TWI542548B - 細微水滑石粒子 - Google Patents
細微水滑石粒子 Download PDFInfo
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Description
本發明係關於一種細微水滑石粒子及其製造方法。
水滑石粒子自先前以來即為人所知,具有優異之酸反應性及陰離子交換性。業界靈活應用該等性質,而將其用於醫藥用製酸劑、吸附劑、聚烯烴系樹脂之觸媒殘餘物之中和劑、氯系樹脂之安定劑等各種領域中。
近年來,奈米粒子提供新用途之例增加,關於水滑石粒子,亦需要奈米等級之微粒子之開發。奈米等級微粒子為非沉澱性且透明性亦變良好,而可用於化妝品、醫藥、塗料等中。
本發明之目的在於提供一種二次粒徑極小之奈米等級之水滑石粒子及其製造方法。又,本發明之目的在於提供一種含有水滑石粒子之樹脂組成物。又,本發明之目的在於提供一種含有水滑石粒子之非沉澱性且透明性優異之分散液。該分散液可用於化妝品、醫藥、塗料等中。
本發明者對製造二次粒徑極小之水滑石粒子之方法進行銳意研究。其結果,發現利用使用直徑300 μm以下之微小珠粒之濕式粉碎機(珠磨機),可獲得平均二次粒徑極小之水滑石粒子,從而完成本發明。
即,本發明係一種水滑石粒子,其藉由動態光散射法測定之平均二次粒徑為5~100 nm。
又,本發明係一種樹脂組成物,其含有100重量份之樹脂、及0.001~300重量份之藉由動態光散射法測定之平均二次粒徑為5~100 nm之水滑石粒子。
又,本發明係一種分散液,其含有100重量份之水、及0.1~100重量份之平均二次粒徑為5~100 nm之水滑石粒子。
又,本發明係一種水滑石粒子之製造方法,該水滑石粒子之藉由動態光散射法測定之平均二次粒徑為5~100 nm,該製造方法之特徵在於:使用珠粒徑為15~300 μm之珠粒對平均二次粒徑為0.1~10 μm之水滑石粒子之漿體進行濕式粉碎。
圖1係本發明(實施例1)之SEM照片。
圖2係實施例2與比較例2之穿透率。
圖3係實施例2與比較例2於可見光區域中之穿透率。
本發明之水滑石粒子之藉由動態光散射法測定之平均二次粒徑為5~100 nm,較佳為5~50 nm,更佳為5~20 nm。
本發明之水滑石粒子之組成並無特別限定,例如較佳為下述式(1)所表示之組成之粒子。
[(M1 2+)y1(M2 2+)y2]1-xMx 3+(OH)2An- x/n.mH2O……(1)
式中,M1 2+表示選自Mg、Zn、Ca、Sr、Cu、Fe、Mn、Co、Ni、Sn、Pb、Cd及Ba等2價金屬中之至少一種以上之2價金屬。
M3+表示Al、Fe等3價金屬之至少一種以上。
An-表示n價陰離子。作為陰離子,例如可列舉:氯離子、碳酸根離子、有機酸根離子等。
x、y1、y2及m分別表示下述式所表示之正數。
0<x≦0.5、0.5≦y1+y2<1、0≦m<2,於上述式(1)中,較佳為M1 2+為Mg及/或Zn,M3+為Al。
本發明之水滑石粒子由於二次粒徑較小,因此可用作非沉澱性且透明性較高之懸浮液型或溶膠型醫藥用製酸劑、塗料、化妝品、吸附劑、聚烯烴系樹脂之觸媒殘餘物之中和劑、氯系樹脂之安定劑。
本發明中使用之水滑石粒子可將其本身調配於合成樹脂中,亦可利用表面處理劑對粒子進行處理而使用。
作為表面處理劑,較佳為選自由高級脂肪酸、高級醇之硫酸酯、鈦酸酯偶合劑、矽烷偶合劑、鋁酸鹽偶合劑、多元醇與脂肪酸之酯、磷酸酯及陰離子系界面活性劑所組成之群中之至少一種。
