JPH02196028A - Production of titanium oxide fine powder - Google Patents
Production of titanium oxide fine powderInfo
- Publication number
- JPH02196028A JPH02196028A JP1012982A JP1298289A JPH02196028A JP H02196028 A JPH02196028 A JP H02196028A JP 1012982 A JP1012982 A JP 1012982A JP 1298289 A JP1298289 A JP 1298289A JP H02196028 A JPH02196028 A JP H02196028A
- Authority
- JP
- Japan
- Prior art keywords
- titanium oxide
- titanium
- powder
- fine powder
- soln
- 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.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 41
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000010936 titanium Substances 0.000 claims abstract description 6
- 239000012452 mother liquor Substances 0.000 claims abstract description 5
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 4
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- -1 Titanium halide Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract description 2
- 239000002341 toxic gas Substances 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 3
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000011882 ultra-fine particle Substances 0.000 description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 238000009835 boiling Methods 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 4
- 238000000635 electron micrograph Methods 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 210000003127 knee Anatomy 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 241000555825 Clupeidae Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004597 plastic additive Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 235000019512 sardine Nutrition 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 229940035289 tobi Drugs 0.000 description 1
- NLVFBUXFDBBNBW-PBSUHMDJSA-N tobramycin Chemical compound N[C@@H]1C[C@H](O)[C@@H](CN)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O[C@@H]2[C@@H]([C@@H](N)[C@H](O)[C@@H](CO)O2)O)[C@H](N)C[C@@H]1N NLVFBUXFDBBNBW-PBSUHMDJSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Composite Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
- 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、酸化チタンの超微粒子から成る粉体の製造方
法に関するものである。本発明により得られる酸化チタ
ン粉体は、ＰＺＴ、ＰＴＣ等の高品位な電子セラミック
スの製造原料や高級化粧品原料、プラスチック添加剤、
塗料、インキ、薬品等の原料として利用されるものであ
る。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing powder consisting of ultrafine particles of titanium oxide. The titanium oxide powder obtained by the present invention can be used as a raw material for manufacturing high-grade electronic ceramics such as PZT and PTC, as a raw material for high-grade cosmetics, as a plastic additive,
It is used as a raw material for paints, inks, chemicals, etc.
〔従来の技術１
酸化チタン粉体の製造方法としては、従来から硫酸法と
塩素法がある。硫酸法は、イルメナイトを硫酸で蒸解し
た後、分離された含水酸化チタンを洗浄の後、８００〜
１０００℃で仮焼、粉砕して粉体としている。塩素法で
は、ＴｉＣβ４を１０００℃位で酸素と反応させて酸化
チタン粒子を生成させて粉体を製造している。[Prior Art 1] Conventionally, methods for producing titanium oxide powder include a sulfuric acid method and a chlorine method. In the sulfuric acid method, after ilmenite is digested with sulfuric acid and the separated hydrous titanium oxide is washed,
It is calcined at 1000°C and ground into powder. In the chlorine method, TiCβ4 is reacted with oxygen at about 1000° C. to produce titanium oxide particles to produce powder.
硫酸法では、含水酸化チタンを１０００℃位の温度で焼
いているため、生成した粒子は大きく成長し、堅く凝集
している。従って、その後の粉砕操作が必要であるが、
機械的粉砕では超微粒子まで粉砕することは現実には不
可能であり、また、粉砕によって不純物のはいる確度が
高く、純度の高い焼結性の優れた粉体な製造することは
困離である。塩素法は純度の高い粉体な作れるが、反応
温度が高いためやはり生成粒子が大きく、活性のある微
粒子粉体な作ることは出来ない。また、塩素法は塩素ガ
スを利用するため反応装置の腐食が激しく、その維持管
理に多くの費用と労力を要する。In the sulfuric acid method, hydrous titanium oxide is baked at a temperature of about 1000°C, so the particles produced grow large and aggregate tightly. Therefore, a subsequent crushing operation is necessary, but
It is actually impossible to grind down to ultra-fine particles using mechanical grinding, and there is a high probability that impurities will be introduced through grinding, making it difficult to produce powder with high purity and excellent sinterability. be. Although the chlorine method can produce powder with high purity, the reaction temperature is high, so the particles produced are large, and it is not possible to produce active microparticle powder. In addition, since the chlorine method uses chlorine gas, the reaction equipment is severely corroded, and its maintenance requires a lot of cost and labor.
上述したように、従来の技術ではいずれも高温熱処理を
しているため、生成された微粒子が強固に結合して大き
な粒子となり、焼結性に優れた高純度の超微粒子粉体を
製造することができなかった。As mentioned above, all conventional techniques involve high-temperature heat treatment, which makes it possible for the generated fine particles to firmly combine to form large particles, producing high-purity ultrafine powder with excellent sinterability. I couldn't do it.
