CN104508054A - 粒状功能化二氧化硅、其制备方法及用途 - Google Patents
粒状功能化二氧化硅、其制备方法及用途 Download PDFInfo
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- CN104508054A CN104508054A CN201380040161.7A CN201380040161A CN104508054A CN 104508054 A CN104508054 A CN 104508054A CN 201380040161 A CN201380040161 A CN 201380040161A CN 104508054 A CN104508054 A CN 104508054A
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- Prior art keywords
- dioxide
- silicon
- additive
- ooc
- organosilane
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Abstract
本发明涉及粒状功能化二氧化硅,其中-Hg孔体积(<4μm)大于0.80ml/g,-dQ3=10%值大于400μm,-dQ3=90%值小于3000μm,-未经超声处理的d50值与经过3分钟超声处理的d50值之比<4.00,并且-碳含量是1.0-15.0重量%。本发明的粒状功能化二氧化硅可用作载体材料,特别是作为酶的载体。
Description
本发明涉及粒状功能化二氧化硅、其制备方法及其用途。
在许多应用领域,例如在农作物保护制品领域、在为活性药物成分的情况下、在制备动物饲料和动物饲料添加剂时或者在食品业,使用载体材料将例如液体或树脂状活性成分转变成自由流动和贮藏稳定的形式。例如WO 2011/117100中所述。
对载体材料的明显需求是其足够高的吸收性能,从而需要使用的载体材料尽可能地少。因此一系列公开,例如DE 102006002765,涉及强化被吸收在载体材料上的材料的含量的工艺。然而,这些工艺非常复杂,并且它们迄今未被以工业规模建立。
对载体材料的另一需求是被吸收的物质具有良好的自由流动性并且因此加工性能良好。此外,在运输、分散和制备被吸收的物质的过程中二氧化硅应具有最小量的粉尘。为了改善自由流动性,EP 0984772 A1和EP 0966207 A1,例如,因此提出使用接近球状并且平均粒径大于150μm的微粒二氧化硅作为载体材料。以这种方式获得的被吸收的物质的确改善了自由流动性,但是该二氧化硅的加工性能不是最佳的。
在固定床催化领域,对载体或载体材料还有其它需求。例如,必需保证固定床反应器中的反应使得反应室中的压降最小化,其中反应物流过反应室,反应室填充负载有催化剂的载体材料的。在其中负载有催化剂的载体材料悬浮在反应介质中的反应的情况下,在反应结束时载体材料必需容易再次除去。最后,流化床反应器中的反应要求被负载的载体材料能够在其中有效地流化。因此显然地,不同的反应器类型对被负载的载体的需求有很大不同并因此也对载体材料的需求也不同。为了满足这些需求,WO2011/117100记载了这样的粒状二氧化硅:Hg孔体积(<4μm)大于0.90ml/g、dQ3=10%大于400μm,同时dQ3=90%小于3000μm并且未经超声暴露的d50与经过3分钟超声暴露的d50之比<4.00,该测定是对400-500μm的颗粒部分进行的。然而,这些二氧化硅的缺点是一些催化活性成分,例如酶或生物催化剂,仅仅不充分地粘附在二氧化硅表面并且很快再次解吸。
EP 1357156 A2公开了硅烷改性的氧化或硅酸盐填料,其中小于75μm的珠粒小于15重量%并且中值粒径为130-500μm。
而且,US 20060084746公开了选自如下的疏水无机氧化物:无定型沉淀二氧化硅、氧化铝和这些无机氧化物的混合物,其中羟基含量是2-15OH/nm2、碳含量0.1-6重量%、甲醇可润湿性15-45%和M1标准白面积小于0.4%。
本发明的目的是提供解吸特性得到改善的二氧化硅,例如酶。
本发明提供了一种粒状功能化二氧化硅,其特征在于:
-Hg孔体积(<4μm)大于0.80ml/g,优选大于0.85ml/g,更优选大于0.90ml/g,甚至更优选大于0.95ml/g,尤其优选大于1.00ml/g,
-dQ3=10%大于400μm,
-dQ3=90%小于3000μm,
-未经超声暴露的d50与经过3分钟超声暴露的d50之比小于4.00,优选小于3.00,更优选小于2.60,甚至更优选小于2.10,尤其优选小于1.60,该测定是对400-500μm的颗粒部分进行的,和
-碳含量是1.0-15.0重量%,优选2.0-14.0重量%,更优选3.0-12.0重量%。
本发明的粒状功能化二氧化硅可以具有5.0-11.0的pH。
足够高的孔隙率保证了本发明的粒状功能化二氧化硅有足够的在中间孔和/或大孔范围内的孔体积,并因此酶对反应物具有良好的可达性,同时,制备本发明的配制物需要最小量的载体材料。
更优选的本发明的粒状功能化二氧化硅的Hg孔体积(<4μm)为0.81-1.50ml/g,更优选0.81ml/g-1.40ml/g,最优选0.81ml/g-1.30ml/g。
本发明的粒状功能化二氧化硅的另一重要性能是其硬度。如果孔隙率高的话,机械性能可能不再得到保证,可能导致在施加于二氧化硅的机械应力下及施加于由二氧化硅制得的配制物的机械应力下,形成的细料增加。在二氧化硅的包装和运输过程中、在配制物的制备过程中、以及在被负载的载体材料的使用过程中的机械应力,通过超声波对悬浮在水中的二氧化硅作用3分钟来模拟。未经超声暴露的d50与经过3分钟超声暴露的d50之比给出通过机械应力将d50降低多少的信息。二氧化硅越硬,超声暴露之后的d50U与未经超声暴露的d50之差越小,即,在理想情况下,未经超声暴露的d50与超声暴露3分钟之后的d50U之比应为1.00。
本发明的粒状功能化二氧化硅尽管其平均粒径高,但是其硬度非常好。
