CN101166796A - 用于硅橡胶基制剂的无机物-中和的煅烧高岭土 - Google Patents
用于硅橡胶基制剂的无机物-中和的煅烧高岭土 Download PDFInfo
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Abstract
本文所公开的是含用至少一种碱性无机化合物处理的煅烧高岭土的无机物-中和的煅烧高岭土、含该无机物-中和的煅烧高岭土的组合物和该无机物-中和的煅烧高岭土在硅橡胶制剂中的用途。本文还公开的是无机物-中和的煅烧高岭土的制备方法和含无机物-中和的煅烧高岭土的硅橡胶制剂的制备方法。
Description
[001]本申请要求2005年2月23日提交的美国临时专利申请第60/654,969号的优选权。
[002]本文公开的是改进的、表面处理的煅烧高岭土(″无机物-中和的煅烧高岭土″)及其用途。本文进一步公开的是含该无机物-中和的煅烧高岭土的组合物,和该无机物-中和的煅烧高岭土在硅橡胶制剂中的用途。本文还进一步公开的是无机物-中和的煅烧高岭土的制备方法,和含无机物-中和的煅烧高岭土的硅橡胶制剂的制备方法。
[003]已知在硅橡胶制剂中使用二氧化硅填充剂,例如结晶二氧化硅、沉淀二氧化硅和热解法二氧化硅。然而,使用二氧化硅填充剂是昂贵的,可增加材料风险观点的忧虑。因此,有必要找到二氧化硅填充剂的替代或扩展,而不损害最终硅橡胶产品的性质。
[004]在聚合作用中例如在硅橡胶制剂中,煅烧高岭土可用作增量填充剂。然而,根据例如聚硅氧烷聚合物的类型和/或特定改性剂的加入,煅烧高岭土不可用作替代和/或增量填充剂,因为它们可延迟或抑制固化过程。换句话说,由于煅烧高岭土对例如硅橡胶制剂固化的有害作用,它的有用性和适用性可能受到限制。
[005]因此,对使用改进的煅烧高岭土的二氧化硅填充剂的替代和/或扩展仍然存在需要,它可显示高水平的强化,但不抑制硅橡胶制剂的固化。
[006]本发明发明人已经惊讶地发现:用至少一种碱性无机化合物处理煅烧高岭土可提供无机物-中和的煅烧高岭土,其可满足至少一种上述需要。在使用自由基引发剂的聚合和交联反应中,本文所公开的无机物-中和的煅烧高岭土例如可用作填充剂、半-增强剂和/或增强剂的补充剂。在一个实施方案中,无机物-中和的煅烧高岭土用于硅橡胶制剂中,例如用于配制耐热硅橡胶。
[007]如J.Am.Chem.Soc,第78卷,第5490-5494页中所公开的,使用Benesi的方法,已经发现具有差固化响应的煅烧高岭土在表面上也具有高度酸性部位或中心。认为当酸性类物质例如路易斯酸电离裂解引发剂,使引发剂惰性时,在聚合物系统中的自由基引发剂和矿物填充剂之间可发生有害的反应。产生的惰性引发剂片段不包含自由基,因此不能启动或增长自由基链反应。例如,在复合硅橡胶系统中,酸裂解可极大地影响交联反应的程度和效能,其可抑制固化或导致差的固化,具有差的橡胶-样性质。
[008]本发明发明人已经惊讶地发现:通过用至少一种碱性无机化合物处理煅烧高岭土,可降低煅烧高岭土的表面酸性(路易斯酸)。因此,在固化过程中可改善无机物-中和的煅烧高岭土的性能。本文所公开的无机物-中和的煅烧高岭土可例如作为补充剂,替代在硅橡胶制剂中用作增强剂的最高达50%的沉淀二氧化硅。
[009]因此,本发明公开的一个方面涉及无机物-中和的煅烧高岭土,该煅烧高岭土包含用至少一种碱性无机化合物处理的煅烧高岭土。
[010]本发明公开的另一个方面提供含无机物-中和的煅烧高岭土的组合物,其中无机物-中和的煅烧高岭土包含用至少一种碱性无机化合物处理的煅烧高岭土。
[011]当用于本文时,术语″无机物-中和的″是指用至少一种碱性无机化合物处理,以便可减弱煅烧高岭土的表面酸性(路易斯酸),即减少高岭土表面上酸性部位的酸势(acid potential)。术语″中和″不是必需表示高岭土表面的pH值为7或接近7。通过各种机制例如典型的酸/碱机制、空间阻断酸性部位的分子结合和酸性部位的其它化学修饰,可实现煅烧高岭土表面酸性的减弱。
[012]如本文所讨论,至少一种碱性无机化合物可选自例如草酸铵、碳酸钠、氢氧化钠和磷酸三钠。在一个实施方案中,至少一种碱性无机化合物可为氨以外的碱性无机化合物。