作為高級脂肪酸,可列舉:硬脂酸、芥子酸、棕櫚酸、月桂酸、山萮酸等碳數10以上之高級脂肪酸。又,可列舉該等高級脂肪酸之鹼金屬鹽。
作為高級醇之硫酸酯,可列舉:硬脂醇硫酸酯、油醇硫酸酯等。
作為鈦酸酯系偶合劑,可列舉:三異硬脂醯基鈦酸異丙酯、三(二辛基焦磷醯氧基)鈦酸異丙酯、三(N-胺基乙基-胺基乙基)鈦酸異丙酯、十三烷基苯磺醯基鈦酸異丙酯等。
作為矽烷偶合劑,可列舉:乙烯基乙氧基矽烷、乙烯基-三(2-甲氧基-乙氧基)矽烷、γ-甲基丙烯醯氧基丙基三甲氧基矽烷、γ-胺基丙基三甲氧基矽烷、β-(3,4-環氧環己基)乙基三甲氧基矽烷、γ-縮水甘油氧基丙基三甲氧基矽烷、γ-巰基丙基三甲氧基矽烷等。
作為鋁酸鹽偶合劑,可列舉乙醯烷氧基二異丙酸鋁等。
作為多元醇與脂肪酸之酯,可列舉:甘油單硬脂酸酯、甘油單油酸酯等。
作為磷酸酯,可列舉:正磷酸與油醇之單酯、二酯或該等之混合物,正磷酸與硬脂醇之單酯、二酯或該等之混合物。又,可列舉該等酯之酸型或鹼金屬鹽或胺鹽等。
作為陰離子系界面活性劑,可列舉:聚乙二醇醚之硫酸酯鹽、醯胺鍵硫酸酯鹽、酯鍵硫酸酯鹽、酯鍵磺酸鹽、醯胺鍵磺酸鹽、醚鍵磺酸鹽、醚鍵烷基芳基磺酸鹽、酯鍵烷基芳基磺酸鹽、醯胺鍵烷基芳基磺酸鹽等。
於使用上述表面處理劑進行細微水滑石粒子之表面塗佈處理時,可藉由其本身公知之濕式或乾式法實施。例如,作為濕式法,只要於細微水滑石粒子之漿體中以液狀或乳膠狀添加該表面處理劑,並以達約100℃之溫度機械地充分混合即可。作為乾式法,只要對細微水滑石粒子利用亨舍爾混合機等混合機於充分攪拌下以液狀、乳
膠狀、固形狀添加表面處理劑,並於加熱或未加熱下充分地進行混合即可。
表面處理劑之添加量可適當地選擇,較佳為基於該水滑石粒子之重量,設為10重量%以下。
經表面處理之水滑石粒子視需要例如可適當地選擇水洗、脫水、造粒、乾燥、粉碎、分級等手段並實施而製成最終製品形態。
本發明之樹脂組成物含有100重量份之樹脂及0.001~100重量份、較佳為0.01~20重量份、更佳為0.1~10重量份之水滑石粒子。
樹脂較佳為熱塑性樹脂。作為其例,可例示:聚乙烯、聚丙烯、乙烯-丙烯共聚合體、聚丁烯、聚(4-甲基-戊烯-1)等之類之C2~C8烯烴(α-烯烴)之聚合體或者共聚合體、該等C2~C8烯烴與二烯之共聚合體類、乙烯-丙烯酸酯共聚合體、聚苯乙烯、ABS(acrylonitrile-butadiene-styrene,丙烯腈-丁二烯-苯乙烯)樹脂、AAS(acrylonitrile-acrylic ester-styrene,丙烯腈-丙烯酸酯-苯乙烯)樹脂、AS(acrylonitrile-styrene,丙烯腈-苯乙烯)樹脂、MBS(methyl methacrylate-butadiene-styrene,甲基丙烯酸甲酯-丁二烯-苯乙烯)樹脂、乙烯-氯乙烯共聚合樹脂、乙烯乙酸乙烯酯共聚合體樹脂、乙烯-氯乙烯-乙酸乙烯酯接枝聚合樹脂、偏二氯乙烯、聚氯乙烯、氯化聚乙烯、氯化聚丙烯、氯乙烯丙烯共聚合體、乙酸乙烯酯樹脂、苯氧基樹脂、聚縮醛、聚醯胺、聚醯亞胺、聚碳酸酯、聚碸、聚苯醚、聚苯硫醚、聚
對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、甲基丙烯酸系樹脂等熱塑性樹脂。