未经超声暴露的d50U与超声暴露3分钟之后的d50之比可以优选是1.00-3.00,更优选1.00-2.60,甚至更优选1.00-2.10,尤其优选1.00-1.60。该测定是对400μm–500μm的颗粒部分进行的。
以dQ3=10%和dQ3=90%表征的粒径分布对保证固定床反应器中良好的流动性是重要的或者对保证流化床反应器中良好的流动性能是重要的。特大颗粒没有足够的比表面积用于反应、溶解和扩散。特小颗粒依次增加流动阻力。本发明的粒状功能化二氧化硅因此dQ3=10%>400μm和dQ3=90%<3000μm。
本发明的粒状功能化二氧化硅因此碳含量可以优选为1.0-9.0,优选1.0-7.5,更优选2.0-7.5。
本发明的粒状功能化二氧化硅可以具有如下官能团:
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、环烷基,
x=1或2。
官能团可以经Si-O-Si键与二氧化硅相连:
(-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]。
粒状功能化二氧化硅可以是热解或沉淀二氧化硅。
本发明还提供了制备本发明粒状二氧化硅的第一种方法,包括以下步骤:
a)提供沉淀或热解二氧化硅,所述沉淀或热解二氧化硅未经超声处理时的平均粒径d50为0.1-350μm,优选BET表面积为30-800m2/g,优选DBP数为140-400g/100g,
b)将得自步骤a)的二氧化硅润湿至干燥失重为30-80重量%,
c)通过挤出、造粒、压实(compaction)或压片(tabletting),使得自步骤b)的二氧化硅成型,
d)将所述成型的二氧化硅体在干燥单元中干燥,
e)以3000μm的筛号筛选造粒或筛选所述颗粒,并用筛号为400μm的筛网筛除细料,和
f)将得自步骤e)的颗粒与表面改性剂反应。
可以将得自步骤a)的沉淀或热解二氧化硅干燥和任选研磨。
替换本发明的上述第一种方法,也可以使用干燥失重为30-80重量%的含水滤饼作为步骤a)的原料。
本发明还提供了制备本发明粒状二氧化硅的第二种方法,包括以下步骤:
i)提供沉淀或热解二氧化硅,所述沉淀或热解二氧化硅的干燥失重<30重量%和未经超声处理时的平均粒径d50为0.1-350μm,优选BET表面积为30-800m2/g,优选DBP数为140-400g/100g;
ii)通过干压实使得自步骤i)的二氧化硅成型,从而得到块料(slugs),优选在两个转辊之间,以0.5kN/cm辊宽-12kN/cm辊宽的比接触压力(specific contact pressure)来进行所述干压实,
iii)以3000μm的筛号筛选造粒或筛选所述块料,并用筛号为400μm的筛网筛除细料,和
iv)使得自步骤iii)的颗粒与表面改性剂反应。
可以将得自步骤i)的沉淀或热解二氧化硅干燥和任选研磨。
在上面所述的本发明所有方法中,通过使颗粒经过用升温,例如70℃-400℃的水蒸气处理可以进一步提高颗粒的硬度。之后,可能需要进一步的干燥步骤。
此外,也可以通过使颗粒与碱性物质接触一段时间以提高颗粒的pH,从而提高颗粒的硬度。该方法记载在DE 102008035867 A1。
此外,通过将得自工艺步骤e)或iii)的颗粒在升温下,优选700℃-1200℃,煅烧一段时间,优选<1h,可以提高颗粒的硬度。
上述硬化颗粒的工艺步骤可以在筛选造粒和筛选工艺步骤之前或之后进行。
本发明第一种方法中的润湿工艺步骤(b)和/或造粒工艺步骤(c)可以在高速强力混合机、捏合机、压实机、盘式造粒机和/或穿孔模压机等中进行。另外,润湿之后可以进行挤出,或者可以直接将含水滤饼挤压。接着可以通过其它合适的方法(例如得自Caleva的spheronizer)改变挤出成型体的几何形状。
本发明第一种方法中的干燥工艺步骤(d)例如可以在干燥箱、流化床干燥器、带式干燥器等中进行。如果需要的话,该干燥成型体接着通过进一步加工,例如以3000μm的筛号筛选或筛选造粒,并用筛号为400μm的筛网筛除细料,可以调整至适当的粒径部分。
本发明第二种方法的成型步骤(ii)优选在压实机中进行,例如在得自Hosokawa Bepex GmbH的设备中,例如Bepex L200/50或AlexanderwerkAG。
本发明两种方法中的筛选造粒(e或iii)可以优选在例如得自Frewitt或Hosokawa Bepex GmbH的筛选磨碎机的设备中进行。筛选可以通过使用所有的已知技术进行,优选通过例如得自公司Vibra、Engelsmann或Allgeier的振动筛选设备。可以进行几次筛选或几个筛选步骤。
步骤f)或iv)中颗粒的反应可以通过任选首先用水对二氧化硅喷雾然后用表面活性剂对二氧化硅喷雾来进行。使用的水可以用酸例如盐酸酸化,使得pH降至7-1,或者使用的水可以用碱碱化使得pH升高至7-14。如果使用许多表面改性剂,它们可以一起施加,也可以分开、连续或者作为混合物。可以将一种或多种表面改性剂在合适溶剂中溶解。喷雾结束之后可以再混合5-30min。
然后,混合物可以在20-400℃的温度下热处理0.1-6h。热处理可以在保护气,例如氮气下进行。热处理也可以在不同温度下分多个阶段进行。
施加表面改性剂和热处理可以在合适的单元中进行或者可以在不同的合适的单元中分开进行。
表面改性剂的施加可以用一相、两相或超声喷嘴进行。
表面改性可以在带有喷雾设备的可加热混合器和干燥器中连续或批次进行。合适的设备例如可以是犁铧(ploughshare)混合器、盘式干燥器、流化床干燥器或移动床干燥器。
使用的表面改性剂可以是有机硅烷类,例如
a)式(RO)3Si(CH2)m-R’的有机硅烷,其中
R=烷基,优选甲基、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’的有机硅烷,其中
R、R’和m各自如上面定义的,并且
R”=烷基、环烷基,
x=1或2,
c)式X3Si(CH2)m-R’的卤代有机硅烷,其中
R’和m各自如上面定义的,并且
X=Cl或Br,
