JPH0489318A - Production of spherical titania - Google Patents
Production of spherical titaniaInfo
- Publication number
- JPH0489318A JPH0489318A JP20387790A JP20387790A JPH0489318A JP H0489318 A JPH0489318 A JP H0489318A JP 20387790 A JP20387790 A JP 20387790A JP 20387790 A JP20387790 A JP 20387790A JP H0489318 A JPH0489318 A JP H0489318A
- Authority
- JP
- Japan
- Prior art keywords
- titania
- butoxide
- ammonia
- water
- particle size
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 11
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 abstract description 39
- 230000007062 hydrolysis Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 8
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 6
- 230000003247 decreasing effect Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- -1 etc. Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000002537 cosmetic Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- ZEIWWVGGEOHESL-UHFFFAOYSA-N methanol;titanium Chemical compound [Ti].OC.OC.OC.OC ZEIWWVGGEOHESL-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000005456 alcohol based solvent Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- KEBCEWNYIWHGPF-UHFFFAOYSA-N butan-1-ol butan-1-olate titanium(4+) Chemical compound C(CCC)O.[O-]CCCC.[O-]CCCC.[O-]CCCC.[O-]CCCC.[Ti+4] KEBCEWNYIWHGPF-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 150000003138 primary alcohols Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、球状チタニアの製造方法に関し、詳しくは化
粧品、塗料等の顔料、触媒、吸着剤、光半導体、更には
還元雰囲気焼成で異色化することにより液晶のスペーサ
ー材として好適な球状チタニアの製造方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing spherical titania, and more specifically, it is used to produce pigments for cosmetics, paints, etc., catalysts, adsorbents, optical semiconductors, and furthermore, to produce unique colors by firing in a reducing atmosphere. This invention relates to a method for producing spherical titania suitable as a spacer material for liquid crystals.
従来、球状チタニアの製造方法として、チタンアルコキ
シドを蒸発せしめ、気相状態下で熱分解して微粒子状チ
タニアを製造する方法（特開昭６０−１８６．４１８号
公報）、チタンテトラエトキ°シト又はチタンテトライ
ソプロポキシドのアルコール溶液を加水分解することに
よりサブミクロンの球状チタニアを製造する方法［Ｃｏ
ｍｕｎｉｃａｔｉｏｎｓ ｏｆ ｔｈｅＡｍｅｒｉｃａ
ｎ Ｃｅｒａｍｉｃ ５ｏｃｉｅｔｙ、Ｃ−１９９，（
１９８２）］、チタンテトラエトキシドのエタノール溶
液に分散剤としてヒドロキシプロピルセルロースを添加
した後、加水分解することによりサブミクロンの球状チ
タニアを製造する方法［Ｊｏｕｒｎａｌ ｏｆ Ａｍｅ
ｒｉｃａｎＣｅｒａｍｉｃ ５ｏｃｉｒｔｙ Ｂｕ
ｌｌｉｔｅｎ、６５．（１２）、 １５７４． （１９
７６）］等が知られている。Conventionally, methods for producing spherical titania include a method in which titanium alkoxide is evaporated and thermally decomposed in a gas phase to produce fine particulate titania (Japanese Unexamined Patent Application Publication No. 186-186-188), titanium tetraethoxylate or A method for producing submicron spherical titania by hydrolyzing an alcohol solution of titanium tetraisopropoxide [Co
communications of theAmerica
n Ceramic 5ociety, C-199, (
1982)], a method for producing submicron spherical titania by adding hydroxypropylcellulose as a dispersant to an ethanol solution of titanium tetraethoxide and then hydrolyzing it [Journal of Ame
ricanCeramic 5ocirty Bu
lliten, 65. (12), 1574. (19
76)] etc. are known.
しかしながら、これらの製造方法では、粒径制御範囲が
狭く、０．１〜１．ｍ程度の球状チタニアしかできず、
化粧品顔料として用いた場合、毛穴、皮溝に入るという
問題点がある。また、チタンテトラエトキシド、チタン
テトライソプロポキシドは加水分解反応速度が速く、大
気中の水分等に対して不安定であり、ドライボックス中
で取り扱わなければならない等、生産工程上のハンドリ
ングが難しいという問題点がある。However, these manufacturing methods have a narrow particle size control range of 0.1 to 1. Only spherical titania of about m size can be produced,
When used as a cosmetic pigment, there is a problem that it gets into the pores and skin grooves. In addition, titanium tetraethoxide and titanium tetraisopropoxide have a fast hydrolysis reaction rate, are unstable against atmospheric moisture, etc., and are difficult to handle during the production process, such as having to be handled in a dry box. There is a problem.