作為聚烯烴,為聚丙烯均聚物、乙烯丙烯共聚合體之類之聚丙烯系樹脂,高密度聚乙烯、低密度聚乙烯、直鏈狀低密度聚乙烯、超低密度聚乙烯、EVA(ethylene vinyl acetate,乙烯乙酸乙烯酯樹脂)、EEA(ethylene ethyl acrylate,乙烯丙烯酸乙酯樹脂)、EMA((ethylene methyl acrylate,乙烯丙烯酸甲酯共聚合樹脂)、EAA(ethylene acrylic acid,乙烯丙烯酸共聚合樹脂)、超高分子量聚乙烯之類之聚乙烯系樹脂,及聚丁烯、聚(4-甲基-戊烯-1)等C2~C6之烯烴(α-乙烯)之聚合體或者共聚合體。該等之中,聚乙烯、聚丙烯、聚丁烯、聚(4-甲基-戊烯-1)或該等之共聚合體尤其適於本發明之組成物。該等聚烯烴含有源自聚合觸媒之鹵素,本發明之組成物對由該鹵素引起之熱劣化極有效。
進而,可列舉:環氧樹脂、酚樹脂、三聚氰胺樹脂、不飽和聚酯樹脂、醇酸樹脂、脲樹脂等熱硬化性樹脂。
又,可例示:EPDM(ethylene-propylene-diene monomer,乙烯-丙烯-二烯單體)、丁基橡膠、異戊二烯橡膠、SBR(styrene-butadiene rubber,苯乙烯-丁二烯橡膠)、NBR(nitrile butadiene rubber,丁腈橡膠)、氯磺化聚乙烯、氟橡膠、溴化丁基橡膠、表氯醇橡膠等含鹵素橡膠等合成橡膠。
樹脂較佳為聚烯烴、聚氯乙烯、聚乙烯醇(PVA,polyvinyl alcohol)、或橡膠。
將細微水滑石粒子調配於樹脂中以製備樹脂組成物之手段並無特別限制,例如只要藉由與將安定劑或填充劑等調配於該等樹脂中之公知慣用之調配手段相同之手段,與其他樹脂調配材料一
同、或者另外儘量均勻地調配於合成樹脂中即可。例如可例示:利用帶型攪拌機、高速攪拌機、捏合機、製粒機、擠壓機等公知混合手段而進行調配之手段;或將以細微水滑石粒子作為有效成分而成之熱劣化劑之懸浮液添加至聚合後之漿體中加以攪拌而混合,並加以乾燥之手段等。
本發明之樹脂組成物除上述成分以外亦可調配慣用之其他添加劑。作為此種添加劑,例如可例示:抗氧化劑、紫外線抑制劑、防靜電劑、顏料、發泡劑、塑化劑、填充劑、增強劑、有機鹵素難燃劑、交聯劑、光安定劑、紫外線吸收劑、滑劑、其他無機系及有機系熱安定劑、水等。
本發明包含使上述樹脂組成物成形而獲得之成形品。
本發明之分散液含有100重量份之水、及0.01~100重量份之藉由動態光散射法測定之平均二次粒徑為5~100 nm之水滑石粒子。水滑石粒子之含量相對於水100重量份,較佳為0.1~50重量份,更佳為1~20重量份。本發明之分散液為非沉澱性且透明性優異,可用於醫藥(製酸劑、鐵劑等)、化妝品(光散射劑、UV(Ultra Violet,紫外線)吸收劑等)、塗料(防銹)等中。
本發明之分散液較佳為含有分散劑。作為分散劑,可列舉六偏磷酸鈉。分散劑之含量相對於水滑石粒子100重量份,較佳為3~30重量份,更佳為5~20重量份,進而較佳為5~10重量份。若於
分散液中含有分散劑,則可抑制水滑石粒子之凝集,且長期將平均二次粒徑維持為較小。
本發明之水滑石粒子可使用平均直徑為15~300 μm之珠粒對平均二次粒徑為0.2~10 μm之水滑石粒子之原料漿體進行濕式粉碎而製造。
原料漿體含有水滑石及介質。作為介質,可列舉水或有機溶劑。作為有機溶劑,具體而言,可列舉:甲苯或二甲苯等芳香族烴類,己烷、環己烷、庚烷等脂肪族烴類,乙酸乙酯、乙酸正丁酯等酯類,乙二醇、丁基賽路蘇、異丙醇、正丁醇、乙醇、甲醇等醇類,丙酮、甲基乙基酮、甲基異丁基酮、環己酮等酮類,四氫呋喃、二烷等醚類,二甲基乙醯胺、二甲基甲醯胺等醯胺類,氯仿、二氯甲烷、四氯化碳等鹵素化合物類,二甲基亞碸,硝基苯等或該等之兩種以上之混合物。視需要亦可進而使用多元醇等粉碎助劑(分散劑)等。