d)式(R”)xX(3-x)Si(CH2)m-R’的卤代有机硅烷,其中R’、R”、X、x和m各自如上面定义的,
e)式(RO)3Si(CH2)m-O(O)C(CH3)C=CH2的有机硅烷,其中R和m各自如上面定义的,
f)式X3Si(CH2)m-O(O)C(CH3)C=CH2的卤代有机硅烷,其中X和m各自如上面定义的,
g)式Xx(R”)(3-x)Si(CH2)m-O(O)C(CH3)C=CH2的有机硅烷,其中X、R”、x和m各自如上面定义的,
h)式(R”)x(RO)(3-x)Si(CH2)m-O(O)C(CH3)C=CH2的有机硅烷,其中R、R”、x和m各自如上面定义的,
和这些表面改性剂的混合物。
优选使用的表面改性剂可以是氨基丙基三乙氧基硅烷、氨基丙基三甲氧基硅烷、N-(2-氨基乙基)-3-氨基丙基甲基二甲氧基硅烷、3-氨基丙基甲基二乙氧基硅烷或3-甲基丙烯酰氧基丙基三甲氧基硅烷。更优选地,使用的表面改性剂可以是氨基丙基三乙氧基硅烷、氨基丙基三甲氧基硅烷或3-甲基丙烯酰氧基丙基三甲氧基硅烷。
就载体或支持体应用而言,市场上大量二氧化硅可用于本发明方法中。其实例有得自Evonik Industries的二氧化硅50、50S、500LS、22、22S、22LS和33。这些二氧化硅–即使专门开发用于载体或支持体–它们自身也不适合或者仅仅不完全适合作为载体或支持体材料。其原因–特别是当为喷雾干燥、喷嘴塔式干燥和/或研磨颗粒的情况下–是其粒径过低,如上面所述范围内的粒径会导致反应器中不希望的压力上升,并且缺少化学或物理连接用的官能团。通过本发明的工艺,这些二氧化硅经过压实,通过本发明的方法控制由此获得的颗粒的粒径和强度,从而获得最佳粒径分布和硬度的颗粒,其在反应器中具有低的流动阻力,或者可以容易地从悬浮体中过滤掉。
除了已经提及的二氧化硅之外,在本发明第一种方法的步骤a)中,例如可以使用得自Evonik Industries的二氧化硅2200、200,得自Rhodia Chimie的38A至X,得自PPG的SC60和SC 72,得自Huber的5170,以及欧洲专利EP 0984772 A1、EP 0966207 A1和EP 0937755 A1中公开的二氧化硅。
本发明方法中使用的二氧化硅可以具有
1.在未经超声处理时平均粒径d50为0.1-350μm,优选0.1-200μm,更优选0.1-150μm,最优选1-50μm,
2.BET表面积为30-800m2/g,优选40-700m2/g,更优选50-600m2/g,最优选150-550m2/g,
3.DBP数为140-400g/(100g),优选140-350g/(100g),更优选190-350g/(100g),最优选290-350g/(100g)。
本发明的第一种方法优选在混合器、捏合机或压实机(任选带有下游挤出机)和下游干燥器、筛选造粒机和筛选机中进行。例如,最初带电的二氧化硅首先可以用液体润湿,例如在得自Eirich GmbH的设备中(除非直接使用滤饼),然后压缩(compressed)或压实,然后挤出并干燥。液体润湿过并压缩或压实过的二氧化硅同样可以被干燥,然后可以进行筛选造粒,然后可以筛选至所需颗粒部分。
最终载体或支持体颗粒的硬度可以通过原料二氧化硅的压缩或压实控制。压实通常可以通过添加水同时引入剪切能来进行。此外,也可以添加水溶液例如纤维素溶液或油,它们适合起颗粒之间的粘合剂的作用。基于密度1.00g/ml,液体可以优选以50-90重量%的比例,更优选以60-90重量%的比例,最优选以65-90重量%的比例添加。此外,在压实期间,可以加入适合起颗粒之间的粘合剂的作用的固体,例如纤维素、蜡或聚合物、或者随后聚合的单体。该固体可以0.1-50重量%的比例添加,优选以0.5-15重量%的比例,更优选以0.5和8重量%的比例。
在一个优选实施方式中,载体或支持体材料可以在不添加粘合剂的情况下经过压缩或压实(步骤c)或ii))。
压实可以优选在10℃-90℃的温度下进行,更优选10℃-70℃。
本明第一种方法中的成型可以优选通过以下方式进行:在混合单元中借助于添加的液体强烈压实原料二氧化硅,直到液体部分排出,并开始颗粒的造粒。由此获得的颗粒(原料颗粒)的粒径可以通过挤出步骤均质化,然后将它们干燥。此外,该湿原料颗粒,不经过挤出步骤,也可以直接干燥,并且例如,通过特征尺寸为3000μm的筛,它将大于该特征尺寸的颗粒研磨。该过程优选在例如得自Frewitt或Hosokawa Bepex GmbH的筛选磨碎机的设备中进行。当将本发明的支持体材料用于悬浮催化领域时,大于通过的筛的特征尺寸的颗粒,可能导致配制物发生不希望的沉淀并使得扩散或反应时间延长。当除去小于400μm的所有筛选部分时也是有益的。如上所述,这些小颗粒对颗粒的流动阻力有副作用并引起固定床反应器中的压降。
筛选可以通过任意已知技术的装置进行,优选通过例如得自Vibra、Engelsmann或Allgeier公司的振动筛选装置进行。可以进行几次筛选或者几个筛选步骤。
在本发明的第二种方法中,二氧化硅的压实优选在具有下游筛选造粒机和筛选机的干燥压实机中进行。初始加入的二氧化硅可以在例如得自Hosokawa Bepex GmbH的设备例如Bepex L200/50或得自AlexanderwerkAG的设备中压实,并且压实的材料可以经过筛选-造粒并且分选至所需颗粒部分。
在本发明第二种方法的步骤ii)中,将干燥原料二氧化硅压实,即压实成块料,它们具有为本发明应用最优化的粒径和硬度。硬度可以通过压实原料二氧化硅时的压力控制。压实优选在0.5-15kN/cm辊宽,更优选3-12kN/cm辊宽,最优选6-10kN/cm辊宽的比接触压力下,并在10℃-90℃,更优选10℃-70℃的温度下进行。此外,在压实期间,可以加入液体,优选水、水溶液如纤维素溶液、或油,它们适合起颗粒之间的粘合剂的作用。该液体可以优选以1-30重量%的比例添加,更优选以1-20重量%的比例,最优选以3-15重量%的比例。此外,在压实期间,可以添加适合起颗粒之间的粘合剂作用的固体,例如纤维素、蜡或聚合物、或者随后聚合的单体。该固体的添加比例为0.1-50重量%,优选0.5-15重量%,更优选0.5-8重量%。
