TW201536686A - 氧化鋅粒子、其等之製造方法、紫外線遮蔽劑及化妝料 - Google Patents
氧化鋅粒子、其等之製造方法、紫外線遮蔽劑及化妝料 Download PDFInfo
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- TW201536686A TW201536686A TW103145670A TW103145670A TW201536686A TW 201536686 A TW201536686 A TW 201536686A TW 103145670 A TW103145670 A TW 103145670A TW 103145670 A TW103145670 A TW 103145670A TW 201536686 A TW201536686 A TW 201536686A
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- Prior art keywords
- zinc oxide
- oxide particles
- ultraviolet shielding
- particles
- coated
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 520
- 239000002245 particle Substances 0.000 title claims abstract description 304
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 259
- 239000002537 cosmetic Substances 0.000 title claims description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 29
- 239000003795 chemical substances by application Substances 0.000 title claims description 24
- 239000000463 material Substances 0.000 title description 7
- 239000011701 zinc Substances 0.000 claims abstract description 40
- 239000006104 solid solution Substances 0.000 claims abstract description 18
- 238000000576 coating method Methods 0.000 claims description 65
- 239000011248 coating agent Substances 0.000 claims description 63
- 239000002002 slurry Substances 0.000 claims description 48
- 239000002994 raw material Substances 0.000 claims description 42
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 41
- 239000007864 aqueous solution Substances 0.000 claims description 36
- 239000011164 primary particle Substances 0.000 claims description 31
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- 150000003608 titanium Chemical class 0.000 claims description 19
- 235000014413 iron hydroxide Nutrition 0.000 claims description 15
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- 238000010304 firing Methods 0.000 claims description 13
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
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- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims 1
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Classifications
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- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
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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
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- 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
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Abstract
提供一種六角板狀之氧化鋅粒子,其無損氧化鋅之電子激發的直接躍遷之性質而進一步提高400nm以下之波長的紫外線之遮蔽率,從而顯著提高UV-B波、UV-A波遮蔽率。
一種氧化鋅粒子,其特徵為:於至少一部分含有由Ti元素及/或Fe元素以及Zn元素構成之固溶體,該氧化鋅粒子之形狀為六角板狀。
Description
本發明係關於一種於至少一部分含有Zn2TiO4、ZnFe2O4所示之固溶體的氧化鋅粒子、其等之製造方法、紫外線遮蔽劑、化妝料。
太陽光所含之紫外線根據波長分類為400~320nm之UV-A波、320~290nm之UV-B波、及290~100nm之UV-C波,UV-A波占照射至地面之全部太陽紫外線量的97%以上,透過玻璃或雲層滲透至肌膚內部之真皮,而成為引起皺紋或鬆弛之光老化的原因。
先前,關於紫外線對策,對曬黑造成強力影響之UV-B波的對策受到重視,近年來,不斷推進對光老化之研究,消費者亦對UV-A波之對策予以關注。
為了高效率地遮蔽UV-A波,必須於製品中大量摻合有機化合物系紫外線吸收劑或無機化合物系紫外線遮蔽劑。另一方面,有機化合物系紫外線吸收劑雖被承認係安全性充分之素材,但於特定之紫外線吸收劑中,亦存在向化妝料中之摻合量受到限定者。根據以上情況,要求僅藉由無機化合物系紫外線遮蔽劑而充分地遮蔽UV-A波。
關於防曬製品中所使用之以氧化鋅或氧化鈦為代表的無機
化合物系紫外線遮蔽劑,藉由紫外線於粉體表面發生散射之效果、紫外線被粉體粒子吸收之效果,而表現其紫外線防禦能力。散射效果來自粒子之折射率或粒子尺寸,吸收效果來自粉體粒子所具有之能帶隙能量(Eg)。由於氧化鋅之Eg為3.2eV,電子激發為直接躍遷,故實質上可高效率地吸收與Eg值對應之388nm以下的波長之光。另一方面,廣泛用作化妝品用途之金紅石型氧化鈦之Eg為3.0eV,但由於氧化鈦之電子激發為間接躍遷,故實質上會高效率地吸收短於對應原本之Eg值的413nm之短波長側之約自320nm以下的光之波長。