原料漿體中之水滑石之平均二次粒子為0.1~10 μm,較佳為0.2~5 μm。平均二次粒子係藉由雷射繞射散射法進行測定。漿體中之水滑石粒子之含量相對於介質100重量份,較佳為0.1~50重量份,更佳為1~20重量份。
濕式珠磨機粉碎所使用之珠粒之平均直徑為15~300 μm,較佳為15~100 μm,更佳為30~50 μm。作為珠粒之材質,可列舉:玻璃、氧化鋁、氧化鋯、鋯石、鋼、氧化鈦。
作為濕式珠磨機粉碎所使用之裝置,可使用藉由旋轉驅動轉子將珠粒與漿體攪拌混合而粉碎漿體中所含之水滑石粒子之濕式
攪拌球磨機。濕式攪拌球磨機具有固定於外殼內之軸上,攪拌填充至外殼內之珠粒與漿體之轉子。又,較佳為具有固定於外殼內之軸上並與軸一同旋轉,藉由離心力之作用自比重較大之珠粒分離比重較小之漿體之分離器。珠粒通常填充外殼內之有效容積之60~80%(鬆容積)而進行運轉。轉子之轉速較佳為以4000~5000 rpm之旋轉進行運轉。
作為濕式攪拌球磨機,較佳為壽工業股份有限公司製造之Ultra Apex Mill UAM-015 1170。Ultra Apex Mill可利用Ultra Centri-Separator,使用0.05 mm或其以下之微小珠粒,且可進行奈米範圍之粉碎。又,藉由利用轉子銷方式之珠粒攪拌,可對水滑石粒子設定最佳之分散力,可防止由奈米範圍中之粒子破壞所引起之再凝集而進行高分散、精密分散。
以下,基於實施例,更詳細地說明本發明。PHR(parts per hundreds of resin)係以相對於樹脂100重量份之各添加物之重量份所表示之值。
實施例中,(a)平均二次粒徑、(b)SEM(Scanning Electron Microscope,掃描式電子顯微鏡)觀察照片、(c)穿透率係藉由下述方法進行。
使用大塚電子製造之ELSZ-2(動態光散射法:動態、電泳光散射法)進行測定。關於測定,係利用超音波對水滑石漿體進行5分鐘處理後進行測定。
使用Hitachi High-Tech公司之S-3000N。試樣係利用超音波對水滑石漿體進行10分鐘處理後,滴加至試樣台上製作並觀測。
使用Hitachi High-Tech公司之分光光度計U-4100。以PET(polyethylene terephthalate,聚對苯二甲酸乙二酯)為基準,將PET之穿透率設為100%而進行測定。
製備1.03 mol/L濃度之氯化鎂與0.239 mol/L濃度之硫酸鋁之混合水溶液{設為A液}、0.753 mol/L濃度之碳酸鈉水溶液{B液}及3.39 N濃度之氫氧化鈉水溶液{C液}。繼而,對A液、B液及C液使用定量泵,將A液:B液以成為4.5:1之體積比之流量注人至反應槽中,利用C液將反應液之pH值保持為9.3~9.6之範圍,反應溫度係於40℃下進行,生成沉澱物。過濾、洗淨後,於離子交換水中進行再次乳化,獲得原料之水滑石漿體。所獲得之水滑石漿體中之水滑石為5.6重量%濃度。所獲得之水滑石粒子係以下述式表示,平均二次粒徑為0.99 μm。
組成:Mg4.3Al2(OH)12.6(CO3).3.5H2O
於所獲得之實施例1之水滑石漿體1.0 kg中添加離子交換水0.4 kg,以水滑石漿體中之水滑石成為4.0重量%濃度之方式加以稀釋。使用UAM-015 1170,添加珠粒徑為50 μm之氧化鋯珠對經稀釋之水滑石漿體進行濕式粉碎而獲得細微水滑石漿體。UAM-015 1170係於轉子轉速4325 rpm下,將漿體流量設為9.6 L/小時進行運轉。
將所獲得之細微水滑石粒子之平均二次粒徑之測定結果示於表1中。又,將細微水滑石之SEM照片示於圖1中。又,將利用超音波對細微水滑石漿體進行分散處理後並放置1天後之平均二次粒徑示於表1中。
