CN101087660A - 用于改进洁牙剂中清洁性和磨损性的分级二氧化硅 - Google Patents
用于改进洁牙剂中清洁性和磨损性的分级二氧化硅 Download PDFInfo
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- CN101087660A CN101087660A CNA2005800446492A CN200580044649A CN101087660A CN 101087660 A CN101087660 A CN 101087660A CN A2005800446492 A CNA2005800446492 A CN A2005800446492A CN 200580044649 A CN200580044649 A CN 200580044649A CN 101087660 A CN101087660 A CN 101087660A
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- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
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Abstract
提供了一种制造沉淀二氧化硅磨料组合物的方法,所述磨料组合物具有优良的清洁性能和较低的磨损性,所述方法包括通过空气分级技术进行的磨料颗粒的反应器后分级。通过设定特定粒径范围,可确定在没有提高所述二氧化硅产品本身的牙质磨损性质的条件下得到更高的薄膜清洁水平。因此,可提供包含该分级磨料二氧化硅产品的洁齿剂,它具有特别理想的清洁效果,从而可改进牙齿抛光、增白等,且对牙齿硬表面没有有害的影响。本发明也包括该选择性处理方法得到的产品和包含该分级二氧化硅产品的洁齿剂。
Description
发明领域
本发明涉及制造磨料组合物的方法,更具体涉及制造沉淀二氧化硅磨料组合物的方法,所述组合物具有优良的清洁性能和更低的磨损性(abrasiveness),该方法包括通过空气分级技术对操作中的磨料颗粒进行反应器后粒度分选(sizing)。通过设定特定的粒径范围,确信可达到更高的薄膜清洁(pellicle film)水平,且没有提高二氧化硅产品本身的牙质磨损性质。因此,可提供包含该分级磨料二氧化硅产品的洁牙剂(dentifrice),其具有特别理想的清洁效果,从而提高牙齿抛光、增白等,且不会对牙齿硬表面产生有害的影响。而且,本发明也包括该选择性处理方法得到的产品和包含该分级二氧化硅产品的洁牙剂。
发明背景
牙膏制造商努力制造具有高清洁性能和低磨损性的洁牙剂。一些配方设计师通过在牙膏配方中加入研磨剂达到了该目标。研磨剂可包含在常规洁牙剂组合物中,以从牙齿表面上除去各种沉淀物,包括薄膜。薄膜紧密粘附,并通常包含褐色或黄色色素,它使得牙齿的外观不太好看。尽管清洁是重要的,但是磨料应该不能太具侵蚀性而破坏到牙齿。理想情况下,有效的洁牙剂磨料最大程度地除去薄膜,同时对牙齿硬表面造成最小程度的磨损和破坏。因此,在这些情况下,洁牙剂的性能与研磨抛光剂组分密切相关。
许多水不溶性研磨抛光剂已经用于或据说用于洁牙剂组合物中。这些研磨抛光剂包含天然和合成研磨颗粒材料。通常已知的合成研磨抛光剂包含无定形沉淀二氧化硅、二氧化硅凝胶、磷酸二钙及其二水合物形式、焦磷酸钙和沉淀碳酸钙(PCC)。洁牙剂用的其它研磨抛光剂包括白垩、碳酸镁、硅酸锆、偏磷酸钾、正磷酸镁、磷酸三钙等。
已将合成的无定形沉淀二氧化硅(具体而言)用作洁牙剂制剂中的研磨组分,因为它们具有清洁能力、相对安全性、与常用洁牙剂组分(例如湿润剂、增稠剂、芳香剂、防龋剂等)的相容性等。通常如下制备合成的沉淀二氧化硅:通过加入无机酸和/或酸性气体(acid gas),从可溶性碱性硅酸盐中去稳定化和沉淀出无定形二氧化硅,该反应的条件使得初始形成的初级颗粒趋向于相互缔合形成许多团聚物(即初级颗粒的离散簇),而不会凝聚成三维凝胶结构体。所得沉淀物通过过滤、清洗和干燥方法与反应混合物中的水性部分分离,然后对干燥的产物进行机械粉碎,以得到合适的粒径。
通常根据总体清洁和磨料品质,制造如上述制备和利用的沉淀二氧化硅磨料,并用于洁牙剂中。尽管前述产品在这些方面具有优良的性质,但是已经注意到它也存在如下缺陷,即不能具有较低磨损水平且没有牺牲薄膜清洁能力(特别是对于容易在龈线(gum line)上出现牙质磨损的使用者而言),同时还需要潜在补充磨料/清洁二氧化硅产品来更有效地抛光和/或牙齿增白。因此,在牙用二氧化硅材料工业中存在需要改进的地方。