该干燥压实可以优选这样进行:干燥的原料二氧化硅在压实单元中于两个转辊之间进行压制(pressed),至少一个辊更优选具有凹进部分例如槽、凹坑或衬垫,其特征尺寸大于待获得的颗粒的尺寸。辊可以是直构型或凹构型。一个更优选的实施方式在于使用至少一种有孔锯齿轮碾机(perforated toothed wheel roller)。此外,可以优选将至少一个辊设计成在辊表面可以产生减压,由此将待压实的二氧化硅吸在辊上。二氧化硅可以通过本领域技术人员已知的任意运输装置供应到压实装置,例如通过运输螺杆、双螺杆等。
压实之后,将所得块料通过特征尺寸为3000μm的筛,在该过程中将大于该特征尺寸的颗粒研磨。该过程优选在例如得自Frewitt或HosokawaBepex GmbH的筛选磨碎机的设备中进行。当将本发明的支持体材料用于悬浮催化领域时,大于通过的该筛的特征尺寸的颗粒,会导致配制物发生不希望的沉积并导致扩散或反应时间延长。此外,将小于400μm的筛选部分除去。如上所述,这些小颗粒对颗粒床的流动阻力有副作用并引起固定床反应器的压降。
对最终的干燥颗粒可能进行的蒸汽处理可以在适合该目的的所有设备中进行,它们例如有带式干燥器、旋转干燥器、干燥箱、流化床干燥器等。颗粒可以暴露于70℃–400℃,优选80℃–300℃,更优选90℃–200℃,最优选106℃–180℃的温度下。该温度下的停留时间可以不超过16h,优选不超过12h,更优选不超过8h,最优选不超过4h。
可能对颗粒进行的煅烧可以在不同设备中进行,例如煅烧炉、带或旋转管煅烧器、或者闪蒸或流化床煅烧器。可以将颗粒暴露于700℃–1200℃,优选800℃–1200℃,更优选800℃–1100℃的温度下。停留时间取决于煅烧温度和所需的颗粒硬度。该过程的停留时间可以是1h,优选20min,更优选小于10min。
本发明还提供了本发明的粒状功能化二氧化硅作为支持体材料,优选酶的载体材料的用途。
最后,本发明提供了一种包含至少一种本发明的粒状功能化二氧化硅和添加剂的配制物。
配制物的添加剂可以与本发明的粒状功能化二氧化硅物理或化学地相连。
本发明的粒状功能化二氧化硅可用于制备配制物,所述添加剂优选是硬化剂或引发剂、交联剂、催化剂、活性药物成分和赋形剂、活性化妆成分和赋形剂、清洁和/或护理组合物、调味剂(flavourings)、芳香剂(aromas)和香味剂(fragrances)、动物饲料或动物饲料添加剂,例如氨基酸、维生素、矿物质、食品或食品添加剂、染料和/或颜料、氨基酸、氧化剂或漂白剂、具有杀微生物,特别是杀真菌或杀细菌作用的添加剂,农业和林业用化学品,和/或混凝土外加剂(concrete admixture)。所述添加剂可以是含水或无水液体,例如油、树脂、溶液、分散体、悬浮体、乳液、蜡、聚合物或熔融物。所述添加剂随后可以经过加热处理、热处理、或者诱导从而结晶、固化、分离或反应。此外,添加剂可以预先或随后干燥。
动物饲料和动物饲料添加剂部分的添加剂包括,例如,维生素、矿物质、羧酸、无机酸、氨基酸、脂肪、油和芳香剂。这些物质更优选是甲酸、乙酸、丙酸、乳酸、磷酸、氯化胆碱溶液、维生素E乙酸酯和植物提取物,例如万寿菊提取物。
农业和林业部分的添加剂包括,例如,被吸收的肥料,例如含硝酸盐-和/或磷酸盐-的肥料、农作物保护组合物、农药,例如除草剂、杀真菌剂或杀虫剂。
化妆品部分的添加剂包括,例如,油如香精油、香味油、护理油、芳香油和硅油、活性抗菌、抗病毒或杀真菌成分,消毒剂和抗微生物剂、除臭剂、抗氧化剂、生物活性物质和生物源活性成分、维生素和维生素复合物、酶和酶类系统如淀粉酶、纤维素酶、脂肪酶和蛋白酶、化妆活性物质如化妆成分和个人卫生产品、洗涤-和清洁-活性物质如各种表面活性剂、洗涤-和/或清洁-活性的无机酸和有机酸、防污和去污活性成分、氧化剂和漂白剂、漂白活化剂、增洁剂和辅助增洁剂、抗再沉积添加剂、发灰和褪色抑制剂、护色活性物质、洗衣护理物质和添加剂、荧光增白剂、泡沫抑制剂、pH调节剂和pH缓冲物。
食品和食品添加剂部分的添加剂包括,例如,被吸收的芳香剂、食品增补剂、维生素、矿物质和氨基酸。
活性药物成分的添加剂包括各种活性药物成分,例如α-蛋白酶抑配制物、阿巴卡韦、阿昔单抗、阿卡波糖、乙酰水杨酸、阿昔洛韦、腺苷、沙丁胺醇、阿地白介素、阿伦膦酸盐、阿夫唑嗪、阿洛司琼、阿普唑仑、阿替普酶、氨溴索、氨磷汀、胺碘酮、氨磺必利、氨氯地平、阿莫西林、苯丙胺、两性霉素、氨苄西林、安普那韦、阿那格雷、阿那曲唑、安克洛酶、抗血友病因子(antihaemophilic factor)、抑肽酶、阿替洛尔、阿托伐他汀、阿托品、氮卓斯汀、阿奇霉素、薁、巴尼地平、倍氯米松、贝那普利、苄丝肼、贝前列素、倍他米松、倍他洛尔、苯扎贝特、比卡鲁胺、没药醇、比索洛尔、肉毒杆菌毒素、溴莫尼定、溴西泮、溴隐亭、布地奈德、布比卡因、安非他酮、丁螺环酮、布托啡诺、卡麦角林、卡泊三烯(calcipotriene)、降钙素、骨化三醇、樟脑、坎地沙坦、坎地沙坦酯、卡托普利、卡马西平、卡比多巴、卡铂、卡维地洛、头孢克洛、头孢羟氨苄、头孢西丁(cefaxitin)、头孢唑林、头孢地尼、头孢吡肟、头孢克肟、头孢美唑、头孢哌酮、头孢替安、头孢唑兰(cefoxopran)、头孢泊肟、头孢丙烯、头孢他啶、头孢布烯、头孢曲松、头孢呋辛、塞来考昔、塞利洛尔、头孢氨苄、西立伐他汀、西替利嗪、氯霉素、西司他丁、西拉普利、西咪替丁、环丙贝特、环丙沙星、西沙必利、顺铂、西酞普兰、克拉霉素、克拉维酸、克林霉素、氯米帕明、氯硝西泮、可乐定、氯吡格雷、克霉唑、氯氮平、色甘酸、环磷酰胺、环孢素、环丙孕酮、达肝素、去铁胺、去氧孕烯、右苯丙胺、地西泮、双氯芬酸、去羟肌苷、洋地黄毒苷、地高辛、双氢麦角胺、地尔硫卓、白喉蛋白、白喉类毒素、丙戊酸、多巴酚丁胺、多西他赛、多拉司琼、多萘哌齐、链道酶-α、多佐胺、多沙唑嗪、去氧氟尿苷、多柔比星、地屈孕酮、依卡倍特、依法韦仑、依那普利、依诺肝素、乙哌立松、依匹斯汀、表柔比星、依替巴肽、促红细胞生成素-α、促红细胞生成素-β、依那西普、炔雌醇(ethynyloestradiol)、依托度酸、依托泊苷、因子VIII、泛昔洛韦、法莫替丁、法罗培南、非洛地平、非诺贝特、非诺多泮、芬太尼、非索非那定、非格司亭、非那雄胺、氟氧头孢、氟康唑、氟达拉滨、氟尼缩松、氟硝西泮、氟西汀、氟他胺、氟替卡松、氟伐他汀、氟伏沙明、促滤泡素-α、促滤泡素-β、福莫特罗、福辛普利、呋塞米、加巴喷丁、钆双胺、更昔洛韦、加替沙星、吉西他滨、孕二烯酮、格拉默、格列本脲、格列美脲、格列吡嗪、格列本脲、戈舍瑞林、格拉司琼、灰黄霉素、乙肝抗原、透明质酸、hycosin、氢氯噻嗪、氢可酮、氢化可的松、氢吗啡酮、羟氯喹、海兰G-F 