TWI593699B - 粒狀官能基化氧化矽,其製法及用途 - Google Patents
粒狀官能基化氧化矽,其製法及用途 Download PDFInfo
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- TWI593699B TWI593699B TW102122526A TW102122526A TWI593699B TW I593699 B TWI593699 B TW I593699B TW 102122526 A TW102122526 A TW 102122526A TW 102122526 A TW102122526 A TW 102122526A TW I593699 B TWI593699 B TW I593699B
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- Prior art keywords
- cerium oxide
- formula
- ooc
- microns
- organodecane
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- 238000000034 method Methods 0.000 title claims description 39
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title description 13
- 239000000377 silicon dioxide Substances 0.000 title 1
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 98
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 94
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Description
本發明係關於粒狀官能基化氧化矽、其製法及用途。
在很多應用領域例如在用於農作物防護之產物部門中、在活性醫藥成份情況中、在動物飼料及動物飼料添加物製造中或在食品工業中,使用載劑材料以將例如液態或樹脂狀活性成份轉化成自由流動及貯存安定型。這例如在WO 2011/117100中描述。
對載劑材料之明顯要求是足夠高之吸收性,以致盡可能少的載劑材料需被使用。一系列之公告例如DE 102006002765因此是關於增進在該載劑材料上之經吸收材料的含量的方法。然而,這些方法是效能是極複雜的且彼迄今尚未在工業規模上被建立。
對該載劑材料之另外的要求是:該吸收物具有良好自由流動且因此具有良好加工性。此外,該氧化矽在該吸收物之運輸、分配及製造過程中應有極少蒙塵度。為改良該
自由流動,例如EP 0984772 A1及EP 0966207 A1因此建議使用具有約球形且具有大於150微米平均粒子尺寸之微粒狀氧化矽作為載劑材料。以此方式獲得之吸收物確實有改良的自由流動,但該氧化矽之加工性並非最理想的。
在固定床催化之領域中,對載劑或載體材料有進一步之額外要求。例如,必須確保:在固定床反應器中之反應在該反應室中造成最小的壓力降,在該反應器中該反應物流過一反應室,其填充已施加觸媒之經負載的載體材料。在經負載觸媒的載體材料係懸浮在反應介質中的反應的情況中,該載體材料必須是在該反應結束時可容易再次移除的。最後,在流化床反應器中之反應要求:該經負載之載體材料可在其內有效率地流化。因此顯然地,不同反應器型式對該經負載之載體有相當不同的要求,且因此也對該載體材料有相當不同要求。為要符合這些要求,WO 2011/117100描述粒狀氧化矽,其具有大於0.9毫升/克之Hg孔體積(<4微米)、大於400微米之dQ3=10%及同時小於3000微米之dQ3=90%且無照射超音波之d50對照射超音波3分鐘後之d50的比率<4.00,此量度是對400至500微米之粒子部份所進行的。然而,這些氧化矽所具有之缺點是一些催化活性成份(例如酵素或生物觸媒)僅不合適地結合在氧化矽表面上且再次太快速地解吸。
EP 1357156 A2揭示經矽烷改質之氧化或矽化的填料,其具有低於15重量%之小於75微米的顆粒部份及在130及500微米之間的中值粒子尺寸。再者,US
20060084746揭示由非結晶之沉澱氧化矽、氧化鋁組成之群所選的疏水性無機氧化物或此等無機氧化物之混合物,其中羥基含量是2-15 OH/平方奈米、碳含量0.1至6重量%、甲醇潤濕度15至45%且M1標準白面積少於0.4%。
本發明之目的是要提供氧化矽,其具有例如改良之酵素解吸特性。
本發明提供一種粒狀官能基化氧化矽,其特徵在於-該Hg孔體積(<4微米)是大於0.80毫升/克,較佳是大於0.85毫升/克,更佳是大於0.90毫升/克,還更佳地大於0.95毫升/克,特佳是大於1.00毫升/克,-dQ3=10%是大於400微米,-dQ3=90%是小於3000微米,-無照射超音波之d50對照射超音波3分鐘後之d50的比率是小於4.00,較佳是小於3.00,更佳是小於2.60,還更佳是小於2.10,特佳是小於1.60,此量度是對400至500微米之粒子部份所進行的,及-碳含量是1.0-15.0重量%,較佳是2.0-14.0重量%,更佳是3.0-12.0重量%。
本發明之粒狀官能基化氧化矽可具有5.0至11.0之pH。
足夠高之孔隙度確保:本發明之粒狀官能基化氧化矽在間隙孔及/或大孔範圍內具有足夠孔體積,且因此該酵
素對於反應物具有良好的接近性,同時需要最小量之載體材料以供製造本發明之調合物。
另外較佳之本發明的粒狀官能基化氧化矽所具有之Hg孔體積(<4微米)是0.81至1.50毫升/克,較佳是0.81至1.40毫升/克,最佳是0.81至1.30毫升/克。
本發明之粒狀官能基化氧化矽的另外重要性質是其硬度。若該孔隙度是高的,則事實可能是機械安定性不再被確保,而可導致在氧化矽及利用氧化矽所製造之調合物上受機械應力情況下增加細物形成。在該氧化矽之包裝及運輸過程中、在該調合物製造過程中、及在該經負載之載體材料的使用過程中,該機械應力藉由對水中懸浮之該氧化矽進行超音波作用3分鐘來模擬。無照射超音波之d50對照射超音波3分鐘後之d50的比率提供與因該機械應力所致之d50的降低程度相關的資訊。該氧化矽愈硬,則在照射超音波後之d50U對無照射超音波之d50間之差異愈小,亦即在理想情況中,無照射超音波之d50對照射超音波3分鐘後之d50U的比率會是1.00。
本發明之粒狀官能基化氧化矽具有極良好之硬度,雖然彼有高的平均粒子尺寸。無照射超音波之d50對照射超音波3分鐘後之d50U的比率較佳可以是1.00至3.00,更佳地1.00至2.60,還更佳地1.00至2.10,特佳地1.00至1.60。此測量係對400微米至500微米之粒子部份所進行的。
特徵在於dQ3=10%及dQ3=90%之粒子尺寸分布對於確保
在固定床反應器中之良好流動性或對於確保在流化床反應器中之良好流化性是重要的。過大之粒子不具有足以用於該反應、解離及擴散的比表面積。反之,過小之粒子增加抗流動性。本發明之粒狀官能基化氧化矽因此具有大於400微米之dQ3=10%及小於3000微米之dQ3=90%。
本發明之粒狀官能基化氧化矽較佳可具有之碳含量是1.0-9.0,較佳是1.0至7.5,更佳是2.0-7.5。