如上所述,目前仍需要具有优良清洁性能同时具有更低磨损值的沉淀二氧化硅组合物,它能用于牙膏组合物中。因此,证实了下述发明满足上述的期望结果。
发明简述
本发明包括无定形沉淀二氧化硅组合物,所述二氧化硅组合物的中值粒径约5-15微米,优选约6-10微米,更优选约7-9微米,粒径跨度小于2,优选约1.25-1.75,更优选约1.25-1.40,粒径β值大于约0.30,优选约0.35-0.50,更优选约0.40-0.50。
本发明也包括洁牙剂,它包含约5-35重量%的上述无定形沉淀二氧化硅组合物,且放射性牙质磨损(RDA)水平约130-200(优选约130-195),薄膜清洁比(pellicle film cleaning ratio,PCR)约100-140(优选约110-140),且PCR:RDA之比约为0.65-1.1,优选约0.68-1.0。
基本上,已认识到提供具有集中特定粒度范围的低结构(low-structure)研磨二氧化硅材料可使得在用包含该材料的洁牙剂清洁牙齿时得到更大的性能均一性。同样地,提供粒径在特定范围内的该材料,可对牙齿表面的特定部位进行适当清洁,且同时没有过度的磨损水平。
发明详述
本文所用所有的份、百分数和比例都用重量表示,除非有其它说明。本文所引用的所有文献通过参考的方式全文插入于此。下面描述了本发明的优选实施方式,它们提供了洁牙剂(例如牙膏)所用的二氧化硅。尽管该二氧化硅的最佳用途是用于洁牙剂,但是该二氧化硅也可用于其它消费产品中。
“混合物”表示两种或多种物质的任何组合,其形式例如但没有局限于均匀混合物、悬浮物、溶液、溶胶、凝胶、分散体或乳液。
“洁牙剂”表示口腔护理产品,例如但没有局限于牙膏、牙粉和假牙乳膏(denture cream)。
“粒径跨度”表示第十体积百分位中的颗粒累积直径(D10)减去第九十百分位中的累积体积(D90),再除以第五十体积百分位中的颗粒直径(D50),即(D10-D90)/D50。更低的跨度表示更窄的粒径分布。
“粒径β值”表示在第二十五体积百分位中的颗粒累积直径(D25)除以第七十五体积百分位中的颗粒直径(D75),即D25/D75。β值越高表示粒径分布越窄。
本发明涉及无定形沉淀二氧化硅组合物,也称为二氧化硅或SiO2,当它用于牙膏或洁牙剂中时可提高清洁和磨损特性。这些研磨二氧化硅不仅通过除去碎片和剩余的污点来清洁牙齿,而且也可抛光牙齿表面。由于本发明的二氧化硅已经经过分级除去了据说清洁效果较低的细颗粒和据说增加磨损的大颗粒,所以它们具有更窄的粒径分布,特别适用于配制具有优良清洁性能和较低磨损性的牙膏。
应在牙膏组合物中加入足量的研磨二氧化硅,这样使得牙膏的放射性牙质磨损(“RDA”)值约为50-250。当RDA小于50时,所述牙膏的清洁性能极小,而RDA大于250时,就会出现牙膏研磨能力太强而沿龈线破坏牙齿牙质的风险。优选地,所述洁牙剂的RDA值应至少约50,例如约70-200之间。
牙膏的RDA取决于磨料的硬度、磨料粒径和磨料在牙膏中的浓度。通过文献“A Laboratory Method for Assessement of Dentifrice Abrasivity”(《评估洁牙剂研磨性的实验室方法》John J.Hefferren,公开于
Journal of Dental Research,第55卷第4期(1976年),第563-573页)中公开的方法测量RDA。也可通过Einlehner方法(在下文详细描述)测量二氧化硅磨损性或硬度。
在本发明中,已经开发了一种研磨无定形二氧化硅,它不仅具有优良的清洁性能,而且磨损性较小。通过对喷雾干燥和研磨的二氧化硅使用反应器后空气分级设备,可生产在给定的PCR范围内具有相对较低的RDA和Einlehner磨损值的研磨二氧化硅材料。
根据下述方法制备本发明的二氧化硅组合物。在该方法中,将已经形成的干燥二氧化硅输入到空气分级器中,以从较细和较粗的颗粒中分离所需的部分。该二氧化硅磨料进料(feed)可以是任意结构(例如非常低到中等结构)的沉淀二氧化硅或二氧化硅凝胶,优选是非常低-低结构的沉淀二氧化硅。本文所用的二氧化硅结构公开在文献“Cosmetic Properties and Structure ofFine-particle Synthetic Precipitated Silicas”(《合成沉淀二氧化硅细粒的美容特性和结构》,S.K.Wason,公开在
Journal of Soc.Cosmet.Chem,第29卷(1978年),第497-521页,其全文以参考引用的方式插入于此)中。本发明的组合物包括亚麻籽油吸收值约为50-90毫升/100克的二氧化硅颗粒。
所述二氧化硅进料可根据美国专利6616916、5869028、4421527和3893840所公开的内容进行制备,所述文献以参考引用的方式全文插入于此。