20、布洛芬、异环磷酰胺、咪达普利、伊米苷酶、亚胺培南、免疫球蛋白、茚地那韦、吲哚美辛、英利昔单抗、胰岛素、人胰岛素、赖脯胰岛素、门冬胰岛素(insulin aspart)、干扰素-β、干扰素-α、碘-125、碘克沙醇、碘海醇、碘美普尔、碘普胺、碘佛醇、羟脯氨酸(ioxoprolene)、异丙托铵、依普黄酮、厄贝沙坦、伊立替康、异山梨醇、异维A酸、伊拉地平、伊曲康唑、氯胺丁钾(potassiumchlorazepate)、氯化钾、酮咯酸、酮替芬、百日咳菌苗、凝血因子IX、拉米夫定、拉莫三嗪、兰索拉唑、拉坦前列素、来氟米特、来格司亭、来曲唑、亮丙瑞林、左旋多巴、左氧氟沙星、左炔诺孕酮、左甲状腺素、利多卡因、利奈唑胺(linezolide)、赖诺普利、碘帕醇(lopamidol)、氯碳头孢、氯雷他定、劳拉西泮、氯沙坦、洛伐他汀、赖氨酸乙酰水杨酸、马尼地平、甲钴胺、甲羟孕酮、甲地孕酮、美洛昔康、四烯甲萘醌、流脑菌苗、促生育素、美罗培南、美沙拉嗪、美他沙酮、二甲双胍、哌甲酯、甲泼尼龙、美托洛尔、咪达唑仑、米力农、米诺环素、米氮平、米索前列醇、米托蒽醌、吗氯贝胺、莫达非尼、莫米松、孟鲁司特、吗尼氟酯、吗啡、莫昔沙星、麦考酚酯、萘丁美酮、纳屈肝素、萘普生、那拉曲坦、奈法唑酮、奈非那韦、奈韦拉平、烟酸、尼卡地平、尼麦角林、硝苯地平、尼鲁米特、尼伐地平、尼莫地平、硝酸甘油、尼扎替丁、炔诺酮、诺氟沙星、奥曲肽、奥氮平、奥美拉唑、昂丹司琼、奥利司他、奥司他韦、雌二醇、雌激素、奥沙利铂、奥沙普秦、奥索利酸、奥昔布宁、紫杉醇、帕利珠单抗、帕米膦酸二钠、胰脂肪酶、帕尼培南、泮托拉唑、对乙酰氨基酚、帕罗西汀、己酮可可碱、培高利特、苯妥英、吡格列酮、哌拉西林、吡罗昔康、普拉克索、普伐他汀、哌唑嗪、普罗布考、黄体酮、普罗帕酮、丙泊酚、丙氧芬、前列腺素、喹硫平、喹那普利、雷贝拉唑、雷洛昔芬、雷米普利、雷尼替丁、瑞格列奈、利血平、利巴韦林、利鲁唑、利培酮、利托那韦、利妥昔单抗、利斯的明、利扎曲普坦、罗非昔布、罗匹尼罗、罗格列酮、沙美特罗、沙奎那韦、沙格司亭、舍雷肽酶、舍曲林、司维拉姆、西布曲明、西地那非、辛伐他汀、生长激素、索他洛尔、螺内酯、司他夫定、舒巴坦、磺胺乙二唑、磺胺甲噁唑、柳氮磺吡啶、舒必利、舒马普坦、他克莫司、他莫昔芬、坦洛新、三唑巴坦、替考拉宁、替莫普利、替莫唑胺、替奈普酶、替诺昔康、替普瑞酮、特拉唑嗪、特比萘芬、特布他林、破伤风类毒素、丁苯那嗪、四氢西泮(tetrazapam)、麝香草酚、噻加宾、替勃龙、替卡西林、噻氯匹定、噻吗洛尔、替罗非班、替扎尼定、妥布霉素、维生素E烟酸酯、托特罗定、托吡酯、托泊替康、托拉塞米、曲马多、群多普利、曲司珠单抗、曲安西龙、三唑仑、曲美布汀、甲氧苄氨嘧啶、曲格列酮、托烷司琼、妥洛特罗、乌诺前列酮、尿促卵泡素、伐昔洛韦、丙戊酸、缬沙坦、万古霉素、文拉法辛、维拉帕米、维替泊芬、氨己烯酸、长春瑞滨、长春西丁、伏格列波糖、华法林、扎鲁司特、扎来普隆、扎那米韦、齐多夫定、佐米曲普坦、唑吡坦、佐匹克隆及它们的衍生物。但是,活性药物成分还应理解为意指其它物质,例如,维生素、维生素原、必需的脂肪酸、植物和动物来源的提取物、植物和动物来源的油、植物药剂制剂和顺势疗法制剂。
配制物中的本发明的粒状功能化二氧化硅尤其可以用作如下动物饲料添加剂的载体,例如甲酸、丙酸、乳酸、磷酸、氯化胆碱溶液、维生素E乙酸酯或植物提取物,例如万寿菊提取物。
此外,配制物中的本发明的粒状功能化二氧化硅可以用作如下化学品的载体材料:三聚氰胺树脂、橡胶添加剂、塑料添加剂、建筑化学品添加剂或油漆添加剂。
配制物中本发明的粒状功能化二氧化硅最优选用作各种催化剂的载体材料。催化剂尤其可以优选为酶或不同酶的组合,例如下面分类的酶:氧化还原酶、转移酶、水解酶、脂肪酶、溶菌酶(lysases)、异构酶和连接酶(按照生物化学和分子生物学的国际联合会的分类目录委员会(Nomenclature Committee of the International Union of Biochemistry andMolecular Biology))的EC(酶委员会)数)。例如通过再组合技术制得的酶变体同样也包括在术语“酶”中。
为了制得配制物,将本发明的粒状功能化二氧化硅与至少一种添加剂接触,使得所述添加剂可以渗透到二氧化硅的孔中。为此,可以使用本领域技术人员已知的各种技术,例如喷涂、滴涂、浸润(saturation)、浸渍、喷雾等。本发明的粒状功能化二氧化硅优选最初加到固体混合单元中,例如捏合机、桨式干燥机、转鼓混合器、立式混合器、桨式混合器、Schugi混合器、水泥混合器、Gericke连续混合器、Eirich混合器和/或筒式(silo)混合器。混合单元中的温度,取决于待吸收的物质的性质和组成,可以优选为5-90℃,更优选10-70℃。混合器内的压力可以优选0.1bar-2bar,更优选0.5bar-1.2bar。
配制物中所有添加剂的含量可以为1-70重量%,优选5-65重量%,更优选5-60重量%,最优选5-20重量%。
本发明的配制物尤其优选用作固定床反应器中的催化剂、多相催化领域中的催化剂、流化床反应器中的催化剂和悬浮反应的催化剂。
所用原料和本发明的粒状二氧化硅的物理化学数据通过以下方法测定:
BET表面积的测定
二氧化硅的比氮表面积(specific nitrogen surface area,下面称之为BET表面积)是按照ISO 9277以多点表面积测定的。所用的测量仪器是得自Micromeritics的the TriStar 3000表面积测量仪。BET表面积通常是在液氮饱和蒸汽压的0.05–0.20的分压范围内测定的。样品是通过在得自Micromeritics的the VacPrep 061加热站中于160℃、真空下加热样品1小时制得的。