本発明者等は、このような高温での熱処理を必要とせず
に超微粒子粉体を製造できる方法を鋭意研究して本発明
を完成した。The present inventors completed the present invention by intensively researching a method for producing ultrafine powder without requiring heat treatment at such high temperatures.
本発明の目的は、従来技術では得られない焼結性の優れ
た高純度の超微粒子（約０．ｌｌ１ｍ以下）から成る粉
体を提供することにある。An object of the present invention is to provide a powder made of highly pure ultrafine particles (approximately 0.11 m or less) with excellent sinterability that cannot be obtained using conventional techniques.
本発明による超微粒子から成る焼結性の良い粉体な利用
することによって、ＰＬＺＴ、Ｐ Ｚ Ｔ 、
Ｂ ａ Ｔ Ｉ Ｏ３、Ｐ ｂ Ｔ
１ ０ ３Ｔ ｉ Ｏｚ等のエレク１−ロセラミックス
を従来よりも効率良く、しかも従来のものより品質の優
れたものを製造することができる。このほか、本発明に
よる粉体は超微粒子より成るため、高級化粧用原料等に
も使用することができ、従来品よりも紫外線特性におい
て優れた製品を製造することができる。By utilizing the powder with good sinterability made of ultrafine particles according to the present invention, PLZT, PZT,
B a T I O3, P b T
It is possible to manufacture electroceramics such as 103T i Oz more efficiently than before and with better quality than conventional ones. In addition, since the powder according to the present invention is composed of ultrafine particles, it can be used as a raw material for high-grade cosmetics, etc., and it is possible to manufacture products that have better ultraviolet properties than conventional products.
本発明は、溶液反応は容器内で行い、塩素のような毒性
のあるガスの使用も発生もないため公害発生の心配もな
く微粒子粉体を製造することができる。また、本発明は
従来技術のような粉砕をする必要がないため経済的であ
る。In the present invention, the solution reaction is carried out in a container, and since toxic gases such as chlorine are not used or generated, fine particle powder can be produced without worrying about pollution. Furthermore, the present invention is economical because it does not require pulverization as in the prior art.
即ち、本発明の第一発明は、水酸化チタンを有機溶剤中
に分散させた後、共沸温度以上で蒸留し、ここに得られ
る水和酸化チタンを母液から分離した後、乾燥、仮焼す
ることを特徴とする酸化チタン微粉体の製造方法に関す
る。That is, in the first aspect of the present invention, titanium hydroxide is dispersed in an organic solvent, then distilled at a temperature higher than the azeotropic temperature, and the resulting hydrated titanium oxide is separated from the mother liquor, followed by drying and calcining. The present invention relates to a method for producing fine titanium oxide powder, characterized in that:
また、本発明の第二発明は、チタンのハロゲン化物ある
いは硫酸チタンな鉱酸酸性の水で稀釈し、加熱して加水
分解し、この加水分解さ１また液に有様溶剤を加λ共沸
温度以トで蒸留した後、生成した水和酸化ｆ−タ：ノを
分離１ツ、仝２１葉、仮焼ｔろ、二）−φ、ｓ’ｔ’ｒ
７１．Ｑ） ｈ・”’）ｌ−’、Ｉ）ｍ ４１．”、、
ｆり゛ノ徹扮体・・７）Ｉ、ｉ’、ｊ ｌ１ｌｊ ｊ
ｉ沈（４［己（１６・、゛）、、：Ｋ ’−、ニア
？： １．ｊ月 （９： イ１訃ｆ’ｌ”］ ”
’ｌ−６７ｊ（ｊ’、ｌｆｉ 化Ｉ′−，□９ ０．
、、ｙ ｉ−ｉ： 、 ４ ハＴＬ、１う゛、
）化％、＜、、；”、’、／、ｂで、１箇’、”、、ｌ
６）ｆ 酸−ｒ′う゛” ｌ容ン（！（Ｉ５．７直Ｉ
）ｊ＋ｊ ；）−た （づ：（−醤７ パ） Ｘ、”
’、’ｆ＜ ）１ ノ）／： ム−？、：
；＼ １１ 、′、 ；多 （４゛、７パ リ、
）ノ リ ヘ カ１１λ−、ン、−プ）２去 Ｔ３
得 １ら ｔｖ、 ６ 、、 ア ル ノ１
リ 、！ｙ： ［、”Ｕ ｌニー、ｊ 、
）′ −に二、ンパ水／゛創ぼＩＩＥ Ｌ、、、、、、
い、高１ｉ度（＋）４’）の７”バイｌ［、ｉ−、、１
い”＞ ’−ｔ” 、ｉ ・づ）、 ′１−５成し、パ
こ゛ノミく醸什−１° し♂・Ｊ“、”Ｒｊｌ’； Ｆ
片部１、＝１’、’−／′ｌ）１′い−１、：）、
、 （（７：４均 ｔｉ、１１ （、何 ；°川 中
（１゛ 介 Ｆｋ 、ｌ、ｌ 、、、Ｍ 、
；１１、゛・小、；鳶１胃 ・５行い １１：［弗
１１１φ／ｉ（ケイ）４、分散ｒ、ニーｔ４−る水酸イ
１）〜イ’ 、”、＞’ （７’、） ｉｆ；ｌ 、Ｔ
暑７ 、ｌ、： １．、３７ （、，４、Ｔ ｉ Ｏ、
とｔ、、、、、、 −（、’−［） 、 Ｘ−（［、５
＋ｔ＋ｏ １ ／璽フイ？ｌが１：い。レー〕１シ徹
Ｕこ １７５ （・ 【°（バ 、 ν１１ｊｉｉ
？舌・’ｆ、Ｉ： Ｉｋ’し手ど １°・１イ １
ｔｌ １．、、ｙ −（−ハ １、 い 。In addition, the second invention of the present invention is to dilute a mineral acid such as a titanium halide or titanium sulfate with acidic water, hydrolyze it by heating, and add a certain solvent to the hydrolyzed solution by azeotroping. After distillation at a temperature below 100 ml, the produced hydrated oxidized f-ta: is separated into 1, 21 leaves, calcined, and 2)-φ, s't'r.
71. Q) h・”')l-', I)m 41.”,,
fri-no-tetsu costume...7) I, i', j l1lj j
i sink (4 [self (16., ゛),,:K'-, near?: 1.j month (9: ii1訃f'l''])
'l-67j(j', lfi cation I'-, □9 0.
,,y ii: , 4 HaTL, 1 U゛,
) conversion%, <,, ;”, ', /, b, 1 item', ",, l
6) f acid-r'u゛'' l yon (! (I5.7 direct I
)j+j ;)-ta (zu: (-sho7 pa) X,”
','f< )1 ノ)/: Mu-? , :
;＼ １１、′、；多（4゛、7Paris、
) no ri he ka11λ-, n, -p)2 left T3
TV, 6, Arno 1
Ri,! y: [,”U lny,j,
)′-Ni2, Npa Water/゛Create IIE L,,,,,,
, high 1i degree (+)4') 7" bil[,i-,,1
">'-t", i ・zu), ``1-5 completed, panicked -1° shi ♂・J'', ``Rjl''; F
Piece part 1, = 1', '-/'l) 1'-1, :),
, ((7:4 uniform ti, 11 (, what; ° Kawanaka (1゛ intervention Fk, l, l,,,M
;11, ゛・small;;Tobi 1 stomach ・5 rows 11: [弗111φ/i (K) 4, dispersion r, knee t4- hydroxyl I1) ~ i','',>'(7', ) if;l,T
Heat 7, l: 1. ,37 (,,4,T i O,
and t, , , , -(,'-[) , X-([,5
+t+o 1/seal hui? l is 1: yes. Le] 1 Shi Toru
Uko 175 (・ [°(ba, ν11jii
? Tongue/'f, I: Ik' hand 1°/1i 1
tl 1. ,,y-(-ha1,i.