於實施例1中獲得之細微水滑石漿體80 g(水滑石粒子之含量為3.2 g)中添加作為分散劑之六偏磷酸鈉0.16 g,獲得添加有分散劑之漿體。水滑石漿體中之水滑石之濃度之計算值為3.99重量%,實測值為3.82重量%。
將所獲得之細微水滑石粒子之平均二次粒徑及利用超音波並放置1天後之平均二次粒徑之測定結果示於表1中。
以成為4.0重量%濃度之方式利用離子交換水使平均二
次粒徑為0.225μm之水滑石(協和化學製造之DHT-4H)再次乳化。於再次乳化漿體80g(水滑石粒子之含量為3.2g)中添加作為分散劑之六偏磷酸鈉0.16g而獲得添加有分散劑之漿體。水滑石漿體中之水滑石之濃度之實測值為3.78重量%。
調配比例如下所述。
使用Kanpe Hapio股份有限公司之水溶性拋光清漆(成分:丙烯酸系樹脂(折射率:1.49)、有機溶劑、水)。於清漆5.44g(以丙烯酸系樹脂計為2.480g)中混合實施例2中獲得之漿體13g(以水滑石粒子計為0.497g),以超音波進行3分鐘分散處理而獲得塗料。
將塗料1ml澆鑄於厚度為125μm之PET板上,自然乾燥一晚而獲得成形品。成形品之厚度為80~120μm。測定所製作之成形品之穿透率。穿透率為98%以上,目測無白濁,無色透明,亦不存在凝集體。本發明之成形品表現出高透明性。
使用比較例1之水滑石粒子,於與實施例3相同之條件
下製造成形品。測定所製造之試樣之穿透率。穿透率為95%以上,但目測產生白濁,且確認到凝集體。
本發明之水滑石粒子之平均二次粒徑為5~100 nm,極細微,於將該粒子調配於樹脂中之情形時,可獲得透明性較高之成形品。又,即便為較少之含量,其效果亦有效。進而由於粒子較小,因此進行成形時之加工性及由提高過濾器通過性所帶來之作業性等優異。又,以較少之添加量作為醫藥用製酸劑、吸附劑、聚烯烴系樹脂之觸媒殘餘物之中和劑、氯系樹脂之安定劑之效果優異。
Claims (6)
- 一種組成物,係含有樹脂、水及藉由動態光散射法測定之平均二次粒徑為5~100nm之水滑石粒子;該組成物中水滑石粒子之含量係:(i)相對於100重量份之水,為0.1~100重量份,且(ii)相對於100重量份之樹脂,為0.001~300重量份。
- 如申請專利範圍第1項之組成物,其中,水滑石粒子之表面係利用選自由高級脂肪酸類、鈦酸酯偶合劑、矽烷偶合劑、鋁酸鹽偶合劑、多元醇與脂肪酸之酯、磷酸酯類、及陰離子系界面活性劑所組成之群中之至少一種表面處理劑進行表面處理。
- 如申請專利範圍第1項之組成物,其中,樹脂為聚烯烴、聚氯乙烯、聚乙烯醇(PVA)或橡膠。
- 一種成形品,其係使申請專利範圍第1項之組成物成形而獲得。
- 如申請專利範圍第4項之成形品,將PET之穿透率設為100%時,其穿透率為98%以上。
- 如申請專利範圍第1項之組成物,其中,水滑石粒子係使用珠粒徑為15~300μm之珠粒將平均二次粒徑為0.1~10μm之水滑石粒子之漿體進行濕式粉碎而製造。
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CN101538019B (zh) * | 2009-04-24 | 2011-04-20 | 山东慧科助剂股份有限公司 | 疏水性纳米水滑石的制备方法 |
JP5396209B2 (ja) * | 2009-09-09 | 2014-01-22 | テイカ株式会社 | 合成ゴム基材の防着剤組成物および防着方法 |