可将干燥的二氧化硅进料以输入分级器之前未研磨的或经研磨的给料的形式加入分级器。可在任何干燥二氧化硅中常规的装置(例如喷雾干燥、喷嘴干燥(例如塔或喷泉(fountain)、急骤干燥、旋转轮干燥或真空/流化床干燥)中干燥所述未研磨的进料。干燥的二氧化硅产品通常应具有1-15重量%的水分。
或者,在输入分级器之前,可用常规粉碎(grind)和研磨(milling)设备来降低干燥二氧化硅的粒径,以得到约为5-25微米的所需粒径,例如约5-15微米。锤子或者摆式轧机可用于一次或多次的研磨(),细碾磨可通过流体能或空气喷射磨机进行。
接着,对干燥的二氧化硅进行空气分级,以得到本发明所述的具有窄粒径分布的二氧化硅。所述二氧化硅的分级通过从所述产品中除去细颗粒和大颗粒使粒径分布变窄。所述分级器的护盖(housing)用作充气装置(plenum),使计量的初级空气通过入口管输入其中。该空气通过两个半转子(rotor halves)和定子顶部之间的窄缝隙进入分级器转子。这些逆向高速流体形成了湍流分散区。进料通过中心管进入系统,所述中心管与径向成角度,以使粗颗粒由于惯性喷射到漩涡的距离最小。刀片的外缘和转子周边之间的空间形成了分级区。将粗产品(由离心场向外排出)用安装在旋风分离器上的喷射泵经粗产物出口输出分级器。旋风分离器的溢流经循环部分返回到所述分级器。细产品与初级空气流经中央出口离开分级器。对所述二氧化硅进行分级,直到该二氧化硅产品具有所需的粒径分布。
描述粒径分布紧密度的两种标准是用Horiba激光散射仪(购自HoribaInstruments,Boothwyn,Pennsylvania)测得的粒径跨度和β值。在给定组合物中,二氧化硅颗粒的粒径分布可在Horiba上表示,它将累积体积百分数作为粒径的函数示出,其中累积体积百分数是粒径分布中粒径小于或等于给定值的体积百分数,粒径是等效(equivalent)球形颗粒的直径。粒径分布中的中值粒径是该粒径分布在Horiba上50%点上的二氧化硅颗粒的粒径(以微米表示)。
对于给定组合物,粒径分布的宽度使用跨度比来表征。所述跨度比定义为在第十体积百分位上颗粒的累积直径(D10)减去第九十百分位上的累积体积,再除以第五十百分位上的粒径(D50),即(D10-D90)/D50。
粒径分布也可用β值表征。所述粒径β值是在第二十五体积百分位上的颗粒累积直径(D25)除以在第七十五体积百分位上的颗粒直径(D75),即D25/D75。β值越高表明粒径分布越窄。
然后,可将该研磨的无定形沉积二氧化硅作为唯一的磨料或者与其它磨料组分一起加入到洁齿剂组合物(例如牙膏)中。
除了磨料组分,所述洁齿剂也可包含一些其它通常用于洁齿剂的组分,例如湿润剂、增稠剂(有时也称为粘合剂、树胶或稳定剂)、抗菌剂、氟化物、甜味剂和共表面活性剂。
湿润剂用于将主体(body)或“口腔织物(mouth texture)”加入到洁齿剂中,以及防止洁齿剂干燥。合适的湿润剂包括聚乙二醇(具有各种不同的分子量)、丙二醇、甘油(丙三醇)、赤藓糖醇、木糖醇、山梨糖醇、甘露醇、乳糖醇和氢化淀粉水解产物,以及这些化合物的组合。
增稠剂可用于本发明的洁齿剂组合物中,以提供使牙膏稳定不会产生相分离的凝胶结构。合适的增稠剂可包括二氧化硅增稠剂、淀粉、淀粉的甘油溶液(glycerite)、卡拉牙胶(刺梧桐树胶)、黄蓍胶、阿拉伯胶、印度胶、金合欢胶(gum acacia)、黄原胶、瓜尔胶、改性硅酸镁铝(veegum)、角叉(菜)胶、海藻酸钠、琼脂、果胶、纤维素、纤维素胶、羧甲基纤维素、羟乙基纤维素、羟丙基纤维素、羟甲基、羟甲基羧丙基纤维素、甲基纤维素、乙基纤维素、硫酸化纤维素、以及这些化合物的组合。粘合剂的常规用量为牙膏组合物的约0-15重量%。
抗菌剂可用于将微生物的存在降低到低于已知的有害水平。合适的抗菌剂包括焦磷酸四钠、安息香酸、苯甲酸钠、苯甲酸钾硼酸酚化合物(例如β-萘酚、氯代百里酚、百里酚、茴香脑、桉叶脑、香芹酚、薄荷脑、苯酚、戊基苯酚、己基苯酚、庚基苯酚、辛基苯酚、己基间苯二酚、氯化月桂基吡啶鎓、氯化肉豆蔻基吡啶鎓、氟化鲸蜡基吡啶鎓、氯化鲸蜡基吡啶鎓、溴化鲸蜡基吡啶鎓。如果存在的话,抗菌剂的含量较好为所述牙膏组合物的约0.1-5重量%。
可将甜味剂加入到牙膏组合物中以使所述产品具有令人愉悦的口味。合适的甜味剂包括糖精(如糖精钠、糖精钾或糖精钙)、环磺酸盐(例如钠盐、钾盐或钙盐)、丁磺氨-K、索马汀(thaumatin)、新橙皮甙二氢查尔酮(neohisperidindihydrochalcone)、氨化甘草素、右旋糖、左旋糖、蔗糖、甘露醇和葡萄糖。