また、硫酸チタニルと尿素を用い、均−沈澱法を利用し
てチタニアを製造する方法〔日本セラミック協会年会予
稿集、 １９０（１９８９）Ｅ等も知られているが、生
成したチタニア粒子の純度が悪いという問題点がある。In addition, a method for producing titania using titanyl sulfate and urea using a homogeneous precipitation method [Proceedings of the Annual Meeting of the Ceramic Society of Japan, 190 (1989) E, etc.] is also known, but the purity of the produced titania particles is There is a problem that it is bad.
そこで、本発明者らは、上記問題点を解決するために鋭
意研究を重ねた結果、チタンテトラ−ｎ−ブトキシドを
エタノール、■−プロパノール又はブタノール溶媒中で
アンモニアの存在下に加水分解することにより、所望の
粒径の高純度の単分散状チタニアを安定的に製造するこ
とができることを見出し、本発明を完成するに至った。Therefore, as a result of extensive research in order to solve the above problems, the present inventors found that titanium tetra-n-butoxide was hydrolyzed in ethanol, -propanol or butanol solvent in the presence of ammonia. They discovered that it is possible to stably produce highly pure monodispersed titania with a desired particle size, and have completed the present invention.
従って、本発明の目的は、０．１〜５趨の範囲の任意の
粒径の高純度単分散球状チタニア粒子を安定的に製造す
る方法を提供することにある。Therefore, an object of the present invention is to provide a method for stably producing high purity monodisperse spherical titania particles having an arbitrary particle size in the range of 0.1 to 5.
すなわち、本発明は、チタンテトラ−ｎ−ブトキシドを
アルコール溶媒中でアンモニア触媒の存在下に加水分解
することを特徴とする球状チタニアの製造方法である。That is, the present invention is a method for producing spherical titania characterized by hydrolyzing titanium tetra-n-butoxide in an alcohol solvent in the presence of an ammonia catalyst.
以下、本発明の球状チタニアの製造方法について具体的
に説明する。Hereinafter, the method for producing spherical titania of the present invention will be specifically explained.
チタニア原料として使用できるチタンアルコキシドは、
反応速度の制御のし易さ、及び湿気に対する安定性の高
さ等の点でチタンテトラ−ｎ−ブトキシドを用いる。Titanium alkoxides that can be used as titania raw materials are:
Titanium tetra-n-butoxide is used because it is easy to control the reaction rate and has high stability against moisture.
本発明において、加水分解に使用する水はチタンテトラ
−ｎ−ブトキシド１モルに対して２モル以上好ましくは
２〜１５モルの範囲である。この範囲より少ないと加水
分解反応が完全に進行しない。In the present invention, the amount of water used for hydrolysis is 2 mol or more, preferably 2 to 15 mol, per 1 mol of titanium tetra-n-butoxide. If the amount is less than this range, the hydrolysis reaction will not proceed completely.
また、この範囲より多いと反応が急激に起こり、凝集体
が生成し易くなるため、水の添加を非常にゆっくりと行
わねばならなくなり、工業的に不利となるので好ましく
ない。Furthermore, if the amount exceeds this range, the reaction occurs rapidly and aggregates are likely to be formed, making it necessary to add water very slowly, which is undesirable from an industrial standpoint.
ところで、チタニアの等電位点はｐＨ７付近であり、酸
又はアルカリの添加によりｐＨを７より大きくするか、
又は小さくすることによりセータ電位を大きくすること
ができる。本発明においては、ゼータ電位を大きくして
粒子間の凝集を防ぎ、安定なゾルを形成すると共に、加
水分解及び縮合反応を速めるためにアンモニアを添加す
る。反応触媒として用いられるアンモニアは、チタンテ
トラ−ｎ−ブトキシド１モルに対して、０．０５〜２モ
ル、好ましくは０．１〜２モルの範囲であり、このとき
のおよそのｐＨは９〜１２である。アンモニアの添加量
がこの範囲より少ないとゼータ電位を十分に大きくでき
ず、粒子間の凝集を防ぐ十分な効果が得られない。また
、この範囲より多いと反応が急激に起こり、凝集体が生
成し易くなる。By the way, the equipotential point of titania is around pH 7, and the pH can be made higher than 7 by adding acid or alkali, or
Alternatively, the theta potential can be increased by decreasing it. In the present invention, ammonia is added to increase the zeta potential to prevent agglomeration between particles and form a stable sol, and to speed up hydrolysis and condensation reactions. The amount of ammonia used as a reaction catalyst is in the range of 0.05 to 2 mol, preferably 0.1 to 2 mol, per 1 mol of titanium tetra-n-butoxide, and the approximate pH at this time is 9 to 12. It is. If the amount of ammonia added is less than this range, the zeta potential cannot be sufficiently increased, and a sufficient effect of preventing aggregation between particles cannot be obtained. Moreover, if the amount exceeds this range, the reaction will occur rapidly and aggregates will be likely to be formed.