（（、仙ｉ ％ａ １ｉＷｌ ｉＪ、ｊｆ’Ａ点；、５
（４：ｌ； ｉ・％ 、）、！、ｊ、イ、） 、ｔｌ、
ｉｔ 、、、Ｑ、、 ｉｉｌ ；１．１ 自’Ｅｔ （
１，）；Ｊ１１点ｊ’ｃ、 ’７） ｉ”％ｎ ｔ：’
） ４．ＩＥ ’、ｅＸ ！’、）、） ？：ｔ ｆｓ
ｃ ：ｉ２Ｓ ’ｔ”ｊ゛〕ｌｈｓ、６沸、ｉ；！、シ
ｌす′し今、くど、覧ｈ ｔｌ５−１０ ’（、’、”
ニーＪ−が）ｔ：・？’ＦＩＡＩＩ′：’（、ｉ；、４
”ｉ“）４二４１．・）Ｘ望ましい７この蒸留−コ・肋
木を終了ぜ１１．めた後、冷却し、生成された酸化ヂク
シを有機溶剤から分離し、ぞ−の後１００℃ｆｌ’ｉｔ
後Ｔ′乾燥、 ３００・・８０（）℃で仮焼！、−（丁
扮体イ、：得る、
７ ＃ （０’ｐ’ｆｆｉ、 ＩＩＬ’、ｙ用いら、ｌ
−１，−１ｕ ６’Ａ ９’ｊ７”剤トｊ、”（ＩＱ、
水１１゛ 疾 ：１ｔｉ ；、ｒ例 ｊｌ′７Ｓ
き イ゛） ？）ｌ の ｉｌ’、、
ｌ’、１ｌｊｉ こＬ ！：ｒ 土 く 、
べ ゛、・・ じ゛、 トノ！ ・−゛・・、
λ ・２）・ン、炭素、・改１〔１（メ［−ζｔ’Ｊ）
’、−、、ｉ’ルｒ ル：ｌ：ｌＵ、１・′ｔ、１
．Ｊｌ、−ｒ：％ Ｑｌニー” フル（１，’） １．
：、” ＆ Ｎ ’ｉ：１別的−＋：２．７、ｊ・ Ｉ
Ｉ’： ｔｌｌｌ）Ｉ”’、’ｆ ６ １−（：
７：ｌ’ ”（：” 、ｑ 、 ｒ−ａ’％２
ら しり’、１ （ｆ！ ：よ、 ノー は：
’＞ トｉｉ 、１ストｊ５、信用□−ｊ□□ ｚ、（
：： ｉ’：ｌ：が−（“きる。シタ゛、ン７ Ｉ’ｔ
’ｌＵ３、ｉｊＢ；晶Ｊ５ｊ−↓ス ｌ・ （′１１
・用１’ｔ’ｒ ’ｉ’ｉ’、ｌ 自 ［−１（〕）
１・；ｉ旨・長 、１“ −（−゛ ・カ’ｌ’、ｌＩ
Ｕ （、Ｊ、 ｌし“ １ｆ−）、
）じ）”ｈ ＪＩＲ水ｊ、’５ ：Ｆ’Ｌ ｊｓｉ’％
’ｔ ４ｉ、７．、−ｊ” ｙ９−、−’ （ｔ ：’
ｌ”＋： ＪＥ Ｌ−”、 ｌ’ｌｊ２ ：／ｌイ゛＼
４１）゛、・ ・ハ（））←゛（（な く 、 １・“
０乍（υ ・’ＪＳ ｂ＜”（’、、’Ｉ ’０．．
−Ｄ）１）：ハ・：、−１，１・ｉ−路１、（いイ゛）
Ｉパ干ルアー、・スの水和ｊｕｔイヒ゛ｉ：ノ］ ”（
Ｆ Ｊ、６ Ｊ’ｌば、（（ハ 、 、、の ’ｈ”
ｆ ＩＩ ｊ’：％ Ｎ ｌ： Ｑ”ｊ］］ｉ、：Ｌ
、、ｌ（＋、（・串？＋（ｉｉ １．ｋ １以 下
（ノ、）２□（：点 （゛・、＄−１゛？醪・１ ７）
と （１阜 に・ 、ｔｌ ・・′、 Ｊ＋、：
、、ｊ ：＝・ ）＋ ブ：〜・ づく 丁旧耳ｉ
、ｉ 、（Ｐ 、Ｉ、４． （、、Ｘル：′ｌ：’、
’・［、：、１’ｒＮ ）！”ト １ （Ｔ ｆ）”Ｃ
’ｌ冒（（１，’、” ｔ：ｌ： 、：！ｆ’、’ｌ−
’（’、）”行ｔ ［−ｊｉ ＜’ｌ、いが１．１；Ｊ
、ｉ ｌ工 ト−ｃ Ｆｉ 、＞： ン！： 、に
’、）；％１．ｌり：白−ｒＦ １ｌｌ）、、：”
、 、芒 ｊ・＼１１ ’ｆ、）ｔ （））（、［・
Ｊ’ｌ；置１、 ’（ＷＱ ′１．Ｉ ・ぢ鳥：ハ
：１．１．１″′呂、 ・：、１、（１−７・）Ｆｌ、
６ ｊｂ２化 −１−り ゛ノ粉体が凝集してしまう
恐れがあるので、 ３００〜８００℃で行うことが望ま
しい。((, Seni %a 1iWl iJ, jf'A point;, 5
(4:l; i・%,),! ,j,i,) ,tl,
it ,,,Q,, iil;1.1 self'Et (
1,); J11 points j'c, '7) i''%n t:'
) 4. IE', eX! ',),)? :t fs
c: i2S 't"j゛]lhs, 6 boiling, i;!, silsu' now, Kudo, viewing h tl5-10 '(,',"
Knee J-ga)t:・? 'FIAII':'(,i;,4
"i")4241.・) After that, it was cooled, the produced oxidized sardines were separated from the organic solvent, and then heated at 100℃ fl'it.