所述牙膏也可优选包含氟化物盐,以防止龋齿的产生和发展。合适的氟化物盐包括氟化钠、氟化钾、氟化锌、氟化锡、氟化锌铵、单氟磷酸钠、单氟磷酸钾、氢氟酸月桂基胺、氢氟酸二乙基氨基乙基辛基酰胺、氟化二癸基二甲基铵、氟化鲸蜡基吡啶鎓、氟化二月桂基吗啉鎓、肌氨酸氟化亚锡、甘氨酸氟化钾、甘氨酸氢氟化物、和单氟磷酸钠。氟化物盐的常规用量约为0.1-5重量%。
也可将表面活性剂用作附加的清洁和发泡剂,它可选自阴离子表面活性剂、两性离子表面活性剂、非离子表面活性剂、两性表面活性剂、和阳离子表面活性剂。阴离子表面活性剂是优选的,例如金属硫酸盐,例如月桂基硫酸钠。
本文所述洁齿剂也可包含许多其它组分,例如脱敏剂、治疗剂(healingagent)、其它防龋剂、螯合剂/掩蔽剂、维生素、氨基酸、蛋白质、其它抗斑剂/抗结石剂、遮光剂、抗生素、抗酶、酶、pH控制剂、氧化剂、抗氧剂、增白剂、着色剂、香料和防腐剂。
最后,水提供了上述添加剂之外的组合物余量。所述水优选是去离子水,且没有杂质。所述洁齿剂可包含约10-40重量%的水,优选20-35重量%。
本发明的优选实施方式
基于下述特定的非限制实施例更详细地描述本发明。
比较例A-B
为了显示本发明的进步性,对2种市售沉淀二氧化硅ZEODENT103和ZEODENT124(分别为比较例A和比较例B)进行表征。这些产品购自J.M.HuberCorporation,Edison,New Jersey。这些样品的物理性质概括在下表2中。
实施例1-2
在实施例1和2中,根据本发明制备适合用于洁齿剂以及其它产品的二氧化硅。
实施例1所用的原料二氧化硅是比较样品A,ZEODENT103。接着,使干燥的沉淀二氧化硅在表1所示条件下,多次通过CCE Technologies,Inc.(Cottage Grove,MN)制造的高效离心空气分级器(Model 205)进行空气分级。
实施例2所用的原料是比较样品B,ZEODENT124二氧化硅,首先对其进行研磨。接着,将研磨的沉淀二氧化硅在表1所示条件下进行空气分级。
表1
实施例1 | 实施例2 | |
转子速度(rpm) | 1550 | 1550 |
流速ΔP(in.H2O) | 4.5 | 4.5 |
空气流速(scfm) | 247 | 247 |
弹射器压力(psig) | 50 | 50 |
分级ΔP(in.Hg) | 6.5 | 7.2 |
如上述制备后,接着测量颗粒二氧化硅的一些性质(包括中值粒径、平均粒径、粒径β值、粒径跨度、%325目剩余物、BET表面积、CTAB表面积、油吸附和Einlehner磨损)。
使用购自Horiba Instruments(Boothwyn,Pennsylvania)的Model LA-910激光散射仪测量粒径。激光束通过透明单元投射,所述透明单元包含悬浮在液体中的移动颗粒流。碰撞到颗粒的光线以一定角度散射,所述角度与其粒径成反比例。所述光检测器阵列测量在一些预定角度的光数量。与所测光通量成正比的电信号用微电脑系统进行处理,形成粒径分布的多通道柱状图。除了粒径跨度((D10-D90)/D50)和β值(D25/D75)之外,还测量中值和平均粒径。
%325筛剩余物如下测定:称重50克二氧化硅,置于包含500-600毫升水的1升烧杯中。使所述二氧化硅颗粒沉入水中,然后充分混合直到所有材料都分散。通过喷嘴(Fulljet 9.5,3/8G,316不锈钢,Spraying Systems Company)将水压调节到20-25psi。喷射时,将所述筛网布(325目筛网,8”直径)放在喷嘴下面4-6英寸,所述烧杯的内容物逐渐倾倒在325目筛网上。冲洗烧杯壁上的剩余材料,并倾倒在筛网上。清洗2分钟,通过扫描移动(sweeping motion)将喷射物(spray)从筛网的一侧移到另一侧。喷射2分钟后(小于筛网开孔的所有颗粒应该都已经漏过筛网),将保留在筛网上的剩余物清洗到一侧,然后用来自喷射瓶(squirt bottle)的水进行清洗将其转移到预称重的铝称量皿中。用所需最少量的水来保证将所有剩余物都转移到称量皿中。静置所述称量皿2-3分钟(剩余物沉淀),然后轻轻倒掉顶部清水。将所述称量皿放入炉(设定在105℃的“Easy-Bake”红外炉或常规炉)中,干燥直到剩余物恒重。将干燥的剩余物样品和称量皿再次称重。如下计算%325剩余物:
%325剩余物=剩余物重量(克)/样品重量(克)×100
使用Brunaur等人,
J.Am.Chem.Soc,60,309(1938)的BET氮气吸附方法测定BET表面积。
二氧化硅的CTAB外表面积如下测定:将CTAB(溴化鲸蜡基三甲基铵)吸附在二氧化硅表面上,通过离心分离多余的量,采用表面活性剂电极以月桂基硫酸钠进行滴定来测量。由吸附的CTAB量确定二氧化硅的外表面积(在吸附之前和之后分析CTAB)。
