CN114423724A - 用于制造耐火陶瓷的未烧组合物 - Google Patents
用于制造耐火陶瓷的未烧组合物 Download PDFInfo
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- CN114423724A CN114423724A CN202080065529.5A CN202080065529A CN114423724A CN 114423724 A CN114423724 A CN 114423724A CN 202080065529 A CN202080065529 A CN 202080065529A CN 114423724 A CN114423724 A CN 114423724A
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Abstract
一种未烧陶瓷组合物,所述未烧陶瓷组合物包含:(i)陶瓷颗粒;(ii)合成聚合物粘合剂,所述合成聚合物粘合剂具有:(a)具有0℃以下的Tg的、来源于软单体的单体单元;(b)具有大于0℃的Tg的、来源于硬的非酸性单体的单体单元;(c)来源于酸性单体的单体单元;和(d)来源于羟基官能化单体的单体单元;以及(iii)水。
Description
本申请要求2019年9月20日提交的美国临时申请62/903,019号的优先权,以引用的方式将其全部内容并入本文。
技术领域
本发明的实施方式涉及未烧陶瓷组合物,所述未烧陶瓷组合物可特别用于制造烧成耐火陶瓷。在一个或多个实施方式中,未烧陶瓷组合物包含苯乙烯-丁二烯基胶乳粘合剂。
背景技术
陶瓷材料通常通过热处理未烧陶瓷组合物来制备,所述未烧陶瓷组合物通常包括无机氧化物,例如氧化镁、氧化铝、二氧化硅、二氧化钛和氧化锆。无机氧化物可连同添加剂(例如分散剂和粘合剂)一起以浆料形式提供。可喷雾干燥所述浆料以生产陶瓷颗粒。所述颗粒可被压制成具有所需形状的、被称为未烧陶瓷的骨料结构(aggregate structure),并随后进行被称为烧结的剧烈热处理。烧结过程将未烧陶瓷转化为具有近乎整体多晶陶瓷相的内聚烧成陶瓷。
粘合剂用于在压制后将未烧陶瓷的陶瓷颗粒保持在所需形状。粘合剂还可以在所述颗粒被压制时提供润滑作用。通常,粘合剂在烧结过程中完全燃烧或蒸发,在烧成陶瓷中不留下微量的粘合剂。尽管如此,粘合剂仍然会显著影响最终生产的烧成陶瓷的性能。
已知有合成聚合物粘合剂。例如,美国专利号5,358,911公开了一种粘合剂,所述粘合剂包含充分水解的乙烯基酯和N-乙烯基酰胺的共聚物。美国专利号3,472,803公开了水性苯乙烯-丁二烯共聚物胶乳乳液可以用作陶瓷粘合剂。特别地,在美国‘803公开了以商品名XR-3100和XR-3113市售的乳液,这些乳液以占最终组合物重量的4%至12%之间的量来提供。
美国专利号4,968,460公开了陶瓷粘合剂,例如包括丙烯酸酯类的酯;SBR型聚合物;乙烯醋酸乙烯酯;NBR;共轭二烯烃;氯乙烯和偏二氯乙烯的均聚物或共聚物;乙烯和偏二氯乙烯的共聚物;乙烯和氯乙烯的共聚物;以及乙烯基芳香聚合物的均聚物。所述粘合剂为乳液,该乳液通常具有约45%至60%的聚合物含量,并且,该聚合物具有-100℃至约+120℃的Tg。
仍然存在改进的粘合剂的需求,该改进的粘合剂为未烧陶瓷组合物和烧成陶瓷材料提供进一步的优点。
发明内容