[013]如本文所公开,可例如在离子化介质例如水中,进行煅烧高岭土的中和处理。在一个实施方案中,使用水性介质例如水将煅烧高岭土浆化,用至少一种碱性无机化合物处理并与之充分混合。在另一个实施方案中,配制至少一种碱性无机化合物的稀水溶液,雾化或喷雾到煅烧高岭土上(雾化或喷雾法)。如本文所公开,雾化法也包括例如在流化床中进行处理。在另一个实施方案中,分别将至少一种无机化合物和煅烧高岭土加到混合的母料中。
[014]可用吸收的Hammett指示剂,例如二亚肉桂基丙酮(dicinnamalacetone)/苯(DCB)酸性指示剂,来测定本文所公开的无机物-中和的煅烧高岭土的中和度,该指示剂广泛用于测定固体例如催化剂的表面酸性。见Benesi,J.Am.Chem.Soc,第78卷,第5490-5494页。
[015]本文所公开的煅烧高岭土可具有中值粒度范围例如约0.5μm至约5.0μm,例如约3.0μm至4.0μm,还例如约3.5μm。锻烧产物的中值粒度可通过例如采用斯托克斯沉降定律的标准试验方法测定。例如,可通过在标准水性介质例如水中充分分散的条件下,用得自美国Micromeritics公司的SEDIGRAPHTM仪器例如SEDIGRAPH 5100测量微粒产物的沉降,来测定煅烧高岭土的中值粒度。
[016]与那些没有无机物-中和的相比,本文所公开的无机物-中和的煅烧高岭土可以更高的装载量混合入聚合物系统例如硅橡胶制剂中,而没有对固化过程的不利影响。另外,当混合入硅橡胶制剂时,本文所公开的无机物-中和的煅烧高岭土可为所得硅橡胶产品提供与广泛用于工业中的二氧化硅填充剂相似的机械特性,甚至可以较低的装载量。例如,与50份本文所公开的无机物-中和的煅烧高岭土混合的硅橡胶的机械特性,可同与50-75份美国Silica公司的Min-U-Sil 5(平均粒度约1.0μm)混合的硅橡胶特性相当,Min-U-Sil 5被认为是用于硅橡胶工业的优质天然二氧化硅补充剂和半-增强剂。
[017]本文还公开的是含本文所公开的无机物-中和的煅烧高岭土的产品。这些产品选自例如聚合物产品和硅橡胶产品。
[018]在一个实施方案中,本发明公开提供包含本文公开的无机物-中和的煅烧高岭土的聚合物产品,无机物-中和的煅烧高岭土可用作填充剂、补充剂和/或增强剂。取决于特定的聚合物系统和期望的最终聚合物产品的物理特性,以最终聚合物产品计,无机物-中和的煅烧高岭土可存在的浓度范围为例如约1至约200phr,例如约1至约100phr重量。
[019]本文所公开的聚合物产品包含至少一种聚合物树脂。术语″树脂″指在成形为塑料制品之前为固体或液体的聚合物材料。本文使用的至少一种聚合物树脂是固化时可形成塑性材料的聚合物树脂。例如,本文公开的聚合物产品选自固化聚合物,例如自由基固化的聚合物和过氧化物固化的聚合物。可用过氧化物如交联剂固化的聚合物包括例如不饱和聚酯、聚氨酯、聚乙烯、聚硅氧烷和弹性体。在一个实施方案中,用于不饱和聚酯的过氧化物可选自例如有机过氧化物,例如二酰基过氧化物(例如癸酰基过氧化物、月桂酰过氧化物和苯甲酰过氧化物);酮过氧化物(例如2,4-戊二酮过氧化物);过氧化酯(例如过氧新癸酸叔丁酯、2,5-二甲基-2,5-二(2-乙基己酰基过氧基)己烷、叔戊基过氧基-2-乙基-己酸酯、叔丁基过氧基-2-乙基-己酸酯、过氧乙酸叔戊酯、过氧乙酸叔丁酯和过苯甲酸叔戊酯);二烷基过氧化物(例如过氧化二枯基、2,5-二甲基-2,5-二-(叔丁基过氧基)己烷、双(叔丁基过氧基)二异丙基-苯、二-叔戊基过氧化物、二-叔丁基过氧化物和2,5-二甲基-2,5-二-(叔丁基过氧基)己炔-3);氢过氧化物(例如氢过氧化枯烯);和过氧缩酮(例如1,1-二-(叔丁基过氧基)-3,3,5-三甲基-环己烷和1,1-二-(叔丁基过氧基)-环己烷)。
[020]本文可使用的至少一种聚合物树脂可选自例如聚烯烃树脂、聚酰胺树脂、聚酯树脂、工程化聚合物、烯丙树脂和热固性树脂。
[021]在另一个实施方案中,本发明公开提供包含本文所公开的无机物-中和的煅烧高岭土的硅橡胶产品。本文所公开的无机物-中和的煅烧高岭土可提供的益处有树脂延伸、橡胶增强和橡胶组合物硬度增加。在本文所公开的硅橡胶产品中,无机物-中和的煅烧高岭土存在的量占橡胶例如约1至约200phr、例如约1至约100phr重量。