又,氧化鐵(赤鐵礦)之Eg為2.2eV,與該值對應之波長為564nm。因此,認為不僅吸收UV-A波,亦吸收作為可見光之400-564nm的波長之光。
又,本發明人等完成六角板狀之氧化鋅粒子(專利文獻1)及其製造方法。專利文獻1所記載之六角板狀的氧化鋅粒子具有良好滑動性、柔焦效果、紫外線遮蔽性及可見光透明性,可較佳地用作化妝料用之紫外線遮蔽劑。又,該等氧化鋅粒子相較於習知之氧化鋅粒子具有較佳之紫外線遮蔽性能,可用作化妝料之紫外線遮蔽成分。然而,若可賦予更優異之紫外線遮蔽性能,則係進而較佳者。
於專利文獻2~5中記載有由鈦酸二鋅微粒子構成之紫外線防禦劑或使氧化鋅粒子含有鐵之紫外線遮蔽劑。然而,該等由於呈不具六角板狀形狀之粒子形狀,因此無法製成於上述具有六角板狀之氧化鋅粒子的形狀之粒子中獲得的具有各種性能之氧化鋅粒子。
[專利文獻1]國際公開2012/147886號
[專利文獻2]日本特開昭63-265819號公報
[專利文獻3]日本特開平9-188517號公報
[專利文獻4]日本特開平5-222317號公報
[專利文獻5]日本特開昭62-275182號公報
本發明之目的在於提供一種氧化鋅粒子,其係具有源自其形狀的較佳性能之六角板狀的氧化鋅粒子,不會明顯損及氧化鋅之電子激發的直接躍遷之性質而進一步提高400nm以下之波長的紫外線之遮蔽率,從而明顯提高UV-B波、UV-A波遮蔽率。
本發明之氧化鋅粒子之特徵為:於至少一部分含有由Ti元素及/或Fe元素以及Zn元素構成之固溶體,上述氧化鋅粒子之形狀為六角板狀。
較佳上述由Ti元素及/或Fe元素以及Zn元素構成之固溶體係被覆成為基材之氧化鋅粒子的表面之被膜。
較佳上述氧化鋅粒子係含有Zn2TiO4及/或ZnFe2O4之氧化鋅粒子,上述氧化鋅粒子之一次粒徑為0.01μm以上。
較佳上述氧化鋅粒子之Ti元素及/或Fe元素之含量相對於氧化鋅粒子100重量%,以TiO2換算及/或Fe2O3換算為5重量%以上30重量%以下。
本發明亦為一種上述氧化鋅粒子之製造方法,其特徵在於具有如下步驟:步驟(1-1):於六角板狀之原料氧化鋅粒子的水性漿料,一面於溫度10℃以上90℃以下之範圍保持pH9±3,一面添加鈦鹽及/或鐵鹽之
水溶液與鹼性水溶液;及步驟(1-2):對藉由上述步驟(1-1)而獲得之被覆氧化鋅粒子進行燒成。
本發明亦為一種上述氧化鋅粒子之製造方法,其特徵在於具有如下步驟:步驟(2-1):將原料氧化鋅粒子添加至溶解有鈦鹽及/或鐵鹽之鋅鹽水溶液中,進行加熱熟成;及步驟(2-2):對藉由上述步驟(2-1)而獲得之含氫氧化鈦及/或氫氧化鐵之六角板狀氧化鋅粒子進行燒成。
本發明亦為一種藉由上述製造方法而獲得之氧化鋅粒子。
本發明亦為一種紫外線遮蔽劑,其特徵在於:含有上述氧化鋅粒子。
本發明亦為一種化妝料,其特徵在於:含有上述氧化鋅粒子。
本發明之氧化鋅粒子無損六角板狀之氧化鋅的電子激發之直接躍遷的性質而進一步提高400nm以下之波長的紫外線之遮蔽率,藉此明顯提高對UV-B波、UV-A波之紫外線遮蔽率。
圖1係表示實施例1之被覆Zn2TiO4的氧化鋅粒子之穿透式電子顯微鏡照片的圖。
圖2係表示實施例1之被覆Zn2TiO4的氧化鋅粒子之X射線繞射光譜的圖。
圖3係表示實施例2之被覆ZnFe2O4的氧化鋅粒子之穿透式電子顯微鏡照片的圖。
圖4係表示實施例2之被覆ZnFe2O4的氧化鋅粒子之X射線繞射光譜的圖。
圖5係表示實施例3之被覆Zn2TiO4+ZnFe2O4的氧化鋅粒子之穿透式電子顯微鏡照片的圖。
圖6係表示實施例3之被覆Zn2TiO4+ZnFe2O4的氧化鋅粒子之X射線繞射光譜的圖。
圖7係表示實施例4之含ZnFe2O4的氧化鋅粒子之穿透式電子顯微鏡照片的圖。
圖8係表示實施例4之含ZnFe2O4的氧化鋅粒子之X射線繞射光譜的圖。
圖9係表示比較例1之成為母體的六角板狀氧化鋅粒子之穿透式電子顯微鏡照片的圖。
圖10係表示比較例2之成為母體的不定形氧化鋅粒子之穿透式電子顯微鏡照片的圖。
圖11係表示比較例3之被覆Zn2TiO4的氧化鋅粒子之穿透式電子顯微鏡照片的圖。
圖12係表示比較例3之被覆Zn2TiO4的氧化鋅粒子之X射線繞射光譜的圖。
圖13係表示比較例4之被覆ZnFe2O4的氧化鋅粒子之穿透式電子顯微鏡照片的圖。
圖14係表示比較例4之被覆ZnFe2O4的氧化鋅粒子之X射線繞射光譜的圖。
圖15係表示對含有實施例1之被覆Zn2TiO4之氧化鋅粒子的塗膜之紫外
線遮蔽率、含有實施例2之被覆ZnFe2O4之氧化鋅粒子的塗膜之紫外線遮蔽率及含有比較例1之氧化鋅粒子之塗膜之紫外線遮蔽率進行比較之波長300~400nm的紫外線波長區域中總光線透射率曲線的圖。
圖16係表示對實施例及比較例之氧化鋅粒子的一次粒徑之測量方法進行圖示的模式圖。
圖17係對六角板狀氧化鋅粒子的縱橫比之測量方法進行圖示的模式圖。
圖18係對不定形之氧化鋅粒子的縱橫比之測量方法進行圖示的模式圖。
圖19係關於紫外線遮蔽率1(%)、紫外線遮蔽率2(%)的說明圖。
以下,詳細地說明本發明。
本發明係下述之氧化鋅粒子:於至少一部分含有由Ti元素及/或Fe元素以及Zn元素構成之固溶體,形狀為六角板狀。即,獲得如下氧化鋅粒子:於具有如專利文獻1所記載的特徵之具有優異性能的氧化鋅粒子中,藉由設為於至少一部分含有由Ti元素及/或Fe元素以及Zn元素構成之固溶體者,使紫外線之吸收特性發生變化,進而提高紫外線遮蔽性能。
被覆或含有本發明之固溶體之氧化鋅粒子兼具氧化鋅的電子激發之直接躍遷的性質與Zn2TiO4、或ZnFe2O4之紫外線遮蔽性能,為前所未有之氧化鋅粒子。
(由Ti元素及/或Fe元素以及Zn元素構成之固溶體)
本發明之氧化鋅粒子於至少一部分含有由Ti元素及/或Fe元素以及Zn元素構成之固溶體。即,係於一部分中具有Zn2TiO4及/或ZnFe2O4者,可為於氧化鋅粒子表面形成有利用該等化合物之被覆者,亦可為於氧化鋅粒子內局部存在由Zn2TiO4及/或ZnFe2O4構成之部分者。由於經Zn2TiO4及/或ZnFe2O4被覆氧化鋅粒子表面而成者其可見光透射率增高,故就摻合於化妝品時透明性更高等觀點而言更佳。
本發明之氧化鋅粒子亦可設為含有上述Ti元素、Fe元素兩者之狀態。又,關於Ti元素及/或Fe元素之含量,相對於氧化鋅粒子100重量%,以TiO2換算及/或Fe2O3換算較佳為5重量%以上30重量%以下,更佳為7重量%以上25重量%以下。若未達5重量%,則就無法充分地獲得提高上述波長400nm以下的紫外線之吸收能的效果方面而言欠佳。若超過30重量%,則就失去氧化鋅粒子所具有的電子激發之直接躍遷的性質方面而言欠佳。對上述氧化鋅粒子之TiO2換算及/或Fe2O3換算之含量係藉由螢光X射線分析裝置ZSX Primus II(理學公司製造)測得之值,所應用之軟體為EZ Scan(SQX)。
於本發明中,Ti元素及/或Fe元素係形成與Zn元素之固溶體者。更佳於Zn2TiO4或ZnFe2O4之通式所示之狀態下存在於氧化鋅粒子中或表面。
形成此種Zn2TiO4及/或ZnFe2O4可藉由X射線繞射而進行確認。如於實施例中亦詳細說明般,對本發明之氧化鋅粒子進行X射線繞射之測量,結果可觀察到ZnO以及Zn2TiO4及/或ZnFe2O4之繞射光譜,藉此,可確認於上述固溶體之狀態下存在Ti元素及/或Fe元素。X射線繞射
係藉由具有銅球管之X射線繞射裝置Ultima III(理學公司製造)進行測量。
關於本發明之氧化鋅粒子,於對成為母體之六角板狀的原料氧化鋅粒子,藉由被覆而形成Zn2TiO4、ZnFe2O4所示之固溶體的情形時,較佳為紫外線遮蔽率高於成為母體之原料氧化鋅粒子者。紫外線存在UV-A波與UV-B波,較佳為對於其任一者或兩者而言,紫外線遮蔽率高於成為母體之原料氧化鋅粒子。具體而言,較佳為下述(被覆氧化鋅粒子之紫外線遮蔽率(%))/(成為被覆氧化鋅粒子之母體的原料氧化鋅粒子之紫外線遮蔽率(%))的比值成為1.1以上。