本發明之粒狀官能基化氧化矽可具有以下官能基:Si[(CH2)m-R']、(R")xSi[(CH2)m-R']、Si[(CH2)m-R']、(R")xSi[(CH2)m-R']、Si[(CH2)m-OOC(CH3)C=CH2]、Si[(CH2)m-OOC(CH3)C=CH2]、(R")(3-x)Si[(CH2)m-OOC(CH3)C=CH2]或(R")xSi[(CH2)m-OOC(CH3)C=CH2],其中m=0、1-20,R'=-NH2、-NH-CH2-CH2-NH2、-N-(CH2-CH2-NH2)2、-NH-CO-N-CO-(CH2)5、-NH-COO-CH3、-NH-COO-CH2-CH3、-NH-(CH2)3Si(OR)3、-NH-(CH2)3-CH3或-NH-CH2-CH2-NH-CH2-CH2-NH2、R"=烷基、環烷基,x=1或2。
以下官能基可經由Si-O-Si鍵結連接該氧化矽:(-O-)3Si[(CH2)m-R']、(-O-)(3-x)(R")xSi[(CH2)m-R']、(-O-)3Si[(CH2)m-R']、(-O-)3-x(R")xSi[(CH2)m-R']、
(-O-)3Si[(CH2)m-OOC(CH3)C=CH2]、(-O-)3Si[(CH2)m-OOC(CH3)C=CH2]、(-O-)x(R")(3-x)Si[(CH2)m-OOC(CH3)C=CH2]或(-O-)(3-x)(R")xSi[(CH2)m-OOC(CH3)C=CH2]。
該粒狀官能基化氧化矽可以是發煙氧化矽或沉澱氧化矽。
本發明另外提供第一種製造本發明之粒狀氧化矽的方法,其包含以下步驟:a)提供沉澱或發煙氧化矽,其具有0.1至350微米之平均粒子尺寸d50,若無超音波處理,較佳地具有30至800平方公尺/克之BET表面積且較佳地具有140至400克/100克之DBP值,b)使步驟a)之氧化矽濕化至30-80重量%之乾燥損失,c)藉由擠出、粒化、壓實或製錠使步驟b)之氧化矽成形,d)在乾燥單元中乾燥該氧化矽成形體,e)以3000微米之篩尺寸篩選粒化或篩選該等顆粒且篩出具有400微米之篩網眼尺寸的細粒,f)使步驟e)之顆粒與表面改質劑反應。
來自步驟a)之沉澱或發煙氧化矽可被乾燥且隨意地研磨。
替代上述依照本發明之第一方法地,也可能使用具有30-80重量%乾燥損失之含水濾餅作為步驟a)之原料。
本發明另外提供第二種製造本發明之粒狀氧化矽的方法,其包含以下步驟:i)提供沉澱或發煙氧化矽,其具有<30重量%之乾燥損失,且具有0.1至350微米之平均粒子尺寸d50,若無超音波處理,較佳地具有30至800平方公尺/克之BET表面積且較佳地具有140至400克/100克之DBP值,ii)藉由乾壓實,較佳在二個轉動的滾筒之間,以每公分滾筒寬0.5千牛頓至每公分滾筒寬12千牛頓的特定接觸壓力,使步驟i)之氧化矽成形以得塊體,iii)以3000微米之篩尺寸篩選粒化或篩選該塊體且篩出具有400微米之篩網眼尺寸的細粒,且iv)使步驟iii)之顆粒與表面改質劑反應。
步驟i)之沉澱或發煙氧化矽可被乾燥且隨意地研磨。
在上述依照本發明之所有方法中,該等粒子之硬度可藉由在高溫例如70℃至400℃下以水蒸氣處理彼等而進一步增加。在此之後,可能需要另外的乾燥步驟。
此外,該等粒子之硬度可藉由彼等與鹼性物質接觸一段時間以提升該等粒子之pH而增加。該方法係描述於DE 102008035867 A1中。
此外,該等粒子之硬度可藉由在高溫(較佳介於700℃至1200℃之間)鍛燒步驟e)或iii)之粒子一段時間(較佳<1小時)而增加。
上述硬化該等粒子之處理步驟可在篩選粒化及篩選之
處理步驟之前或之後進行。
依照本發明之第一方法的濕化處理步驟(b)及/或粒化處理步驟(c)可以在高速強化混合器、捏合機、壓實機、平盤型粒化機及/或穿孔塑模壓機或類似機器中進行。可選擇地,該濕化後接著是擠出,或含水濾餅可直接被擠出。經擠出之成形體隨後可藉由另外合適的處理(例如得自Caleva之團球機(spheronizer))改變幾何形狀。
依照本發明之第一方法的乾燥處理步驟(d)可例如在乾燥櫥、流化床乾燥機、帶式乾燥機或類似機器中進行。若需要,經乾燥之成形體隨後可藉由另外處理(例如以3000微米之篩尺寸篩選或篩選粒化)被調節至合適之粒子尺寸部份且篩出具有400微米網眼尺寸的細粒。
依照本發明之第二方法的成形步驟(ii)較佳在壓實機(例如在得自Hosokawa Bepex GmbH之設備中,諸如在Bepex L200/50中,或在Alexanderwerk AG之設備中)進行。
依照本發明之二方法的篩選粒化(e或iii)較佳可在諸如在得自Frewitt或Hosokawa Bepex GmbH之篩選磨機等設備中進行。該篩選可利用所有已知的技術進行,較佳利用得自諸如Vibra、Engelsmann或Allgeier等公司之震動篩進行。可能進行數次篩選或數次篩選步驟。
在步驟f)或iv)中該等顆粒之反應可藉由隨意地首先以水,而後以表面改質劑噴灑該氧化矽而進行。所用之水可用酸(例如氫氯酸)來酸化至pH7-1,或所用之水可
用鹼來鹼化至pH7-14。若使用多種表面改質劑,彼可分開地、順序地或以混合物形式施加在一起。該表面改質劑可溶在適合溶劑中。該噴灑結束後接著是混合另外的5至30分鐘。然後該混合物可在20至400℃之溫度下熱處理0.1至6小時之時間。該熱處理可在保護性氣體例如氮氣下進行。該熱處理也可在多於一個階段中於不同溫度下進行。該表面改質劑之施加及該熱處理可以在一合適單元中進行或分開地在不同的合適單元中進行。可利用單相、二相或超音波噴嘴進行該表面改質劑之施加。該表面改質可連續地或分批地在具有噴灑裝置之可加熱混合器或乾燥機中進行。適合之設備可以是例如犁型混合器、平盤型乾燥機、流化床乾燥器或移動床乾燥機。
所用之表面改質劑可以是有機矽烷,例如a)式(RO)3Si(CH2)m-R'之有機矽烷類,其中R=烷基,較佳是甲基、乙基或丙基,m=0、1-20,R'=-NH2、-NH-CH2-CH2-NH2、-N-(CH2-CH2-NH2)2、-NH-CO-N-CO-(CH2)5、-NH-COO-CH3、-NH-COO-CH2-CH3、-NH-(CH2)3Si(OR)3、-NH-(CH2)3-CH3或-NH-CH2-CH2-NH-CH2-CH2-NH2,b)式(R")x(RO)(3-x)Si(CH2)m-R'之有機矽烷類,其中R、R'及m分別如以上所定義且R"=烷基、環烷基,
x=1或2,c)式X3Si(CH2)m-R'之鹵有機矽烷類,其中R'及m分別如以上所定義,且X=Cl或Br,d)式(R")xX(3-x)Si(CH2)m-R'之鹵有機矽烷類,其中R'、R"、X、x及m分別如以上所定義,e)式(RO)3Si(CH2)m-O(O)C(CH3)C=CH2之有機矽烷類,其中R及m分別如以上所定義,f)式X3Si(CH2)m-O(O)C(CH3)C=CH2之鹵有機矽烷類,其中X及m分別如以上所定義,g)式Xx((R")(3-x)Si(CH2)m-O(O)C(CH3)C=CH2之有機矽烷類,其中X、R"、x及m分別如以上所定義,h)式(R")x(RO)(3-x)Si(CH2)m-O(O)C(CH3)C=CH2之有機矽烷類,其中R、R"、x及m分別如以上所定義,及這些表面改質劑之混合物。
較佳地,所用之表面改質劑可以是胺基丙基三乙氧基矽烷、胺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、3-胺基丙基甲基二乙氧基矽烷或3-甲基丙烯醯基氧基丙基三甲氧基矽烷。更佳地,所用之表面改質劑可以是胺基丙基三乙氧基矽烷、胺基丙基三甲氧基矽烷或3-甲基丙烯醯基氧基丙基三甲氧基矽烷。
對於載劑或載體應用而言,可以在依照本發明之方法中使用市面上很多的氧化矽。其實例是得自Evonik Industries之氧化矽SIPERNAT® 50、SIPERNAT® 50S、
