JP2002047012A - Method of manufacturing titanium oxide - Google Patents
Method of manufacturing titanium oxideInfo
- Publication number
- JP2002047012A JP2002047012A JP2000230779A JP2000230779A JP2002047012A JP 2002047012 A JP2002047012 A JP 2002047012A JP 2000230779 A JP2000230779 A JP 2000230779A JP 2000230779 A JP2000230779 A JP 2000230779A JP 2002047012 A JP2002047012 A JP 2002047012A
- Authority
- JP
- Japan
- Prior art keywords
- titanium
- titanium oxide
- ammonia
- titanium compound
- purity
- 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
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 31
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title abstract description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 40
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 24
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 11
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 abstract description 16
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 abstract description 4
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 abstract description 4
- 230000001678 irradiating effect Effects 0.000 abstract description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 12
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 description 6
- 239000001569 carbon dioxide Substances 0.000 description 6
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000001747 exhibiting effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical compound [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005468 ion implantation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 102100033040 Carbonic anhydrase 12 Human genes 0.000 description 1
- 102100033041 Carbonic anhydrase 13 Human genes 0.000 description 1
- 102100032566 Carbonic anhydrase-related protein 10 Human genes 0.000 description 1
- 102100033029 Carbonic anhydrase-related protein 11 Human genes 0.000 description 1
- LLQPHQFNMLZJMP-UHFFFAOYSA-N Fentrazamide Chemical compound N1=NN(C=2C(=CC=CC=2)Cl)C(=O)N1C(=O)N(CC)C1CCCCC1 LLQPHQFNMLZJMP-UHFFFAOYSA-N 0.000 description 1
- 101000867855 Homo sapiens Carbonic anhydrase 12 Proteins 0.000 description 1
- 101000867860 Homo sapiens Carbonic anhydrase 13 Proteins 0.000 description 1
- 101000867836 Homo sapiens Carbonic anhydrase-related protein 10 Proteins 0.000 description 1
- 101000867841 Homo sapiens Carbonic anhydrase-related protein 11 Proteins 0.000 description 1
- 101001075218 Homo sapiens Gastrokine-1 Proteins 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- -1 for example Chemical compound 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Physical Water Treatments (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は酸化チタンの製造方
法に関するものであり、詳細には、ＮＯｘや有機溶剤の
分解除去、河川や湖沼の清浄化に用いられる光触媒体と
して利用可能な酸化チタンの製造方法に関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing titanium oxide, and more particularly, to a method for producing titanium oxide which can be used as a photocatalyst used for decomposing and removing NOx and organic solvents and for cleaning rivers and lakes. It relates to a manufacturing method.
【０００２】[0002]
【従来の技術】酸化チタンが示す光触媒作用によって、
大気中の悪臭物質や水中の有機溶剤、界面活性剤を分解
除去することが検討されている。最近では、汎用性、利
便性から光源に可視光線を使った分解除去方法が注目さ
れ、可視光線を照射したときに高い触媒活性を示す酸化
チタンの開発が期待されている。2. Description of the Related Art The photocatalysis of titanium oxide is
Decomposition and removal of atmospheric odor substances, organic solvents and surfactants in water are being studied. Recently, attention has been paid to a decomposition and removal method using visible light as a light source from the viewpoint of versatility and convenience, and development of titanium oxide exhibiting high catalytic activity when irradiated with visible light is expected.
【０００３】このような酸化チタンの製造方法として、
例えば、酸化チタンにＶ、Ｃｒのような金属のイオンを
イオン注入法で導入する方法が知られている。しかし、
イオン注入法では、真空容器を備えた装置が必要であっ
た。また、製造装置の大型化が難しく、量産化が難しい
ため、製造コストが高くなることがあった。[0003] As a method for producing such titanium oxide,
For example, a method is known in which ions of a metal such as V and Cr are introduced into titanium oxide by an ion implantation method. But,
In the ion implantation method, a device equipped with a vacuum vessel was required. In addition, since it is difficult to increase the size of the manufacturing apparatus and to mass-produce it, the manufacturing cost may be increased.
【０００４】[0004]
【発明が解決しようとする課題】本発明の目的は、可視
光線を照射することによって高い触媒活性を示す酸化チ
タンを、真空容器を備えた特定の装置を用いることなく
簡易に製造する方法を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a method for easily producing titanium oxide having high catalytic activity by irradiating visible light without using a specific apparatus equipped with a vacuum vessel. Is to do.
