JP2019034881A - 酸化亜鉛コアシェル粒子の製造方法、その方法により製造された酸化亜鉛コアシェル粒子及びその粒子を含む紫外線遮蔽組成物 - Google Patents
酸化亜鉛コアシェル粒子の製造方法、その方法により製造された酸化亜鉛コアシェル粒子及びその粒子を含む紫外線遮蔽組成物 Download PDFInfo
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- zinc oxide
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 199
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 99
- 239000002245 particle Substances 0.000 title claims abstract description 86
- 239000011258 core-shell material Substances 0.000 title claims abstract description 79
- 239000000203 mixture Substances 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 74
- IWLXWEWGQZEKGZ-UHFFFAOYSA-N azane;zinc Chemical compound N.[Zn] IWLXWEWGQZEKGZ-UHFFFAOYSA-N 0.000 claims abstract description 65
- 239000012266 salt solution Substances 0.000 claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 45
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 37
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- 239000013067 intermediate product Substances 0.000 claims abstract description 27
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 26
- 239000011575 calcium Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 9
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 8
- 239000011667 zinc carbonate Substances 0.000 claims description 8
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 8
- 235000004416 zinc carbonate Nutrition 0.000 claims description 8
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 4
- SNMGLCMOPMWGTP-UHFFFAOYSA-L zinc azane hydrogen carbonate Chemical compound N.[Zn++].OC([O-])=O.OC([O-])=O SNMGLCMOPMWGTP-UHFFFAOYSA-L 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000378 calcium silicate Substances 0.000 claims description 2
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 54
- 239000001569 carbon dioxide Substances 0.000 description 27
- 229910002092 carbon dioxide Inorganic materials 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 25
- 230000000694 effects Effects 0.000 description 17
- 239000011701 zinc Substances 0.000 description 12
- 238000000862 absorption spectrum Methods 0.000 description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 9
- 238000002835 absorbance Methods 0.000 description 9
- 229910052725 zinc Inorganic materials 0.000 description 9
- 239000004579 marble Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 229910052570 clay Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 208000000453 Skin Neoplasms Diseases 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 201000000849 skin cancer Diseases 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
- C09C1/022—Treatment with inorganic compounds
- C09C1/024—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
- A61K8/27—Zinc; 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
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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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
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/025—Calcium sulfates
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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
