CN111479881B - 用于制造涂覆的二氧化钛颗粒的方法、涂覆的二氧化钛颗粒及包含其的产品 - Google Patents

用于制造涂覆的二氧化钛颗粒的方法、涂覆的二氧化钛颗粒及包含其的产品 Download PDF

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Publication number
CN111479881B
CN111479881B CN201880081145.5A CN201880081145A CN111479881B CN 111479881 B CN111479881 B CN 111479881B CN 201880081145 A CN201880081145 A CN 201880081145A CN 111479881 B CN111479881 B CN 111479881B
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titanium dioxide
coated
range
product
particles
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CN111479881A (zh
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拉尔夫-约翰·拉明马基
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Venator Germany GmbH
Weinert P & A Finland
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Huntsman P&A Germany GmbH
Weinert P & A Finland
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3653—Treatment with inorganic compounds
    • C09C1/3661—Coating
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29—Titanium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • 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
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3081—Treatment with organo-silicon compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/69—Particle size larger than 1000 nm
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/60—Particulates further characterized by their structure or composition
    • A61K2800/61—Surface treated
    • A61K2800/62—Coated
    • A61K2800/621—Coated by inorganic compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/60—Particulates further characterized by their structure or composition
    • A61K2800/65—Characterized by the composition of the particulate/core
    • A61K2800/651—The particulate/core comprising inorganic material
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/86—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by NMR- or ESR-data
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/10—Solid density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • Animal Behavior & Ethology (AREA)
  • Epidemiology (AREA)
  • Birds (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Dermatology (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Paints Or Removers (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Cosmetics (AREA)
CN201880081145.5A 2017-10-17 2018-10-15 用于制造涂覆的二氧化钛颗粒的方法、涂覆的二氧化钛颗粒及包含其的产品 Expired - Fee Related CN111479881B (zh)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP17196845.6 2017-10-17
EP17196845 2017-10-17
PCT/EP2018/078019 WO2019076790A1 (en) 2017-10-17 2018-10-15 PROCESS FOR PRODUCING COATED TITANIUM DIOXIDE PARTICLES, COATED TITANIUM DIOXIDE PARTICLES, AND PRODUCTS COMPRISING SAID PARTICLES

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Publication Number Publication Date
CN111479881A CN111479881A (zh) 2020-07-31
CN111479881B true CN111479881B (zh) 2022-10-14

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US (1) US20200248000A1 (enExample)
EP (1) EP3697852A1 (enExample)
JP (1) JP2020537710A (enExample)
KR (1) KR20200084870A (enExample)
CN (1) CN111479881B (enExample)
AU (1) AU2018352064A1 (enExample)
BR (1) BR112020007518A2 (enExample)
CA (1) CA3079301A1 (enExample)
MX (1) MX2020003630A (enExample)
TW (1) TW201927921A (enExample)
UA (1) UA126505C2 (enExample)
WO (1) WO2019076790A1 (enExample)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7326934B2 (ja) * 2019-07-03 2023-08-16 住友大阪セメント株式会社 酸化チタン粉体、並びに、それを用いた分散液および化粧料
CN114829508A (zh) * 2019-12-18 2022-07-29 克洛诺斯国际有限公司 包含未干燥的涂覆二氧化钛的印刷油墨
US12435228B2 (en) 2019-12-18 2025-10-07 Kronos International, Inc. Printing ink containing undried, coated titanium dioxide
CN112452295B (zh) * 2020-12-09 2021-07-09 广州市飞雪材料科技有限公司 一种维生素载体用二氧化硅吸附剂及其制备方法
CN113088105B (zh) * 2021-03-22 2022-05-24 龙佰集团股份有限公司 一种高耐候钛白粉及制备方法
RU2760442C1 (ru) * 2021-03-25 2021-11-25 Федеральное государственное автономное образовательное учреждение высшего образования «Южно-Уральский государственный университет (национальный исследовательский университет)» ФГАОУ ВО «ЮУрГУ (НИУ)» Способ получения смешанного фотокатализатора на основе оксида титана
CN113372736B (zh) * 2021-06-08 2022-04-22 正太新材料科技有限责任公司 一种二氧化钛包覆材料、其制备方法及应用
KR102655036B1 (ko) * 2022-12-30 2024-04-08 (주)젠텍 백탁 및 자외선 차단 효과가 향상된 화장료 조성물용 하이브리드 이산화티탄 안료의 제조 방법