具体地,精确称量约0.5克二氧化硅,并将其放入装有100.00毫升CTAB溶液(5.5克/升)的250毫升烧杯中,在电动搅拌板上混合30分钟,然后以10000rpm离心15分钟。将1毫升10%Triton X-100加入到置于100毫升烧杯中的5毫升澄清上清液中。用0.1N HCl调节pH到3.0-3.5,采用表面活性剂电极(Brinkmann SUR15O1-DL)以0.0100M月桂基硫酸钠滴定样品,以确定终点。
使用亚麻籽油通过抹除(rubout)法测量油吸附。在该测试中,将油与二氧化硅样品混合,在光滑表面上用抹刀刮擦(rub)直到形成干硬性油灰状浆料。通过测量要得到铺展时会卷曲的浆料混合物所需的油量,可计算二氧化硅的油吸附值-该值表示完全饱和二氧化硅吸附容量的每单位重量二氧化硅所需的油体积。如下计算油吸附值:
油吸附=吸附的油(毫升)/二氧化硅重量(克)×100
=油(毫升)/100克二氧化硅 (II)
使用Einlehner AT-1000 Abrader测量Brass Einlehner(BE)磨损值。在该测试中,对Fourdrinier黄铜(brass)金属丝网筛进行称重,并暴露于10%水性二氧化硅悬浮液的作用下,旋转(revolution)固定次数,然后,确定每100000次旋转后从Fourdrinier金属丝网筛损失的黄铜的毫克数,作为磨损量()。该测试所需的一次性用品(disposable supply)(黄铜筛网、耐磨板和PVC管)购自Duncan Associates(Rutland,Vermont),商品名为“Einlehner TestKit“。特别地,黄铜筛网(Phosphos Bronze P.M.)如下制备:在热肥皂水(0.5%Alconox)的超声浴中清洗5分钟,然后在自来水中清洗,并在装有150毫升水的烧杯中再次超声浴清洗。将所述筛网在自来水中再次清洗,在105℃的炉中干燥20分钟,在干燥器中冷却并称重。用镊子处理筛网,防止皮肤油污染筛网。Einlehner测试圆柱体装有耐磨板和称重的筛网(红线侧向下-无磨损侧),并夹紧于适当位置。耐磨板可使用25次测试,或者直到用坏;称重的筛网一次性使用。
通过混合100克二氧化硅和900克去离子水得到10%二氧化硅浆料,将其倾倒入Einlehner测试圆柱体中。将Einlehner PVC管放在搅拌轴上。PVC管有5个已编号的位置。对于每次测试,PVC管的位置累进,直到使用5次,然后丢弃。重新装配Einlehner磨损仪,将该仪器设定为运转87000次旋转。每次测试耗时约49分钟。完成一次循环后,取下筛网,在自来水中清洗,置于装有水的烧杯中、置于超声浴中2分钟,用去离子水清洗,并在105℃的炉中干燥20分钟。使干燥的丝网在干燥器中冷却并再次称重。每个样品进行两次测试,结果取平均,并表示为每100000次旋转损失的毫克数。对于10%浆料,以每100000次旋转损失的毫克数为单位的结果表征为10%黄铜Einlehner(BE)磨损值。这些测量和测试的结果概括在下表2中。
表2
实施例1 | 实施例2 | 比较例A | 比较例B | |
中值粒径(微米) | 8.1 | 8.0 | 9.4 | 8.3 |
平均粒径(微米) | 8.2 | 8.7 | 13.1 | 11.2 |
粒径β值 | 0.45 | 0.41 | 0.19 | 0.24 |
粒径跨度 | 1.47 | 1.61 | 3.01 | 2.73 |
%325剩余物 | 0.0 | 0.0 | 1.2 | 0.4 |
BET表面积(米2/克) | -- | 53 | 39 | 73 |
CTAB表面积(米2/克) | 22 | 48 | 32 | 42 |
油吸附(毫升/100克) | 59 | 74 | 70 | 72 |
Einlehner磨损(毫克) | 13.10 | 6.38 | 18.92 | 8.57 |
如表2所示,实施例1-2中制备的二氧化硅相比比较例A-B具有更小的中值粒径和平均粒径。更低的粒径跨度和更高的粒径β值表明,实施例1-2中的二氧化硅具有更窄的粒径分布。实施例1-2也具有更低的Einlehner磨损值,同时也足以进行研磨以用于生产具有可接收的或良好的清洁性能的牙膏。相反地,比较例A-B具有更宽的粒径分布,且磨损性更强。
为了说明其在消费产品中的功效,将实施例1-2的二氧化硅磨料以粉末的形式加入到四种不同的牙膏组合物(编号1-4)中,每一种中二氧化硅的加入量为20%和35%。然后,将这些组合物的性能与用比较例A-B的二氧化硅配制的牙膏组合物5-8的性能进行比较,其中牙膏组合物5-8中的每一种中二氧化硅含量为20和35%。8种牙膏组合物列在下表3中。