於本說明書中,紫外線遮蔽率係基於對藉由實施例中記載之方法製作的塗膜所測得之總光線透射率而算出之值。
(總光線透射率1、總光線透射率2)
於本說明書中,於實施例中詳細說明之總光線透射率1(%)、總光線透射率2(%)係藉由分光光度計V-570(日本分光公司製造)對所製作之塗膜進行測量而得之值。再者,總光線透射率1(%)之值為波長300nm下的總光線透射率之值,總光線透射率2(%)之值為波長360nm下之總光線透射率之值。總光線透射率1(%)之值越小,意指對UV-B之波長的紫外線之紫外線遮蔽效果越高,總光線透射率2(%)之值越小,意指對UV-A之波長的紫外線之紫外線遮蔽效果越高。
(紫外線遮蔽率1、紫外線遮蔽率2)
於本說明書中,基於上述總光線透射率,藉由下式算出紫外線遮蔽率。
紫外線遮蔽率1(%)=100%-總光線透射率1(%)
紫外線遮蔽率2(%)=100%-總光線透射率2(%)
即,紫外線遮蔽率1(%)之值係指對波長300nm下之紫外線的遮蔽率,該值越大,意指對UV-B波之紫外線遮蔽性越高。
又,紫外線遮蔽率2(%)之值係指對波長360nm下之紫外線的遮蔽率,該值越大,意指對UV-A波之紫外線遮蔽性越高。
關於總光線透射率1(%)、總光線透射率2(%)、紫外線遮蔽率1(%)、紫外線遮蔽率2(%),為了更容易理解有關各自之關係性,而將說明圖隨附於圖19。
((含有被覆氧化鋅粒子之塗膜的紫外線遮蔽率1(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率1(%))的比)
本說明書中,於本發明之氧化鋅粒子藉由被覆而形成Zn2TiO4、ZnFe2O4所示之固溶體之情形時,較佳UV-B波之((含有被覆氧化鋅粒子之塗膜的紫外線遮蔽率1(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率1(%))的比)成為1.1以上。
((含有被覆氧化鋅粒子之塗膜的紫外線遮蔽率2(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率2(%))的比)
本說明書中,於本發明之氧化鋅粒子藉由被覆而形成Zn2TiO4、ZnFe2O4所示之固溶體的情形時,較佳UV-A波之((含有被覆氧化鋅粒子之塗膜的紫外線遮蔽率2(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率2(%))的比)成為1.1以上。
(氧化鋅粒子之形狀)
本發明之氧化鋅粒子係具有六角板狀之形狀者。亦如專利文獻1中所記載,此種形狀之氧化鋅粒子具有優異紫外線遮蔽性能,且藉由自具有特定粒子形狀所獲得之物理效果,作為化妝料素材而發揮出優異功能。更具體而言,係可獲得由六角板狀之形狀所獲得的光滑觸感,另外於柔焦性方面亦優異之粒子。本發明之氧化鋅粒子具有此種優異效果,於六角板狀氧化鋅粒子中,使400nm以下之區域中的紫外線吸收能變得更優異。
上述具有六角板狀形狀之氧化鋅粒子並無特別限定,較佳為如以下詳細說明者。
本發明之氧化鋅粒子的一次粒徑較佳為0.01μm以上。藉由適當控制氧化鋅粒子之一次粒徑,可選擇性地賦予良好滑動性、柔焦效果、紫外線遮蔽性、可見光透明性等各種性能。上述一次粒徑更佳為0.02μm以上,進而較佳為0.03μm以上。
上述一次粒徑之上限並無特別限定,例如較佳為100μm以下,更佳為50μm以下,進而較佳為25μm以下。
本說明書中之一次粒徑係藉由穿透式電子顯微鏡JEM-2100(日本電子公司製造)照片之2000~50000倍的視野中之定方向徑(夾著粒子之一定方向的兩條平行線之間隔;不論對圖像上之何種形狀之粒子均於一定方向上進行測量)進行定義之粒徑(μm),係測量TEM照片內之250個一次粒子之定方向徑,求出其累積分佈之平均值而得者。關於上述一次粒徑之測量方法,隨附圖16。
進而,本發明之六角板狀氧化鋅粒子的縱橫比較佳為2.5以上。即,係具有六角板狀之形狀的氧化鋅粒子,藉由此種形狀,尤其是用
於化妝料中之情形時,滑動良好,可獲得優異之使用感。關於本發明中之六角板狀氧化鋅粒子之縱橫比如下所述:於穿透式電子顯微鏡JEM-2100(日本電子公司製造)照片之2000~50000倍的視野中,對六角板狀氧化鋅粒子之六角形狀面朝向近前之粒子,對以其定方向徑(夾著粒子之一定方向的兩條平行線之間隔;對圖像上之六角形狀面朝向近前之粒子,於一定方向上進行測量)所定義之粒徑(μm)測量250個粒子而獲得平均值,將該平均值設為L,並對六角板狀氧化鋅粒子之側面朝向近前之粒子(視為長方形之粒子),對其厚度(μm)(長方形之短邊之長度)測量250個粒子而獲得平均值,將該平均值設為T,此時,其等之值的比:以L/T所求出之值。關於上述縱橫比之測量方法,隨附圖17。上述縱橫比更佳為2.7以上,進而較佳為3.0以上。
再者,關於本說明書之比較例中粒子形狀不定形的粒子之縱橫比如下所述:於穿透式電子顯微鏡JEM-2100(日本電子公司製造)照片之2000~50000倍的視野中,對250個不定形之粒子測量粒子的長徑與通過長徑之中心的短徑,並求出長徑與短徑之長度的比:長徑/短徑,將其累積分佈之平均值作為縱橫比而求出。關於不定形之粒子的縱橫比之測量方法,示於圖18。
(製造方法)
本發明之氧化鋅粒子並未特別限定製造方法,例如可列舉:對藉由專利文獻1中記載之方法而獲得的原料氧化鋅粒子,利用含有Fe、Ti之化合物而實施處理的方法;於專利文獻1中記載之六角板狀氧化鋅粒子的製造方法(包括將微粒子氧化鋅於鋅鹽水溶液中熟成之步驟在內之氧化鋅的製
造方法)中,於鐵離子、鈦離子之存在下進行反應的方法等。
更具體而言,尤佳為如下製造方法之任一種:該製造方法(製造方法1)之特徵在於具有如下步驟:步驟(1-1):於六角板狀之原料氧化鋅粒子的水性漿料,一面保持pH、溫度之條件,一面添加鈦鹽及/或鐵鹽之水溶液與鹼性水溶液;及步驟(1-2):對藉由上述步驟(1-1)而獲得之被覆氧化鋅粒子進行燒成;該製造方法(製造方法2)之特徵在於具有如下步驟:步驟(2-1):將氧化鋅粒子添加至溶解有鈦鹽、及/或鐵鹽之鋅鹽水溶液中,進行加熱熟成;及步驟(2-2):對藉由上述步驟(2-1)而獲得之含氫氧化物的六角板狀氧化鋅粒子進行燒成。
以下,對該等製造方法進行詳細說明。
(製造方法1)
上述製造方法如下:將六角板狀之原料氧化鋅粒子添加至液體介質中製成水性漿料,於該水性漿料中,使鈦鹽及/或鐵鹽析出至原料氧化鋅粒子之表面,藉此形成表面被覆,對其進行燒成而形成被覆。對藉由此種製造方法而獲得之被覆氧化鋅粒子,利用X射線繞射進行分析,結果明確得知並非由氧化鈦、氧化鐵形成之被覆,而由以Ti元素及/或Fe元素以及Zn元素構成之固溶體形成被覆。
於該步驟中所使用之作為原料氧化鋅粒子的六角板狀氧化鋅粒子可較佳地使用藉由專利文獻1記載之製造方法而獲得者。
專利文獻1中記載之氧化鋅粒子之製造方法為漿料中之反應,但可於進行該反應後,直接供給至本發明之製造方法,亦可於進行過濾、水洗、
乾燥、燒成等步驟後,再次使之分散於水性介質中,藉此製成水性漿料。
於上述漿料中,上述六角板狀之原料氧化鋅粒子較佳設為10~500g/l之濃度。
構成漿料之液體介質較佳為水或水與水溶性有機溶劑之混合液體,最佳為水。於使用水與水溶性有機溶劑之混合液體的情形時,作為水溶性有機溶劑,可使用甲醇、乙醇等低級醇;丙酮等可以任意比例與水混合之溶劑,關於水溶性有機溶劑之使用量,相對於混合溶劑總量較佳為1~30重量%。
於漿料之製備時,亦可視需要使用分散劑。
作為上述鈦鹽,並無特別限定,例如可列舉:如硫酸鈦、四異丙醇鈦(titanium tetraisopropoxide)之類的四烷醇鈦(titanium tetraalkoxide)、四氯化鈦等。
