanium hydroxide or titanium dioxide of the present invention preferably has an MIU value of 0.6 or less and an MMD value of 0.04 or less. By being in the said range, it is preferable at the point which can obtain cosmetics with a favorable feeling of use.
本発明の水酸化チタン又は二酸化チタンは、その製造方法を特に限定されるものではなく、公知の水酸化チタン又は二酸化チタンの製造方法において、製造条件を適宜設定して好適な製造条件を選択することによって得ることができる。また、製造条件を調整することによって、（ａ）〜（ｃ）、（ａ）／（ｂ）、（ｂ）／（ｃ）の値、比表面積、ＭＩＵ値、ＭＭＤ値等を調整することができる。更に、製造条件を調整することによって、ルチル型二酸化チタンとすることも、アナタース型二酸化チタンとすることもできる。 The production method of the titanium hydroxide or titanium dioxide of the present invention is not particularly limited, and in the known production method of titanium hydroxide or titanium dioxide, suitable production conditions are selected by appropriately setting the production conditions. Can be obtained. Further, by adjusting the manufacturing conditions, the values (a) to (c), (a) / (b), (b) / (c), specific surface area, MIU value, MMD value, etc. can be adjusted. it can. Furthermore, it can be set as a rutile type titanium dioxide or an anatase type titanium dioxide by adjusting manufacturing conditions.
焼成時には、比較的低温で結晶性を高めるための各種フラックス、ルチル化を促進するための助剤、焼結を防止するための焼結防止剤等の添加剤の存在下に行うものであってもよい。本発明の水酸化チタン又は二酸化チタンは比較的容易に表面積、結晶形状を変化させることができるため、用途に応じて必要とされる形状を比較的容易に得ることができる点でも好ましいものである。 During firing, it is carried out in the presence of additives such as various fluxes for enhancing crystallinity at relatively low temperatures, auxiliary agents for promoting rutileization, and sintering inhibitors for preventing sintering. Also good. Since the titanium hydroxide or titanium dioxide of the present invention can change the surface area and crystal shape relatively easily, it is also preferable in that the required shape can be obtained relatively easily depending on the application. .
本発明の水酸化チタン又は二酸化チタンは、化粧料、塗料、インキ、樹脂組成物等に配合することができる。本発明の水酸化チタン又は二酸化チタンを化粧料に配合すると、皮膚への伸展性、すなわち、すべり性がよく、使用感が非常に良好となる。また、塗料、インキのフィラーとして用いた場合、棒状形状であることにより膜強度が大きくなるとともに、表面のすべり性の改善も期待でき、更に、吸着能の高さによる環境汚染物質の吸着も期待できる。そして更に、光触媒や触媒の担体に使用した場合、内部が空洞であることから化合物の吸着能に優れることとなり、高い触媒活性を発揮することが期待されるものである。 The titanium hydroxide or titanium dioxide of the present invention can be blended in cosmetics, paints, inks, resin compositions and the like. When the titanium hydroxide or titanium dioxide of the present invention is blended into a cosmetic, the extensibility to the skin, that is, the slipperiness is good and the feeling of use becomes very good. In addition, when used as a filler for paints and inks, the rod-like shape increases the film strength, and can be expected to improve the slipperiness of the surface. In addition, it is also expected to adsorb environmental pollutants due to its high adsorption capacity. it can. Further, when used as a photocatalyst or a catalyst carrier, the inside is hollow, so that the compound adsorption ability is excellent, and high catalytic activity is expected to be exhibited.
本発明の水酸化チタン又は二酸化チタンは、特殊な形状を有するものであり、このような形状に由来する優れたすべり性、吸着能を有するものである。このような機能を有することから、化粧料、光触媒、塗料、インキ、樹脂組成物等に使用したときに、好適に使用することができる。 The titanium hydroxide or titanium dioxide of the present invention has a special shape, and has excellent slipperiness and adsorption ability derived from such a shape. Since it has such a function, it can be suitably used when used in cosmetics, photocatalysts, paints, inks, resin compositions and the like.
以下に本発明を実施例により更に具体的に説明するが、本発明はこれら実施例のみに限定されるものではない。また実施例中、「部」は特に断りのない限り「質量部」を意味する。 Examples The present invention will be described more specifically with reference to examples. However, the present invention is not limited to these examples. In the examples, “parts” means “parts by mass” unless otherwise specified.
（実施例）
硫酸チタニルを原料とした通常の二酸化チタンの製造方法における製造条件を調整することによって、長径方向に通孔を有する棒状である二酸化チタンを得た。得られた二酸化チタンの電子顕微鏡写真を図1及び図２に示した。なお、図１及び図２は同一の二酸化チタンを測定したものであるが、倍率が相違している。
(Example)
By adjusting the production conditions in the usual titanium dioxide production method using titanyl sulfate as a raw material, a rod-like titanium dioxide having through holes in the major axis direction was obtained. An electron micrograph of the obtained titanium dioxide is shown in FIGS. 1 and 2 show the same titanium dioxide, but the magnification is different.