After T' drying, calcination at 300...80()℃! , -(Ding tai ii, : get, 7 # (0'p'ffi, IIL', y use et al., l
-1, -1u 6'A 9'j7"agentj,"(IQ,
Water 11゛ Speed: 1ti ;, r example jl'7S
Kiii)? )l's il',,
l', 1lji koL! :r soil,
Be,... Ji, Tono!・−゛・・、
λ ・2)・N, Carbon,・Kai 1 [1 (Me[−ζt'J)
', -,, i'le r le:l:lU,1・'t,1
．． Jl, -r:% Ql knee'' full (1,') 1.
:,”&N'i:1separate-+:2.7,j・I
I': tllll)I"','f 6 1-(:
7:l'"(:", q, r-a'%2
Ra Shiri', 1 (f!: Yo, no is:
'> To ii, 1st j5, credit □−j□□ z, (
:: i':l:ga-(“kiru.shita・n7 I't
'lU3, ijB; Akira J5j-↓su l・ ('11
・For 1't'r 'i'i', l self [-1(])
1・;i , long , 1 “ −(−゛ ・KA'l', lI
U (, J, lshi" 1f-), )ji)"h JIR water j,'5 :F'L jsi'%
't 4i, 7. , -j'' y9-, -'(t:'
l"+: JE L-", l'lj2:/lii゛\
41)゛、・・Ha()）←゛((without 、１・“
0乍(υ ・'JS b<”(',,'I '0..
-D) 1): C:, -1,1・i-path 1, (ii)
I dry the lure, the hydration of the water juhi:ノ] ”(
F J, 6 J'lba, ((ha, ,,'h'
f II j':% N l: Q"j]]i,:L
,,l(+,(・skewer?+(ii 1.k 1 or less
（ノ、）２□（：Point （゛・、＄−1゛?Moromi・1 7）
and (1 day..., tl...', J+,:
,,j :=・ )+ bu :〜・ Zuku Ding old ear i
,i,(P,I,4.(,,Xle:'l:',
'・[,:,1'rN)! "T 1 (T f)"C
'l-
'(',)'' line t [-ji <'l, iga1.1;J
, il 工 ト ーc FI , ＞: N! : , to
',);%1. 1ll: White-rF 1ll),,:”
, , awn j・\11 'f,)t ())(,[・
J'l; Put 1, '(WQ '1.I ・Dibird: Ha: 1.1.1'''ro, ・:, 1, (1-7・) Fl,
Since there is a risk that the powder may aggregate, it is desirable to carry out the reaction at a temperature of 300 to 800°C.
第二発明の４ハロゲン化チタンあるいは硫酸チタン溶液
を鉱酸酸性溶液で稀釈する際の、これらのチタン化合物
の濃度はＴ ｉ Ｏｓとしてｏ、ｉ〜０．５ｏ＋ｏｌ／
Ｉ２で、稀釈後の酸濃度は２Ｎ以上であればよいが、好
ましくは４Ｎ以上とする。このように稀釈したＴ １４
＊含有溶液を加熱沸騰して、Ｔ ｉ”と水との加水分
解を十分に行う、加水分解後に有機溶剤を加えて共沸蒸
留を行う。When diluting the titanium tetrahalide or titanium sulfate solution of the second invention with an acidic mineral acid solution, the concentration of these titanium compounds as T i Os is o, i ~ 0.5 o + ol/
In I2, the acid concentration after dilution may be 2N or more, but preferably 4N or more. T14 diluted in this way
*The containing solution is heated to boiling to sufficiently hydrolyze Ti" and water. After hydrolysis, an organic solvent is added to perform azeotropic distillation.
共沸蒸留は、第一発明の時と同様に行う、使用する有機
溶剤としては、第一発明と同じでよいが、水への溶解度
の小さいものを用いるのがこの方法の後の操作に都合が
よい。The azeotropic distillation is carried out in the same manner as in the first invention. The organic solvent used may be the same as in the first invention, but it is convenient for the subsequent operations of this method to use one with low solubility in water. Good.
蒸留操作の終了後、生成した水和酸化物を濾過あるいは
遠心分離等の方法により分離後、第一発明と同様の操作
を行い粉体を得る。After the distillation operation is completed, the produced hydrated oxide is separated by a method such as filtration or centrifugation, and then the same operation as in the first invention is performed to obtain a powder.