また、チタンテトラ−ｎ−ブトキシド以外のチタンテト
ラアルコキシドを用いた場合、アンモニアを添加すると
加水分解及び縮合反応が速くなりすぎて粒子が球形に成
長しないという問題があるため、ゼータ電位を大きくし
て粒子間の凝集を防ぐという手法が使えない。In addition, when titanium tetraalkoxide other than titanium tetra-n-butoxide is used, there is a problem that when ammonia is added, the hydrolysis and condensation reactions become too fast and the particles do not grow into spherical shapes, so the zeta potential is increased. Methods to prevent agglomeration between particles cannot be used.
なお、アンモニアは、アンモニウムガスであっても水溶
液としても用いてもよいが、水溶液として用いた場合は
、水溶液中に含まれる水は上記加水分解用の水として扱
われる。Note that ammonia may be used as ammonium gas or as an aqueous solution, but when used as an aqueous solution, the water contained in the aqueous solution is treated as the water for the above-mentioned hydrolysis.
また、本発明において使用できるアルコール溶媒は、エ
タノール、１−プロパノール及びｎ−ブタノールである
。これら以外の溶媒、例えばメタノールを用いると、チ
タンメトキシドが析出してしまい、ｎ−ペンチルアルコ
ール等炭素数５以上の第１アルコールを用いると、水と
の相溶性が極端に悪く、添加する水の量が制約を受ける
ので好ましくない。また、５ｅｅ−ブタノール等の第２
アルコールを用いると加水分解速度が速くなり、チタニ
ア粒子の凝集物が生成し易くなる。Further, alcohol solvents that can be used in the present invention are ethanol, 1-propanol, and n-butanol. If a solvent other than these, such as methanol, is used, titanium methoxide will precipitate, and if a primary alcohol with a carbon number of 5 or more, such as n-pentyl alcohol, is used, the compatibility with water will be extremely poor, and the water added will result in the precipitation of titanium methoxide. This is not preferable because the amount of In addition, secondary compounds such as 5ee-butanol
When alcohol is used, the rate of hydrolysis becomes faster and aggregates of titania particles are more likely to be formed.
アルコール溶媒の使用量は、チタンテトラ−ｎブトキシ
ド１モルに対して１〜２０１．好ましくは３〜１２ｆで
ある。アルコール溶媒の使用量が１１に満たない場合は
凝集粒子が生成し易く、また、２０１を越えると粒子の
生成速度が遅くなり、実用性に乏しくなる。The amount of alcohol solvent used is 1 to 201.0% per mole of titanium tetra-n-butoxide. Preferably it is 3 to 12 f. If the amount of alcohol solvent used is less than 11, aggregated particles are likely to be produced, and if it exceeds 201, the rate of particle production becomes slow, making it impractical.
本発明の加水分解反応は、チタンテトラ−ｎ−ブトキシ
ドのアルコール溶液に水を添加することにより行うこと
ができ、反応が完結した後、濾過、乾燥して単分散球状
チタニア粒子を得ることができる。The hydrolysis reaction of the present invention can be carried out by adding water to an alcoholic solution of titanium tetra-n-butoxide, and after the reaction is completed, it can be filtered and dried to obtain monodisperse spherical titania particles. .
チタニアの粒子径は加水分解反応の条件を適宜選択する
ことにより制御することができる。例えば、水の濃度を
低くすると粒径を大きくすることができ、濃度を高くす
れば粒径を小さくすることができる。また、アンモニア
の濃度を低くすると粒径を大きくすることができ、濃度
を高くすれば粒径を小さくすることができる。更に、水
又はアルコールで希釈した水の滴下速度を小さくすると
粒径を大きくすることができ、滴下速度を大きく、又は
、−括添加すると粒径を小さくすることができる。The particle size of titania can be controlled by appropriately selecting the conditions for the hydrolysis reaction. For example, decreasing the concentration of water can increase the particle size, and increasing the concentration can decrease the particle size. Further, if the concentration of ammonia is lowered, the particle size can be increased, and if the concentration is increased, the particle size can be decreased. Further, the particle size can be increased by decreasing the dropping rate of water or water diluted with alcohol, and the particle size can be decreased by increasing the dropping rate or adding at once.