如下制备这些牙膏样品。通过混合下述组分形成第一混合物:甘油和山梨糖醇、聚乙二醇(CARBOWAX600,购自Union Carbide Corporation,Danbury,CT)、羧甲基纤维素(例如CEKOL2000,购自Noviant,Arnhem,The Netherlands,或者CMC-7MXF,购自Hercules Corporation,Wilmington,DE的Aqualon分公司),然后搅拌第一混合物直到组分溶解。通过混合下述组分形成第二混合物:去离子水、焦磷酸四钠、糖精钠、氟化钠,然后搅拌直到所述组分溶解。然后混合所述第一混合物和第二混合物,同时搅拌形成预混物。将所述预混物放入Ross混合器(130LDM型,Charles Ross & Co.,Haupeauge,NY),将二氧化硅增稠剂、二氧化钛和二氧化硅磨料加入到预混物中,所述预混物在非真空条件下混合。然后抽30英寸真空,每种样品混合15分钟,接着加入月桂基硫酸钠和香料。所得混合物在降低的混合速度下搅拌5分钟。根据下述配方制备八种不同的牙膏组合物,所述数量以克为单位:
表3
组分 | 牙膏组合物编号 | |||||||
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | |
甘油,99.5% | 11 | 9.683 | 11 | 9.683 | 11 | 9.683 | 11 | 9.683 |
山梨糖醇,70% | 40.007 | 28.718 | 40.007 | 28.718 | 40.007 | 27.718 | 40.007 | 28.718 |
去离子水 | 20 | 17.806 | 20 | 17.806 | 20 | 17.806 | 20 | 17.806 |
Carbowax 600 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 |
CMC-7MXF | 1.2 | 1 | 1.2 | 1 | 1.2 | 1 | 1.2 | 1 |
焦磷酸四钠 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
糖精钠 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
氟化钠 | 0.243 | 0.243 | 0.243 | 0.243 | 0.243 | 0.243 | 0.243 | 0.243 |
Zeodent165二氧化硅增稠剂 | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 |
实施例1磨料 | 20 | 35 | - | - | - | - | - | - |
实施例2磨料 | - | - | 20 | 35 | - | - | - | - |
比较例A磨料 | - | - | - | - | 20 | 35 | - | - |
比较例B磨料 | - | - | - | - | - | - | 20 | 35 |
TiO2 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
月桂基硫酸钠 | 1.2 | 1.2 | 1.2 | 1.2 | 1.2 | 1.2 | 1.2 | 1.2 |
香料 | 0.65 | 0.65 | 0.65 | 0.65 | 0.65 | 0.65 | 0.65 | 0.65 |
总量 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 |
如上述制备牙膏组合物1-8之后,如下述确定RDA和PCR性质。用Hefferen,Journal of Dental Res.,1976年7-8月,55(4),第563-573页所示的方法以及Wason的美国专利4340583、4420312和4421527(这些公开文献和专利文献以引用的方式全文插入于此)所述的方法确定本发明所用沉淀二氧化硅组合物的放射性牙质磨损(RDA)值。
用于分析牙膏组合物的PCR测试参见“In Vitro Removal of Stain WithDentifrice”(《用洁牙剂体外去除污点》G.K.Stookey等人的J.DentalRes.,61,1236-9,1982年)。
每种牙膏组合物测量3次PCR和RDA,结果取平均。RDA和PCR测量的平均结果以及这些测量值的比值概括在下表4中。
表4
牙膏性质
牙膏组合物编号 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