得られた二酸化チタンの電子顕微鏡写真に基づいて画像中の任意の１００個の粒子について長径（ａ）、短径（ｂ）、中空径（ｃ）を測定し、これに基づいてアスペクト比（ａ）／（ｂ）及び中空比（ｂ）／（ｃ）を算出した。これらの値を表１に示した。 The major axis (a), minor axis (b), and hollow diameter (c) of any 100 particles in the image are measured based on the obtained electron micrograph of titanium dioxide, and the aspect ratio (a ) / (B) and hollow ratio (b) / (c). These values are shown in Table 1.
更に、上記実施例によって得られた二酸化チタン及びこの二酸化チタンを得る工程において、焼成前に得られた水酸化チタンのそれぞれについて、比表面積（ＢＥＴ法）とＸＲＤ測定を行った。結果を図３及び図４に示した。焼成後の二酸化チタンは比表面積２２０ｍ２／ｇで、２Θ＝２５度付近にアナタース型の二酸化チタン由来のピークが観測されたが、焼成前の水酸化チタンは比表面積３５０ｍ２／ｇで、二酸化チタン由来のピークがみられなかった。 Furthermore, in the step of obtaining titanium dioxide obtained by the above-mentioned Examples and titanium dioxide, specific surface area (BET method) and XRD measurement were performed for each of the titanium hydroxide obtained before firing. The results are shown in FIGS. The titanium dioxide after firing had a specific surface area of 220 m 2 / g, and a peak derived from anatase-type titanium dioxide was observed around 2Θ = 25 ° C., but the titanium hydroxide before firing had a specific surface area of 350 m 2 / g, A peak derived from titanium was not observed.
上記実施例によって得られた長径方向に通孔を有する棒状である二酸化チタンの滑り性及び吸着性能を以下に示す方法によって測定した。結果を表２及び図５に示した。なお、表２においては、同様の方法によって測定した各種の顔料の摩擦特性値を比較データとして示した。更に、図５においては超微粒子アナタース型酸化チタン（ＳＳＰ−２５ 堺化学工業社製）を使用して同じ試験を行った場合の結果を示した。 The slipperiness and adsorption performance of titanium dioxide, which is rod-shaped having through holes in the major axis direction obtained in the above examples, were measured by the following methods. The results are shown in Table 2 and FIG. In Table 2, the friction characteristic values of various pigments measured by the same method are shown as comparative data. Furthermore, in FIG. 5, the result at the time of performing the same test using ultrafine particle | grains anatase type titanium oxide (SSP-25 Sakai Chemical Industry Co., Ltd.) was shown.
（滑り性の測定方法）
スライドガラスに両面テープを貼付し、粘着面に試料を載せる。化粧用スポンジで試料を均一に伸ばし、摩擦子をセットして測定を行った。なお、測定はカトーテック株式会社製ＫＥＳ−ＳＥ摩擦テスターを使用して行い、ＳＥＮＳ：Ｈ，摩擦子移動速度１．０ｍｍ／ｓｅｃ、摩擦静荷重２５ｇの条件で、摩擦子としてシリコンセンサーを使用して行った。
(Slip measurement method)
Apply double-sided tape to the slide glass and place the sample on the adhesive surface. The sample was uniformly stretched with a cosmetic sponge, and a measurement was performed by setting a friction piece. The measurement was performed using a KES-SE friction tester manufactured by Kato Tech Co., Ltd., using a silicon sensor as a friction element under the conditions of SENS: H, friction element moving speed 1.0 mm / sec, and static friction load 25 g. I went.
表２の結果から、実施例によって得られた本発明の二酸化チタンは滑り性良好であることが明らかとなった。 From the results in Table 2, it was revealed that the titanium dioxide of the present invention obtained by the examples had good slipperiness.