SIPERNAT® 500LS、SIPERNAT® 22、SIPERNAT® 22S、SIPERNAT® 22LS及SIPERNAT® 33。這些氧化矽即使特別地為載劑或載體應用而發展,彼等也不適合或僅在不足之程度上適合用來作為載劑或載體材料。特別是在噴乾、噴嘴塔乾燥及/或研磨粒子的情況中,此現象之理由是其過低之粒子尺寸而如以上所列述的可在反應器中導致非所欲之壓力上升,及沒有用於化學或物理連結之官能基。藉由依照本發明之方法,進行這些氧化矽之壓實,所得之粒子的粒子尺寸及強度因此受依照本發明之方法所控制,以致獲得具有最理想粒子尺寸分布及硬度之粒子,其在該反應器中具有低的抗流動性且可容易地由懸浮液濾出。
除了已提及之氧化矽之外,在依照本發明之第一方法的步驟a)中,可能使用例如得自Evonik Industries之矽石SIPERNAT® 2200、Aerosil® 200、得自Rhodia Chimie之Tixosil® 38 A至X、得自PPG之HiSil ® SC 60及HiSil ® SC 72、得自Huber之Hubersil® 5170及在歐洲專利EP 0984772 A1、EP 0966207 A1及EP 0937755 A1中所揭示之氧化矽。
依照本發明之方法中所用的氧化矽可具有:1. 0.1至350微米,較佳地0.1至200微米,更佳地0.1至150微米,且最佳地1至50微米之無超音波處理之平均粒子尺寸d50,2. 30至800平方公尺/克,較佳地40至700平方公尺
/克,更佳地50至600平方公尺/克,且最佳地150至550平方公尺/克之BET表面積,3. 140至400克/(100克),較佳地140至350克/(100克),更佳地190至350克/(100克),最佳地290至350克/(100克)之DBP值。
依照本發明之第一方法較佳是在混合器、捏合機或壓實機(隨意地與下游之擠出機)及下游乾燥機、篩選粒化機及篩中進行。例如,起初裝填之氧化矽首先可在例如一得自Eirich GmbH之設備中用液體濕化(除非是直接使用濾餅),然後壓縮或壓實,然後擠出且乾燥。經液體濕化且壓縮或壓實之氧化矽可同樣地被乾燥,然後可進行篩選粒化,然後彼可篩選至所要之粒子部份。
最後之載劑或載體粒子的硬度可受原料氧化矽之壓縮或壓實措施來控制。該壓實通常可以藉由添加水且同時導入切變能量來進行。此外,也可能添加水溶液(諸如纖維素溶液)或油類,其係適合作為粒子間之黏合劑。該液體基於1.00克/毫升之密度,較佳可以50至90重量%之比例,更佳地以60至90重量%之比例且最佳地以65至90重量%之比例被添加。此外,在該壓實期間,可能添加適合在粒子間作為黏合劑之固體(例如纖維素、蠟或聚合物)或隨後可被聚合之單體。該固體添加比例可以是0.1至50重量%,較佳是0.5至15重量%,更佳是0.5至8重量%。
在一較佳具體例中,該載劑或載體材料可在不添加黏
合劑之情況下被壓縮或壓實(步驟c)或ii))。
該壓實較佳可以在10℃至90℃,更佳在10℃至70℃之溫度下進行。
在依照本發明之第一方法中的成形較佳可藉由以下方式進行:在該混合單元中於所添加之液體的輔助下密集地壓實該原料氧化矽,直至有部份液體排出及開始粒子之粒化。由此所得之顆粒(原料顆粒)的粒子尺寸可藉由擠出步驟均勻化,然後彼可被乾燥。此外,該濕化之原料顆粒在省略該擠出步驟時也可直接被乾燥且例如通過具有3000微米特性尺寸之篩,而將比該特性篩尺寸大的粒子研成粉末。該通過較佳在諸如得自Frewitt或Hosokawa Bepex GmbH之篩磨機等設備中進行。比該通過篩之特性尺寸大的粒子在使用本發明之載體材料於懸浮催化領域中的情況下可導致該調合物之非所欲的沉澱且導致長的擴散或反應時間。當所有小於400微米之篩部份被移除時,則是另外有利的。如上述,這些小粒子對粒子之抗流動性有不良影響且在固定床反應器中導致壓力降。
可以利用所有已知的技術,較佳利用得自諸如Vibra、Engelsmann或Allgeier等公司之震動篩進行該篩選。可能進行數次篩選或篩選步驟。
在依照本發明之第二方法中,該氧化矽之壓實較佳是在具有下游篩選粒化器及篩之乾燥壓實機中進行。起初裝填之氧化矽可例如在得自Hosokawa Bepex GmbH之設備諸如Bepex L200/50或得自Alexanderwerk AG之設備中被
壓實,且壓實的材料可被篩選粒化且分成所要的粒子部份。
在依照本發明之第二方法的步驟ii)中,乾燥的原料氧化矽被壓實,亦即加壓成具有對於本發明之應用最理想之粒子尺寸及硬度的塊體。硬度可受將該原料氧化矽壓實之壓力所控制。較佳以每公分滾筒寬0.5至15千牛頓,更佳以每公分滾筒寬3至12千牛頓,且最佳以每公分滾筒寬6至10千牛頓的特定接觸壓力及在10℃至90℃,更佳地10℃至70℃之溫度下進行該壓實。此外,在該壓實期間,可能添加液體,較佳添加水、水溶液(諸如纖維素溶液)或油類,這些適合作為粒子間之黏合劑。該液體之添加比例較佳可以是1至30重量%,更佳是1至20重量%,且最佳是3至15重量%。此外,在該壓實期間,可能添加適合作為粒子間之黏合劑的固體(例如纖維素、蠟或聚合物)或隨後可被聚合之單體。該固體添加比例是0.1至50重量%,較佳是0.5至15重量%,更佳是0.5至8重量%。
此乾燥壓實較佳進行方式可以是使該乾燥的原料氧化矽在壓實單元中於二轉動的滾筒間加壓,其中至少一個滾筒更佳具有凹部諸如溝槽、窪部或墊,其特性尺寸大於所要獲得之粒子尺寸。該滾筒可具有直的或凹的構型。另外特佳之具體例在於使用至少一個經穿孔之齒輪滾筒。此外,當至少一個滾筒被構成以致在該滾筒表面可產生低壓時,則可以是有利的,藉該壓力該待壓實之氧化矽被捲在
該滾筒上。可利用對精於此技藝者已知的所有輸送裝置(例如輸送螺桿、雙螺桿等)將該氧化矽供應至該壓實單元。
在該壓實之後,所得之塊體通過具有3000微米之特性尺寸的篩,在此過程中比該特性篩尺寸大之粒子被研成粉末。該通過較佳在諸如得自Frewitt或Hosokawa Bepex GmbH之篩磨機的設備中進行。比該通過篩之特性尺寸大的粒子在使用本發明之載體材料於懸浮催化領域中的情況下可導致該調合物之非所欲的沉澱且導致長的擴散或反應時間。此外,比400微米小之篩部份被移除。如上述,這些小粒子對粒子之抗流動性有不良影響且在固定床反應器中導致壓力降。
對最終乾燥之顆粒之可能的蒸氣處理可在適合此目的之所有設備中完成,這些是例如帶式乾燥機、旋轉乾燥機、乾燥櫥、流化床乾燥機等。該顆粒可曝於70℃-400℃,較佳地80℃-300℃,更佳地90℃-200℃且最佳地106℃-180℃之溫度下。在此溫度下之滯留時間可以是至高16小時,較佳地至高12小時,更佳地至高8小時,最佳地至高4小時。
該等粒子之可能的煅燒可以在不同設備(例如鍛燒爐、帶式或旋轉管式鍛燒爐)或在快速或流化床鍛燒爐中進行。該顆粒可曝於700℃-1200℃,較佳地800℃-1200℃,更佳地800℃-1100℃之溫度下。滯留時間視該煅燒時間及所要之粒子硬度而定。在該方法中之滯留時間可以是
1小時,較佳是20分鐘,更佳是小於10分鐘。
本發明另外提供本發明之粒狀官能基化氧化矽作為載體材料的用途,較佳用於酵素。
最後,本發明提供一種調合物,其包含至少一種本發明之粒狀官能基化氧化矽及添加劑。
該調合物之添加劑可以化學地或物理地結合本發明之粒狀官能基化氧化矽。
本發明之粒狀官能基化氧化矽可用以製造調合物,該添加劑較佳是硬化劑或起始劑、交聯劑、觸媒、活性醫藥成份及賦形劑、活性化妝成份及賦形劑、清潔及/或照護組成物、調味、香氣及香味劑、動物飼料或動物飼料添加劑、例如胺基酸、維生素、礦物質、食品或食品添加劑、染料及/或顏料、胺基酸、氧化或漂白劑、具有微生物(特別是黴菌或細菌)作用之添加劑、農業及林業用化學品及/或混凝土摻合物。該添加劑可以是水性或非水性液體,例如油類、樹脂、溶液、分散液、懸浮液、乳濁液、蠟、聚合物或熔體。該添加劑隨後可被熱處理、熱處理或使之結晶、固化、分離或反應。此外,該添加劑可預先或稍後乾燥。