作為上述鐵鹽,並無特別限定,例如可列舉:乙酸亞鐵、三乙酸鐵、氯化亞鐵、氯化鐵、硫酸亞鐵、硫酸鐵、硝酸亞鐵、硝酸鐵等。
關於上述鈦鹽及/或鐵鹽之水溶液,鈦鹽及/或鐵鹽之濃度較佳為50~300g/l。藉由使用上述範圍內之水溶液,不會降低生產性,且可於成為母體之原料氧化鋅粒子表面均勻地形成被覆層,就該方面而言較佳。
上述鈦鹽及/或鐵鹽之水溶液並非需要鈦鹽及/或鐵鹽與水以外之成分者,但可於不損及本發明之效果之範圍內摻合其他成分。
作為上述鹼性水溶液中之鹼性化合物,並無特別限定,可使用氫氧化鈉、氫氧化鉀、氨等。上述鹼性水溶液之濃度並無特別限定,例
如可設為5~30重量%。
於上述步驟(1-1)中,一面保持pH及溫度之條件,一面添加鈦鹽及/或鐵鹽之水溶液與鹼性水溶液。藉此,藉由均勻地析出鈦及/或鐵,可較佳地達成目標。
作為上述pH與溫度之條件,較佳一面維持pH9±3、溫度10℃以上90℃以下之條件,一面添加上述鈦鹽及/或鐵鹽之水溶液與上述鹼性水溶液。反應時間並無特別限定,例如能以10~360分鐘進行。
關於上述鈦鹽及/或鐵鹽之水溶液與上述鹼性水溶液之添加,較佳為於成為添加對象之上述漿料的液面之不同位置同時添加各水溶液的方法。藉由同時進行添加,可於成為母體之氧化鋅粒子的表面形成形狀、粒徑均勻之氫氧化鈦粒子及/或形狀、粒徑均勻之氫氧化鐵粒子的被覆。作為此種添加之方法,並無特別限定,例如可列舉藉由泵連續地添加一定量之方法等。上述水溶液之添加量較佳設為與目標氧化鋅粒子中之鈦、鐵的量相應之量。於在上述漿料中同時添加上述鈦鹽及/或鐵鹽之水溶液與鹼水溶液時,較佳預先對上述漿料進行攪拌。藉此,可於氧化鋅粒子表面形成均勻之氫氧化鈦粒子及/或氫氧化鐵粒子。上述漿料之攪拌可藉由使用攪拌機等通常之攪拌方法而進行。
其後,對進行了上述步驟(1-1)之漿料進行過濾,視需要進行水洗、乾燥,藉此可獲得被覆氫氧化物之氧化鋅粒子。對以上述方式獲得之被覆氫氧化物的氧化鋅粒子於步驟(1-2)中進行燒成。藉此,形成由Ti元素及/或Fe元素以及Zn元素構成之固溶體。
於上述步驟(1-2)中,燒成溫度較佳為400~900℃。若為
500℃以上,則就結晶性高,紫外線遮蔽效果增高之方面而言較佳。步驟(1-2)中之燒成氣體環境並無特別限定,可列舉:大氣、氧氣、氮氣、二氧化碳、氫氣、氬氣、甲烷等。燒成時間亦取決於燒成溫度,但較佳為1~50小時。
(製造方法2)
上述製造方法2具有步驟(2-1):於溶解有鈦鹽及/或鐵鹽之鋅鹽水溶液中,將原料氧化鋅粒子加熱熟成。
於上述步驟(2-1)中,作為可使用之鈦鹽、鐵鹽,可分別列舉上述者。
作為鋅鹽,並無特別限定,可列舉:硫酸鋅、硝酸鋅、乙酸鋅、氯化鋅、甲酸鋅等。
上述鋅鹽水溶液中之鋅鹽的濃度較佳為0.005~4.0mol/l。上述鋅鹽水溶液中之鈦鹽及/或鐵鹽的濃度較佳為50~300g/l。
構成上述鋅鹽水溶液之液體介質較佳為水或水與水溶性有機溶劑之混合液體,最佳為水。於使用水與水溶性有機溶劑之混合液體的情形時,作為水溶性有機溶劑,可使用甲醇、乙醇等低級醇;丙酮等可以任意比例與水混合之溶劑,關於水溶性有機溶劑之使用量,相對於混合溶劑總量較佳為1~30重量%。
於漿料之製備時,亦可視需要使用分散劑。
作為製造方法2中之原料氧化鋅粒子,並非限定於六角板狀者,可使用任意形狀之氧化鋅粒子。
可將上述原料氧化鋅粒子添加至鋅鹽水溶液中,並進行攪拌、分散,藉此製成漿料狀,並於該漿料中進行反應。
上述原料氧化鋅粒子相對於漿料總量較佳設為10~500g/l
之濃度。反應溫度較佳為10~110℃,反應時間較佳為0.5~24小時。進行上述步驟(2-1)之漿料的pH較佳為5.5~13.5。
其後,對進行了上述步驟(2-1)之漿料進行過濾,視需要進行水洗、乾燥,藉此可獲得含氫氧化物之氧化鋅粒子。對以上述方式獲得的含氫氧化物之氧化鋅粒子於步驟(2-2)中進行燒成。藉此,形成由Ti元素及/或Fe元素以及Zn元素構成之固溶體。
於上述步驟(2-2)中,燒成溫度較佳為400~900℃。若為500℃以上,則就結晶性高,紫外線遮蔽效果增高之方面而言較佳。步驟(2-2)中之燒成氣體環境並無特別限定,可列舉:大氣、氧氣、氮氣、二氧化碳、氫氣、氬氣、甲烷等。燒成時間亦取決於燒成溫度,但較佳為1~5小時。
(表面處理)
本發明之氧化鋅粒子亦可為進而實施過表面處理者。作為上述表面處理,並無特別限定,可列舉:形成選自由矽氧化物、矽氧化物之水合物、鋁之氧化物及鋁之氫氧化物組成之群中至少1種化合物之皮膜的表面處理、利用撥水性有機化合物之表面處理、利用矽烷偶合劑、鈦偶合劑等偶合劑之表面處理等。亦可組合進行該等之2種以上之表面處理。
形成選自由上述矽氧化物、矽氧化物之水合物、鋁之氧化物及鋁之氫氧化物組成之群中之至少1種化合物的皮膜可藉由如下方法等而進行:藉由水解或加熱分解等使Si源化合物及/或Al源化合物析出至粉體表面。作為上述Si源化合物及/或Al源化合物,可使用四烷氧矽烷或其水解縮合物、矽酸鈉、矽酸鉀、烷醇鋁(aluminium alkoxide)或其水解縮合物、鋁酸鈉等容易地轉化為SiO2或Al(OH)3、Al2O3之化合物等。
作為上述水解,並無特別限定,可列舉使用硫酸、鹽酸、乙酸、硝酸等酸之方法。使用該水分散體的二氧化矽之處理方法中的中和方法可為於分散體中添加酸後添加Si源化合物及/或Al源化合物之方法、於分散體中添加Si源化合物及/或Al源化合物後添加酸之方法、於分散體中同時添加Si源化合物及/或Al源化合物與酸之方法中之任一種。
作為上述利用撥水性有機化合物之處理,並無特別限定,例如可列舉:聚矽氧油、烷基矽烷、鈦酸烷基酯(alkyl titanate)、鋁酸烷基酯(alkyl aluminate)、聚烯烴、聚酯、金屬皂、胺基酸、胺基酸鹽等。其中,就化學穩定性而言,較佳為聚矽氧油。作為該聚矽氧油之具體例,可列舉:利用二甲基聚矽氧烷(例如信越化學工業製造之KF-96A-100cs、Wacker asahikasei silicone製造之DM10)、甲基氫聚矽氧烷(例如信越化學工業製造之KF-99P、道康寧東麗股份有限公司製造之SH1107C)、(二甲聚矽氧烷(dimethicone)/甲聚矽氧烷(methicone))共聚物(例如信越化學工業製造之KF-9901)、甲基苯基聚矽氧(例如信越化學工業製造之KF-50-100cs)、胺基改質聚矽氧(例如信越化學工業製造之KF-8015、道康寧東麗股份有限公司製造之JP-8500 Conditioning Agent、Wacker asahikasei silicone製造之ADM6060)、三乙氧基矽烷基乙基聚二甲基矽烷氧基乙基二甲聚矽氧烷(例如信越化學工業製造之KF-9908)、三乙氧基矽烷基乙基聚二甲基矽烷氧基乙基己基二甲聚矽氧烷(例如信越化學工業製造之KF-9909)之處理等。
作為利用上述矽烷偶合劑之處理,可列舉:乙烯基三(2-甲氧基乙氧基)矽烷、乙烯基三氯矽烷、乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、2-(3,4-環氧環己基)乙基三甲氧基矽烷、3-環氧丙氧基丙基三甲氧基
矽烷、3-環氧丙氧基丙基甲基二乙氧基矽烷、3-環氧丙氧基丙基三乙氧基矽烷、對苯乙烯基三甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二乙氧基矽烷、3-甲基丙烯醯氧基丙基三乙氧基矽烷、3-丙烯醯氧基丙基三甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基甲基二甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基三甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基三乙氧基矽烷、3-胺基丙基三甲氧基矽烷、3-胺基三乙氧基矽烷、3-三乙氧基矽烷基-N-(1,3-二甲基-亞丁基)丙基胺、N-苯基-3-胺基丙基三甲氧基矽烷、N-(乙烯基苄基)-2-胺基乙基-3-胺基丙基三甲氧基矽烷鹽酸鹽、3-脲基丙基三乙氧基矽烷、3-氯丙基三甲氧基矽烷、3-巰基丙基甲基二甲氧基矽烷、3-巰基丙基三甲氧基矽烷、雙(三乙氧基矽烷基丙基)四硫醚、3-異氰酸酯基丙基三乙氧基矽烷、四甲氧基矽烷、四乙氧基矽烷、甲基三甲氧基矽烷、甲基三乙氧基矽烷、苯基三乙氧基矽烷、六甲基二矽氮烷、己基三甲氧基矽烷、癸基三甲氧基矽烷。