（吸着性能の測定方法）
上記実施例によって得られた長径方向に通孔を有する棒状である二酸化チタン５ｇとイソプロピルアルコール１０ｇとを遊星ミルで１０分間混合した。上記工程によって得られたペーストを１５ｃｍ角のガラス板にバーコーターによって塗布した。６時間放置して溶剤を揮発させた後、中心波長３５０ｎｍの紫外線ランプ（東芝ライテック社製、１０Ｗ）を５Ｗ／ｃｍ２の強度で４時間照射し、有機物を完全に分解した。上記酸化チタン被膜を形成したガラス板を６０ｃｍ×６０ｃｍ×１５ｃｍの容器に入れ、容器内の気体中の濃度が５００ｐｐｍとなる割合でアセトアルデヒドを封入した。室温で上記容器を保持し、一定時間ごとに容器内のガスをサンプリングして、ガスクロマトグラフィーによってアセトアルデヒド濃度を測定した。
(Measurement method of adsorption performance)
5 g of rod-like titanium dioxide having through holes in the major axis direction obtained in the above examples and 10 g of isopropyl alcohol were mixed in a planetary mill for 10 minutes. The paste obtained by the above process was applied to a 15 cm square glass plate with a bar coater. After leaving it to stand for 6 hours to volatilize the solvent, an ultraviolet lamp (manufactured by Toshiba Lighting & Technology, 10 W) with a central wavelength of 350 nm was irradiated for 4 hours at an intensity of 5 W / cm 2 to completely decompose the organic matter. The glass plate on which the titanium oxide film was formed was placed in a 60 cm × 60 cm × 15 cm container, and acetaldehyde was enclosed at a ratio of 500 ppm in the gas in the container. The container was held at room temperature, the gas in the container was sampled at regular intervals, and the acetaldehyde concentration was measured by gas chromatography.
図５に示された結果から、本発明の二酸化チタンは、比表面積が大きく吸着能に優れると言われている超微粒子チタンよりも良好な吸着性能を有することが明らかである。 From the results shown in FIG. 5, it is clear that the titanium dioxide of the present invention has better adsorption performance than ultrafine particle titanium, which is said to have a large specific surface area and excellent adsorption ability.
本発明の水酸化チタン又は二酸化チタンは、化粧料、塗料、インキ、樹脂組成物への添加剤；光触媒；触媒の担体等において使用することができる。 The titanium hydroxide or titanium dioxide of the present invention can be used in cosmetics, paints, inks, additives to resin compositions; photocatalysts; catalyst carriers and the like.
Claims (8)
短径（ｂ）：１≦ｂ≦１０μｍ
中空径（ｃ）：０．５≦ｃ≦８μｍ
アスペクト比（ａ）／（ｂ）：２≦（ａ）／（ｂ）≦５０
中空比（ｂ）／（ｃ）：１．５≦（ｂ）／（ｃ）≦１０
を満たす請求項１記載の水酸化チタン又は二酸化チタン。 Long diameter (a): 5 ≦ a ≦ 100 μm
Minor axis (b): 1 ≦ b ≦ 10 μm
Hollow diameter (c): 0.5 ≦ c ≦ 8 μm
Aspect ratio (a) / (b): 2 ≦ (a) / (b) ≦ 50
Hollow ratio (b) / (c): 1.5 ≦ (b) / (c) ≦ 10
The titanium hydroxide or titanium dioxide according to claim 1 satisfying
A resin composition comprising the titanium hydroxide or titanium dioxide according to claim 1, 2 or 3.
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| JP2013023676A (en) * | 2011-07-26 | 2013-02-04 | General Co Ltd | White ink for inkjet |
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|---|---|---|---|---|
| JPH10152323A (en) * | 1996-09-30 | 1998-06-09 | Chubu Electric Power Co Inc | Crystal titania and its production |
| JP2004175586A (en) * | 2002-11-25 | 2004-06-24 | Fujikura Ltd | Method of manufacturing titanium oxide nanotube |
| JP2004175587A (en) * | 2002-11-25 | 2004-06-24 | Fujikura Ltd | Method of manufacturing titanium oxide nanotube |
| WO2004057064A1 (en) * | 2002-12-21 | 2004-07-08 | Juridical Foundation Osaka Industrial Promotion Organization | Oxide nanostructure, method for producing same, and use thereof |
| JP2005289932A (en) * | 2004-04-02 | 2005-10-20 | Pola Chem Ind Inc | Fibrous hollow inorganic compound particle and cosmetic containing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10152323A (en) * | 1996-09-30 | 1998-06-09 | Chubu Electric Power Co Inc | Crystal titania and its production |
| JP2004175586A (en) * | 2002-11-25 | 2004-06-24 | Fujikura Ltd | Method of manufacturing titanium oxide nanotube |
| JP2004175587A (en) * | 2002-11-25 | 2004-06-24 | Fujikura Ltd | Method of manufacturing titanium oxide nanotube |
| WO2004057064A1 (en) * | 2002-12-21 | 2004-07-08 | Juridical Foundation Osaka Industrial Promotion Organization | Oxide nanostructure, method for producing same, and use thereof |
| JP2005289932A (en) * | 2004-04-02 | 2005-10-20 | Pola Chem Ind Inc | Fibrous hollow inorganic compound particle and cosmetic containing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2013023676A (en) * | 2011-07-26 | 2013-02-04 | General Co Ltd | White ink for inkjet |
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