JP5732040B2 (ja) * | 2010-03-09 | 2015-06-10 | 協和化学工業株式会社 | 合成樹脂用充填剤の発泡障害を抑制する剤および方法 |
GB201005931D0 (en) * | 2010-04-09 | 2010-05-26 | Isis Innovation | Immune modulation |
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2013
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- 2013-03-25 WO PCT/JP2013/059789 patent/WO2013147284A1/ja active Application Filing
- 2013-03-25 EP EP13767674.8A patent/EP2832695A4/en not_active Withdrawn
- 2013-03-25 US US14/377,600 patent/US20150010652A1/en not_active Abandoned
- 2013-03-25 CN CN201380012731.1A patent/CN104169219B/zh not_active Expired - Fee Related
- 2013-03-25 JP JP2014508250A patent/JP5911153B2/ja not_active Expired - Fee Related
- 2013-03-25 KR KR1020147022373A patent/KR101975628B1/ko active IP Right Grant
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
USD967686S1 (en) | 2006-10-05 | 2022-10-25 | Lowe's Companies, Inc. | Tool handle |
Also Published As
Publication number | Publication date |
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RU2014143055A (ru) | 2016-05-20 |
CN104169219A (zh) | 2014-11-26 |
JPWO2013147284A1 (ja) | 2015-12-14 |
KR20140138628A (ko) | 2014-12-04 |
RU2600378C2 (ru) | 2016-10-20 |
US20150010652A1 (en) | 2015-01-08 |
CN104169219B (zh) | 2016-02-10 |
TW201345838A (zh) | 2013-11-16 |
WO2013147284A1 (ja) | 2013-10-03 |
JP5911153B2 (ja) | 2016-04-27 |
KR101975628B1 (ko) | 2019-05-07 |
US20160264429A1 (en) | 2016-09-15 |
EP2832695A1 (en) | 2015-02-04 |
EP2832695A4 (en) | 2015-08-26 |
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