本发明的一个或多个实施方式提供了一种未烧陶瓷组合物,所述未烧陶瓷组合物包含:i)陶瓷颗粒;ii)合成聚合物粘合剂,所述合成聚合物粘合剂具有:(a)来源于软单体的单体单元;(b)来源于硬的非酸性单体的单体单元;(c)来源于酸性单体的单体单元;和(d)来源于羟基官能化单体的单体单元;以及iii)水。
本发明的其它实施方式还提供了一种制备陶瓷产品的方法,所述方法包括以下步骤:i)将陶瓷颗粒与水性乳液掺混,从而形成未烧陶瓷组合物,所述水性乳液包含水和聚合物颗粒,所述聚合物颗粒具有:(a)来源于至少一种软单体的单体单元;(b)来源于至少一种硬的非酸性单体的单体单元;(c)来源于至少一种酸性单体的单体单元;和(d)来源于至少一种羟基官能化单体的单体单元;ii)将所述未烧陶瓷组合物成形为陶瓷生坯;以及iii)烧结所述陶瓷生坯。
附图说明
图1为示出了本发明实施例和比较例的粉碎细料和未烧断裂模量(MOR)的图。
图2为示出了本发明实施例和比较例的粉碎细料和未烧断裂模量(MOR)的图。
图3为示出了本发明实施例和比较例的挤出棒吸水率结果的图。
图4为示出了本发明实施例和比较例的挤出棒干燥收缩率和烧成收缩率结果的图。
图5为示出了本发明实施例和比较例的压制棒烧成断裂模量(MOR)结果的图。
具体实施方式
本发明的实施方式至少部分基于改进的未烧陶瓷组合物的发现。所述未烧陶瓷组合物可特别用于制造烧成耐火陶瓷。未烧陶瓷组合物包含合成聚合物粘合剂。所述聚合物粘合剂可为未烧陶瓷组合物和由该未烧陶瓷组合物制成的烧成耐火陶瓷提供有利的性能平衡,例如润滑性、粘合性、塑化性、分散性、压缩性、生坯强度、烧成强度和足够的烧除性。根据本发明的实施方式,所述聚合物粘合剂由胶乳提供,所述胶乳包含具有如下单体单元的聚合物颗粒:来源于至少一种软单体的单体单元;来源于至少一种硬的非酸性单体的单体单元;来源于至少一种酸性单体的单体单元;以及来源于至少一种羟基官能化单体的单体单元。在一个或多个实施方式中,所述聚合物粘合剂可包括苯乙烯-丁二烯基胶乳粘合剂。尽管现有技术教导了用于未烧陶瓷组合物的某些合成聚合物粘合剂,但相对于已知的合成聚合物粘合剂,本文公开的所述聚合物粘合剂提供了一个或多个优点。
未烧陶瓷组合物
本发明的未烧陶瓷组合物包含耐火基体成分(refractory base component)、合成聚合物粘合剂、任选的水以及任选的其它通常包含在未烧陶瓷组合物中的组分。
聚合物粘合剂
如上所提议的那样,所述合成聚合物粘合剂由胶乳提供,因此,所述聚合物粘合剂可称为胶乳粘合剂或乳液粘合剂。本领域技术人员理解,胶乳是一种水性乳液,其中聚合物颗粒分散在水中(即,聚合物颗粒和水的非均相混合物)。在一个或多个实施方式中,乳液中可存在两种或多种组成不同的聚合物颗粒的混合物。
在一个或多个实施方式中,胶乳的聚合物颗粒的特征在于:具有约-50℃至约60℃、在其它实施方式中约-45℃至约85℃、在其它实施方式中约-10℃至约40℃、在其它实施方式中约-15℃至约25℃以及在其它实施方式中约18℃至约20℃的Tg。在一个或多个实施方式中,所述聚合物颗粒的特征在于:具有约20℃的Tg。可使用DSC技术基于胶乳的干燥样品或膜测定Tg。
在一个或多个实施方式中,胶乳的聚合物颗粒的特征在于:基于颗粒的总重量,具有约55%至约100%、在其它实施方式中约70%至约95%、在其它实施方式中约75%至约90%、在其它实施方式中约60%至约90%的凝胶含量。可根据溶剂(如THF或甲苯)中的不溶性组分测定凝胶。