【０００５】[0005]
【課題を解決するための手段】本発明者等は酸化チタン
の製造方法について検討を行った結果、本発明を完成す
るに至った。Means for Solving the Problems The present inventors have studied the method for producing titanium oxide, and as a result, have completed the present invention.
【０００６】すなわち本発明は、純度９９％以上のチタ
ン化合物と、該チタン化合物を中和するための必要量を
超える量のアンモニアを混合し反応させ、得られた生成
物を焼成することを特徴とする酸化チタンの製造方法を
提供するものである。That is, the present invention is characterized in that a titanium compound having a purity of 99% or more and an amount of ammonia exceeding a necessary amount for neutralizing the titanium compound are mixed and reacted, and the obtained product is calcined. And a method for producing titanium oxide.
【０００７】[0007]
【発明の実施の形態】以下、本発明を詳細に説明する。
本発明で用いられるチタン化合物としては、アンモニア
との反応により水酸化チタンを生成するチタンの化合物
であればよく、例えば、三塩化チタン〔ＴｉＣｌ3〕、
四塩化チタン〔ＴｉＣｌ4〕、硫酸チタン〔Ｔｉ（Ｓ
Ｏ4）2・ｍＨ2Ｏ、０≦ｍ≦２０〕、オキシ硫酸チタン
〔ＴｉＯＳＯ4・ｎＨ2Ｏ、０≦ｎ≦２０〕、オキシ塩化
チタン〔ＴｉＯＣｌ2〕が挙げられ、中でも、オキシ硫
酸チタンの適用が推奨される。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.
The titanium compound used in the present invention may be any titanium compound that produces titanium hydroxide by reacting with ammonia, for example, titanium trichloride [TiCl 3 ],
Titanium tetrachloride [TiCl 4 ], titanium sulfate [Ti (S
O 4 ) 2 .mH 2 O, 0 ≦ m ≦ 20], titanium oxysulfate [TiOSO 4 .nH 2 O, 0 ≦ n ≦ 20] and titanium oxychloride [TiOCl 2 ]. Is recommended.
【０００８】これらのチタン化合物は、純度が高いもの
が好ましく、純度９９重量％以上である。チタン化合物
の純度が９９重量％未満であると、高い光触媒活性を示
す酸化チタンを得ることが困難となる。チタン化合物の
純度は、例えば、三塩化チタンではＪＩＳ Ｋ８４０１
−１９９２、四塩化チタンではＪＩＳ Ｋ８４６０−１
９９２、の方法により求めることができ、オキシ硫酸チ
タンではＴｉＯ2、ＳＯ3の主要成分およびＳｉＯ2、Ｐ2
Ｏ5、Ｎｂ2Ｏ5のような他の成分を測定し、それぞれの
含有量をＡ1、Ａ2、Ａ3、Ａ4、Ａ5とし、下式 純度（％）＝〔（Ａ1＋Ａ2）／（Ａ1＋Ａ2＋Ａ3＋Ａ4＋
Ａ5）〕×１００ により算出することができる。These titanium compounds preferably have high purity, and have a purity of 99% by weight or more. If the purity of the titanium compound is less than 99% by weight, it becomes difficult to obtain titanium oxide having high photocatalytic activity. The purity of the titanium compound is, for example, JIS K8401 for titanium trichloride.
-1992, JIS K8460-1 for titanium tetrachloride
992, and in titanium oxysulfate, the main components of TiO 2 and SO 3 and SiO 2 , P 2
Other components such as O 5 and Nb 2 O 5 were measured, and their contents were defined as A 1 , A 2 , A 3 , A 4 , and A 5 , respectively, and the following purity (%) = [(A 1 + A 2) / (A 1 + A 2 + A 3 + A 4 +
A 5 )] × 100.