（作 用）
本発明の特徴は、水酸化チタンあるいは水和酸化チタン
をそのまま乾燥するのでなく、有機溶剤に接しせしめな
がら脱水を行い、有機溶剤分子に包まれた水和酸化物粒
子を取り出して乾燥させている点にある。このような方
法を行っているため、コロイドとしての粒子の一つ一つ
が互いに強固に結合することなく粉体とすることができ
るのである。また、仮焼温度も３００〜８００℃でよい
ため、強固に凝集した粒子のない粉体を得ることができ
る。(Function) The feature of the present invention is that, instead of drying titanium hydroxide or hydrated titanium oxide as it is, it is dehydrated while being brought into contact with an organic solvent, and hydrated oxide particles wrapped in organic solvent molecules are extracted. The point is that it is dried. Because this method is used, each colloidal particle can be made into a powder without strongly bonding to each other. Further, since the calcination temperature may be 300 to 800°C, a powder free of strongly agglomerated particles can be obtained.
以下、実施例をもって本発明を更に詳細に説明するが、
本発明はこれらに限定されるものではない。Hereinafter, the present invention will be explained in more detail with reference to Examples.
The present invention is not limited to these.
実施例Ｉ
Ｔ ｉ Ｏ＊として０．３ｍｏｌ／Ｉ２に相当するＴ
ｉ Ｃ１２４を水５００ｍ １２に加えてから十分に撹
拌しながらアンモニア水を加えて水酸化チタンを得た。Example I T corresponding to 0.3 mol/I2 as T i O*
i C124 was added to 500 m 12 of water, and then aqueous ammonia was added with sufficient stirring to obtain titanium hydroxide.
この水酸化チタンを母液から遠心分離法で分離後、直ち
に１リツトルのイソアミルアルコール中に分散させ、加
熱蒸留して、沸点が１０５℃の点で蒸留を停止し、静置
後、沈降物を濾過分離し、 １００℃で十分に乾燥の後
、 ５００℃で１時間仮焼してＴｉＯ□の超微粒子粉体
を得た。After separating this titanium hydroxide from the mother liquor by centrifugation, it is immediately dispersed in 1 liter of isoamyl alcohol, heated and distilled, and the distillation is stopped when the boiling point reaches 105°C. After standing still, the precipitate is filtered. It was separated, thoroughly dried at 100°C, and then calcined at 500°C for 1 hour to obtain ultrafine powder of TiO□.
得られた酸化チタン微粉体の電子顕微鏡写真を第１図に
示す、また、比較のため市販の酸化チタン微粉体（チタ
ン工業■製）の電子顕微鏡写真を第２図に示す６第１図
の顕微鏡写真かられかるように、本実施例で得られたＴ
ｉ Ｏ２は粒径０．１μｍ以下、より具体的には０．
０２μｍ〜０．０５μｍの超微粒子粉体である。An electron micrograph of the obtained titanium oxide fine powder is shown in Fig. 1, and for comparison, an electron micrograph of a commercially available titanium oxide fine powder (manufactured by Titan Kogyo ■) is shown in Fig. 6. As can be seen from the micrograph, the T obtained in this example
i O2 has a particle size of 0.1 μm or less, more specifically 0.1 μm or less.
It is an ultrafine powder of 0.02 μm to 0.05 μm.
実施例２
実施例１と同様にして、遠心分離後の水酸化チタンを１
リツトル中のオクタツール中に入れ、界面活性剤を１０
ｍβ加えてから撹拌したのち蒸留し、沸点が１１０°Ｃ
となった時点で蒸留を止め、以後は実施例１と同様に行
いＴ ｉ Ｏｚの超微粒子粉体な得た。得られた超微粒
子粉体は粒径０．ｌｕ、ｍ以下で、大部分が０．０２ｇ
ｍ 〜０．０５ｇ、 ｍのものであった。Example 2 In the same manner as in Example 1, titanium hydroxide after centrifugation was
Add 10% surfactant to Octatool in a small bottle.
After adding mβ, stirring and distilling, the boiling point is 110°C.
Distillation was stopped at the time when , and the rest was carried out in the same manner as in Example 1 to obtain ultrafine powder of T i Oz. The obtained ultrafine powder has a particle size of 0. lu, m or less, mostly 0.02g
m~0.05g, m.