PCR | 123 | 128 | 111 | 116 | 115 | 123 | 109 | 122 |
RDA | 181 | 195 | 144 | 144 | 225 | 249 | 170 | 205 |
PCR/RDA | 0.68 | 0.66 | 0.77 | 0.81 | 0.51 | 0.49 | 0.64 | 0.60 |
如表4所示,在所有例子中包含本发明二氧化硅的牙膏(牙膏组合物1-4)相比相应的对照牙膏(牙膏组合物5-8)都具有相等的PCR值。令人吃惊的是,本发明牙膏组合物1-4的RDA值比对应的对照牙膏组合物5-8低26-61分。此外,本发明分级二氧化硅产品的计算所得比值明显高于比较例的二氧化硅产品,这表明其相对于当前所用磨料具有明显的改进。
本领域的普通技术人员可以理解,上述实施方法可在没有离开本发明范围的情况下进行一些变化。因此,可以理解,本发明并没有局限于所述特定的实施方式,而是覆盖所附权利要求书所限定的本发明精神和范围内所有改变。
Claims (20)
1.一种包含无定形沉淀二氧化硅颗粒的组合物,所述组合物中的所述二氧化硅颗粒的中值粒径约为5-15微米,粒径跨度小于2,粒径β值大于0.3。
2.如权利要求1所述的组合物,其特征在于,所述组合物中的所述二氧化硅颗粒的中值粒径约为6-10微米,粒径跨度约为1.25-1.75,粒径β值约为0.35-0.50。
3.如权利要求2所述的组合物,其特征在于,所述组合物中的所述二氧化硅颗粒的中值粒径约为7-9微米,粒径跨度约为1.25-1.65,粒径β值约为0.40-0.50。
4.如权利要求1所述的组合物,其特征在于,所述二氧化硅颗粒的亚麻籽油吸附值约为50-90毫升/100克。
5.如权利要求2所述的组合物,其特征在于,所述二氧化硅颗粒的亚麻籽油吸附值约为50-90毫升/100克。
6.如权利要求3所述的组合物,其特征在于,所述二氧化硅颗粒的亚麻籽油吸附值约为50-90毫升/100克。
7.一种洁齿剂制剂,它包含约5-35重量%的权利要求1所述的组合物。
8.一种洁齿剂制剂,它包含约5-35重量%的权利要求2所述的组合物。
9.一种洁齿剂制剂,它包含约5-35重量%的权利要求3所述的组合物。
10.一种洁齿剂制剂,它包含约5-35重量%的权利要求4所述的组合物。
11.一种洁齿剂制剂,它包含约5-35重量%的权利要求5所述的组合物。
12.一种洁齿剂制剂,它包含约5-35重量%的权利要求6所述的组合物。
13.一种包含权利要求1所述组合物的洁齿剂,所述洁齿剂的放射性牙质磨损(RDA)水平约为130-200之间,薄膜清洁比(PCR)约为100-140之间。
14.如权利要求13所述的洁齿剂,其特征在于,所述洁齿剂的RDA水平约为130-195之间,PCR约为110-140之间。
15.一种包含权利要求2所述组合物的洁齿剂,所述洁齿剂的RDA水平约为130-200之间,PCR约为100-140之间。
16.如权利要求15所述的洁齿剂,其特征在于,所述洁齿剂的RDA水平约为130-195之间,PCR约为110-140之间。
17.一种包含权利要求3所述组合物的洁齿剂,所述洁齿剂的RDA水平约为130-200之间,PCR约为100-140之间。
18.如权利要求17所述的洁齿剂,其特征在于,所述洁齿剂的RDA水平约为130-195之间,PCR约为110-140之间。
19.如权利要求13所述的洁齿剂,其特征在于,所述洁齿剂的PCR/RDA约为0.65-1.1。
20.如权利要求13所述的洁齿剂,其特征在于,所述洁齿剂的PCR/RDA约为0.68-1.0。
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CN105208997A (zh) * | 2013-03-15 | 2015-12-30 | J.M.休伯有限公司 | 具有低研磨性的高清洁性二氧化硅及其制备方法 |
CN111278774A (zh) * | 2017-08-29 | 2020-06-12 | 赢创运营有限公司 | 用于控制rda的球形二氧化硅粒径 |
CN117323241A (zh) * | 2023-10-24 | 2024-01-02 | 金三江(肇庆)硅材料股份有限公司 | 一种口腔用二氧化硅颗粒及其制备方法和应用 |
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GB0525369D0 (en) | 2005-12-14 | 2006-01-18 | Ineos Silicas Ltd | Silicas |