【０００９】本発明では、上で示したチタン化合物と、
該チタン化合物を中和するための必要量を超える量のア
ンモニアを混合し反応させる。アンモニアの量は、チタ
ン化合物を中和するための必要量に対し、通常１．２倍
以上、好ましくは２倍以上であり、また２０倍以下、さ
らには１０倍以下が適当である。ここで、チタン化合物
を中和するために必要なアンモニア量とは、水の存在下
でチタン化合物を水酸化チタンに変えるのに必要な化学
量論量のアンモニアを意味し、具体的には、チタン化合
物１モルあたりのアンモニアのモル数で表して、そのチ
タン化合物１分子中に含まれる酸基の数Ｂとその価数Ｃ
を掛けた値（Ｂ×Ｃ）となる。例えば、三塩化チタンで
は３モル倍、四塩化チタンでは４モル倍、硫酸チタンで
は４モル倍、オキシ硫酸チタンでは２モル倍、オキシ塩
化チタンでは２モル倍のアンモニアが中和のための必要
量となる。チタン化合物を中和するための必要量を超え
る量のアンモニアを反応に用いることによって、可視光
線の照射によって高い触媒活性を示す酸化チタンを得る
ことができる。[0009] In the present invention, the titanium compound shown above,
An amount of ammonia exceeding a necessary amount for neutralizing the titanium compound is mixed and reacted. The amount of ammonia is usually 1.2 times or more, preferably 2 times or more, and more preferably 20 times or less, and more preferably 10 times or less, with respect to the amount required for neutralizing the titanium compound. Here, the amount of ammonia necessary to neutralize the titanium compound means a stoichiometric amount of ammonia required to convert the titanium compound to titanium hydroxide in the presence of water, and specifically, The number B of acid groups contained in one molecule of the titanium compound and the valence C thereof, expressed as the number of moles of ammonia per mole of the titanium compound
Is multiplied by (B × C). For example, the required amount of ammonia for neutralization is 3 mole times for titanium trichloride, 4 mole times for titanium tetrachloride, 4 mole times for titanium sulfate, 2 mole times for titanium oxysulfate, and 2 mole times for titanium oxychloride. Becomes By using ammonia in the reaction in an amount exceeding the amount required for neutralizing the titanium compound, it is possible to obtain titanium oxide having high catalytic activity by irradiation with visible light.
【００１０】チタン化合物とアンモニアとの反応は、通
常６０℃以下の温度で行われる。この際の温度は低いほ
ど好ましく、例えば、４０℃以下、さらには−５℃以下
が一層好ましい。反応は、例えば、反応容器にチタン化
合物を入れ、攪拌下、アンモニア水のようなアンモニア
を添加し、混合する方法、反応容器にアンモニアを入
れ、攪拌下、チタン化合物を添加し、混合する方法、ま
たは、反応容器にチタン化合物とアンモニアとを同時に
導入し、混合する方法で行うことができる。[0010] The reaction between the titanium compound and ammonia is usually carried out at a temperature of 60 ° C or lower. The temperature at this time is preferably as low as possible, for example, 40 ° C. or lower, more preferably −5 ° C. or lower. The reaction is, for example, a method of adding a titanium compound to a reaction vessel and adding ammonia such as aqueous ammonia under stirring and mixing, a method of adding ammonia to a reaction vessel and adding the titanium compound under stirring and mixing, Alternatively, the method can be carried out by simultaneously introducing and mixing a titanium compound and ammonia into a reaction vessel.
【００１１】チタン化合物とアンモニア水とを混合して
反応させるときには、次工程の焼成の前に、生成物であ
る水酸化チタンを含むスラリーを固液分離することが好
ましい。固液分離することによって、高い光触媒活性を
示す酸化チタンを得ることができる。固液分離は、例え
ば、濾過、デカンテーションで行うことができる。When the titanium compound and the aqueous ammonia are mixed and reacted, it is preferable to separate the slurry containing the product, titanium hydroxide, into solid and liquid before firing in the next step. By performing solid-liquid separation, titanium oxide exhibiting high photocatalytic activity can be obtained. The solid-liquid separation can be performed by, for example, filtration and decantation.
【００１２】次に、反応により得られた生成物を焼成す
る。焼成は、３００℃以上、さらには３５０℃以上で行
うことが好ましく、６００℃以下、さらには５００℃以
下で行うことが適当である。焼成温度が高くなり過ぎる
と、得られる酸化チタンの触媒活性が低下することがあ
る。Next, the product obtained by the reaction is calcined. The firing is preferably performed at 300 ° C. or higher, more preferably 350 ° C. or higher, and suitably 600 ° C. or lower, and more preferably 500 ° C. or lower. If the firing temperature is too high, the catalytic activity of the resulting titanium oxide may decrease.