在動物飼料或動物飼料添加劑部門中之添加劑包括維生素、礦物質、羧酸、礦物酸、胺基酸、脂肪、油類及香氣。這些更佳是甲酸、乙酸、丙酸、乳酸、磷酸、氯化膽素溶液、維生素E乙酸酯及植物萃取物例如萬壽菊萃取物。
在農業及林業部門中的添加劑包括例如經吸收之肥料(例如含氮及/或磷脂肥料)、農作物保護用組成物、殺蟲劑(例如除草劑、殺真菌劑或殺昆蟲劑)。
在化妝產品部門中之添加劑包括例如油類(諸如精油、香料油、護理油、清香油及聚矽氧油)、活性抗菌、抗病毒或抗真菌的成份、消毒及抗菌物質、除臭劑、抗氧化劑、生物活性物質及生源活性成份、維生素及維生素錯合物、酵素及酵素系統(諸如澱粉酶、纖維素酶、脂酶及蛋白酶)、化妝活性物質(諸如化妝品及個人衛生產品之成份)、清洗及清潔活性物質(諸如所有種類之表面活性劑)、清洗及/或清潔活性之無機及有機酸、除污及脫污活性成份、氧化劑及漂白劑、漂白活化劑、填充劑及輔填充劑、抗再沉澱添加劑、灰色化及褪色抑制劑、彩色保護用之活性物質、洗衣保護用之物質及添加劑、光學增亮劑、泡沫抑制劑、pH改質劑及pH緩衝物質。
在食品及食品添加劑部門中之添加劑包括例如經吸收之香氣、食品補給劑、維生素、礦物質及胺基酸。
選自活性醫藥成份之添加劑包括所有種類之活性醫藥成份,例如α-蛋白酶抑制劑、阿巴卡維(abacavir)、阿昔克斯碼(abciximab)、阿卡波糖、乙醯水楊酸、阿賽可羅維(acyclovir)、腺合苷、羥甲叔丁腎上腺素、阿迪斯白血球素(aldesleukin)、阿蘭卓內特(alendronate)、阿福若辛(alfuzosin)、阿羅色重(alosetron)、三氮二氮平、阿特波勒斯(alteplase)、
溴環己胺醇、阿米福斯丁(amifostine)、乙胺碘呋酮、阿米沙坡來得(amisulpride)、安羅地平(amlodipine)、羥氨苄青黴素、安非他命、雙性黴素、安比西林、安波瑞納為(amprenavir)、阿那雷理得(anagrelide)、阿納斯錯唑(anastrozole)、暗克羅德(ancrod)、抗血友病因子、抑肽酶、氨醯心安、阿托伐施特丁(atorvastatin)、阿托平、阿渃拉施丁(azelastine)、阿奇黴素、甘菊藍、巴尼迪平(barnidipine)、氯地米松(beclomethasone)、貝納渃波(benazepril)、羥苄絲肼(benserazide)、貝拉波施特(beraprost)、貝它米松(betamethasone)、貝它梭醇(betaxolol)、貝沙非伯(bezafibrate)、比卡魯醯胺(bicalutamide)、甜沒藥醇、比梭波醇(bisoprolol)、肉毒桿菌素、波瑞模尼定(brimonidine)、溴吡二氮(bromoazepam)、溴麥角環肽(bromocriptine)、布得梭尼得(budesonide)、布皮乏卡因(bupivacaine)、丁氯苯丙酮、丁螺環酮、環丁二羥嗎南、卡波勾藍(cabergoline)、鈣波三烯(calcipotriene)、抑鈣素、鈣化三醇、樟腦、堪低沙坦(candesartan)、刊底沙鉭西勒克施提耳(cilexetil)、巰基甲基氧丙基天旋脯氨酸(captopril)、卡巴馬平(carbamazepine)、碳度巴(carbidopa)、碳鉑(carboplatin)、卡法地羅(carvedilol)、氯頭孢菌素、氯羥苄頭孢菌素、甲氧噻吩頭孢菌素(cefaxitin)、頭孢菌素、頭孢低尼
(cefdinir)、頭孢批每(cefepime)、頭孢克肪(cefixime)、賽每他唑(cefmetazole)、頭孢哌酮(cefoperazone)、頭孢提胺(cefotiam)、頭孢酮基普蘭(cefoxopran)、頭孢帕肟(cefpodoxime)、頭孢普(cefprozil)、頭孢它日地每(ceftazidime)、頭孢替布坦(ceftibuten)、頭孢揣沙酮(ceftriaxone)、頭孢氨呋肟(cefuroxime)、塞內昔布(celecoxib)、二乙脲心安(celiprolol)、乙酸頭孢菌素(cephalexin)、色瑞法施它丁(cerivastatin)、色替瑞辛(cetirizine)、氯黴素、西拉施它丁(cilastatin)、西拉薩普(cilazapril)、組織胺拮抗劑(cimetidine)、西酞普蘭(ciprofibrate)、西普氯沙辛(ciprofloxacin)、西沙普萊德(cisapride)、順鉑(cisplatin)、景普朗(citalopram)、開羅理黴素(clarithromycin)、棒酸(clavulanic acid)、克林達黴素(clindamycin)、氯米帕明(clomipramine)、可納賽潘(clonazepam)、可尼丁(clonidine)、可皮都銳(clopidogrel)、氯三苯甲咪唑(clotrimazole)、可撒平(clozapine)、可偌木林(cromolyn)、環磷醯胺、環孢素、環丙孕酮、達特帕因(dalteparin)、去鐵胺(deferoxamine)、地梭佳斯挫(desogestrel)、右旋安非他命、苯甲二氮焯(diazepam)、雙氯酚酸(diclofenac)、待達諾辛(didanosine)、毛地黃毒苷、長葉毛地黃苷、二氫麥角胺、治定贊(diltiazem)、白喉蛋白、白喉類毒素、雙丙戊酸(divalproex)、多巴酚丁
胺(dobutamine)、多色它克(docetaxel)、多拉瑟創(dolasetron)、多奈派齊(donepezil)、去氧核醣酶-α、多若醯胺(dorzolamide)、多沙若辛(doxazosin)、5'-去氧-5-氟尿苷、阿黴素、6-去氫逆孕銅、依卡貝(ecabet)、西寧(efavirenz)、依那拉瑞(enalapril)、依諾沙帕因(enoxaparin)、依配瑞松(eperisone)、依皮那施丁(epinastine)、表阿黴素、依銻沸巴銻得(eptifibatide)、紅血球生成素-α、紅血球生成素-β、依他那色(etanercept)、乙炔基雌二醇、依托多勒克(etodolac)、依托泊苷(etoposide)、因子VIII、泛昔洛韋(famciclovir)、法莫替丁(famotidine)、法若片(faropenem)、非羅地平(felodipine)、非諾沸伯(fenofibrate)、非諾多潘(fenoldpam)、酞太尼枸椽酸鹽(fentanyl)、非克梭非那定(fexofenadine)、費格拉施(filgrastim)、費那施特(finasteride)、福羅目(flomoxef)、氟康唑(fluconazole)、氟達拉濱(fludarabine)、9-去氟膚輕鬆(flunisolide)、氟尼錯潘(flunitrazepam)、氟西汀(fluoxetine)、N-3-[三氟甲基-4-硝基]苯基異丁醯胺、氟提可松(fluticasone)、氟乏施特丁(fluvastatin)、氟伏沙明、促卵泡激素-α、促卵泡激素-β、佛莫特醇(formoterol)、佛西諾波(fosinopril)、呋喃苯胺酸(furosemide)、佳巴潘丁(gabapentin)、佳多二醯胺(gadodiamide)、甘西勒維(ganciclovir)、佳替佛克沙