- C09C1/04—Compounds of zinc
- C09C1/043—Zinc oxide
-
- 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
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- 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
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- General Health & Medical Sciences (AREA)
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- Epidemiology (AREA)
- Birds (AREA)
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
Description
A=加熱前のアンモニア濃度(%)、即ち、加熱前の第1の混合物または第2の混合物におけるアンモニアの重量パーセント濃度
B=加熱後のアンモニア濃度(%)、即ち、加熱後の第1の混合物または第2の混合物におけるアンモニアの重量パーセント濃度
C=加熱時間(min)即ち、アンモニアの除去時間
D=加熱前の二酸化炭素濃度(g/L)、即ち、加熱前の第1の混合物または第2の混合物の1リットル中の二酸化炭素の量
E=加熱後の二酸化炭素濃度(g/L)、即ち、加熱後の第1の混合物または第2の混合物の1リットル中の二酸化炭素の量
F=加熱時間(min)、即ち、二酸化炭素の除去時間
金属工業において生じた亜鉛含有廃棄物を、水酸化アンモニウムと二酸化炭素とを含有する水溶液に混合して(混合物の重量比は、亜鉛:アンモニア:二酸化炭素=10g/L:7〜12g/L:7〜9g/L)、亜鉛を溶出し、そして、その混合物に含有する重金属を除去することにより、亜鉛イオン濃度が9.55wt%の亜鉛アンモニア錯塩溶液を得る。該亜鉛アンモニア錯塩は、Zn(NH3)n(HCO3)2であり、nは整数1〜6である。
下記の工程により実施例1〜5の酸化亜鉛コアシェル粒子を製造する。
実施例6〜10の酸化亜鉛コアシェル粒子は、大理石の粉を40.7g使用すること以外、実施例1〜5と同じ条件及び工程で製造された。
下記の工程により比較例1の酸化亜鉛コアシェル粒子を製造する。
A.UV−可視光の吸光度スペクトル
実施例1〜5と比較例1との酸化亜鉛コアシェル粒子それぞれを直径3cmの透明の試料セルに、厚さが1cmになるまで添加した後、UV−可視光分光光度計(HITACHI 3900)で、各実施例及び比較例それぞれを600nm/minの速度で500nmから250nmまでスキャンして、各波長の透過率を測定する。そして、計算ソフトにより吸光度に換算して、吸光度スペクトルの図を得た。
B. 紫外線吸光度の増加率の計算
図1〜図5により、実施例1〜5と比較例1との酸化亜鉛コアシェル粒子それぞれの最大紫外線吸光度は、340nm〜360nmの範囲内にあることが分かった。
G=紫外線吸光度の増加率(%)
H=実施例の最大紫外線吸光度
I=比較例1の最大紫外線吸光度
走査型電子顕微鏡で、実施例1〜3、5及び比較例1の酸化亜鉛コアシェル粒子を観察し、その画像を、図6〜10に示した。
Claims (13)
- カルシウム含有材料を第1の亜鉛アンモニア錯塩溶液に混合して第1の混合物を得る第1の工程と、
前記第1の混合物を加熱してアンモニアを除去することにより、第1の中間産物を得る第2の工程と、
前記第1の中間産物を第2の亜鉛アンモニア錯塩溶液に混合して第2の混合物を得る第3の工程と、
前記第2の混合物を加熱してアンモニアを除去した後、乾燥処理により、第2の中間産物を得る第4の工程と、
前記第2の中間産物を焼成して酸化亜鉛コアシェル粒子を得る第5の工程と、を含むことを特徴とする酸化亜鉛コアシェル粒子の製造方法。 - 340℃〜360℃の範囲内の焼成で前記第5の工程を行うことを特徴とする請求項1に記載の酸化亜鉛コアシェル粒子の製造方法。
- アンモニアの除去速度が0.02%/min〜0.09%/min範囲内になるように、前記第2の工程及び前記第4の工程それぞれにおける加熱を行うことを特徴とする請求項1または請求項2に記載の酸化亜鉛コアシェル粒子の製造方法。
- 前記第2の工程及び前記第4の工程それぞれにおける加熱を80℃〜100℃の範囲内で行うことを特徴とする請求項1〜請求項3のいずれか一項に記載の酸化亜鉛コアシェル粒子の製造方法。
- 前記第1の工程における第1の亜鉛アンモニア錯塩溶液及び前記第3の工程における第2の亜鉛アンモニア錯塩溶液は、すべて亜鉛イオン濃度が8wt%〜20wt%の範囲内にあるものを使用することを特徴とする請求項1〜請求項4のいずれか一項に記載の酸化亜鉛コアシェル粒子の製造方法。
- 前記第1の工程における第1の亜鉛アンモニア錯塩溶液及び前記第3の工程における第2の亜鉛アンモニア錯塩溶液は、前記第1の亜鉛アンモニア錯塩溶液と前記第2の亜鉛アンモニア錯塩溶液との重量比が1:3〜3:1の範囲内となるように使用することを特徴とする請求項1〜請求項5のいずれか一項に記載の酸化亜鉛コアシェル粒子の製造方法。
- 前記第2の工程で得る第1の中間産物は、前記カルシウム含有材料のコアと、コアの表面に形成された炭酸亜鉛フレークと、を含むことを特徴とする請求項1〜請求項6のいずれか一項に記載の酸化亜鉛コアシェル粒子の製造方法。
- 前記第1の工程においては、亜鉛アンモニア重炭酸錯塩溶液を前記第1の亜鉛アンモニア錯塩溶液として使用することを特徴とする請求項1〜請求項7のいずれか一項に記載の酸化亜鉛コアシェル粒子の製造方法。
- 前記第5の工程で得る酸化亜鉛コアシェル粒子は、前記カルシウム含有材料のコアと、コアの表面に形成された酸化亜鉛フレークのシェルと、を含むことを特徴とする請求項1〜請求項8のいずれか一項に記載の酸化亜鉛コアシェル粒子の製造方法。
- 前記第3の工程においては、亜鉛アンモニア重炭酸錯塩溶液を前記第2の亜鉛アンモニア錯塩溶液として使用することを特徴とする請求項1〜請求項9のいずれか一項に記載の酸化亜鉛コアシェル粒子の製造方法。
- 前記第1の工程においては、前記カルシウム含有材料として、炭酸カルシウム含有材料、酸化カルシウム含有材料、ケイ酸カルシウム含有材料、塩化カルシウム含有材料、硫酸カルシウム含有材料からなる群より少なくとも1つ選ばれるものを使用することを特徴とする請求項1〜請求項10のいずれか一項に記載の酸化亜鉛コアシェル粒子の製造方法。
- 請求項1〜請求項11のいずれか一項に記載の酸化亜鉛コアシェル粒子の製造方法により製造された酸化亜鉛コアシェル粒子。
- 請求項12に記載の酸化亜鉛コアシェル粒子を含む紫外線遮蔽組成物。
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