在一个或多个实施方式中,胶乳的聚合物颗粒的特征在于:具有约50nm至约350nm、在其它实施方式中约70nm至约300nm、在其它实施方式中约125nm至约250nm、在其它实施方式中约160nm至约220nm的算术平均粒径(mean average particle size)。在一个或多个实施方式中,聚合物颗粒的特征在于:具有约165nm、在其它实施方式中约220nm、在其它实施方式中约180nm的算术平均粒径。可根据一般已知的试验测定算术平均粒径。
在一个或多个实施方式中,胶乳的特征在于:具有约5.5至约11.0、在其它实施方式中约6.0至约9.5、在其它实施方式中约7.5至约10、在其它实施方式中约8至约9的pH。在一个或多个实施方式中,可通过添加一种或多种碱中和胶乳粘合剂,所述碱例如氢氧化钾、碳酸氢钠、氢氧化铵、氢氧化钠、有机胺(例如三甲胺)和2-氨基-2-甲基-1-丙醇(以商品名AMP-95TM市售)。可根据本领域技术人员通常已知的试验测定pH。
在一个或多个实施方式中,胶乳的特征在于:具有约25cps至约3000cps、在其它实施方式中约50cps至约1500cps、在其它实施方式中约15cps至约500cps、在其它实施方式中约15cps至约3000cps的粘度。在一个或多个实施方式中,胶乳的特征在于:具有小于1000cps、在其它实施方式中小于500cps、在其它实施方式中小于300cps的粘度。可在25℃下使用布鲁克菲尔德粘度计测定粘度。
在一个或多个实施方式中,胶乳的特征在于:具有约30wt.%至约65wt.%、在其它实施方式中约40wt.%至约60wt.%、在其它实施方式中约44wt.%至约56wt.%的固体含量。固体含量可通过使用干燥胶乳粘合剂样品的微波CEM或烘箱进行测定,所述样品通过重量分析进行称重,直到获得恒定重量。
在一个或多个实施方式中,从其中获得聚合物粘合剂的胶乳包含聚合物颗粒,所述聚合物颗粒具有来源于至少一种软单体的单体单元、来源于至少一种硬的非酸性单体的单体单元、来源于至少一种酸性单体的单体单元以及来源于至少一种羟基官能化单体的单体单元。在一个或多个实施方式中,水性乳液包含一种或多种表面活性剂。
软单体包括在聚合(即,均聚)时产生弹性聚合物或具有低于约0℃、优选低于约-35℃、且更优选低于约-55℃的Tg的聚合物的那些单体。合适的软单体包括共轭二烯、丙烯酸丁酯、丙烯酸2-乙基己酯、丙烯酸羟乙酯、二甲基丙烯酸酯、聚乙二醇二丙烯酸酯、丙烯酸烷基酯、叔碳酸乙烯酯(vinyl versatates)衍生的单体以及它们的混合物。示例性的共轭二烯包括1,3-丁二烯、异戊二烯、1,3-戊二烯、1,3-己二烯、2,3-二甲基-1,3-丁二烯、2-乙基-1,3-丁二烯、2-甲基-1,3-戊二烯、3-甲基-1,3-戊二烯、4-甲基-1,3-戊二烯和2,4-己二烯。
硬的非酸性单体包括不含羧酸官能团且在聚合(即,均聚)时产生热塑性聚合物或具有超过约0℃、优选超过约75℃、且更优选超过约90℃的Tg的那些聚合物的那些单体。合适的硬的非酸性单体包括乙烯基芳香单体,例如苯乙烯、α-甲基苯乙烯、叔丁基苯乙烯、烷基取代的苯乙烯、二乙烯基苯和多不饱和二乙烯基化合物。其它合适的硬的非酸性单体包括丙烯酸酯,例如甲基丙烯酸甲酯、甲基丙烯酸丁酯,醋酸乙烯酯及它们的混合物。其它合适的硬的非酸性单体还包括丙烯酰胺,例如甲基丙烯酰胺,2-丙烯酰胺基-2-甲基丙烷磺酸以及该酸的盐(例如,钠、钾或铵盐)。
酸性单体包括既具有羧酸基团、又具有可聚合基团的那些单体。酸性单体可以包括硬单体和软单体两种。合适的酸性单体包括α,β-不饱和羧酸和乙烯基叔碳酸(vinylversatic acids)。示例性α,β-不饱和羧酸包括衣康酸、甲基丙烯酸、柠康酸、肉桂酸、丙烯酸、富马酸、马来酸和来源于酸酐(例如马来酸酐)的酸。