前述したように、生成するチタニア粒子のゼータ電位を
大きくして、粒子間の凝集を防ぐためには、アンモニア
の添加量は多い方が好ましい。したがって、大きなチタ
ニア粒子を製造するためには、アンモニア濃度は高く保
ち、水の濃度及び滴下速度で制御することが好ましい。As described above, in order to increase the zeta potential of the titania particles to be produced and prevent agglomeration between particles, it is preferable to add a large amount of ammonia. Therefore, in order to produce large titania particles, it is preferable to keep the ammonia concentration high and control it by controlling the water concentration and dropping rate.
以下、実施例及び比較例に基づいて、本発明を更に詳し
く説明する。Hereinafter, the present invention will be explained in more detail based on Examples and Comparative Examples.
実施例１〜５
チタンテトラ−ｎ−ブトキシド１モルに対して、アルコ
ールを第１表に示す割合で反応容器に仕込み、そこに水
とアンモニアとアルコールを第１表に示す割合で混合し
たものを添加した後、静置して沈澱したチタニア粒子を
得た。Examples 1 to 5 For 1 mole of titanium tetra-n-butoxide, alcohol was charged into a reaction vessel in the proportions shown in Table 1, and water, ammonia, and alcohol were mixed therein in the proportions shown in Table 1. After the addition, the titania particles were left to stand and precipitated.
得られた球状チタニア粒子を走査型電子顕微鏡（ＳＥＭ
）で観察したところ、各粒子はほぼ真球であった。平均
粒子径を第１表に示す。The obtained spherical titania particles were subjected to a scanning electron microscope (SEM).
), each particle was almost perfectly spherical. The average particle diameter is shown in Table 1.
比較例１
チタンテトライソプロポキシド１モルに対して、イソプ
ロパノールを１００モルの割合で反応容器に仕込み、そ
こに水とアンモニアとイソプロパノールを混合したもの
を１０モル／ｈの速度で添加した後静置して沈澱したチ
タニア粒子を濾過、乾燥した後、ＳＥＭで観察したとこ
ろ、サブミクロンのチタニア粒子の凝集物であった。Comparative Example 1 Isopropanol was charged into a reaction vessel at a ratio of 100 mol to 1 mol of titanium tetraisopropoxide, and a mixture of water, ammonia, and isopropanol was added thereto at a rate of 10 mol/h, and then left to stand. The precipitated titania particles were filtered and dried, and then observed with a SEM, which revealed that they were aggregates of submicron titania particles.
比較例２
チタンテトラ−ｎ−ブトキシド１モルに対して、５ｅｃ
−ブタノールを８５モルの割合で反応容器に仕込み、そ
こに水３モルとアンモニア０．４モルと５ｅｃ−ブタノ
ール１５モルを混合したものを一括添加し、沈澱したチ
タニア粒子を濾過、乾燥した後、ＳＥＭで観察したとこ
ろミサブミクロンのチタニア粒子の凝集物であった。Comparative Example 2 5ec for 1 mole of titanium tetra-n-butoxide
- Butanol was charged in a reaction container at a ratio of 85 moles, a mixture of 3 moles of water, 0.4 moles of ammonia, and 15 moles of 5ec-butanol was added thereto at once, and the precipitated titania particles were filtered and dried. When observed with SEM, it was found to be an aggregate of submicron titania particles.
比較例３
チタンテトラ−ｎ−ブトキシド１モルに対して、ｎ−フ
タノール１５モルを混合したものを、２モル／ｈの速度
で、反応容器中の水６モルとアンモニア０゜１モルとｎ
−ブタノール８５モルに滴下し、沈澱したチタニア粒子
を濾過、乾燥した後、ＳＥＭで観察したところ、３趨程
度の球状粒子とサブミクロンのチタニア粒子の凝集物と
の混合物であった。Comparative Example 3 A mixture of 15 moles of n-phthanol and 1 mole of titanium tetra-n-butoxide was mixed with 6 moles of water, 0.1 mole of ammonia, and 1 mole of ammonia in a reaction vessel at a rate of 2 moles/h.
- When the precipitated titania particles were added dropwise to 85 mol of butanol and filtered and dried, they were observed by SEM and were found to be a mixture of about 3 spherical particles and an aggregate of submicron titania particles.