【００１３】本発明の酸化チタンの製造方法では、通
常、結晶構造がアナターゼ型である粒子状酸化チタンが
得られる。この酸化チタンは波長が４３０ｎｍ以上であ
る可視光線の照射によって高い触媒活性を示すので、そ
のまま、またはこれを成形加工することにより、大気中
のＮＯｘの分解、悪臭物質・カビの分解除去、または水
中の有機溶剤の分解除去に適用することができる。In the method for producing titanium oxide of the present invention, a particulate titanium oxide having an anatase crystal structure is usually obtained. This titanium oxide exhibits high catalytic activity when irradiated with visible light having a wavelength of 430 nm or more. Therefore, as it is or by molding it, it can decompose NOx in the air, decompose and remove malodorous substances and mold, or use it in water. Can be applied to the decomposition and removal of organic solvents.
【００１４】[0014]
【実施例】以下、実施例により本発明をさらに詳細に説
明するが、本発明は本実施例に限定されるものではな
い。 実施例１ １Ｌフラスコに水４０ｇを入れた後、攪拌下、ＳｉＯ2
含有量０．０１１重量％、Ｐ2Ｏ5含有量０．０３４重量
％、Ｎｂ2Ｏ5含有量０．０３重量％、純度９９．９３％
のオキシ硫酸チタン水和物（添川理化学製）６０ｇを添
加し溶解した。この溶液を７０℃のエバポレーターによ
り水を除去して濃縮してオキシ硫酸チタンを得た。一
方、２５％アンモニア水（試薬特級、和光純薬工業製）
２７０ｇを水１８０ｇで希釈し１５％アンモニア水を調
製した。この１５％アンモニア水を−３０℃の冷却槽で
冷却した後、４００ｒｐｍで攪拌しながら、そこに、上
で得られたオキシ硫酸チタンを添加、混合し、反応させ
てスラリーを得た。このスラリーを濾過し、得られた水
酸化チタンを洗浄、乾燥した後、４００℃の空気中で１
時間焼成して、粒子状酸化チタンを得た。このとき、ア
ンモニアの量は、用いたオキシ硫酸チタンを中和するた
めの必要量の８倍であった。EXAMPLES The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples. Example 1 After charging 40 g of water into a 1 L flask, SiO 2 was stirred under stirring.
Content 0.011% by weight, P 2 O 5 content 0.034% by weight, Nb 2 O 5 content 0.03% by weight, purity 99.93%
60 g of titanium oxysulfate hydrate (manufactured by Soekawa Rikagaku Co., Ltd.) was added and dissolved. The solution was concentrated by removing water with an evaporator at 70 ° C. to obtain titanium oxysulfate. On the other hand, 25% ammonia water (special grade reagent, manufactured by Wako Pure Chemical Industries)
270 g was diluted with 180 g of water to prepare 15% ammonia water. After cooling this 15% ammonia water in a cooling bath at -30 ° C, the titanium oxysulfate obtained above was added thereto, mixed and reacted while stirring at 400 rpm to obtain a slurry. This slurry was filtered, and the obtained titanium hydroxide was washed and dried.
After firing for a time, particulate titanium oxide was obtained. At this time, the amount of ammonia was eight times the necessary amount for neutralizing the used titanium oxysulfate.