羟基官能化单体包括具有羟基官能团的那些单体,其中羟基官能团不与附加的酸基团结合(即,不发生空间相互作用)。某些羟基官能化单体还可包括羟基官能团与羰基不共享碳原子的那些单体。某些羟基官能化单体还可以包括不包含附加的酸基团的那些单体。
在一个或多个实施方式中,羟基官能化单体可由下式定义:
其中,R1为酯键或亚烃基,并且其中,R2为氢或甲基。在特定的实施方式中,R1为酯键或芳香基。在一个或多个实施方式中,R1通常以使得1-二烯双键与聚合物主链反应的化合物为特征。酯键中烷氧基的示例性烷基包括乙基和丙基。R1的示例性芳香基包括苄基和苯基。
在特定的实施方式中,R1为烷氧基中具有乙基的酯键,且R2为氢,使得羟基官能化单体为丙烯酸羟乙酯。
在一个或多个实施方式中,R1为烷氧基中具有乙基的酯键,且R2为甲基,使得羟基官能化单体为甲基丙烯酸羟乙酯。
在一个或多个实施方式中,R1为苯基,且R2为氢,使得羟基官能化单体为羟基苯乙烯。羟基苯乙烯可以为4-羟基苯乙烯或3-羟基苯乙烯。
在一个或多个实施方式中,如本领域技术人员通常所知,羟基官能化单体由环氧化物在两步反应中制成。
如本领域所知,可调整用于合成聚合物颗粒的各种单体的相对量,以实现本文所述的期望的性能。此外,还可以调控转化时间、聚合温度、链转移剂的类型和水平等,尤其是控制凝胶度。
在一个实施方式中,基于聚合物颗粒的总重量,聚合物颗粒可包含约5wt.%至约75wt.%、在其它实施方式中约15wt.%至约60wt.%、在其它实施方式中约15wt.%至约45wt.%以及在其它实施方式中约20wt.%至约45wt.%的来源于软单体的单元。
在一个实施方式中,基于聚合物颗粒的总重量,聚合物颗粒可包含约25wt.%至约95wt.%、在其它实施方式中约40wt.%至约85wt.%、在其它实施方式中约45wt.%至约85wt.%以及在其它实施方式中约55wt.%至约80wt.%的来源于硬的非酸性单体的单元。
在一个或多个实施方式中,基于聚合物颗粒的总重量,聚合物颗粒可包含约0.05wt.%至约12wt.%、在其它实施方式中约0.1wt.%至约12wt.%、在其它实施方式中约0.1wt.%至约5wt.%以及在其它实施方式中约0.1wt.%至约2wt.%的含酸官能团(即,羧酸基)的单元。在一个或多个实施方式中,基于聚合物颗粒的总重量,聚合物颗粒可包含小于10wt.%、在其它实施方式中小于8wt.%、在其它实施方式中小于5wt.%的带有酸官能团(即,羧酸基)的单元。可根据合成聚合物所用的含酸单体的重量或通过FTIR技术测定酸含量。
在一个实施方式中,基于聚合物颗粒的总重量,聚合物颗粒可包含约0.1wt.%至约10wt.%、在其它实施方式中约0.1wt.%至约8wt.%、在其它实施方式中约0.5wt.%至约6wt.%以及在其它实施方式中约1.0wt.%至约4wt.%的来源于软单体的单元。
在特定的实施方式中,胶乳粘合剂包含具有来源于1,3-丁二烯的单体单元、来源于苯乙烯的单体单元、来源于衣康酸的单体单元、来源于甲基丙烯酸的单体单元、来源于丙烯酸羟乙酯的单体单元以及来源于烷基硫醇的单体单元的聚合物颗粒。
胶乳粘合剂的制备方法
在一个或多个实施方式中,可通过采用常规乳液聚合技术制备提供胶乳粘合剂的胶乳组合物。乳液聚合在美国专利号5,166,259和6,425,978中描述,其通过引用并入本文。