[022]本文还公开的是硅橡胶制剂,该硅橡胶制剂包含:
含无机物-中和的煅烧高岭土的至少一种填充剂,其中无机物-中和的煅烧高岭土包含用至少一种无机化合物处理的煅烧高岭土,该无机化合物的量足以降低煅烧高岭土表面酸性部位的活性;和
至少一种聚硅氧烷聚合物。
[023]本文还公开的是无机物-中和的煅烧高岭土的制备方法,该方法包括用至少一种碱性无机化合物处理煅烧高岭土。这样的处理可在离子化介质中进行。离子化介质可选自例如水性介质,例如水。处理的实例包括喷水、雾化、混合、在流化床或者桨式搅拌机中涂覆和在蒸气磨中处理。以在处理中的煅烧高岭土计,至少一种碱性无机化合物存在的量等于或大于0.1%重量,例如约0.1%至约5.0%,例如约0.5%至约2.5%,还例如约2.0%重量。
[024]在一个实施方案中,处理操作包括在水中将煅烧高岭土浆化,将所得的煅烧高岭土与至少一种碱性无机化合物混合。另外,本文公开的方法还可包括将用至少一种碱性无机化合物处理的煅烧高岭土干燥,例如盘式干燥、喷雾干燥和在流化床干燥器中干燥,和粉碎。
[025]本文甚至还公开的是硅橡胶产品的制备方法,该方法包括将无机物-中和的煅烧高岭土加入硅橡胶制剂中,其中硅橡胶制剂包含至少一种聚硅氧烷弹性体和至少一种引发剂,和无机物-中和的煅烧高岭土包含用至少一种碱性无机化合物处理的煅烧高岭土。另外,硅橡胶制剂还可包括至少一种选自例如沉淀二氧化硅、结晶二氧化硅和热解法二氧化硅的其它填充剂。
[026]本文还公开的是硅橡胶产品的制备方法,该方法包括将煅烧高岭土和至少一种碱性无机化合物加入硅橡胶制剂中,其中硅橡胶制剂包含至少一种聚硅氧烷弹性体和至少一种引发剂。在一个实施方案中,基本上同时加入煅烧高岭土和至少一种碱性无机化合物。在另一个实施方案中,煅烧高岭土在至少一种碱性无机化合物之前加入。在还另一个实施方案中,煅烧高岭土可在至少一种碱性无机化合物之后加入。另外,硅橡胶制剂还可包括至少一种选自例如沉淀二氧化硅、结晶二氧化硅和热解法二氧化硅的另外填充剂。
[027]本文中,所有量、百分比和范围均表达为近似值。
[028]通过以下非限定性实施例进一步说明本发明,这些实施例仅仅用于作为本发明的示例。
实施例
实施例1:
[029]用分别相对于煅烧高岭土重量为2%重量的草酸铵处理的中值粒度约1.5μm的商品煅烧高岭土A、中值粒度约0.5μm的商品煅烧高岭土B和中值粒度约1.5μm的商品煅烧高岭土C,与硅橡胶制剂中中值粒度约1.0μm的商品热解法二氧化硅比较。商品煅烧高岭土A、B和C的样品分别在水中浆化,固体浓度为35%,然后搅拌淤浆,同时按相对于煅烧高岭土重量为2%重量的处理水平加入草酸铵溶液,允许反应约1小时。然后将该混合物在70-90℃时盘式干燥,并微粉化三次。硅橡胶制剂包含100phr的SWS-725、0.6phr的Luperox500 R(引发剂)和以下所示各种量的填充剂。用50phr、75phr和100phr的商品热解法二氧化硅作对照。用相对于煅烧高岭土重量为2%重量的草酸铵处理的50phr、75phr和100phr的各商品煅烧高岭土A、B或C用于比较。在实验室中,使用标准2-辊碾磨机,不加热进行混合。在340和1000psi下,将聚合物压模/固化10分钟。测定所得硅橡胶的物理特性,包括Shore“A”硬度、拉伸断裂强度(tensile atbreak)、断裂伸长率和100%、200%和300%时的模量。根据ASTM D2240用A型硬度计测量Shore“A”硬度。根据ASTM D 412方法A测量拉伸断裂强度和断裂伸长率。用Instron 1120装置测量100%、200%和300%时的模量。结果显示于表1。
[030]表1
[031]如表1所示,随着填充剂例如本发明的填充剂(即2%草酸铵处理的商品煅烧高岭土A、B和C)负载水平的增加,最终硅橡胶的shore″A″硬度和模量增加。本领域已知模量值表明抗拉伸的内部强度或能力。
[032]另外,如表1所示,在50phr、75phr或100phr的各混合水平,与本发明的填充剂即用2%草酸铵处理的商品煅烧高岭土A、B和C混合的最终硅橡胶的Shore“A”硬度和模量,优于与商品热解法二氧化硅混合的那些。因此,结果表明本文公开的无机物-中和的煅烧高岭土可用于替代热解法二氧化硅填充剂在硅橡胶制剂中的使用。