DBP吸收值的测定
DBP吸收值(DBP数),是二氧化硅吸收率的量度,是基于标准DIN53601如下测定。
将12.50g的水分含量3-10%的二氧化硅(如果需要的话,通过在干燥箱中于105℃干燥来调整水分含量)加入到得自Brabender的C吸收计的捏合室中。在C吸收计上的测量是在PC的支持下如下进行的:使用软件BRABENDER自动油吸收体系1.1.2版,并且利用测量的转矩曲线的固定阻尼。
当为滤饼的情况下,在使用之前,在干燥箱中于105℃将它们干燥至水分含量减至≤10%,并通过3mm筛,然后通过300μm筛。
在左手捏合机桨的圆周速度为125rpm时,使用形成C吸收计的部件的Titronic通用滴管(得自Schott),将邻苯二甲酸二丁酯于室温下以4ml/min的速度滴加至捏合室。C吸收计的控制软件将捏合机和DBP计量停止的断开点定义为转矩0.6Nm。
下式用于计算DBP吸收值[g/100g]:
其中
DBP:DBP吸收值[g/100g]
V:消耗的DBP[ml]
D:DBP密度[g/ml](1.047g/ml,20℃)
E:二氧化硅的初始重量[g]
K:根据湿度校正表的校正值[g/100g]
DBP吸收是对无水的干燥二氧化硅定义的。当使用未干燥的二氧化硅的情况下,计算DBP吸收时应考虑校正值K。该值可以用下面的校正表确定。
表:邻苯二甲酸二丁酯吸收(无水)的湿度校正表
实施例:
如果二氧化硅的水分含量是5.8%的话,将33g/100g的校正值K加到如上所述分析的值上作为DBP吸收值。二氧化硅的水分含量是通过本文后面所述的“水分含量的测定”方法测定的。
通过激光衍射测量粒径的样品的制备
使用激光衍射测定粉末状固体的粒径分布基于以下现象:颗粒根据其大小在所有方向以不同的强度图形散射或衍射来自单色激光束的光。被照射的颗粒的直径越小,单色激光束的散射或衍射角越大。
通过激光衍射测定粒径的样品制备:
由于一些样品颗粒的尺寸超过所用仪器的测量范围,并且未经超声暴露的d50与经过3分钟的超声暴露之后的d50U之比取决于原料粒径(较小的材料颗粒具有较高的所述尺寸比例),测量之前从样品中筛选出400μm–500μm的颗粒部分。该操作使得不同材料的稳定性能够可靠地比较从而获得物质特定稳定性的描述。筛选是用得自Haver&Boecker,59302Oelde的HAVER EML 200Digital Plus筛选机进行的,它配备有400μm和500μm筛。将5g原料施加在位于上面的500μm筛,并以1.0的振幅设置筛选2分钟。将400μm-500μm的颗粒部分用于进一步分析。
400μm-500μm颗粒部分对比较而言是重要的,如果这样的颗粒部分不是本发明载体或支持体材料的粒径分布的一部分,如下制得相应的筛选部分:借助得自Eweka GmbH,Heusenstamm的TG2S筛选造粒机将足量的原料以100次振动/min通过500μm筛,然后通过400μm筛筛选。该筛选是如上所述完成的。
未经超声暴露的d
50
测定
当为亲水二氧化硅的情况下,通过LS 230激光衍射系统(得自Beckman Coulter;测量范围0.04–2000μm)和液体模块(Small VolumeModule Plus,120ml,得自Beckman Coulter,具有集成超声指),借助0.05%m/m的去离子水中的二磷酸四钠作为分散液,制备样品进行分析(模块的冲洗等),并且当为水可润湿性不足的二氧化硅的情况下,用乙醇/水混合物(体积比1:1)作为分散液。
在开始分析之前,必需将激光衍射系统加热2小时。之后,用分散液将SVM模块冲洗3次。
应设定与颗粒分析相关的以下参数:
使用抹刀添加二氧化硅筛选部分(400–500μm)直到达到LS 230激光衍射仪给出“OK”信息所需的测量浓度。在没有超声暴露的情况下通过泵循环将二氧化硅悬浮体分散60秒钟之后,室温下进行分析。
由原料数据曲线,软件基于Fraunhofer模型(Fraunhofer.rfd文件)计算粒径分布和未经超声暴露的d50(中位值)。
以100%的振幅超声处理3分钟之后的d
50U
测定
借助于集成在SVM模块(Vibra Cell VCX 130超声处理器,得自Sonics,具有CV 181超声转换器和6mm超声尖头)中的超声指,以100%的振幅,同时在液体模块中进行泵循环,通过超声处理180秒钟将存在于LS 230激光衍射计中的二氧化硅悬浮体再次分散,并如上所述进行分析。
由原料数据曲线,软件基于Fraunhofer模型(Fraunhofer.rfd文件)计算粒径分布和经过3分钟超声暴露之后的d50U(中位值)。
通过动态图像评价来测定粒径
在动态图像评价中,将散装(bulk)材料流向下流入光源与照相机之间。测定颗粒的投影面积,用计算机程序进行数字化并转化成粒径。
dQ3=10%和dQ3=90%的测定
为了测量粒径,使用得自RETSCH Technology GmbH,Haan的CAMSIZER。借助于带有贮罐漏斗的DR 100-40计量通道将颗粒供应到测量仪器。为了进行图像评价,使用3.12d版的软件。
开始分析之前,让仪器加热2h。保证照明单元前面的玻璃保护和照相机没有灰尘。将漏斗与计量通道之间的距离调整至最大粒径的大约3倍。将计量通道直接放置在测量仪器的上方。将约150ml的样品加入到漏斗中。根据图1在分析任务文件(*.afg)中记录分析参数。
为了调节测量通道,根据图2将下面设置记录在软件中。
评价数字化图像时,由min(xc)值计算x值。根据图3不使用形状因子(form factors)。
在基本参数中测定dQ3=10%和dQ3=90%的输出(图4)。
不借助拟合文件(fitting files)进行分析数据的拟合。
水分含量的测定
按照ISO 787-2测定二氧化硅的水分含量。为此,将1-4g的样品在干燥箱中于(105±2)℃干燥2小时并根据ISO说明进行评价。该干燥失重主要由物理结合的水组成。