在一个或多个实施方式中,乳液聚合技术可利用单次进料间歇聚合法,在其它实施方式中可以使用可采用连续搅拌反应釜(CSTR)的连续系统,在其它实施方式中可以使用半间歇或连续进料法,在其它实施方式中可以使用增量法。在一个或多个实施方式中,通过采用增量聚合技术制备聚合物颗粒。在一个或多个实施方式中,这包括使用聚合物种子,例如在合适的表面活性剂存在下,通过衣康酸和苯乙烯聚合制备的聚合物种子。一旦制备所述种子后,加入增量添加的软单体、硬的非酸性单体、酸性单体、羟基官能化单体、引发剂、链转移剂和表面活性剂。美国专利号6,425,978中记载了相似技术,该专利通过引用并入本文中。
在一个或多个实施方式中,聚合物颗粒的聚合可在约45℃至约90℃、在其它实施方式中在约55℃至约75℃的温度下进行。
通常,有用的聚合法采用自由基引发剂的使用,在表面活性剂存在下引发单体聚合。在一个或多个实施方式中,可采用自由基引发剂。
在一个或多个实施方式中,示例性的有用的自由基引发剂包括过硫酸铵、过硫酸钠、过硫酸钾、叔丁基过氧化氢和二叔丁基异丙苯。可以使用多种自由基引发剂。在一个或多个实施方式中,所述引发剂可与一种或多种还原剂(例如铁盐、胺、抗坏血酸、抗坏血酸钠盐和甲醛次硫酸钠)结合使用。可以使用任意适当量的引发剂和还原剂。
在一个或多个实施方式中,有用的表面活性剂包括磺基琥珀酸烷基酯的碱金属盐。合适的磺基琥珀酸烷基酯的碱金属盐包括磺基琥珀酸二己酯钠、磺基琥珀酸二辛酯钠、辛烷磺酸钠、烷基酚乙氧基化物、脂肪醇乙氧基化物、烷基聚葡糖苷、烷基磷酸酯。合适的表面活性剂包括商标名为AerosolTM MA-80(Cytec)、GemtexTM 80(Finetex)和MM-80TM(Uniqema)的那些表面活性剂。
在一个或多个实施方式中,有用的表面活性剂包括烷基硫酸酯的盐和有机二磺酸酯的盐。合适的烷基硫酸酯的盐包括十二烷基硫酸钠、以商品名为Stepanol WA和TexaponTM(Cognis)、PolystepTM B-3(Stepan)、PolystepTM B-5(Stepan)或RhodaponTM UB(Rhodia)获得。合适的有机二磺酸酯的盐包括十二烷基二苯醚二磺酸钠,以商品名Dowfax 2A1以及StepanolTM AM、PolystepTM B-7(Stepan)、RhodaponTM L-22EP(Rhodia)、DowfaxTM 2A1(Dow)、CalfaxTM DB-45(Pilot)、RhodacalTM DSB(Rhodia)和AerosolTM DPOS-45(Cytec)获得。
其它合适的表面活性剂包括月桂醇聚醚硫酸钠、月桂醇聚醚-3(又名三甘醇十二烷基醚)、月桂醇聚醚-4(又名PEG-4月桂基醚)、月桂醇聚醚-5(又名PEG-5月桂基醚)、月桂醇聚醚-6(又名PEG-6月桂基醚)、月桂醇聚醚-7(又名PEG-7月桂基醚)、月桂基醚硫酸钠、月桂醇聚醚-12硫酸钠(又名PEG(12)月桂基醚硫酸盐)和月桂醇聚醚-30硫酸钠(又名PEG(30)月桂基醚硫酸盐)。其它醚烷基硫酸盐以商品名为PolystepTM B40(Stepan)和GenapolTMTSM获得。
除上述表面活性剂外,可与乳液聚合一起使用的其它表面活性剂(除所述表面活性剂外或代替所述表面活性剂)包括烷基硫酸酯/盐、磺基琥珀酸烷基酯/盐、磺酸烷基芳基酯/盐、α-烯烃磺酸酯/盐、脂肪酸盐或松香酸盐、NPE、磺酸烷基芳基酯/盐、烷基酚乙氧基化物和脂肪醇乙氧基化物。在一个或多个实施方式中,表面活性剂包括磺基琥珀酸二己酯钠和磺基琥珀酸二辛酯钠的混合物。可以调整混合物以控制或获得所需的临界胶束浓度。