【００１５】密閉式のガラス製反応容器（直径８ｃｍ、
高さ１０ｃｍ、容量約０．５Ｌ）内に、直径５ｃｍのガ
ラス製シャーレを設置し、そのシャーレ上に、上で得ら
れた粒子状酸化チタン０．３ｇを置いた。反応容器内を
酸素と窒素との体積比が１：４である混合ガスで満た
し、アセトアルデヒドを１３．４μｍｏｌ封入し、反応
容器の外から可視光線を照射した。可視光線の照射に
は、５００Ｗキセノンランプ（商品名：オプティカルモ
ジュレックスＳＸ−ＵＩ５００ＸＱ、ランプＵＸＬ−５
００ＳＸ、ウシオ電機製）に、波長約４３０ｎｍ以下の
紫外線をカットするフィルター（商品名：Ｙ−４５、東
芝硝子製）と波長約８３０ｎｍ以上の赤外線をカットす
るフィルター（商品名：スーパーコールドフィルター、
ウシオ電機製、）とを装着したものを光源として用い
た。可視光線の照射によりアセトアルデヒドが分解する
と、二酸化炭素が発生するので二酸化炭素の濃度を光音
響マルチガスモニタ（１３１２型、ＩＮＮＯＶＡ製）で
経時的に測定し、濃度変化より算出した二酸化炭素の生
成速度により、酸化チタンのアセトアルデヒドに対する
光触媒作用を評価した。この例における二酸化炭素の生
成速度は酸化チタン１ｇあたり１８９．９μｍｏｌ／ｈ
であった。A closed glass reaction vessel (diameter 8 cm,
A glass petri dish having a diameter of 5 cm was placed within a height of 10 cm and a capacity of about 0.5 L), and 0.3 g of the particulate titanium oxide obtained above was placed on the petri dish. The inside of the reaction vessel was filled with a mixed gas having a volume ratio of oxygen to nitrogen of 1: 4, acetaldehyde was filled in at 13.4 μmol, and visible light was irradiated from outside the reaction vessel. For irradiation of visible light, a 500 W xenon lamp (trade name: Optical Modlex SX-UI500XQ, lamp UXL-5)
00SX, manufactured by Ushio Inc.), a filter that cuts ultraviolet rays having a wavelength of about 430 nm or less (trade name: Y-45, manufactured by Toshiba Glass) and a filter that cuts infrared rays having a wavelength of about 830 nm or more (trade name: Super Cold Filter,
Ushio Inc.) was used as the light source. When acetaldehyde is decomposed by irradiation with visible light, carbon dioxide is generated. The concentration of carbon dioxide is measured over time with a photoacoustic multi-gas monitor (Type 1312, manufactured by INNOVA), and the carbon dioxide generation rate is calculated from the change in concentration. The photocatalytic action of titanium oxide on acetaldehyde was evaluated. In this example, the production rate of carbon dioxide was 189.9 μmol / h per 1 g of titanium oxide.
Met.
【００１６】実施例２ １Ｌフラスコに水１００ｇを入れた後、攪拌下、ＳｉＯ
2含有量０．０１１重量％、Ｐ2Ｏ5含有量０．０３４重
量％、Ｎｂ2Ｏ5含有量０．０３重量％、純度９９．９３
％のオキシ硫酸チタン水和物（添川理化学製）６０ｇを
添加し溶解した。この溶液を７０℃のエバポレーターに
より水を除去して濃縮してオキシ硫酸チタンを得た。２
５％アンモニア水（試薬特級、和光純薬工業製）６８ｇ
を−３０℃の冷却槽で冷却した後、４００ｒｐｍで攪拌
しながら、そこに、上で得られたオキシ硫酸チタンを添
加、混合し、反応させてスラリーを得た。このスラリー
を濾過し、得られた水酸化チタンを洗浄、乾燥した後、
４００℃の空気中で１時間焼成して、粒子状酸化チタン
を得た。このとき、アンモニアの量は、用いたオキシ硫
酸チタンを中和するための必要量の２倍であった。上で
得られた粒子状酸化チタンにつき、実施例１と同様にし
てアセトアルデヒドに対する光分解作用を評価した。二
酸化炭素の生成速度は酸化チタン１ｇあたり９３．８８
μｍｏｌ／ｈであった。Example 2 After 100 g of water was put into a 1 L flask, the mixture was mixed with SiO 2 under stirring.
2 content 0.011% by weight, P 2 O 5 content 0.034% by weight, Nb 2 O 5 content 0.03% by weight, purity 99.93
60 g of titanium oxysulfate hydrate (manufactured by Soegawa Rikagaku) was added and dissolved. The solution was concentrated by removing water with an evaporator at 70 ° C. to obtain titanium oxysulfate. 2
68 g of 5% aqueous ammonia (special grade reagent, manufactured by Wako Pure Chemical Industries)
Was cooled in a cooling bath at −30 ° C., and while stirring at 400 rpm, the titanium oxysulfate obtained above was added thereto, mixed and reacted to obtain a slurry. This slurry was filtered, and the obtained titanium hydroxide was washed and dried.
Calcination was performed in air at 400 ° C. for 1 hour to obtain particulate titanium oxide. At this time, the amount of ammonia was twice the amount required for neutralizing the used titanium oxysulfate. With respect to the particulate titanium oxide obtained above, the photolytic action on acetaldehyde was evaluated in the same manner as in Example 1. The production rate of carbon dioxide was 93.88 per gram of titanium oxide.