二氧化硅的pH的测定
以含水悬浮体在室温下测定二氧化硅的pH。预先用研钵和槌将粒状样品研磨或者将粒状样品碾碎。将95g的去离子水加入到5g的二氧化硅中。悬浮体通过磁性搅拌器搅拌5分钟。之后直接借助在预期测定范围内校正的pH计(Metrohm 780pH计),精确测量悬浮体的pH至一位小数点。
水银孔体积≤4μm的测定
该方法是按照DIN 66133基于水银侵入,使用得自Micromeritics的AutoPore IV 9520系统进行的。
该方法原理是基于测量注入多孔固体的水银体积作为施加的压力的函数。这仅仅包括水银在施加的压力下(最大414MPa)能够渗透的孔(Ritter和Drake法)。
非润湿性液体仅仅在压力下渗透到多孔系统内。消耗的压力与孔口的内径成反比。就圆柱形孔而言,孔半径rp与压力p之间的关系由Washburn等式给出:
rp:孔半径
p:压力
σ:表面张力(480mN/m*)
θ:水银的接触角(140°*)
*根据DIN 66133
水银孔体积≤4μm是根据直径从≤4μm到AutoPore IV 9520水银孔隙计(最大压力414MPa)的测定极限的所有孔的累积孔体积计算的。
以下实施例用于详细描述本发明,而非限制其范围。
碳含量的测定
通过LECO元素分析仪(型号:CS 244或CS 600)测定碳含量。将氧化物称重到陶瓷坩埚中,配备有燃烧添加剂并在感应炉中于氧气流下加热。这将存在的碳氧化为CO2。通过红外线检测仪将该气体量定量。在实际测定之前,用合适的参照材料进行仪器的校正。
步骤
将约50-150mg的样品材料准确称重至1mg,加入到陶瓷坩埚中。该样品材料用约1g的Lecocel II(钨-锡(10%)合金粉)和约0.7g的铁填料覆盖。接着,用盖盖住坩埚。诱导炉设置至最大功率并用氧气冲洗10s。将坩埚插入诱导炉之后,开始自动测定和评价。就每一样品而言,进行多次测定。结果以重量%记录。
该分析法的碳检测极限是300μg/g。
夯实密度的测定
按照DIN EN ISO 787-11测定夯实密度。
灼烧损失的测定
基于ISO 3262-1测定灼烧损失。与ISO 3262-1的差别在于
-代替白金皿或瓷皿,使用陶瓷坩埚(porcelain crucibles或fusioncrucibles)测,
-称重约0.5g(500mg)而不是约2g的待测二氧化硅,
-待测材料预先不经干燥;相反,通过基于ISO 787-2的干燥失重的单独测定进行湿度校正。
实施例
对比例1
在混合器(R02,得自Eirich)中,添加220ml水/100g二氧化硅,将得自Evonik Industries的50S混合和压实。室温下使用10升混合容器,其配备有销型(pin-type)搅拌器混合工具。为了获得混合器的最佳填充量,最初加入1kg的50S。以20m/s的搅拌器的圆周速度将水均匀加入1分钟。板总是以1档运行。之后,销型搅拌器在40m/s下运转。一旦形成所需聚集体尺寸就停止该步骤。所得颗粒在160℃在干燥箱中干燥至恒重,然后通过筛选分级至400–1250μm。为了测定,就单个实验,制得400–500μm的筛选部分;将其用于接下来的硬度和孔隙率测定。
实施例1和2
最初将得自对比例的颗粒加入到犁铧混合器中并通过双相喷嘴喷雾(载体气:氮气),同时与表面改性剂混合。喷雾接触之后再混合15分钟。
然后,该混合物在干燥箱中进行热处理(热处理)。
下表1列出了实施例1和2的制备的精确实验参数。
表1
*:SM=表面改性剂、
A=3-氨基丙基三乙氧基硅烷、
B=3-甲基丙烯酰氧基丙基三甲氧基硅烷
表2a和2b包含本发明表面改性的二氧化硅和对比二氧化硅的物理化学数据。
表2a
表2b
负载有硅油的支持体的解吸实验
1.配制物(被吸收的物质)的制备
将8g的DOW DC 20050cs硅油称重到烧杯中,加入10g的粒状二氧化硅(干燥失重<=6%),然后通过刮刀混合直到获得干且自由流动的被吸收的物质。由此获得的被吸收的物质于室温(23℃)下贮藏14天。
·对比配制物1:5g的对比例1+4g的DC20050cs硅油
·本发明配制物1:5g的实施例1+4g的DC20050cs硅油
·本发明配制物2:5g的实施例2+4g的DC20050cs硅油
2.解吸倾向的测定
通过将10g的Triton X160溶解在490g的去离子水中制得表面活性剂溶液。
·在50ml离心管中填充20ml的表面活性剂溶液,并加入9g的实验1中记载的配制物。
·将离心管翻转10次并静置5min。
·上清液经200μm筛倾析到称重过的玻璃盘中。
·保留的被吸收的物质的量再次分散到20ml的表面活性剂溶液中,该提取摇动步骤重复总共5次(5x 20ml的表面活性剂溶液)。将每次倾析的液体体积收集在玻璃盘中。
·将收集的倾析表面活性剂溶液在110℃干燥3h并精确称量剩余物。
·作为空白(用于测定没有硅油的剩余物的量),将5g的对比例1分散在100ml的表面活性剂溶液中,然后倾析并干燥。
3.结果(样品在室温下贮藏14天)
如下计算释放的硅油的百分数:
((剩余物–空白)x 100)/4=释放[%]
结果
·空白:1.409g的剩余物
·对比例1:3.38g的剩余物=>49.3%释放
·实施例1:1.60g的剩余物=>4.8%释放
·实施例2:2.02g的剩余物=>15.3%释放
本发明的实施例显示释放低得多并因此吸收较高。
Claims (20)
1.粒状功能化二氧化硅,其特征在于,
-Hg孔体积(<4μm)大于0.80ml/g,
-dQ3=10%大于400μm,
-dQ3=90%小于3000μm,
-未经超声暴露的d50与经过3分钟超声暴露的d50之比<4.00,该测定是对400-500μm的颗粒部分进行的,和
-碳含量是1.0-15.0重量%。
2.如权利要求1所述的粒状功能化二氧化硅,其特征在于,所述二氧化硅的pH为5.0-11.0。
3.如权利要求1或2所述的粒状功能化二氧化硅,其特征在于,未经超声暴露的d50与经过3分钟超声暴露的d50之比为1.00-3.00,该测定是对400-500μm的颗粒部分进行的.