[033]除非另有说明,本说明书和权利要求书中使用的所有表示数量的数字应理解为在所有情况下均被术语″约″修正。因此,除非相反地说明,下面的说明书和权利要求书提出的数字参数均为近似值,可以根据本发明希望获得的理想特性而改变。
[034]本领域的技术人员通过考虑本说明书和实施本文所公开的发明,本发明的其它实施方案将是显而易见的。说明书和实施例仅作为示例考虑,本发明的真实范围和宗旨由权利要求限定。
Claims (48)
1.一种无机物-中和的煅烧高岭土,所述无机物-中和的煅烧高岭土包含用一定量的至少一种碱性无机化合物处理的煅烧高岭土,所述量足以降低该煅烧高岭土表面酸性部位的活性。
2.权利要求1的无机物-中和的煅烧高岭土,其中所述至少一种碱性无机化合物选自草酸铵、碳酸钠、氢氧化钠和磷酸三钠。
3.权利要求1的无机物-中和的煅烧高岭土,其中所述处理在离子化介质中进行。
4.权利要求3的无机物-中和的煅烧高岭土,其中所述离子化介质为水。
5.权利要求1的无机物-中和的煅烧高岭土,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量等于或大于0.1%重量。
6.权利要求5的无机物-中和的煅烧高岭土,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.1%-5.0%重量。
7.权利要求6的无机物-中和的煅烧高岭土,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.5%-2.5%重量。
8.权利要求7的无机物-中和的煅烧高岭土,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为2.0%重量。
9.一种包含无机物-中和的煅烧高岭土的组合物,其中所述无机物-中和的煅烧高岭土包含用一定量的至少一种无机化合物处理的煅烧高岭土,所述量足以降低该煅烧高岭土表面酸性部位的活性。
10.权利要求9的组合物,其中所述至少一种碱性无机化合物选自草酸铵、碳酸钠、氢氧化钠和磷酸三钠。
11.权利要求9的组合物,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量等于或大于0.1%重量。
12.权利要求11的组合物,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.1%-5.0%重量。
13.权利要求12的组合物,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.5%-2.5%重量。
14.权利要求13的组合物,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为2.0%重量。
15.一种产品,所述产品包含无机物-中和的煅烧高岭土,其中所述无机物-中和的煅烧高岭土包含用一定量的至少一种无机化合物处理的煅烧高岭土,所述量足以降低该煅烧高岭土表面酸性部位的活性。
16.权利要求15的产品,其中所述至少一种碱性无机化合物选自草酸铵、碳酸钠、氢氧化钠和磷酸三钠。
17.权利要求15的产品,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量等于或大于0.1%重量。
18.权利要求17的产品,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.1%-5.0%重量。
19.权利要求18的产品,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.5%-2.5%重量。
20.权利要求19的产品,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为2.0%重量。
21.权利要求15的产品,其中所述无机物-中和的煅烧高岭土在该产品中存在的浓度为1-200phr。
22.权利要求21的产品,其中所述无机物-中和的煅烧高岭土在该产品中存在的浓度为1-100phr。