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2885366A (en) * 1956-06-28 1959-05-05 Du Pont Product comprising a skin of dense, hydrated amorphous silica bound upon a core of another solid material and process of making same
EP0406194A1 (en) * 1989-06-26 1991-01-02 Kemira Oy Process for coating titanium dioxide pigments
JPH10130527A (ja) * 1996-10-28 1998-05-19 Ishihara Sangyo Kaisha Ltd 二酸化チタン顔料及びその製造方法
CN1430653A (zh) * 2000-04-12 2003-07-16 千年无机化学公司 二氧化钛颜料的连续生产方法
CN106459611A (zh) * 2014-05-23 2017-02-22 亨斯迈P And A英国有限公司 涂覆的二氧化钛分散体

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4125412A (en) * 1976-09-09 1978-11-14 E. I. Du Pont De Nemours And Company Process for the production of durable titanium dioxide pigment
JP2739227B2 (ja) * 1989-02-15 1998-04-15 テイカ株式会社 二酸化チタン顔料及びその製造方法
FI89900C (fi) 1990-03-01 1993-12-10 Kemira Oy Nytt framstaellningsfoerfarande av titandioxid
US6695906B2 (en) * 2000-04-12 2004-02-24 Millennium Inorganic Chemicals, Inc. Continuous processes for producing titanium dioxide pigments
US6784401B2 (en) * 2001-01-30 2004-08-31 Illinois Tool Works Inc. Welding electrode and method for reducing manganese in fume
JP5207426B2 (ja) * 2006-06-30 2013-06-12 学校法人神奈川大学 化粧料及びその製造方法
MX352876B (es) * 2007-02-01 2017-12-13 Sol Gel Tech Ltd Metodo para preparar particulas que comprenden recubrimiento de oxido de metal y particulas con recubrimiento de oxido de metal.
JP2010006629A (ja) * 2008-06-25 2010-01-14 Ishihara Sangyo Kaisha Ltd 二酸化チタン微粒子及びその製造方法
US8840719B2 (en) * 2011-03-09 2014-09-23 Tronox Llc Titanium dioxide pigments and manufacturing method
JP6269439B2 (ja) * 2013-11-01 2018-01-31 信越化学工業株式会社 酸化チタン含有コーティング組成物及び被覆物品

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2885366A (en) * 1956-06-28 1959-05-05 Du Pont Product comprising a skin of dense, hydrated amorphous silica bound upon a core of another solid material and process of making same
EP0406194A1 (en) * 1989-06-26 1991-01-02 Kemira Oy Process for coating titanium dioxide pigments
JPH10130527A (ja) * 1996-10-28 1998-05-19 Ishihara Sangyo Kaisha Ltd 二酸化チタン顔料及びその製造方法
CN1430653A (zh) * 2000-04-12 2003-07-16 千年无机化学公司 二氧化钛颜料的连续生产方法
CN106459611A (zh) * 2014-05-23 2017-02-22 亨斯迈P And A英国有限公司 涂覆的二氧化钛分散体

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KR20200084870A (ko) 2020-07-13
MX2020003630A (es) 2020-11-09
RU2020115957A (ru) 2021-11-19
RU2020115957A3 (enExample) 2022-04-18
WO2019076790A1 (en) 2019-04-25
JP2020537710A (ja) 2020-12-24
US20200248000A1 (en) 2020-08-06
TW201927921A (zh) 2019-07-16
CA3079301A1 (en) 2019-04-25
CN111479881A (zh) 2020-07-31
EP3697852A1 (en) 2020-08-26
BR112020007518A2 (pt) 2020-10-06
AU2018352064A1 (en) 2020-05-21
UA126505C2 (uk) 2022-10-19

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