μmol / h.
【００１７】比較例１ １Ｌフラスコに水３６０ｇを入れた後、攪拌下、ＳｉＯ
2含有量０．０１１重量％、Ｐ2Ｏ5含有量０．０３４重
量％、Ｎｂ2Ｏ5含有量０．０３重量％、純度９９．９３
％のオキシ硫酸チタン水和物（添川理化学製）９０ｇを
添加し溶解した。この溶液を氷水で冷却した後、４００
ｒｐｍで攪拌しながら、２５％アンモニア水５０ｇを添
加、混合し、反応させてスラリーを得た。このスラリー
を濾過し、得られた水酸化チタンを洗浄、乾燥し、４０
０℃の空気中で１時間焼成して、粒子状酸化チタンを得
た。このとき、アンモニアの量は、用いたオキシ硫酸チ
タンを中和するための必要量と同じであった。上で得ら
れた粒子状酸化チタンにつき、実施例１と同様にしてア
セトアルデヒドに対する光分解作用を評価した。二酸化
炭素の生成速度は酸化チタン１ｇあたり０．６６μｍｏ
ｌ／ｈであった。COMPARATIVE EXAMPLE 1 After placing 360 g of water in a 1 L flask, the mixture was mixed with SiO 2 under stirring.
2 content 0.011% by weight, P 2 O 5 content 0.034% by weight, Nb 2 O 5 content 0.03% by weight, purity 99.93
90 g of titanium oxysulfate hydrate (manufactured by Soekawa Rikagaku) was added and dissolved. After cooling this solution with ice water, 400
While stirring at rpm, 50 g of 25% aqueous ammonia was added, mixed and reacted to obtain a slurry. This slurry was filtered, and the obtained titanium hydroxide was washed, dried, and dried.
Calcination was performed in air at 0 ° C. for 1 hour to obtain particulate titanium oxide. At this time, the amount of ammonia was the same as the amount required for neutralizing the used titanium oxysulfate. With respect to the particulate titanium oxide obtained above, the photolytic action on acetaldehyde was evaluated in the same manner as in Example 1. The generation rate of carbon dioxide is 0.66 μmo / g of titanium oxide.
1 / h.
【００１８】[0018]
【発明の効果】本発明によれば、可視光線を照射するこ
とによって高い触媒活性を示す酸化チタンを簡易に製造
することができる。According to the present invention, titanium oxide exhibiting high catalytic activity can be easily produced by irradiating visible light.
フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ０２Ｆ 1/30 Ｃ０２Ｆ 1/30 Ｆターム(参考） 4D037 AA05 AB11 BA16 BB09 CA12 4G047 CA02 CB05 CC03 CD03 4G069 AA02 AA08 AA09 BA04A BA04B BA48A BB01C BB08C BB10C BB20C BC50C BD01C BD02C BD06C BD12C CA05 CA10 CA11 CA13 EA02Y EC22Y FB05 FB08 FB30 FC03 FC07 Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat II (reference) C02F 1/30 C02F 1/30 F term (reference) 4D037 AA05 AB11 BA16 BB09 CA12 4G047 CA02 CB05 CC03 CD03 4G069 AA02 AA08 AA09 BA04A BA04B BA48A BB01C BB08C BB10C BB20C BC50C BD01C BD02C BD06C BD12C CA05 CA10 CA11 CA13 EA02Y EC22Y FB05 FB08 FB30 FC03 FC07
Claims (2)
タン化合物を中和するための必要量を超える量のアンモ
ニアを混合し反応させ、得られた生成物を焼成すること
を特徴とする酸化チタンの製造方法。1. An oxidation method comprising mixing and reacting a titanium compound having a purity of 99% or more with ammonia in an amount exceeding a necessary amount for neutralizing the titanium compound, and calcining the obtained product. Manufacturing method of titanium.
方法。2. The method according to claim 1, wherein the reaction is carried out at a temperature of 60 ° C. or lower.