23.权利要求15的产品,所述产品选自固化聚合物。
24.权利要求23的产品,其中所述固化聚合物选自自由基固化的聚合物和过氧化物固化的聚合物。
25.一种硅橡胶制剂,所述制剂包含:
至少一种包含无机物-中和的煅烧高岭土的填充剂,其中所述无机物-中和的煅烧高岭土包含用一定量的至少一种无机化合物处理的煅烧高岭土,所述量足以降低该煅烧高岭土表面酸性部位的活性;和
至少一种聚硅氧烷聚合物。
26.权利要求25的硅橡胶制剂,其中所述至少一种碱性无机化合物选自草酸铵、碳酸钠、氢氧化钠和磷酸三钠。
27.权利要求25的硅橡胶制剂,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量等于或大于0.1%重量。
28.权利要求27的硅橡胶制剂,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.1%-5.0%重量。
29.权利要求28的硅橡胶制剂,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.5%-2.5%重量。
30.权利要求29的硅橡胶制剂,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为2.0%重量。
31.权利要求25的硅橡胶制剂,其中所述无机物-中和的煅烧高岭土在该硅橡胶制剂中存在的浓度为1-200phr。
32.权利要求31的硅橡胶制剂,其中所述无机物-中和的煅烧高岭土在该硅橡胶制剂中存在的浓度为1-100phr。
33.一种无机物-中和的煅烧高岭土的制备方法,所述方法包括用一定量的至少一种无机化合物处理煅烧高岭土,所述量足以降低该煅烧高岭土表面酸性部位的活性,其中所述处理在离子化介质中进行。
34.权利要求33的方法,其中所述离子化介质为水性介质。
35.权利要求34的方法,其中所述离子化介质为水。
36.权利要求33的方法,其中所述处理操作包括用所述煅烧高岭土和水形成淤浆,并将所得的煅烧高岭土淤浆和所述至少一种无机化合物混合。
37.权利要求33的方法,其中所述至少一种碱性无机化合物选自草酸铵、碳酸钠、氢氧化钠和磷酸三钠。
38.权利要求33的方法,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量等于或大于0.1%重量。
39.权利要求38的方法,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.1%-5.0%重量。
40.权利要求39的方法,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为0.5%-2.5%重量。
41.权利要求40的方法,其中在所述处理中以煅烧高岭土计,所述至少一种碱性无机化合物的量为2.0%重量。
42.权利要求33的方法,所述方法还包括将所述用至少一种无机化合物处理的煅烧高岭土干燥和粉碎。
43.一种硅橡胶产品的制备方法,所述方法包括将无机物-中和的煅烧高岭土加入硅橡胶制剂中,其中所述硅橡胶制剂包含至少一种聚硅氧烷聚合物和至少一种引发剂,且所述无机物-中和的煅烧高岭土包含用一定量的至少一种碱性无机化合物处理的煅烧高岭土,所述量足以降低该煅烧高岭土表面酸性部位的活性。
44.权利要求43的方法,其中所述硅橡胶制剂还包含至少一种二氧化硅填充剂。
45.权利要求44的方法,其中所述至少一种二氧化硅填充剂选自沉淀二氧化硅、结晶二氧化硅和热解法二氧化硅。
46.一种硅橡胶产品的制备方法,所述方法包括将煅烧高岭土和一定量的至少一种碱性无机化合物加入硅橡胶制剂中,所述量足以降低所述煅烧高岭土表面酸性部位的活性,其中所述硅橡胶制剂包含至少一种聚硅氧烷聚合物和至少一种引发剂。
47.权利要求46的方法,其中所述硅橡胶制剂还包含至少一种二氧化硅填充剂。
48.权利要求47的方法,其中所述至少一种二氧化硅填充剂选自沉淀二氧化硅、结晶二氧化硅和热解法二氧化硅。
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EP (1) | EP1856212A1 (zh) |