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US8858699B2 (en) | 2006-07-13 | 2014-10-14 | Unimin Corporation | Ultra fine nepheline syenite powder and products for using same |
US20080015104A1 (en) * | 2006-07-13 | 2008-01-17 | Unimin Corporation | Ultrafine nepheline syenite |
US7757976B2 (en) * | 2007-02-07 | 2010-07-20 | Unimin Corporation | Method of processing nepheline syenite powder to produce an ultra-fine grain size product |
BRPI0814106A2 (pt) * | 2007-07-09 | 2015-02-03 | Unimin Corp | Pó de sienito de nefelina com tamanho de partícula controlado e método de produzir o mesmo |
CA2720666C (en) * | 2008-04-17 | 2014-02-25 | Unimin Corporation | Powder formed from mineral or rock material with controlled particle size distribution for thermal films |
MY151227A (en) | 2008-05-16 | 2014-04-30 | Colgate Palmolive Co | Oral compositions and uses thereof |
US8551457B2 (en) | 2008-11-25 | 2013-10-08 | The Procter & Gamble Company | Oral care compositions comprising spherical fused silica |
ES2560202T3 (es) * | 2008-11-25 | 2016-02-17 | The Procter & Gamble Company | Composiciones para el cuidado bucal con sílice fundida |
TWI407975B (zh) | 2009-12-17 | 2013-09-11 | Colgate Palmolive Co | 在牙用配製物中控制包覆並釋放疏水性活性物質之高潔淨力及低磨損性的二氧化矽材料 |
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US20120301522A1 (en) * | 2011-05-19 | 2012-11-29 | Isp Investments Inc. | Peroxide-stabilized abrasive tooth whitening compositions, process for preparing and method of use |
IN2015DN02997A (zh) | 2012-11-05 | 2015-09-25 | Procter & Gamble | |
EP3171850B1 (en) * | 2014-07-21 | 2018-12-26 | Colgate-Palmolive Company | Abrasive oral care composition |
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CN105208997A (zh) * | 2013-03-15 | 2015-12-30 | J.M.休伯有限公司 | 具有低研磨性的高清洁性二氧化硅及其制备方法 |
CN111278774A (zh) * | 2017-08-29 | 2020-06-12 | 赢创运营有限公司 | 用于控制rda的球形二氧化硅粒径 |
CN117323241A (zh) * | 2023-10-24 | 2024-01-02 | 金三江(肇庆)硅材料股份有限公司 | 一种口腔用二氧化硅颗粒及其制备方法和应用 |
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