Priority Applications (10)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000230779A JP2002047012A (en) | 2000-07-31 | 2000-07-31 | Method of manufacturing titanium oxide |
| DE60121261T DE60121261T2 (en) | 2000-07-31 | 2001-03-29 | Process for producing titanium oxide |
| CA002342665A CA2342665A1 (en) | 2000-07-31 | 2001-03-29 | Titanium oxide production process |
| EP01302973A EP1178011B1 (en) | 2000-07-31 | 2001-03-29 | Titanium oxide production process |
| TW090107457A TWI230689B (en) | 2000-07-31 | 2001-03-29 | Titanium oxide production process |
| US09/820,367 US6726891B2 (en) | 2000-07-31 | 2001-03-29 | Titanium oxide production process |
| KR1020010016536A KR100705990B1 (en) | 2000-07-31 | 2001-03-29 | Titanium oxide production process |
| EP05020936A EP1614659A3 (en) | 2000-07-31 | 2001-03-29 | Titanium oxide production process |
| CN011178973A CN1217862C (en) | 2000-07-31 | 2001-03-29 | Method for prepn. of titanium oxide |
| AU31404/01A AU781450B2 (en) | 2000-07-31 | 2001-03-29 | Titanium oxide production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000230779A JP2002047012A (en) | 2000-07-31 | 2000-07-31 | Method of manufacturing titanium oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2002047012A true JP2002047012A (en) | 2002-02-12 |
| JP2002047012A5 JP2002047012A5 (en) | 2007-08-16 |
Family
ID=18723694
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000230779A Pending JP2002047012A (en) | 2000-07-31 | 2000-07-31 | Method of manufacturing titanium oxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2002047012A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1338564A2 (en) | 2002-02-25 | 2003-08-27 | Sumitomo Chemical Co.,Ltd. | Titanium oxide precursor and production method thereof, and production method of titanium oxide using the precursor |
| JP2006312572A (en) * | 2005-05-09 | 2006-11-16 | Nippon Chem Ind Co Ltd | Granular titanium oxide, its manufacturing method and optical glass |
| JP2008516880A (en) * | 2004-10-14 | 2008-05-22 | トクセン ユー．エス．エー．、インコーポレイテッド | Method for synthesizing nano-sized titanium dioxide particles |
| US7521391B2 (en) | 2004-03-17 | 2009-04-21 | Sumitomo Chemical Company, Limited | Coating composition of photocatalyst |
| EP2130587A2 (en) | 2008-06-05 | 2009-12-09 | Sumitomo Chemical Company, Limited | Photocatalyst dispersion liquid and process for producing the same |
| EP2281628A2 (en) | 2009-08-07 | 2011-02-09 | Sumitomo Chemical Company, Limited | Method for producing noble metal-supported photocatalyst particles |
| DE102010045549A1 (en) | 2009-09-16 | 2011-08-25 | Sumitomo Chemical Company, Limited | Photocatalyst composite and using this photocatalytically active product |
| CN113842854A (en) * | 2021-08-24 | 2021-12-28 | 深圳市银宝山新科技股份有限公司 | Reaction device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1338564A2 (en) | 2002-02-25 | 2003-08-27 | Sumitomo Chemical Co.,Ltd. | Titanium oxide precursor and production method thereof, and production method of titanium oxide using the precursor |
| US7521391B2 (en) | 2004-03-17 | 2009-04-21 | Sumitomo Chemical Company, Limited | Coating composition of photocatalyst |
| JP2008516880A (en) * | 2004-10-14 | 2008-05-22 | トクセン ユー．エス．エー．、インコーポレイテッド | Method for synthesizing nano-sized titanium dioxide particles |
| JP2006312572A (en) * | 2005-05-09 | 2006-11-16 | Nippon Chem Ind Co Ltd | Granular titanium oxide, its manufacturing method and optical glass |
| EP2130587A2 (en) | 2008-06-05 | 2009-12-09 | Sumitomo Chemical Company, Limited | Photocatalyst dispersion liquid and process for producing the same |
| EP2281628A2 (en) | 2009-08-07 | 2011-02-09 | Sumitomo Chemical Company, Limited | Method for producing noble metal-supported photocatalyst particles |
| DE102010045549A1 (en) | 2009-09-16 | 2011-08-25 | Sumitomo Chemical Company, Limited | Photocatalyst composite and using this photocatalytically active product |
| CN113842854A (en) * | 2021-08-24 | 2021-12-28 | 深圳市银宝山新科技股份有限公司 | Reaction device |
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