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CN114316359A (zh) * | 2021-12-22 | 2022-04-12 | 内蒙古超牌新材料股份有限公司 | 低真密度高岭土橡胶补强填料及其制备方法 |
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GB0315409D0 (en) * | 2003-07-01 | 2003-08-06 | Imerys Minerals Ltd | Particulate clay materials and polymer compositions incorporating the same |
GB0328236D0 (en) * | 2003-12-05 | 2004-01-07 | Dow Corning | Method of making kaolin containing silicone rubber compositions |
EP1765201A4 (en) * | 2004-06-28 | 2013-01-23 | Arthrosurface Inc | SYSTEM FOR THE BENDING AREA |
USD900311S1 (en) | 2018-05-18 | 2020-10-27 | Baxter International Inc. | Dual chamber flexible container |
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US3573945A (en) * | 1965-07-06 | 1971-04-06 | Ppg Industries Inc | Process for improving pigmentary metal oxides |
US4677141A (en) * | 1981-01-26 | 1987-06-30 | Dow Corning Corporation | Method of improving heat stability of pigmentable silicone elastomer |
US4806167A (en) * | 1986-10-14 | 1989-02-21 | E.C.C. America Inc. | Kaolin aggregation using combination of organic and inorganic bases |
US5089056A (en) * | 1989-04-21 | 1992-02-18 | Thiele Kaolin Company | Opacifying kaolin pigments and process for making same by reacting with sodium hydroxide in water |
US20050203236A1 (en) * | 2004-03-09 | 2005-09-15 | Christina Prowell | Reinforcing filler for silicone rubber and sealants |
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CN114316359A (zh) * | 2021-12-22 | 2022-04-12 | 内蒙古超牌新材料股份有限公司 | 低真密度高岭土橡胶补强填料及其制备方法 |
CN114316359B (zh) * | 2021-12-22 | 2023-08-18 | 内蒙古超牌新材料股份有限公司 | 低真密度高岭土橡胶补强填料及其制备方法 |
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US20090023849A1 (en) | 2009-01-22 |
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