4.如权利要求1或2所述的粒状功能化二氧化硅,其特征在于,所述二氧化硅的Hg孔体积(<4μm)大于0.90ml/g。
5.如权利要求1或2所述的粒状功能化二氧化硅,其特征在于,所述二氧化硅的Hg孔体积(<4μm)为0.81-1.50ml/g。
6.如权利要求1或2所述的粒状功能化二氧化硅,其特征在于,所述二氧化硅含有以下官能团:
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、环烷基,
x=1或2。
7.制备如权利要求1-6中任一项所述的粒状功能化二氧化硅的方法,其包括以下步骤:
a)提供沉淀或热解二氧化硅,所述沉淀或热解二氧化硅未经超声处理时的平均粒径d50为0.1-350μm,
b)将得自步骤a)的二氧化硅润湿至干燥失重为30-80重量%,
c)通过挤出、造粒、压实或压片,使得自步骤b)的二氧化硅成型,
d)将所述成型的二氧化硅体在干燥单元中干燥,
e)以3000μm的筛号筛选造粒或筛选所述颗粒,并用筛号为400μm的筛网筛除细料,和
f)使得自步骤e)的颗粒与表面改性剂反应。
8.如权利要求7所述的方法,其特征在于,使用干燥失重为30-80重量%的含水滤饼作为步骤a)的原料。
9.如权利要求7所述的方法,其特征在于,在步骤c)中,将二氧化硅在高速强力混合机中压实和造粒。
10.制备如权利要求1-6中任一项所述的粒状功能化二氧化硅的方法,其包括以下步骤:
i)提供沉淀或热解二氧化硅,所述沉淀或热解二氧化硅的干燥失重<30重量%,并且在未经超声处理时的平均粒径d50为0.1-350μm,
ii)通过干压实使得自步骤i)的二氧化硅成型,从而得到块料,优选在两个转辊之间,以0.5kN/cm辊宽-12kN/cm辊宽的比接触压力来进行所述干压实,
iii)以3000μm的筛号筛选造粒或筛选所述块料,并用筛号为400μm的筛网筛除细料,和
iv)使得自步骤iii)的颗粒与表面改性剂反应。
11.如权利要求7-10中任一项所述的方法,其特征在于,除去小于400μm的所有筛选部分。
12.如权利要求7和10中任一项所述的方法,其特征在于,成型步骤c)或ii)是在没有添加粘合剂的情况下进行的。
13.如权利要求7和10中任一项所述的方法,其特征在于,步骤f)或iv)中所用的改性剂是至少一种有机硅烷。
14.如权利要求13述的方法,其特征在于,使用以下有机硅烷中的至少一种或所述有机硅烷的混合物作为改性剂:
a)式(RO)3Si(CH2)m-R’的有机硅烷、
b)式(R”)x(RO)(3-x)Si(CH2)m-R’的有机硅烷、
c)式X3Si(CH2)m-R’的卤代有机硅烷、
d)式(R”)xX(3-x)Si(CH2)m-R’的卤代有机硅烷、
e)式(RO)3Si(CH2)m-OOC(CH3)C=CH2的有机硅烷、
f)式X3Si(CH2)m-OOC(CH3)C=CH2的卤代有机硅烷、
g)式Xx(R”)(3-x)Si(CH2)m-OOC(CH3)C=CH2的有机硅烷、或
h)式(R”)x(RO)(3-x)Si(CH2)m-OOC(CH3)C=CH2的有机硅烷,
其中
R=烷基,优选甲基、乙基或丙基,
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、环烷基,
X=Cl或Br,
x=1或2,
m=0、1–20。
15.如权利要求1-6中任一项所述的粒状二氧化硅用于制备配制物的用途。
16.配制物,其含有至少一种如权利要求1-6中任一项所述的粒状二氧化硅和添加剂。
17.如权利要求16所述的配制物,其特征在于,所使用的添加剂是至少一种催化活性物质。
18.如权利要求16和17中任一项所述的配制物,其特征在于,所述配制物中含有的所述添加剂的比例为1-70重量%。
19.如权利要求16所述的配制物,其特征在于,所使用的添加剂包括硬化剂或引发剂、交联剂、催化剂、活性药物成分和赋形剂、活性化妆成分和赋形剂、清洁和/或护理组合物、调味剂、芳香剂和香味剂、动物饲料或动物饲料添加剂、维生素、矿物质、食品或食品添加剂、染料和/或颜料、氨基酸、氧化剂或漂白剂、具有杀微生物作用的添加剂、农业和林业用化学品,和/或混凝土外加剂。
20.如权利要求19所述的配制物,其特征在于,所述添加剂是酶。
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US20160082415A1 (en) | 2016-03-24 |
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BR112014032729A2 (pt) | 2017-06-27 |
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