辛(gatifloxacin)、浸西塔濱(gemcitabine)、孕二烯酮(gestodene)、哥拉替南(glatiramer)、優降糖(glibenclamide)、格理美派若(glimepiride)、吡磺環己脲(glipizide)、格來不得(glyburide)、枸色雷林(goserelin)、格藍色創(granisetron)、灰黃黴素、B型肝炎抗原、玻尿酸、海可辛(hycosin)、氫氯苯噻噠嗪、二氫可待因酮(hydrocodone)、氫皮質酮、氫嗎啡酮(hydromorphone)、羥基氯奎因(hydroxychloroquine)、海蘭G-F 20、異丁苯丙酸、依弗醯胺、依咪達波(imidapril)、依咪露色醇(imiglucerase)、依咪噴印(imipenem)、免疫球蛋白、克率滿(indinavir)、美洒辛(indomethacin)、英利昔單抗、胰島素、人類胰島素、理施波(lidpro)胰島素、阿施帕特(aspart)胰島素、干擾素-β、干擾素-α、碘-125、艾歐山醇(iodixanol)、艾歐亥可梭(iohexol)、艾歐美坡醇(iomeprol)、艾歐波米得(iopromide)、艾歐佛梭(ioversol)、艾歐撒波林(ioxoprolene)、異丙托醇(ipratropium)、益瑞發豐(ipriflavone)、依貝沙坦(irbesartan)、依瑞諾帖勘(irinotecan)、異山梨醇(isosorbide)、異全反視黃酸、依施拉地平(isradipine)、伊曲康唑(itraconazole)、氯吖配酸鉀(potassium chlorazepate)、氯化鉀、凱特羅拉(ketorolac)、凱特銻分(ketotifen)、百日咳疫苗、凝血因子IX、拉米弗定
(lamivudine)、拉莫區精(lamotrigine)、蘭梭波唑(lansoprazole)、拉塔諾普施特(latanoprost)、勒弗糯米得(leflunomide)、勒諾拉施定(lenograstim)、勒措唑(letrozole)、流波利得(leuprolide)、左旋多巴、左旋氟辛(levofloxacin)、左旋諾佳施翠(levonorgestrel)、左旋甲狀腺素、利多卡因(lidocaine)、理聶若利得(linezolide)、理西諾波(lisinopril)、落帕米多(lopamidol)、落拉卡貝(loracarbef)、落拉塔定(loratadine)、落拉磐(lorazepam)、落沙坦(losartan)、落法施特丁(lovastatin)、離胺酸乙醯水楊酸、馬尼地平(manidipine)、美可巴拉明(mecobalamin)、甲羥助孕酮、美及施措(megestrol)、每落科西肯(meloxicam)、美那特傳農(menatetrenone)、腦膜炎球菌疫苗、美諾措平(menotropin)、美若片(meropenem)、美沙胺(mesalamine)、5-(3,5-二甲苯氧甲基)-2-惡唑啉酮(metaxalone)、美佛明(metformin)、派醋甲酯、甲基去氧皮質醇、1-異丙氨基-3-對甲氧乙苯氧基-2-丙酮(metoprolol)、米達唑(midazolam)、米瑞農(milrinone)、二甲胺四環素(minocycline)、米它撒平(mirtazapine)、米沙坡施投(misoprostol)、雙羥葱醌(mitoxantrone)、莫洛貝米得(moclobemide)、莫待芬寧(modafinil)、莫美它松(mometasone)、盟帖路喀(montelukast)、摩尼弗馬特
(morniflumate)、嗎啡、模克西洛沙辛(moxifloxacin)、黴酚酸鹽、那布美同(nabumetone)、那卓帕林(nadroparin)、甲氧萘丙酸(naproxen)、那拉催坦(naratriptan)、內發若恫(nefazodone)、內非那維(nelfinavir)、內維拉平(nevirapine)、菸鹼酸、硝吡胺甲酯(nicardipine)、麥角溴菸鹼酯、利心平(nifedipine)、尼露醯胺(nilutamide)、利心平(nilvadipine)、尼莫地平(nimodipine)、硝化甘油、尼撒替定(nizatidine)、炔諾酮、諾氟沙辛、體抑素胜肽、奧氮平、歐美波唑(omeprazole)、翁單色創(ondansetron)、歐理施特(orlistat)、歐色塔米韋(oseltamivir)、雌二醇、雌激素、草酸鉑(oxaliplatin)、4,5-二苯-2-唑丙酸、氧林酸(oxolinic acid)、α-環己基-α-羥基苯乙酸二乙氨基丁炔酯(oxybutynin)、紫杉醇、帕力威入莫(palivizumab)、帕米壯特(pamidronate)、胰脂肪酶(pancrelipase)、帕尼片(panipenem)、潘托波唑(pantoprazole)、乙醯胺苯酚、帕羅西汀、己酮可可鹼(pentoxifylline)、波哥力得(pergolide)、苯妥英、皮歐力塔松(pioglitazone)、氧哌嗪青黴素(piperacillin)、吡氧噻嗪(piroxicam)、拉米配梭(pramipexole)、派拉乏施特汀(pravastatin)、哌唑嗪(prazosin)、4,4-(異丙叉二硫)-雙(2,6-二特丁基酚)(probucol)、孕酮、苯丙醯苯心安
(propafenone)、異丙酚(propofol)、丙氧苯、前列腺素、誇太平(quetiapin)、規那波(quinapril)、拉貝帕唑(rabeprazole)、拉洛西芬(raloxifene)、拉米瑞(ramipril)、呋喃硝胺(ranitidine)、瑞帕利尼得(repaglinide)、蛇根鹼、利巴韋林(ribavirin)、利露唑(riluzole)、利培酮、利托納韋(ritonavir)、利妥昔單抗(rituximab)、利乏提明(rivastigmin)、利沙催坦(rizatriptan)、羅非可西(rofecoxib)、羅披尼羅耳(ropinirole)、羅西力塔松(rosiglitazone)、沙美特羅(salmeterol)、服妥美(saquinavir)、沙拉莫施定(sargramostim)、蠶酵素(serrapeptase)、舍曲林、(sevelamer)、(sibutramine)、(sildenafil)、(simvastatin)、(somatropin)、(sotalol)、螺甾內酯、(stavudine)、(sulbactam)、(sulfaethidole)、磺胺甲異噁唑、水楊酸偶氮磺胺吡啶(sulfasalazine)、止嘔靈(sulpiride)、沙馬翠坦(sumatriptan)、它羅利莫施(tacrolimus)、他莫西芬(tamoxifen)、倘舒羅辛(tamsulosin)、它梭巴倘(tazobactam)、貼可蘭因(teicoplanin)、替莫卡利(temocapril)、替莫唑胺(temozolomide)、替內替拉施(tenecteplase)、替諾西勘(tenoxicam)、替坡農(teprenone)、特梭辛(terazosin)、特必那分(terbinafine)、特布它林(terbutaline)、破傷風類毒素、丁苯喹嗪(tetrabenazine)、替措撒盤(tetrazapam)、茴香油、太
