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1. WO2019189307 - TITANIUM OXIDE PARTICLES AND MANUFACTURING METHOD THEREFOR

Publication Number WO/2019/189307
Publication Date 03.10.2019
International Application No. PCT/JP2019/013090
International Filing Date 27.03.2019
IPC
C01G 23/053 2006.1
CCHEMISTRY; METALLURGY
01INORGANIC CHEMISTRY
GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F94
23Compounds of titanium
04Oxides; Hydroxides
047Titanium dioxide
053Producing by wet processes, e.g. hydrolysing titanium salts
CPC
C01G 23/0536
CCHEMISTRY; METALLURGY
01INORGANIC CHEMISTRY
GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
23Compounds of titanium
04Oxides; Hydroxides
047Titanium dioxide
053Producing by wet processes, e.g. hydrolysing titanium salts
0536by hydrolysing chloride-containing salts
C01G 23/0538
CCHEMISTRY; METALLURGY
01INORGANIC CHEMISTRY
GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
23Compounds of titanium
04Oxides; Hydroxides
047Titanium dioxide
053Producing by wet processes, e.g. hydrolysing titanium salts
0536by hydrolysing chloride-containing salts
0538in the presence of seeds
C01P 2002/60
CCHEMISTRY; METALLURGY
01INORGANIC CHEMISTRY
PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
2002Crystal-structural characteristics
60Compounds characterised by their crystallite size
C01P 2004/03
CCHEMISTRY; METALLURGY
01INORGANIC CHEMISTRY
PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
2004Particle morphology
01depicted by an image
03obtained by SEM
C01P 2004/51
CCHEMISTRY; METALLURGY
01INORGANIC CHEMISTRY
PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
2004Particle morphology
51Particles with a specific particle size distribution
C01P 2004/52
CCHEMISTRY; METALLURGY
01INORGANIC CHEMISTRY
PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
2004Particle morphology
51Particles with a specific particle size distribution
52highly monodisperse size distribution
Applicants
  • 石原産業株式会社 ISHIHARA SANGYO KAISHA, LTD. [JP]/[JP]
Inventors
  • 友成 雅則 TOMONARI Masanori
  • 井田 清信 IDA Kiyonobu
  • 細川 拓也 HOSOKAWA Takuya
Agents
  • 特許業務法人浅村特許事務所 ASAMURA PATENT OFFICE, P.C.
Priority Data
2018-06235528.03.2018JP
Publication Language Japanese (ja)
Filing Language Japanese (JA)
Designated States
Title
(EN) TITANIUM OXIDE PARTICLES AND MANUFACTURING METHOD THEREFOR
(FR) PARTICULES D'OXYDE DE TITANE ET SON PROCÉDÉ DE PRODUCTION
(JA) 酸化チタン粒子及びその製造方法
Abstract
(EN) The present invention manufactures titanium oxide particles that have a small degree of aggregation (size of aggregate particle diameter relative to primary particle diameter) and are not readily sintered by heating. The present invention has: a step in which an alkali and a solution including a carboxylic acid and a titanium (oxy)chloride are mixed, and the titanium (oxy)chloride is hydrolyzed by neutralization; and a step in which, after the hydrolysis by neutralization, the solution is heated to a temperature of 80°C or more and 110°C or less, and the titanium (oxy)chloride remaining in the solution is hydrolyzed by heating. It is thus possible to obtain titanium oxide particles that have a small degree of aggregation and a range of 1-35 for the ratio (D90/BET diameter) between the 90% cumulative mass particle size distribution diameter (D90) (nm) as measured by a dynamic light-scattering particle diameter distribution measurement device and the BET diameter (nm) as calculated from the specific surface area of the titanium oxide particles.
(FR) La présente invention consiste à fabriquer des particules d'oxyde de titane qui ont un faible degré d'agrégation (taille de diamètre de particule d'agrégat par rapport au diamètre de particule primaire) et ne sont pas facilement frittées par chauffage. La présente invention comprend : une étape dans laquelle un alcali et une solution comprenant un acide carboxylique et un chlorure de titane (oxy) sont mélangés, et le chlorure de titane (oxy) est hydrolysé par neutralisation; et une étape dans laquelle, après l'hydrolyse par neutralisation, la solution est chauffée à une température de 80°C ou plus et de 110°C ou moins, et le chlorure de titane (oxy) restant dans la solution est hydrolysé par chauffage. Il est ainsi possible d'obtenir des particules d'oxyde de titane qui ont un faible degré d'agrégation et une plage de 1 à 35 pour le rapport (D90/diamètre BET) entre le diamètre de distribution de taille de particule de masse cumulative de 90 % (D90) (nm) telle que mesuré par un dispositif de mesure de distribution de diamètre de particule par diffusion dynamique de la lumière et le diamètre BET (nm) tel que calculé à partir de la surface spécifique des particules d'oxyde de titane.
(JA) 凝集の程度(一次粒子径に対する凝集粒子径の大きさ)が小さく、加熱による焼結が進みにくい酸化チタン粒子を製造する。 カルボン酸と(オキシ)塩化チタンとを含む溶液と、アルカリとを混合して(オキシ)塩化チタンを中和加水分解する工程と、次いで、中和加水分解後の溶液を80℃以上110℃以下の温度に加熱して、前記溶液に残存する(オキシ)塩化チタンを熱加水分解する工程と、を有する。これにより、動的光散乱式粒子径分布測定装置により測定した90%累積質量粒度分布径(D90)(nm)と前記酸化チタン粒子の比表面積から算出したBET径(nm)との比(D90/BET径)が1~35の範囲の、凝集程度の小さな酸化チタン粒子を得ることができる。
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