作為上述利用鈦偶合劑之處理,可列舉:鈦酸四異丙酯、鈦酸四正丁酯、鈦酸丁酯二聚物、鈦酸四(2-乙基己基)酯、鈦酸四甲酯、乙醯丙酮酸鈦、四乙醯丙酮酸鈦、乙醯乙酸乙酯鈦、辛二醇鈦(titanium octanediolate)、乳酸鈦(titanium lactate)、三乙醇胺鈦、聚羥基鈦硬脂酸酯。
於進行上述表面處理之情形時,表面處理較佳以相對於處理後之粉體的總量成為1~10重量%之比例進行。藉由設為該範圍內者,就提高滑動性,且提高耐濕性,提高於樹脂中之分散性的方面而言較佳。
(用途)
本發明之氧化鋅粒子亦可與其他成分混合而摻合於化妝料、油墨、塗
料、塑膠等中。尤其是由於具有上述特性,故就可獲得穩定性及紫外線遮蔽效果優異之化妝料的方面而言較佳。
(於化妝料領域中之使用)
作為上述化妝料,並無特別限定,藉由在此種複合粉體中視需要混合化妝品原料,可獲得防曬劑等防紫外線用化妝料;粉底等底妝(base makeup)化妝料;唇膏等重點彩妝(point makeup)化妝料等。又,由於係具有紫外線遮蔽能之特徵者,因此係在用於化妝品中之情形時具有優異性能者。
上述化妝料可設為油性化妝料、水性化妝料、O/W型化妝料、W/O型化妝料之任意形態。
上述化妝料亦可為併用於化妝品領域中可使用之任意水性成分、油性成分者。作為上述水性成分及油性成分,並無特別限定,例如亦可為含有油劑、界面活性劑、保濕劑、高級醇、金屬離子封阻劑、天然及合成高分子、水溶性及油溶性高分子、紫外線遮蔽劑、各種萃取液、有機染料等色劑、防腐劑、抗氧化劑、色素、增黏劑、pH調整劑、香料、冷感劑、止汗劑、殺菌劑、皮膚活化劑、各種粉體等成分者。
上述油劑並無特別限定,例如可例示:天然動植物油脂(例如橄欖油、貂油、蓖麻油、棕櫚油、牛油、月見草油、椰油、可可油、澳洲胡桃油等);蠟(例如荷荷芭油、蜂蠟、羊毛脂、巴西棕櫚蠟、堪地里拉蠟等);高級醇(例如月桂醇、硬脂醇、鯨蠟醇、油醇等);高級脂肪酸(例如月桂酸、棕櫚酸、硬脂酸、油酸、山萮酸、羊毛脂脂肪酸等;高級脂肪族烴(例如液態石蠟、固態石蠟、角鯊烷、凡士林、地蠟、微晶蠟等);合成酯油(例如硬脂酸丁酯、月桂酸己酯、己二酸二異丙酯、癸二酸二異丙
酯、肉豆蔻酸辛基十二烷基酯、肉豆蔻酸異丙酯、棕櫚酸異丙酯、異辛酸鯨蠟酯、二癸酸新戊二醇酯);聚矽氧衍生物(例如甲基聚矽氧、甲基苯基聚矽氧等聚矽氧油)等。進而,亦可摻合油溶性維生素、防腐劑、美白劑等。
作為上述界面活性劑,可列舉:親油性非離子界面活性劑、親水性非離子界面活性劑等。作為上述親油性非離子界面活性劑,並無特別限定,例如可列舉:山梨糖醇酐單油酸酯、山梨糖醇酐單異硬脂酸酯、山梨糖醇酐單月桂酸酯、山梨糖醇酐單棕櫚酸酯、山梨糖醇酐單硬脂酸酯、山梨糖醇酐倍半油酸酯(sorbitan sesquioleate)、山梨糖醇酐三油酸酯(sorbitan trioleate)、山梨糖醇酐五-2-乙基己酸二甘油酯、山梨糖醇酐四-2-乙基己酸二甘油酯等山梨糖醇酐脂肪酸酯類,單棉籽油脂肪酸甘油酯、單芥子酸甘油酯、倍半油酸甘油酯、單硬脂酸甘油酯、α,α'-油酸焦麩胺酸甘油酯、蘋果酸單硬脂酸甘油酯等甘油聚甘油脂肪酸酯類,單丙二醇硬脂酸酯等丙二醇脂肪酸酯類,氫化蓖麻油衍生物,甘油烷基醚等。
作為親水性非離子界面活性劑,並無特別限定,例如可列舉:POE山梨糖醇酐單油酸酯、POE山梨糖醇酐單硬脂酸酯、POE山梨糖醇酐四油酸酯等POE山梨糖醇酐脂肪酸酯類,POE山梨糖醇單月桂酸酯、POE山梨糖醇單油酸酯、POE山梨糖醇五油酸酯、POE山梨糖醇單硬脂酸酯等POE山梨糖醇脂肪酸酯類,POE甘油單硬脂酸酯、POE甘油單異硬脂酸酯、POE甘油三異硬脂酸酯等POE甘油脂肪酸酯類,POE單油酸酯、POE二硬脂酸酯、POE單二油酸酯、二硬脂酸乙二醇酯等POE脂肪酸酯類,POE月桂醚、POE油醚、POE硬脂醚、POE山萮醚、POE2-辛基十二烷基醚、POE
二氫膽固醇醚等POE烷基醚類,POE辛基苯醚、POE壬基苯醚、POE二壬基苯醚等POE烷基苯醚類,普朗尼克(pluronic)等普洛尼克(pluaronic)型類,POE-POP鯨蠟醚、POE-POP2-癸基十四烷基醚、POE-POP單丁醚、POE-POP氫化羊毛脂、POE-POP甘油醚等POE-POP烷基醚類,特窗(tetronic)等四POE-四POP乙二胺縮合物類,POE蓖麻油、POE氫化蓖麻油(POE hydrogenated castor oil)、POE氫化蓖麻油單異硬脂酸酯、POE氫化蓖麻油三異硬脂酸酯、POE氫化蓖麻油單焦麩胺酸單異硬脂酸二酯、POE氫化蓖麻油順丁烯二酸等POE蓖麻油氫化蓖麻油衍生物,POE山梨糖醇蜂蠟等POE蜂蠟-羊毛脂衍生物,椰油脂肪酸二乙醇醯胺、月桂酸單乙醇醯胺、脂肪酸異丙醇醯胺等烷醇醯胺,POE丙二醇脂肪酸酯,POE烷基胺,POE脂肪醯胺,蔗糖脂肪酸酯,POE壬基苯基甲醛縮合物,烷基乙氧基二甲基氧化胺,磷酸三油酯等。
作為其他界面活性劑,例如亦可於在穩定性及皮膚刺激性方面沒有問題之範圍內摻合脂肪酸皂、高級烷基硫酸酯鹽、POE月桂基硫酸三乙醇胺、烷基醚硫酸酯鹽等陰離子界面活性劑,烷基三甲基銨鹽、烷基吡啶鎓鹽、烷基四級銨鹽、烷基二甲基苄基銨鹽、POE烷基胺、烷基胺鹽、聚胺脂肪酸衍生物等陽離子界面活性劑,及咪唑啉系兩性界面活性劑、甜菜鹼系界面活性劑等兩性界面活性劑。
作為上述保濕劑,並無特別限定,例如可列舉:木糖醇、山梨糖醇、麥芽糖醇、軟骨素硫酸、透明質酸、硫酸黏多糖(mucoitinsulfuric acid)、括樓仁酸(carolinic acid)、動脈膠原蛋白(atelocollagen)、膽固醇基-12-羥基硬脂酸酯、乳酸鈉、膽鹽、dl-吡咯啶酮羧酸鹽、短鏈可溶性膠原蛋白、
二甘油(EO)PO加成物、十六夜薔薇(chestnut rose)萃取物、洋蓍草(Achillea millefolium)萃取物、黃香草木樨萃取物等。
作為上述高級醇,並無特別限定,例如可列舉:月桂醇、鯨蠟醇、硬脂醇、山萮醇、肉豆蔻醇、油醇、鯨蠟硬脂醇等直鏈醇,單硬脂基甘油醚(鯊肝醇)、2-癸基十四烷醇、羊毛脂醇、膽固醇、植固醇、己基十二烷醇、異硬脂醇、辛基十二烷醇等支鏈醇等。
作為金屬離子封阻劑,並無特別限定,例如可列舉:1-羥基乙烷-2,1-二膦酸、1-羥基乙烷-1,1-二膦酸四鈉鹽、檸檬酸鈉、聚磷酸鈉、偏磷酸鈉、葡萄糖酸、磷酸、檸檬酸、抗壞血酸、琥珀酸、乙二胺四乙酸等。
作為上述天然之水溶性高分子,並無特別限定,例如可列舉:阿拉伯膠、黃蓍膠、聚半乳糖、瓜爾膠、刺槐豆膠、刺梧桐樹膠、角叉菜膠、果膠、瓊脂、榅桲籽(榅桲)、海藻膠(algae colloid)(褐藻萃取物)、澱粉(大米、玉米、馬鈴薯、小麥)、甘草酸等植物系高分子,黃原膠、葡聚糖、琥珀醯聚糖(succinoglucan)、聚三葡萄糖等微生物系高分子,膠原蛋白、酪蛋白、白蛋白、明膠等動物系高分子。
作為半合成之水溶性高分子,並無特別限定,例如可列舉:羧甲基澱粉、甲基羥丙基澱粉等澱粉系高分子,甲基纖維素、硝化纖維素、乙基纖維素、甲基羥丙基纖維素、羥乙基纖維素、纖維素硫酸鈉、羥丙基纖維素、羧甲基纖維素鈉(CMC)、纖維素結晶、纖維素粉末等纖維素系高分子,海藻酸鈉、海藻酸丙二醇酯等海藻酸系高分子等。
作為合成之水溶性高分子,並無特別限定,例如可列舉:聚乙烯醇、聚乙烯基甲醚、聚乙烯基吡咯啶酮等乙烯基系高分子,聚乙二醇