実施例３
Ｔ ｉ Ｏａとして０．５ｍｏｌ／βに相当する量のＴ
ｉ Ｃ１２４を水１０００ｍβ中に加えてから塩酸で
４Ｎに調整し、１０時間加熱沸騰させて十分に白濁させ
る０次いで、ブクノールを５００ｍ １２加えて蒸留し
、沸点が１００℃の点で蒸留を停止し、遠心分離法で沈
降物を分離した後、実施例１と同様に行いＴ ｉ Ｏ２
の超微粒子粉体を得た。得られた超微粒子粉体は、上記
実施例１および２と同様に粒径０．ｌＬＬｍ以下で、９
０％以上が０．０２μｍ〜０．０５μｍのものであった
。Example 3 An amount of T equivalent to 0.5 mol/β as T i Oa
i Add C124 to 1000 mβ of water, adjust to 4N with hydrochloric acid, boil for 10 hours and make it sufficiently cloudy. Next, add 500 m of Buknor and distill it, and stop the distillation when the boiling point is 100°C. , After separating the sediment by centrifugation, the same procedure as in Example 1 was carried out to obtain T i O2
An ultrafine powder was obtained. The obtained ultrafine particle powder had a particle size of 0.5 mm as in Examples 1 and 2 above. lLLm or less, 9
0% or more had a diameter of 0.02 μm to 0.05 μm.
実施例４
上記実施例で得られたＴ ｉ Ｏ２超微粒子粉体を静水
圧法で成形後、１３００ ’Ｃで２時間焼成した。得ら
れた焼結体のカサ比重は、４．１８であった。これに対
し、市販品のＴｉＯ□粉体を同様にして成形し、焼成し
た焼結体のカサ比重は３．８５であった。この結果が示
すように、本発明ｊ・こより得られた超微粉体の焼結体
は、比重が大ぎく緻密であり、非常に優れた物性および
機械特性を示す。Example 4 The T i O2 ultrafine particle powder obtained in the above example was molded by a hydrostatic pressure method and then calcined at 1300'C for 2 hours. The bulk specific gravity of the obtained sintered body was 4.18. On the other hand, a sintered body obtained by molding and firing a commercially available TiO□ powder in the same manner had a bulk specific gravity of 3.85. As shown by these results, the sintered body of ultrafine powder obtained from the method of the present invention has a high specific gravity and is very dense, and exhibits very excellent physical and mechanical properties.
以上述べたように、上記各実施例で得られた酸化チタン
微粉体は、いずれも粒径０．１μｍ以下の超微粒子粉体
であり、焼結材料として使用したとき良好な圧粉性を示
し、得られた焼結体は真比重に近い高密度体であった。As mentioned above, the titanium oxide fine powder obtained in each of the above examples is an ultrafine powder with a particle size of 0.1 μm or less, and exhibits good compactability when used as a sintering material. The obtained sintered body was a high-density body with close to true specific gravity.
第１図は実施例１によって得た酸化チタン微粉体の電子
顕微鏡写真、
第２図は市販の酸化チタン微粉体の電子顕微鏡写真を示
す。FIG. 1 shows an electron micrograph of the titanium oxide fine powder obtained in Example 1, and FIG. 2 shows an electron micrograph of the commercially available titanium oxide fine powder.
Claims (2)
温度以上で蒸留し、ここに得られる水和酸化チタンを母
液から分離した後、乾 燥、仮焼することを特徴とする酸化チタン微粉体の製造
方法。(1) Oxidation characterized by dispersing titanium hydroxide in an organic solvent and then distilling it above the azeotropic temperature, separating the resulting hydrated titanium oxide from the mother liquor, followed by drying and calcining. A method for producing titanium fine powder.
酸性の水で稀釈し、加熱して加水分解し、この加水分解
された液に有機溶剤を加え共沸温度以上で蒸留した後、
生成した水和酸化チタンを分離し、乾燥、仮焼すること
を特徴とする酸化チタン微粉体の製造方法。(2) Titanium halide or titanium sulfate is diluted with mineral acidic water, heated and hydrolyzed, an organic solvent is added to this hydrolyzed liquid, and the mixture is distilled at a temperature higher than the azeotropic temperature.