佳濱(tiagabine)、7-甲異炔諾酮(tibolone)、羧噻吩青黴素(ticarcillin)、氯苄噻啶(ticlopidine)、噻嗎心安(timolol)、替羅費伴(tirofiban)、咪噻二唑(tizanidine)、妥布黴素(tobramycin)、菸酸生育酚、托特定(tolterodin)、托吡酯(topiramate)、拓撲替康(topotecan)、胺吡磺異丙脲(torasemide)、反胺苯環醇(tramadol)、傳多拉波(trandolapril)、措施圖入嗎(trastuzumab)、去炎松(triamcinolone)、三唑喃(triazolam)、脆美布汀(trimebutine)、甲氧苄氨嘧啶(trimethoprim)、措利他松(troglitazone)、措吡色隆(tropisetron)、叔丁氯喘通(tulobuterol)、優諾波施通(unoprostone)、優羅佛利措平(urofollitropin)、發拉賽克羅維(valacyclovir)、丙戊酸(valproic acid)、乏沙坦(valsartan)、萬古黴素、文拉法辛(venlafaxine)、佛瑞帕米(verapamil)、佛特波分(verteporfin)、微佳巴春(vigabatrin)、長春瑞濱(vinorelbine)、長春乙酯(vinpocetine)、(viglibose)、殺鼠靈(warfarin)、札非路卡施(zafirlukast)、札勒隆(zaleplon)、札那米韋(zanamivir)、日多夫定(zidovudine)、若米崔坦(zolmitriptan)、若琵登(zolpidem)、吡嗪哌酯(zopiclone)及其衍生物。然而,也了解活性醫藥成份是指其他物質諸如維生素、維生素原、必須脂肪酸、源自植物及動物之萃取物、源自植物及動物之油、植物性藥物製
劑及順勢療法的製劑。
在該調合物中之本發明的粒狀官能基化氧化矽尤其可用來作為動物飼料添加劑(例如甲酸、丙酸、乳酸、磷酸、氯化膽鹼溶液、維生素E乙酸酯或植物萃取物例如萬壽菊萃取物)的載劑。
此外,在該調合物中之本發明的粒狀官能基化氧化矽可被用來作為化學產品(三聚氰胺樹脂、橡膠添加劑、塑膠添加劑、建築化學品之添加劑或塗料添加劑)之載劑材料。
在該調合物中之本發明的粒狀官能基化氧化矽最佳被用來所有種類之觸媒的載體材料。該等觸媒特佳可以是酵素或不同種類之酵素的混合物,例如選自氧化還原酶、轉移酶、水解酶、脂酶、離酶(lysases)、異構酶及結合酶之類的酵素(依照生化及分子生物國際聯盟之命名委員會的EC(酵素委任)的編號)。例如藉由重組技術所製造之酵素變體同樣地應被包括在"酵素"用語中。
為製造該調合物,本發明之粒狀官能基化氧化矽與至少一種添加劑接觸,以使該添加劑能滲入該氧化矽之孔中。為此目的,可能利用在此技藝中已知之所有技術,例如噴灑施加、滴式施加、飽和、浸漬、噴嘴噴灑等。本發明之粒狀官能基化氧化矽較佳在起初被裝填於固體混合單元中,例如捏合機、槳式乾燥機、滾動混合器、垂直混合器、槳式混合器、沙及(Schugi)混合器、水泥混合器、蓋力克(Gericke)連續混合器、艾氏混合器及/或倉型混
合器。在該混合單元中之溫度依照待吸收之物質的本質及組成,較佳可以在5至90℃之間,更佳在10至70℃之間。在該混合器中之壓力較佳可以在0.1巴至2巴之間,更佳在0.5巴至1.2巴之間。
在該調合物中之所有添加劑的含量可以是在1至70重量%,較佳在5至65重量%之間,更佳在5至60重量%之間,最佳在5至20重量%之間。
本發明之調合物特佳可以用來作為在固定床反應器中、在雜相催化領域中、在流化床反應器中及用於懸浮液中之反應的觸媒。
所用之原料及本發明之粒狀氧化矽的物理化學數據藉由以下方法測定:
氧化矽之比氮表面積(下文中稱為BET表面積)係依照ISO 9277測定為多點表面積。所用之測量儀是得自Micromeritics之TriStar 3000表面積測量儀。該BET表面積一般是在液態氮之飽和蒸氣壓的0.05-0.20的分壓範圍內測定。該樣品係藉由在得自Micromeritics之VacPrep 061加熱站中於160℃真空下加熱該樣品1小時而製備。
DBP吸收(DBP值)-該氧化矽之吸收性的量度-是在如下之標準DIN 53601的基礎上被測定。
12.50克之具有3-10%之水含量的氧化矽(若需要則水含量藉由在乾燥櫥中105℃下乾燥而調節)被導入得自Brabender之C吸收計的捏合室中。在該吸收計上之測量係在使用BRABENDER Automatic Oil Absorption System Version 1.1.2(其具有所測量之力矩曲線的固定阻尼)的PC支援下進行。
在濾餅之情況中,其係在使用前在乾燥櫥中於105℃下乾燥至≦10%之水含量,且通過3毫米篩,然後通過300微米篩。
在左手邊之捏合機之槳的圓周速度為125rpm之下,形成該C吸收計之零件的Titronic Universal滴定管(得自Schott)被使用以在室溫下以4毫升/分鐘之速率將鄰苯二甲酸二丁酯逐滴添加至該捏合室中。在該C吸收計之控制軟體停止該捏合機及DBP測量時的關機點設定在0.6Nm之力矩下。
下式用來計算該DBP吸收率[克/100克]
其中
DBP:DBP吸收率[克/100克]
V:消耗之DBP[毫升]
D:DBP密度[克/毫升](在20℃下1.047克/毫升)
E:開始實之氧化矽重量[克]
K:依照水校正表之校正值[克/100克]
該DBP吸收率係對無水乾燥之氧化矽定義。在使用未乾燥之氧化矽的情況中,為供計算該DBP吸收率,應將該校正值K列入考慮。可以使用以下校正值決定此值。
若氧化矽之水含量是5.8%,為供DBP吸收率,則33克/100克之校正值K被加至上述之分析值。氧化矽之水含量藉由在本文中稍後所述之“水含量測定”方法來測定。
用以測定粉狀固體之粒子尺寸分布的雷射繞射的應用是基於粒子將來自單色雷射光束之光散射或繞射在全部方
向上且依照其尺寸有不同強度圖形的現象。待照射之粒子的直徑愈小,則該單色雷射光束之散射或繞射角度愈大。
供利用雷射繞射之粒子尺寸測量的樣品的製備:因為一些樣品粒子尺寸超過所用儀器之測量範圍且無照射超音波之d50對照射超音波3分鐘後之d50U的比率係依照開始之粒子尺寸而定(較小之材料粒子擁有較高比率之所述尺寸),在該測量前要將400微米-500微米之粒子部份從該樣品篩出。此操作使不同材料之安定性能可靠地被比較以獲得關於特定物質之安定性的陳述。該篩選係利用得自Haver & Boecker,59302 Oelde之HAVER EML 200 Digital Plus篩選機進行,該篩選機係配備400微米及500微米之篩。5克原料被施加至上方之500微米篩上,且以1.0之振幅設定篩選2分鐘。在400微米至500微米間之粒子部份被用於另外的分析。
若該400微米至500微米的部份(其對於比較是重要的)並非本載劑或載體材料的粒子尺寸分布的部份,對應之篩部份係藉由以下方式產生:在得自Eweka GmbH,Heusenstamm之TG2S篩選粒化機的輔助下使足量之原料在100震動/分鐘下通過500微米之篩,然後通過400微米之篩使其篩出。該篩選係如上述地完成。
在親水性氧化矽的情況中,製備該樣品以供分析(該模組之清洗等),該分析係利用LS 230雷射繞射系統
(得自Beckman Coulter;測量範圍0.04-2000微米)及液體模組(得自Beckman Coulter之Small Volume Module Plus,120毫升,其附帶整合的超音波指),且在作為分散液體之去離子水中的0.05% m/m二磷酸四鈉幫助下;且在不充分水可潤濕之氧化矽的情況中係利用乙醇/水混合物(體積比率1:1)作為分散液體。在該分析開始前,該雷射繞射系統必須預熱2小時。此後,該SVM模組必須用該分散液體清洗3次。以下與該粒子相關之參數必須被設定:
分析時間:60秒
測量次數:1次
泵速度:75%
光學模式:夫朗和斐(Fraunhofer)
PIDS功能:停止的
偏位測量:啟動的
調整:自動
背景測量:啟動的
設定樣品濃度:啟動的
使用刮勺以添加該氧化矽篩選部份(400-500微米)直至達到使該LS 230雷射繞射給予"OK"訊息所需之測量濃度。在藉由抽送循環以分散該氧化矽懸浮液60秒而無超音波照射之後,在室溫下進行該分析。由該原始數據的曲線,該軟體基於夫朗和斐模式(夫朗和斐rfd檔案)計算該粒子尺寸分布及無照射超音波之d50(中值)。