20,000、40,000、60,000等聚氧乙烯系高分子,聚氧乙烯聚氧丙烯共聚物共聚合系高分子、聚丙烯酸鈉、聚丙烯酸乙酯、聚丙烯醯胺等丙烯酸系高分子,聚甘油、聚伸乙基亞胺、陽離子聚合物、羧基乙烯基聚合物、烷基改質羧基乙烯基聚合物、(丙烯酸羥基乙酯/丙烯醯基二甲基牛磺酸Na)共聚物、(丙烯酸Na/丙烯醯基二甲基牛磺酸Na)共聚物、(丙烯醯基二甲基牛磺酸銨/乙烯基吡咯啶酮)共聚物、(丙烯醯基二甲基牛磺酸銨/山萮醇聚醚-25甲基丙烯酸酯)交聯聚合物等。
作為無機之水溶性高分子,並無特別限定,例如可列舉:膨潤土、矽酸鋁鎂(veegum)、合成鋰皂石、鋰膨潤石、矽酸酐等。
作為紫外線遮蔽劑,並無特別限定,例如可列舉:對胺基苯甲酸(以下簡稱為PABA)、PABA單甘油酯、N,N-二丙氧基PABA乙酯、N,N-二乙氧基PABA乙酯、N,N-二甲基PABA乙酯、N,N-二甲基PABA丁酯等苯甲酸系紫外線遮蔽劑;N-乙醯基鄰胺基苯甲酸高薄荷酯(homo menthyl N-acetyl anthranilate)等鄰胺苯甲酸系紫外線遮蔽劑;柳酸戊酯、柳酸酯(menthyl salicylate)、柳酸高酯(homo menthyl salicylate)、柳酸辛酯、柳酸苯酯、柳酸苄酯、對異丙醇苯基柳酸酯等柳酸系紫外線遮蔽劑;肉桂酸辛酯、4-異丙基肉桂酸乙酯、2,5-二異丙基肉桂酸甲酯、2,4-二異丙基肉桂酸乙酯、2,4-二異丙基肉桂酸甲酯、對甲氧基肉桂酸丙酯、對甲氧基肉桂酸異丙酯、對甲氧基肉桂酸異戊酯、對甲氧基肉桂酸2-乙氧基乙酯、對甲氧基肉桂酸環己酯、α-氰基-β-苯基肉桂酸乙酯、α-氰基-β-苯基肉桂酸2-乙基己酯、單-2-乙基己醯基-二對甲氧基肉桂酸甘油酯等肉桂酸系紫外線遮蔽劑;2,4-二羥基二苯甲酮、2,2'-二羥基-4-甲氧基二苯甲酮、2,2'-二羥基-4,4'-二甲氧基
二苯甲酮、2,2',4,4'-四羥基二苯甲酮、2-羥基-4-甲氧基二苯甲酮、2-羥基-4-甲氧基-4'-甲基二苯甲酮、2-羥基-4-甲氧基二苯甲酮-5-磺酸鹽、4-苯基二苯甲酮、2-乙基己基-4'-苯基-二苯甲酮-2-羧酸酯、2-羥基-4-正辛氧基二苯甲酮、4-羥基-3-羧基二苯甲酮等二苯甲酮系紫外線遮蔽劑;3-(4'-甲基亞苄基)-d,l-樟腦、3-亞苄基-d,l-樟腦、4-咪唑丙烯酸、4-咪唑丙烯酸乙酯、2-苯基-5-甲基苯并唑、2,2'-羥基-5-甲基苯基苯并三唑、2-(2'-羥基-5'-第三辛基苯基)苯并三唑、2-(2'-羥基-5'-甲基苯基)苯并三唑、二雙亞苄肼(dibenzalazine)、聯大茴香甲醯基甲烷(dianisoyl methane)、4-甲氧基-4'-第三丁基二苯甲醯甲烷、5-(3,3-二甲基-2-亞降莰基(norbornylidene))-3-戊烷-2-酮等。
作為其他藥劑成分,並無特別限定,例如可列舉:維生素A油、視黃醇、棕櫚酸視黃醇、肌醇、鹽酸吡哆醇、菸鹼酸苄酯、菸鹼醯胺、菸鹼酸DL-α-生育酚酯、抗壞血酸磷酸鎂、2-O-α-D-吡喃葡萄糖-L-抗壞血酸、維生素D2(麥角鈣化固醇鈣化醇)、dl-α-生育酚、乙酸-dl-α-生育酚酯、泛酸、生物素等維生素類;雌二醇、乙炔基雌二醇等激素;精胺酸、天冬醯胺酸、胱胺酸、半胱胺酸、甲硫胺酸、絲胺酸、白胺酸、色胺酸等胺基酸;尿囊素(allantoin)、薁等抗炎劑、熊果苷等美白劑;鞣酸等收斂劑;L-薄荷腦、樟腦等清涼劑;或硫、鹽酸溶菌酶、鹽酸吡哆醇等。
作為各種萃取液,並無特別限定,例如可列舉:蕺菜萃取物、黃柏萃取物、黃香草木樨萃取物、野芝麻(Lamium album var.barbatum)萃取物、甘草萃取物、芍藥萃取物、肥皂草(saponaria officinalis)萃取物、絲瓜萃取物、金雞納樹萃取物、虎耳草萃取物、苦參萃取物、日本萍蓬草萃取物、茴香萃取物、報春花(oxlip)萃取物、薔薇萃取物、地黃萃取物、檸檬萃
取物、紫根(lithospermum root)萃取物、蘆薈萃取物、甜旗草(sweet flag)萃取物、桉樹萃取物、木賊(field horsetail)萃取物、鼠尾草萃取物、麝香草萃取物、茶葉萃取物、海藻萃取物、黃瓜萃取物、丁香(cloves)萃取物、樹莓萃取物、柏蜂草(melissa)萃取物、胡蘿蔔萃取物、馬栗(horse chestnut)萃取物、桃萃取物、桃葉萃取物、桑樹萃取物、矢車菊(knapweed)萃取物、金縷梅萃取物、胎盤萃取物、胸腺萃取物、蠶絲萃取液等。
作為上述各種粉體,可列舉:鐵丹、黃氧化鐵、黑氧化鐵、雲母鈦、被覆氧化鐵之雲母鈦、被覆氧化鈦之玻璃薄片等光亮性著色顏料,雲母、滑石、高嶺土、絹雲母、二氧化鈦、二氧化矽等無機粉末或聚乙烯粉末,尼龍粉末、交聯聚苯乙烯、纖維素粉末、聚矽氧粉末等有機粉末等。較佳為了提高官能特性、提高化妝持續性,而藉由聚矽氧類、氟化合物、金屬皂、油劑、醯基麩胺酸鹽等物質利用公知之方法對粉末成分之一部分或全部進行疏水化處理而使用。又,亦可將不屬於本發明之其他複合粉體者混合而使用。
(於油墨領域中之使用)
於使用本發明之氧化鋅粉末作為向油墨中之添加成分之情形時,可列舉:氧化鈦、鐵丹、銻紅、鎘黃、鈷藍、鐵藍、群青、碳黑、石墨等有色顏料,及碳酸鈣、高嶺土、黏土、硫酸鋇、氫氧化鋁、滑石等體質顏料。進而,作為有機顏料,可併用可溶性偶氮顏料、不溶性偶氮顏料、偶氮色澱(azo lake)顏料、縮合偶氮顏料、銅酞青顏料、縮合多環顏料等顏料成分;蟲膠樹脂、丙烯酸系樹脂、苯乙烯-丙烯酸系樹脂、苯乙烯-順丁烯二酸樹脂、苯乙烯-丙烯酸-順丁烯二酸樹脂、聚胺甲酸酯樹脂、聚酯樹脂、聚醯胺樹脂
等黏合劑樹脂;水混合性有機溶劑等而使用。
(於塗料領域中之使用)
於使用本發明之氧化鋅粉末作為向塗料組成物中之添加成分之情形時,可併用丙烯酸系樹脂、聚酯樹脂、環氧樹脂等塗膜形成樹脂;著色顏料、體質顏料、光亮性顏料等各種顏料;硬化觸媒、表面調整劑、消泡劑、顏料分散劑、塑化劑、造膜助劑、紫外線吸收劑、抗氧化劑等而使用。又,塗料中之樹脂可為具有硬化性者,亦可為不具有硬化性者。
[實施例]
以下,基於實施例更詳細地說明本發明。再者,本發明並不限定於以下之實施例。
(實施例1)
將一次粒徑1.05μm之六角板狀氧化鋅(XZ-1000F,堺化學工業公司製造)150g添加至水723.21g中,並充分地攪拌,藉此獲得ZnO濃度200g/l之水性漿料。繼而,一面攪拌漿料,一面升溫至40℃後,一面維持該溫度,一面添加5重量%之NaOH水溶液,藉此將漿料之pH調整為10。一面保持漿料之溫度40℃、pH10之條件,一面歷時180分鐘對上述漿料同時添加TiO2換算濃度為45.5g/l之硫酸鈦水溶液330ml(相對於母體ZnO以TiO2換算計相當於10重量份之量),及用於中和該硫酸鈦水溶液的5重量%之NaOH水溶液。中和結束後,進行熟成30分鐘,然後進行過濾、水洗,並於120℃乾燥12小時,藉此獲得成為母體之一次粒徑1.05μm的六角板狀氧化鋅粒子表面經氫氧化鈦被覆而成之被覆氫氧化鈦的氧化鋅粒子。繼而,利用電爐於700℃將所獲得之被覆氫氧化鈦的氧化鋅粒子燒成2小時,
藉此獲得一次粒徑1.07μm的被覆Zn2TiO4之六角板狀氧化鋅粒子。利用穿透式電子顯微鏡JEM-2100(日本電子公司製造)觀察所獲得之粒子的尺寸、形態。將所獲得之電子顯微鏡照片示於圖1。又,藉由X射線繞射裝置Ultima III(理學公司製造)對所獲得之粒子進行分析。將所獲得之X射線繞射光譜示於圖2。又,將所獲得之粒子之物性及塗膜之物性示於表1。確認到(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率1(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率1(%))的比值成為1.6,(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率2(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率2(%))的比值成為1.2,所獲得之氧化鋅粒子相對於母體之原料氧化鋅粒子而言,對UV-B波、UV-A波之紫外線遮蔽性均提高。