A method for producing fine titanium oxide powder, which comprises separating, drying, and calcining the produced hydrated titanium oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1012982A JP2805202B2 (en) | 1989-01-21 | 1989-01-21 | Method for producing titanium oxide fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1012982A JP2805202B2 (en) | 1989-01-21 | 1989-01-21 | Method for producing titanium oxide fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02196028A true JPH02196028A (en) | 1990-08-02 |
| JP2805202B2 JP2805202B2 (en) | 1998-09-30 |
Family
ID=11820413
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1012982A Expired - Lifetime JP2805202B2 (en) | 1989-01-21 | 1989-01-21 | Method for producing titanium oxide fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2805202B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5744126A (en) * | 1995-06-02 | 1998-04-28 | Miyoshi Kasei, Inc. | Cosmetics containing silicone surface-modified particles of titanium oxide and zinc oxide |
| US6156324A (en) * | 1996-05-16 | 2000-12-05 | Miyoshi Kasei, Inc. | Compositions for cosmetics and cosmetics |
| EP1160202A1 (en) * | 2000-05-24 | 2001-12-05 | Sumitomo Chemical Company, Limited | Titanium hydroxide, photocatalyst produced from the same and photocatalytic coating agent |
| KR100343395B1 (en) * | 1999-05-28 | 2002-07-15 | 유석범 | Method for production of titanium dioxide ultrafine powders with rutile phase from titanium sulfate |
| EP1323676A3 (en) * | 1999-06-30 | 2004-01-21 | Sumitomo Chemical Company, Limited | Titanium oxide, photocatalyst comprising same and photocatalytic coating agent |
| KR100450225B1 (en) * | 2001-08-31 | 2004-09-24 | 재단법인 포항산업과학연구원 | Fabrication method of nanoscale-porous body |
-
1989
- 1989-01-21 JP JP1012982A patent/JP2805202B2/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5744126A (en) * | 1995-06-02 | 1998-04-28 | Miyoshi Kasei, Inc. | Cosmetics containing silicone surface-modified particles of titanium oxide and zinc oxide |
| US6156324A (en) * | 1996-05-16 | 2000-12-05 | Miyoshi Kasei, Inc. | Compositions for cosmetics and cosmetics |
| KR100343395B1 (en) * | 1999-05-28 | 2002-07-15 | 유석범 | Method for production of titanium dioxide ultrafine powders with rutile phase from titanium sulfate |
| EP1323676A3 (en) * | 1999-06-30 | 2004-01-21 | Sumitomo Chemical Company, Limited | Titanium oxide, photocatalyst comprising same and photocatalytic coating agent |
| EP1160202A1 (en) * | 2000-05-24 | 2001-12-05 | Sumitomo Chemical Company, Limited | Titanium hydroxide, photocatalyst produced from the same and photocatalytic coating agent |
| KR100450225B1 (en) * | 2001-08-31 | 2004-09-24 | 재단법인 포항산업과학연구원 | Fabrication method of nanoscale-porous body |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2805202B2 (en) | 1998-09-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102659149B (en) | Preparation method for monodisperse high-purity alpha-Al2O3 powder | |
| Yang et al. | Preparation of rutile titania nanocrystals by liquid method at room temperature | |
| JP2017515786A (en) | Method for preparing nanometer titanium dioxide | |
| CN101333002B (en) | Titanium dioxide nanometer powder with special appearance and method for preparing same | |
| CN101973578A (en) | Water-based sol-gel method for preparing high-purity monodisperse barium titanate nanopowder | |
| CN104591259B (en) | Engraftment type nano-zinc oxide and production process thereof | |
| CN104894636B (en) | The preparation method of eight potassium titanate crystal whiskers | |
| CN103588246A (en) | Preparation process for nano zirconia powder | |
| CN109721357A (en) | A kind of Zirconium oxide powder and its preparation method and application that the nanometer yttrium that monodisperse granularity is controllable is stable | |
| JP3198494B2 (en) | Conductive oxide particles and method for producing the same | |
| JPH02196028A (en) | Production of titanium oxide fine powder | |
| KR101152382B1 (en) | Manufacturing method of titanium oxide improved whiteness | |
| WO2015030388A1 (en) | Method for preparing titanium carbide powder | |
| Nagabhushana et al. | An efficient and a novel route for the synthesis of titania via solution combustion of peroxotitanic acid | |
| CN113860350A (en) | Method for preparing thorium dioxide nano material based on molten salt method and thorium dioxide nano material obtained by method | |
| CN103274460B (en) | Method for preparing rutile phase titanium dioxide sub-microsphere through selective dispergation | |
| CA2377241C (en) | Processing aqueous titanium solutions to titanium dioxide pigment | |
| JPH05163022A (en) | Spherical anatase titanium oxide and its production | |
| CN108002435B (en) | Method for improving production quality of titanium dioxide by sulfuric acid process | |
| JP3324164B2 (en) | Indium oxide powder, method for producing the same, and method for producing ITO sintered body | |
| JPH04280815A (en) | Fine particulate alkali titanate and its production | |
| CN107140690A (en) | It is a kind of to improve the method that bismuth ferrotitanium type oxide nano-powder is reunited | |
| CN207129969U (en) | The preparation system of nano titanium oxide | |
| CN106865600B (en) | A kind of preparation method of size tunable stannic oxide nano powder | |
| KR20000075055A (en) | Method for production of titanium dioxide ultrafine powders with rutile phase from titanium sulfate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313117 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| EXPY | Cancellation because of completion of term |