本発明によれば、０．１〜５趨の範囲の任意の粒径を有
する高純度の単分散球状チタニアを安定的に製造するこ
とができ、このような高純度の単分散球状チタニア粒子
は化粧品、触媒、吸着剤、光半導体として特に有用であ
る。According to the present invention, it is possible to stably produce high-purity monodisperse spherical titania having an arbitrary particle size in the range of 0.1 to 5, and such high-purity monodisperse spherical titania particles It is particularly useful in cosmetics, catalysts, adsorbents, and optical semiconductors.
特許出願人 新日鐵化学株式会社Patent applicant: Nippon Steel Chemical Co., Ltd.
Claims (3)
中でアンモニア触媒の存在下に加水分解することを特徴
とする球状チタニアの製造方法。(1) A method for producing spherical titania, which comprises hydrolyzing titanium tetra-n-butoxide in an alcohol solvent in the presence of an ammonia catalyst.
ル、プロパノール又はｎ−ブタノールを用いることを特
徴とする請求項１記載の球状チタニアの製造方法。(2) The method for producing spherical titania according to claim 1, characterized in that ethanol, propanol, or n-butanol is used as the alcohol solvent for the hydrolysis reaction.
に水を添加することを特徴とする請求項１記載の球状チ
タニアの製造方法。(3) The method for producing spherical titania according to claim 1, characterized in that water is added to the alcohol solution of titanium tetra-n-butoxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20387790A JPH0489318A (en) | 1990-08-02 | 1990-08-02 | Production of spherical titania |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20387790A JPH0489318A (en) | 1990-08-02 | 1990-08-02 | Production of spherical titania |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0489318A true JPH0489318A (en) | 1992-03-23 |
Family
ID=16481197
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20387790A Pending JPH0489318A (en) | 1990-08-02 | 1990-08-02 | Production of spherical titania |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0489318A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009001472A (en) * | 2007-06-25 | 2009-01-08 | Seiko Epson Corp | Functional material and its manufacturing process |
| US7601327B2 (en) | 2004-11-23 | 2009-10-13 | E.I. Du Pont De Nemours And Company | Mesoporous oxide of hafnium |
| US7601326B2 (en) | 2004-11-23 | 2009-10-13 | E. I. Du Pont De Nemours And Company | Mesoporous oxide of zirconium |
| US7858066B2 (en) | 2007-05-08 | 2010-12-28 | E.I. Du Pont De Nemours And Company | Method of making titanium dioxide particles |
| US7988947B2 (en) | 2004-11-23 | 2011-08-02 | E. I. Du Pont De Nemours And Company | Mesoporous oxide of titanium |
| US8377414B2 (en) | 2004-11-23 | 2013-02-19 | E I Du Pont De Nemours And Company | Mesoporous amorphous oxide of titanium |
| JP2013530121A (en) * | 2010-05-26 | 2013-07-25 | インダストリ−ユニヴァーシティ コオペレーション ファウンデイション ソガン ユニヴァーシティ | NOVEL MANUFACTURING METHOD OF TITANIUM DIOXIDE PARTICLES AND TITANIUM DIOXIDE PARTICLES BY THE |
-
1990
- 1990-08-02 JP JP20387790A patent/JPH0489318A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7601327B2 (en) | 2004-11-23 | 2009-10-13 | E.I. Du Pont De Nemours And Company | Mesoporous oxide of hafnium |
| US7601326B2 (en) | 2004-11-23 | 2009-10-13 | E. I. Du Pont De Nemours And Company | Mesoporous oxide of zirconium |
| US7988947B2 (en) | 2004-11-23 | 2011-08-02 | E. I. Du Pont De Nemours And Company | Mesoporous oxide of titanium |
| US8221655B2 (en) | 2004-11-23 | 2012-07-17 | E. I. Du Pont De Nemours And Company | Mesoporous oxide of titanium |
| US8377414B2 (en) | 2004-11-23 | 2013-02-19 | E I Du Pont De Nemours And Company | Mesoporous amorphous oxide of titanium |
| US7858066B2 (en) | 2007-05-08 | 2010-12-28 | E.I. Du Pont De Nemours And Company | Method of making titanium dioxide particles |
| JP2009001472A (en) * | 2007-06-25 | 2009-01-08 | Seiko Epson Corp | Functional material and its manufacturing process |
| JP2013530121A (en) * | 2010-05-26 | 2013-07-25 | インダストリ−ユニヴァーシティ コオペレーション ファウンデイション ソガン ユニヴァーシティ | NOVEL MANUFACTURING METHOD OF TITANIUM DIOXIDE PARTICLES AND TITANIUM DIOXIDE PARTICLES BY THE |
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