(實施例2)
將一次粒徑1.05μm之六角板狀氧化鋅(XZ-1000F,堺化學工業公司製造)150g添加至水723.21g中,並充分地攪拌,藉此獲得ZnO濃度200g/l之水性漿料。繼而,一面攪拌漿料,一面升溫至30℃後,一面維持該溫度,一面添加5重量%之NaOH水溶液,藉此將漿料之pH調整為10。一面保持漿料之溫度30℃、pH10之條件,一面歷時180分鐘對上述漿料同時添加Fe2O3換算濃度為38.8g/l之硫酸鐵(七水硫酸亞鐵)水溶液387ml(相對於母體ZnO以Fe2O3換算計相當於10重量份之量),及用於中和該硫酸鐵水溶液的5重量%之NaOH水溶液。中和結束後,進行熟成30分鐘,然後進行過濾、水洗,並於120℃乾燥12小時,藉此獲得成為母體之一次粒徑1.05μm的六角板狀氧化鋅粒子表面經氫氧化鐵被覆而成的被覆氫氧化鐵
之氧化鋅粒子。繼而,利用電爐於600℃將所獲得之被覆氫氧化鐵之氧化鋅粒子燒成2小時,藉此獲得一次粒徑1.06μm的被覆ZnFe2O4之六角板狀氧化鋅粒子。利用穿透式電子顯微鏡JEM-2100(日本電子公司製造)觀察所獲得之粒子之尺寸、形態。將所獲得之電子顯微鏡照片示於圖3。又,藉由X射線繞射裝置Ultima III(理學公司製造)對所獲得之粒子進行分析。將所獲得之X射線繞射光譜示於圖4。又,將所獲得的粒子之物性及塗膜之物性示於表1。確認到(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率1(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率1(%))的比值成為1.7,(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率2(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率2(%))的比值成為1.3,所獲得之氧化鋅粒子相對於母體之原料氧化鋅粒子而言,對UV-B波、UV-A波之紫外線遮蔽性均提高。
(實施例3)
將一次粒徑1.05μm之六角板狀氧化鋅(XZ-1000F,堺化學工業公司製造)150g添加至水723.21g中,並充分地攪拌,藉此獲得ZnO濃度200g/l之水性漿料。繼而,一面攪拌漿料,一面升溫至40℃後,一面維持該溫度,一面添加5重量%之NaOH水溶液,藉此將漿料之pH調整為10。一面保持漿料之溫度40℃、pH10之條件,一面歷時180分鐘對上述漿料同時添加TiO2換算濃度為45.5g/l之硫酸鈦水溶液165ml(相對於母體ZnO以TiO2換算計相當於5重量份之量)、Fe2O3換算濃度為38.8g/l之硫酸鐵(七水硫酸亞鐵)水溶液194ml(相對於母體ZnO以Fe2O3換算計相當於5重量份之量),及用於中和該硫酸鈦水溶液及該硫酸鐵水溶液的5重量%之NaOH水
溶液。
中和結束後,進行熟成30分鐘,然後進行過濾、水洗,並於120℃乾燥12小時,藉此獲得成為母體之一次粒徑1.05μm之六角板狀氧化鋅粒子表面經氫氧化鈦及氫氧化鐵被覆而成的被覆氫氧化鈦及氫氧化鐵之氧化鋅粒子。繼而,利用電爐於700℃將所獲得之被覆氫氧化鈦及氫氧化鐵之氧化鋅粒子燒成2小時,藉此獲得一次粒徑1.07μm之被覆Zn2TiO4+ZnFe2O4之六角板狀氧化鋅粒子。利用穿透式電子顯微鏡JEM-2100(日本電子公司製造)觀察所獲得之粒子之尺寸、形態。將所獲得之電子顯微鏡照片示於圖5。又,藉由X射線繞射裝置Ultima III(理學公司製造)對所獲得之粒子進行分析。將所獲得之X射線繞射光譜示於圖6。又,將所獲得之粒子之物性及塗膜的物性示於表1。確認到(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率1(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率1(%))的比值成為1.6,(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率2(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率2(%))的比值成為1.2,所獲得之氧化鋅粒子相對於母體之原料氧化鋅粒子而言,對UV-B波、UV-A波之紫外線遮蔽性均提高。
(實施例4)
將乙酸鋅二水合物(細井化學工業公司製造之乙酸鋅)66.51g溶解於水中,而以使乙酸鋅二水合物之濃度成為0.5mol/l之方式製備乙酸鋅水溶液1200ml。繼而,對乙酸鋅水溶液1200ml,添加乙酸鐵(II)(和光純藥工業公司製造)9.68g,使之完全溶解。繼而,藉由對上述水溶液將一次粒徑
0.02μm之氧化鋅(FINEX-50,堺化學工業公司製造)40g再漿化(repulp),而製成漿料。繼而,一面攪拌該漿料,一面歷時65分鐘升溫至95℃,並一面攪拌一面於95℃熟成1小時。熟成後,進行過濾、水洗。繼而,將所獲得之固形物於3公升水中再漿化而製成漿料,一面攪拌一面升溫至95℃,並一面攪拌一面於95℃加熱洗淨30分鐘。加熱洗淨後,進行過濾、水洗,於110℃乾燥12小時,藉此獲得含有氫氧化鐵的含氫氧化鐵之六角板狀氧化鋅粒子。繼而,利用電爐於600℃將所獲得之含氫氧化鐵之氧化鋅粒子燒成2小時,藉此獲得一次粒徑0.07μm之含ZnFe2O4之氧化鋅粒子。利用穿透式電子顯微鏡JEM-2100(日本電子公司製造)觀察所獲得之粒子的尺寸、形態。將所獲得之電子顯微鏡照片示於圖7。又,藉由X射線繞射裝置Ultima III(理學公司製造)對所獲得之粒子進行分析。將所獲得之X射線繞射光譜示於圖8。又,將所獲得之粒子之物性及塗膜的物性示於表1。
(比較例1)
將一次粒徑1.05μm之六角板狀氧化鋅(XZ-1000F,堺化學工業公司製造)製成比較對象之紫外線遮蔽劑。將粒子之穿透式電子顯微鏡照片示於圖9。又,將粒子之物性及塗膜之物性示於表1。再者,該粒子亦為實施例1、2及3中獲得之成為被覆氧化鋅粒子的母體之原料氧化鋅粒子。
(比較例2)
利用電爐於550℃將一次粒徑0.02μm之氧化鋅(FINEX-50,堺化學工業公司製造)50g燒成2小時,藉此製備一次粒徑0.11μm的不定形之氧化鋅粒子,而製成比較對象之紫外線遮蔽劑。將粒子之穿透式電子顯微鏡照片示於圖10。又,將所獲得之粒子的物性及塗膜之物性示於表1。再者,
該粒子亦為比較例3及4中獲得之成為被覆氧化鋅粒子的母體之原料氧化鋅粒子。
(比較例3)
將比較例2中獲得之氧化鋅粒子即一次粒徑0.11μm的不定形之氧化鋅粒子30g添加至水144.64g中,充分地攪拌,藉此獲得ZnO濃度200g/l之水性漿料。繼而,一面攪拌漿料,一面升溫至40℃後,一面維持該溫度,一面添加5重量%之NaOH水溶液,藉此將漿料之pH調整為10。一面保持漿料之溫度40℃、pH10之條件,一面歷時180分鐘對上述漿料同時添加TiO2換算濃度為45.5g/l之硫酸鈦水溶液132ml(相對於母體ZnO以TiO2換算計相當於20重量份之量),及用於中和該硫酸鈦水溶液的5重量%之NaOH水溶液。中和結束後,進行熟成30分鐘,然後進行過濾、水洗,並於120℃乾燥12小時,藉此獲得成為母體之一次粒徑0.11μm的不定形氧化鋅粒子表面經氫氧化鈦被覆而成的被覆氫氧化鈦之氧化鋅粒子。繼而,利用電爐於700℃將所獲得之被覆氫氧化鈦之氧化鋅粒子燒成2小時,藉此獲得一次粒徑為0.12μm的被覆Zn2TiO4之氧化鋅粒子。利用穿透式電子顯微鏡JEM-2100(日本電子公司製造)觀察所獲得之粒子的尺寸、形態。將所獲得之電子顯微鏡照片示於圖11。又,藉由X射線繞射裝置Ultima III(理學公司製造)對所獲得之粒子進行分析。將所獲得之X射線繞射光譜示於圖12。又,將所獲得的粒子之物性及塗膜之物性示於表1。確認到(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率1(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率1(%))的比值成為1.0,(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率2(%))/(含有成為被覆
氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率2(%))的比值成為0.9,所獲得之氧化鋅粒子相對於母體之原料氧化鋅粒子而言,對UV-B波、UV-A波之紫外線遮蔽性均未提高。
(比較例4)
將比較例2之氧化鋅粒子即一次粒徑0.11μm的不定形之氧化鋅粒子30g添加至水144.64g中,充分地攪拌,藉此獲得ZnO濃度200g/l之水性漿料。繼而,一面攪拌漿料,一面升溫至30℃後,一面維持該溫度,一面添加5重量%之NaOH水溶液,藉此將漿料之pH調整為10。
一面保持漿料之溫度30℃、pH10之條件,一面歷時180分鐘對上述漿料同時添加Fe2O3換算濃度為38.8g/l之硫酸鐵(七水硫酸亞鐵)水溶液154ml(相對於母體ZnO以Fe2O3換算計相當於20重量份之量),及用於中和該硫酸鐵水溶液的5重量%之NaOH水溶液。中和結束後,進行熟成30分鐘,然後進行過濾、水洗,並於120℃乾燥12小時,藉此獲得成為母體之一次粒徑0.11μm的不定形氧化鋅粒子表面經氫氧化鐵被覆而成的被覆氫氧化鐵之氧化鋅粒子。繼而,利用電爐於600℃將所獲得的被覆氫氧化鐵之氧化鋅粒子燒成2小時,藉此獲得一次粒徑0.11μm的被覆ZnFe2O4之氧化鋅粒子。利用穿透式電子顯微鏡JEM-2100(日本電子公司製造)觀察所獲得之粒子的尺寸、形態。將所獲得之電子顯微鏡照片示於圖13。又,藉由X射線繞射裝置Ultima III(理學公司製造)對所獲得之粒子進行分析。將所獲得之X射線繞射光譜示於圖14。又,將所獲得之粒子的物性及塗膜之物性示於表1。確認到(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率1(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽
率1(%))的比值成為1.0,(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率2(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率2(%))的比值成為1.0,所獲得之氧化鋅粒子相對於母體之原料氧化鋅粒子而言,對UV-B波、UV-A波之紫外線遮蔽性均未提高。
(評價方法)
(所獲得之粒子之組成)
圖2、4、6、8、12、14中所示之X射線繞射光譜及表1中所獲得之粒子的組成係表示藉由具有銅管球之X射線繞射裝置Ultima III(理學公司製造)進行分析而得之結果者。
(紫外線遮蔽率之測量方法)
(塗膜之製作)
將實施例或比較例之粒子2g、清漆10g(ACRYDIC A-801-P,DIC公司製造)、乙酸丁酯5g(特級試劑,和光純藥工業公司製造)、二甲苯5g(特級純正,純正化學公司製造)、及玻璃珠38g(1.5mm,Potters-Ballotini公司製造)放入至容積75ml之蛋黃醬瓶中,充分攪拌,其後固定於塗料調節器5410型(RED DEVIL公司製造)上,施加振動90分鐘而進行分散處理,藉此製作塗料。繼而,將所製作之塗料少量滴加至載玻片(長度、寬度、厚度=76mm、26mm、0.8~1.0mm,松浪硝子工業公司製造)上,利用棒式塗佈機(No.579棒No.6,安田精機製作所公司製造)製作塗膜。將所製作之塗膜於20℃乾燥12小時,其後用於測量。
使用實施例1的被覆Zn2TiO4之氧化鋅粒子、實施例2的被覆ZnFe2O4之氧化鋅粒子及比較例1的氧化鋅粒子,藉由上述摻合分別製作塗膜,將利用分光光度計V-570(日本分光公司製造)對各塗膜所測得的光之波長300~400nm之紫外線波長區域中的總光線透射率曲線加以比較,令其結果示於圖15。再者,總光線透射率雖亦根據粒徑而不同,但由表1可知,實施例1之粒子、實施例2之粒子及比較例1之粒子的一次粒徑大致
相等。
根據圖15之結果明瞭本發明之氧化鋅粒子相較於習知之六角板狀氧化鋅粒子具有更優異的紫外線遮蔽性能。
又,根據表1之(含有被覆氧化鋅粒子的塗膜之紫外線遮蔽率(%))/(含有成為被覆氧化鋅粒子之母體之原料氧化鋅粒子的塗膜之紫外線遮蔽率(%))的比,明瞭關於使用六角板狀氧化鋅粒子作為原料氧化鋅粒子之實施例1、2及3的被覆氧化鋅粒子,相較於原料氧化鋅粒子,紫外線遮蔽性成為更優異者。
又,關於上述比,於比較例3及4中,明瞭紫外線遮蔽率1及2均為1.0以下,紫外線遮蔽率未必藉由Zn2TiO4或ZnFe2O4之被覆而提高。並且,實施例1、2及3之被覆氧化鋅粒子得上述比為1.2以上,尤其於紫外線遮蔽率1方面為1.6以上,因此亦明瞭藉由本發明之被覆而實現紫外線遮蔽能之大幅提高。
進而,雖然粒徑越小紫外線遮蔽率越增高,但由於滑動性變差,故作為化妝品材料尤其欠佳。比較例1之氧化鋅粒子因形狀與粒徑而滑動性良好,但如表1所示,紫外線遮蔽率低,比較例3及4之被覆氧化鋅粒子由於粒徑小,故雖然紫外線遮蔽率增高,但無法獲得較佳之滑動性。
實施例1、2及3之被覆氧化鋅粒子為六角板狀形狀,且為1μm左右之粒徑,故具有高滑動性,於紫外線遮蔽率方面亦高於粒徑、形狀相同之比較例1。即,明瞭實施例1、2及3之被覆氧化鋅粒子兼具高紫外線遮蔽率與較佳之滑動性。如上所述,本發明之氧化鋅粒子係同時兼具高滑動性、柔焦效果、及高紫外線遮蔽率的優異氧化鋅粒子。
[產業上之可利用性]
本發明之氧化鋅粒子可摻合於化妝料、油墨、塗料等中。
Claims (9)
- 一種氧化鋅粒子,其於至少一部分含有由Ti元素及/或Fe元素以及Zn元素構成之固溶體,該氧化鋅粒子之形狀為六角板狀。
- 如申請專利範圍第1項之氧化鋅粒子,其中,由Ti元素及/或Fe元素以及Zn元素構成之固溶體係被覆成為基材之氧化鋅粒子的表面之被膜。
- 如申請專利範圍第1或2項之氧化鋅粒子,其係含有Zn2TiO4或ZnFe2O4之氧化鋅粒子,該氧化鋅粒子之一次粒徑為0.01μm以上。
- 如申請專利範圍第1、2或3項之氧化鋅粒子,其中,Ti元素及/或Fe元素之含量相對於氧化鋅粒子100重量%,以TiO2換算及/或Fe2O3換算為5重量%以上30重量%以下。
- 一種申請專利範圍第1、2、3或4項之氧化鋅粒子之製造方法,具有如下步驟:步驟(1-1):於六角板狀之原料氧化鋅粒子之水性漿料,一面於溫度10℃以上90℃以下之範圍保持pH9±3,一面添加鈦鹽及/或鐵鹽之水溶液與鹼性水溶液;及步驟(1-2):對藉由該步驟(1-1)而獲得之被覆氧化鋅粒子進行燒成。
- 一種申請專利範圍第1、2、3或4項之氧化鋅粒子之製造方法,具有如下步驟:步驟(2-1):將原料氧化鋅粒子添加至溶解有鈦鹽及/或鐵鹽之鋅鹽水溶液中,進行加熱熟成;及 步驟(2-2):對藉由該步驟(2-1)而獲得之含氫氧化鈦及/或氫氧化鐵之氧化鋅粒子進行燒成。
- 如申請專利範圍第1、2、3或4項之氧化鋅粒子,係藉由申請專利範圍第5或6項之製造方法而獲得。
- 一種紫外線遮蔽劑,含有申請專利範圍第1、2、3、4或7項之氧化鋅粒子。
- 一種化妝料,含有申請專利範圍第1、2、3、4、7或8項之氧化鋅粒子。
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