在該LS 230雷射繞射機中所呈現之氧化矽懸浮液再次藉由在該SVM模組(得自Sonics之Vibra Cell VCX 130超音波處理器,其具有CV 181超音波轉換器及6毫米超音波尖端)中整合之超音波指,在100%振幅下超音波處理180秒,同時在該液體模組中抽送循環,且如上述被分析。
由該原始數據曲線,該軟體基於夫朗和斐模式(夫朗和斐rfd檔案)計算該粒子尺寸分布及照射超音波3分鐘後之d50U(中值)。
在動力影像評估時,蓬鬆材料流向下落在光源與照相機之間。該等粒子經偵測為投影區、利用電腦程式數位化且轉換成粒子尺寸。
為測量該粒子尺寸,使用得自RETSCH Technology GmbH,Haan之CAMSIZER。該等粒子在具有貯存槽漏斗之DR100-40計量通道的幫助下被供應至該測量儀。為供該影像評估,應使用在3.12d版中所供應之軟體。
在該分析開始前,使該儀器預熱2小時。這確保玻璃在照明單元前防護且該照相機沒有灰塵。在漏斗與計量通道之間的距離被調整成該最大粒子尺寸之約3倍。該計量
通道置於該測量儀正上方。約150毫升之樣品被導入該漏斗。以下之用於分析的參數被記錄在該分析工作檔案(*.afg)中:
為調節該計量通道,以下設定被記錄在該軟體中:
在該數位化影像的評估中,x值係由最小(xc)值計算。沒有使用形成因素。
dQ3=10%及dQ3=90%之輸出係以基礎參數測定。
在擬合檔案的幫助下並不進行分析數據之擬合。
氧化矽之水含量係依照ISO 787-2測定。為此目的,1-4克之樣品量在乾燥櫥中於(105±2)℃下乾燥2小時且依照該ISO說明書評估。此乾燥損失主要由物理結合之水所構成。
該氧化矽之pH係以水性懸浮液形式在室溫下被測定。粒狀樣品預先利用研缽及杵研磨或壓碎。將95克之去離子水添加至5克氧化矽。該懸浮液利用磁性攪拌器攪拌5分鐘。在此之後,立刻在被校正於預期測量範圍中之pH計(Metrohm 780 pH計)的幫助下,該懸浮液之pH精確地測量至小數點右邊第一位。
該方法是基於依照DIN 66133的汞侵入,使用得自Micromeritics之AutoPore IV 9520系統。該方法原則是基於與所施加之壓力相關之經注入多孔性固體中之汞體積的測量。此僅涵蓋在所施加之壓力(最大414MPa)下汞可滲入之孔(李特-德雷克(Ritter and Drake)方法)。
非潤濕之液體僅在壓力下滲入孔系統中。待施加之壓力與該孔洞之淨寬成反比。對於圓柱形孔而言,孔半徑rp與壓力p之間的關係藉由華許本(Washburn)等式所給予:
rp:孔半徑
p:壓力
σ:表面張力(480mN/m*)
θ:汞之接觸角度(140° *),*依照DIN 66133
≦4微米之汞孔體積係由具有直徑≦4微米降至該AutoPore IV 9520汞孔隙計(最大壓力414MPa)之偵測限度的所有孔的累計孔體積所計算的。
以下實例意欲詳細說明本發明卻不限制其範圍。
利用LECO元素分析儀(型號:CS 244或CS 600)測定碳含量。該氧化物被秤入陶瓷坩鍋中,提供燃燒添加劑且在氧流下於感應爐中加熱。此方法將所存在之碳氧化成CO2。此氣體量利用紅外偵測器定量化。在真實測量前,該儀器之校正係利用合適參考物質進行。
將精確至1毫克之約50克至150毫克的樣品材料秤入陶瓷坩鍋中。該樣品材料用約1克之Lecocel II(10%之鎢-錫合金粉末)及約0.7克之鐵屑覆蓋。然後,該坩鍋用蓋子關上。該感應爐設定至最大功率且用氧沖洗10秒。然後在該坩鍋已放入該感應爐之後,啟動自動測量及
評估。對於每一樣品而言,進行多重測定。結果報告之單位係重量%。
此分析方法之碳偵測限度是300微克/克。
敲緊密度係依照DIN EN ISO 787-11測定。
點燃損失係在ISO 3262-1之基礎上被測定。與ISO 3262-1的差異是:-並非鉑盤或磁盤,而是使用磁坩鍋或熔解坩鍋以供測定,-秤入約0.5克(500毫克)而非約2克之待測試的氧化矽,-待檢驗之材料並未預先乾燥,反之,該水份校正係基於ISO 787-2,藉由乾燥損失之分開的測定而進行。
得自Evonik Industries之SIPERNAT® 50 S在混合機(得自Eirich之R02)中混合且壓實,且每100克氧化矽添加220毫升之水。在室溫下使用配備釘型攪拌器混合裝置之10升混合槽。為要獲得該混合機的最理想填充程度,在起初裝填1公斤之SIPERNAT® 50 S。在20公尺/
秒之該攪拌器之圓周速度下在1分鐘內均勻地添加水。之後,該板總以段數1運轉。之後,該針型攪拌器以40公尺/秒操作。一旦已形成所要之黏聚物,即停止該程序。在乾燥櫥中於160℃下將所得之顆粒乾燥至固定重量,然後藉由篩選分級至400-1250微米。為供測試之目的,對於個別測試而言,製造400-500微米之篩選部份;彼被用於稍後之硬度及孔隙度測試。
得自該比較用實例之顆粒在起初被裝填於犁型混合機中且利用二相噴嘴噴灑(載劑氣體:氮),同時與該表面改質劑混合。該噴灑結束後接著混合另外15分鐘。
然後該混合物在乾燥櫥中受熱處理(加熱處理)。
用於製造實例1及2之確實的實驗參數在以下表1中列出。
表2a及2b含有本發明之經表面改質的氧化矽及比較用氧化矽的物理化學數據。
將8克之DOW DC 200 50cs聚矽氧油秤入燒杯中,添加10克之粒狀氧化矽(乾燥損失≦6%),然後利用刮勺混合直至獲得乾燥且自由流動之吸收物。所得之該吸收物在室溫(23℃)下貯存14天。
‧比較用調合物1:5克之比較用實例1+4克之DC200 50cs聚矽氧油
‧本發明之調合物1:5克之實例1+4克之DC200 50cs聚矽氧油
‧本發明之調合物2:5克之實例2+4克之DC200 50cs聚矽氧油
‧藉由溶解10克之Triton X160於490克之去離子水
中製備表面活性劑溶液。
‧50毫升之離心管被填充20毫升之表面活性劑溶液,且添加9克之在1中所述之調合物。
‧該離心管被翻轉10次且靜置5分鐘。
‧將該上清液通過200微米之篩,傾倒於經秤重之玻璃盤中。
‧所保留之吸收物的量再次被分散在20毫升之表面活性劑溶液中,且萃取搖盪步驟共重覆5次(5×20毫升之表面活性劑溶液)。每次所傾倒之液體的體積被收集在該玻璃盤中。
‧所收集之傾倒的表面活性劑溶液在110℃下乾燥3小時且殘留物被精確地秤重。
‧作為空白組(為測定在無聚矽氧油之情況下的殘留物的量),5克之比較用實例1被分散在100毫升表面活性劑溶液中,然後傾倒且乾燥。
所釋出之聚矽氧油的百分比計算如下:((殘留物-空白組)×100)/4=釋出(%)
‧空白組:1.409克之殘留物
‧比較用實例1:3.38克之殘留物=>49.3%之釋出
‧實例1:1.60克之殘留物=>4.8%之釋出
‧實例2:2.02克之殘留物=>15.3%之釋出
本發明之實例顯示甚降低之釋出及因此更高之吸收。
Claims (18)
- 一種粒狀官能基化氧化矽,其特徵在於-該Hg孔體積(<4微米)是大於0.80毫升/克,-dQ3=10%是大於400微米,-dQ3=90%是小於3000微米,-無照射超音波之d50對照射超音波3分鐘後之d50的比率是<4.00,此量度是對400至500微米之粒子部份所進行的,及-碳含量是1.0-15.0重量%,其中該粒狀官能基化氧化矽含有以下官能基:Si(CH2)m-R'、(R")xSi(CH2)m-R'、Si(CH2)m-R'、(R")xSi(CH2)m-R'、Si(CH2)m-OOC(CH3)C=CH2、Si(CH2)m-OOC(CH3)C=CH2、(R")(3-x)Si(CH2)m-OOC(CH3)C=CH2或(R")xSi(CH2)m-OOC(CH3)C=CH2,其中m=0、1-20,R'=-NH-CH2-CH2-NH2、-N-(CH2-CH2-NH2)2、-NH-CO-N-CO-(CH2)5、-NH-COO-CH3、-NH-COO-CH2-CH3、-NH-(CH2)3Si(OR)3、-NH-(CH2)3-CH3或-NH-CH2-CH2-NH-CH2-CH2-NH2、R"=烷基、環烷基,x=1或2。
- 如申請專利範圍第1項之粒狀官能化氧化矽,其中其具有在5.0至11.0範圍內之pH。
- 如申請專利範圍第1或2項之粒狀官能化氧化矽,其中彼所具有之無照射超音波之d50對照射超音波3分鐘後之d50的比率是1.00至3.00,此量度是對400至500微米之粒子部份所進行的。
- 如申請專利範圍第1或2項之粒狀官能化氧化矽,其中其所具有Hg孔體積(<4微米)是大於0.90毫升/克。
- 如申請專利範圍第1或2項之粒狀官能化氧化矽,其中其所具有Hg孔體積(<4微米)是0.81至1.50毫升/克。
- 一種製造如申請專利範圍第1至5項之粒狀官能基化氧化矽之方法,其包含以下步驟:a)提供沉澱或發煙氧化矽,其具有0.1至350微米之平均粒子尺寸d50,無超音波處理,b)使步驟a)之氧化矽濕化至30-80重量%之乾燥損失,c)藉由擠出、粒化、壓實或製錠使步驟b)之氧化矽成形,d)在乾燥單元中乾燥該氧化矽成形體,e)以3000微米之篩尺寸篩選粒化或篩選該等顆粒且篩出具有400微米之篩網眼尺寸的細粒,f)使步驟e)之顆粒與表面改質劑反應,其中使用以下有機矽烷類之至少一種或該有機矽烷類之混合物作為改質劑 a)式(RO)3Si(CH2)m-R'之有機矽烷類,b)式(R")x(RO)(3-x)Si(CH2)m-R'之有機矽烷類,c)式X3Si(CH2)m-R'之鹵有機矽烷類,d)式(R")xX(3-x)Si(CH2)m-R'之鹵有機矽烷類,e)式(RO)3Si(CH2)m-OOC(CH3)C=CH2之有機矽烷類,f)式X3Si(CH2)m-OOC(CH3)C=CH2之鹵有機矽烷類,g)式Xx((R")(3-x)Si(CH2)m-OOC(CH3)C=CH2之有機矽烷類,或h)式(R")x(RO)(3-x)Si(CH2)m-OOC(CH3)C=CH2之有機矽烷類,其中R=烷基,較佳是甲基、乙基或丙基,R'=-NH-CH2-CH2-NH2、-N-(CH2-CH2-NH2)2、-NH-CO-N-CO-(CH2)5、-NH-COO-CH3、-NH-COO-CH2-CH3、-NH-(CH2)3Si(OR)3、-NH-(CH2)3-CH3或-NH-CH2-CH2-NH-CH2-CH2-NH2,R"=烷基、環烷基,X=Cl或Br,x=1或2, m=0、1-20。
- 如申請專利範圍第6項之方法,其中使用具有30-80重量%之乾燥損失的含水濾餅作為步驟a)之原料。
- 如申請專利範圍第6項之方法,其中在步驟c)中之氧化矽在高速強化混合器中被壓實且粒化。
- 一種製造如申請專利範圍第1至5項之粒狀官能基化氧化矽的方法,其包含以下步驟:i)提供沉澱或發煙氧化矽,其具有<30重量%之乾燥損失,且具有0.1至350微米之平均粒子尺寸d50,無超音波處理,ii)藉由乾壓實,較佳在二個轉動的滾筒之間,以每公分滾筒寬0.5千牛頓至每公分滾筒寬12千牛頓的特定接觸壓力,使步驟i)之氧化矽成形以得塊體,iii)以3000微米之篩尺寸篩選粒化或篩選該塊體且篩出具有400微米之篩網眼尺寸的細粒,且iv)使步驟iii)之顆粒與表面改質劑反應,其中使用以下有機矽烷類之至少一種或該有機矽烷類之混合物作為改質劑a)式(RO)3Si(CH2)m-R'之有機矽烷類,b)式(R")x(RO)(3-x)Si(CH2)m-R'之有機矽烷類,c)式X3Si(CH2)m-R'之鹵有機矽烷類,d)式(R")xX(3-x)Si(CH2)m-R'之鹵有機矽烷類, e)式(RO)3Si(CH2)m-OOC(CH3)C=CH2之有機矽烷類,f)式X3Si(CH2)m-OOC(CH3)C=CH2之鹵有機矽烷類,g)式Xx((R")(3-x)Si(CH2)m-OOC(CH3)C=CH2之有機矽烷類,或h)式(R")x(RO)(3-x)Si(CH2)m-OOC(CH3)C=CH2之有機矽烷類,其中R=烷基,較佳是甲基、乙基或丙基,R'=-NH-CH2-CH2-NH2、-N-(CH2-CH2-NH2)2、-NH-CO-N-CO-(CH2)5、-NH-COO-CH3、-NH-COO-CH2-CH3、-NH-(CH2)3Si(OR)3、-NH-(CH2)3-CH3或-NH-CH2-CH2-NH-CH2-CH2-NH2,R"=烷基、環烷基,X=Cl或Br,x=1或2,m=0、1-20。
- 如申請專利範圍第6至9項中任一項之方法,其中所有小於400微米之篩部份被移除。
- 如申請專利範圍第6及9項中任一項之方法,其中成形步驟c)或ii)係在不添加黏合劑之情況下進行。
- 如申請專利範圍第6及9項中任一項之方法,其 中在步驟f)或iv)中所用之改質劑是至少一種有機矽烷。
- 一種如申請專利範圍第1至5項中任一項之粒狀氧化矽於製造調合物之用途。
- 一種調合物,其包含如申請專利範圍第1至5項中任一項之至少一種粒狀氧化矽及添加劑。
- 如申請專利範圍第14項之調合物,其中所用之添加劑是至少一種催化活性物質。
- 如申請專利範圍第14及15項中任一項之調合物,其中該調合物含有比例在1至70重量%之間的添加劑。
- 如申請專利範圍第14項之調合物,其中所用之添加劑包含硬化劑或起始劑、交聯劑、觸媒、活性醫藥成份及賦形劑、活性化妝成份及賦形劑、清潔及/或照護組成物、調味、香氣及香味劑、動物飼料或動物飼料添加劑、維生素、礦物質、食品或食品添加劑、染料及/或顏料、胺基酸、氧化或漂白劑、具有微生物作用之添加劑、農業及林業用化學品及/或混凝土摻合物。
- 如申請專利範圍第17項之調合物,其中該添加劑是酵素。
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PT2867310T (pt) | 2018-06-06 |
CA2878095A1 (en) | 2014-01-03 |
EP2867310B1 (de) | 2018-04-18 |
CA2878095C (en) | 2020-03-31 |
BR112014032729B1 (pt) | 2021-06-29 |
MY194070A (en) | 2022-11-10 |
EP2867310A1 (de) | 2015-05-06 |
US11458454B2 (en) | 2022-10-04 |
JP2015527285A (ja) | 2015-09-17 |
CN104508054B (zh) | 2016-08-31 |
TW201418269A (zh) | 2014-05-16 |
BR112014032729A2 (pt) | 2017-06-27 |
US20160082415A1 (en) | 2016-03-24 |
TR201807287T4 (tr) | 2018-06-21 |
HUE038697T2 (hu) | 2018-11-28 |
PL2867310T3 (pl) | 2018-09-28 |
KR102023556B1 (ko) | 2019-09-23 |
CN104508054A (zh) | 2015-04-08 |
ES2671268T3 (es) | 2018-06-05 |
DE102012211121A1 (de) | 2014-01-02 |
KR20150032724A (ko) | 2015-03-27 |
WO2014001088A1 (de) | 2014-01-03 |
MX2015000130A (es) | 2015-05-07 |
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