在一个或多个实施方式中,基于水性乳液的总重量,水性乳液可包括约0.1wt.%至约10wt.%、在其它实施方式中约1wt.%至约6wt.%以及在其它实施方式中约2wt.%至约4wt.%的表面活性剂。换言之,在一个或多个实施方式中,表面活性剂以约0.2重量份表面活性剂/100重量份聚合物至约1.0重量份表面活性剂/100重量份聚合物、在其它实施方式中以约0.25重量份表面活性剂/100重量份聚合物至约0.65重量份表面活性剂/100重量份聚合物、在其它实施方式中以约0.35重量份表面活性剂/100重量份聚合物至约0.55重量份表面活性剂/100重量份聚合物、在其它实施方式中以约0.40重量份表面活性剂/100重量份聚合物至约0.50重量份表面活性剂/100重量份聚合物以及在其它实施方式中以约0.44重量份表面活性剂/100重量份聚合物至约0.48重量份表面活性剂/100重量份聚合物的量存在,其中表面活性剂重量份指活性表面活性剂含量。
根据所使用的聚合技术,更具体而言,根据所使用的表面活性剂的类型和数量,上述聚合产生的胶乳可以用作未烧陶瓷组合物的胶乳粘合剂组合物。作为一种选择,可在聚合后添加表面活性剂以形成胶乳粘合剂组合物。在一个或多个实施方式中,该表面活性剂可以是本文所述的胶乳粘合剂中的相同表面活性剂。
在一个或多个实施方式中,聚合中使用链转移剂。可使用共轭二烯单体的乳液聚合中通常使用的任意链转移剂。示例性链转移剂包括烷基硫醇(例如,以商品名SulfoleTM市售)、四氯化碳、四溴化碳、C2-C22正烷基醇、C2-C22支链醇和2,4-二苯基-4-甲基-1-戊烯。
在一个或多个实施方式中,基于聚合物颗粒的总重量,聚合物颗粒包含约0至约2.5wt.%、在其它实施方式中约0至约1.5wt.%以及在其它实施方式中约0.2wt.%至约1.0wt.%的链转移剂。
在一个或多个实施方式中,尤其是在胶乳粘合剂发泡的情况下,胶乳粘合剂可包含特征为起泡剂的一种或多种表面活性剂。合适的起泡剂包括磺基琥珀酸单酰硬脂胺二钠,以商品名AerosolTM 18、AerosolTM A18P(Cytec)、MonawetTM SNO(Uniqema)、OctosolTM18(Tiarco)和StanfaxTM 318、StanfaxTM 319、StanfaxTM 377(Para-Chem)获得。这些特征为起泡剂的表面活性剂可与上述一种或多种表面活性剂或者增稠剂(例如羧甲基纤维素钠)结合使用。
耐火基体成分
如上所述,本发明的未烧陶瓷组合物包含耐火基体成分。在一个或多个实施方式中,未烧陶瓷组合物包含两种或多种耐火基体成分。
合适的耐火基体成分也可称为陶瓷颗粒、陶瓷材料或陶瓷基体成分,包括但不限于镁氧化物(氧化镁)、铝氧化物(氧化铝)、硅氧化物(二氧化硅)、钛氧化物、锆氧化物、铁氧化物、钙氧化物、氢氧化钙、粘土、砖材料或其两种或多种的混合物。一种或多种耐火基体成分也可以水提供,所述水独立于一种或多种胶乳粘合剂的水。在一个或多个实施方式中,一种或多种耐火基体成分作为含水化合物(例如水合硅酸铝(Al2O3·2SiO2·2H2O))提供。
如本领域技术人员通常所知,粘土是一种细粒度的天然岩石或土壤材料,其包括一种或多种粘土矿物且具有可选的微量石英(SiO2)、金属氧化物(例如,Al2O3、MgO)和有机物质。如本领域技术人员通常所知,粘土矿物是含水的层状硅酸铝,任选地含有铁、镁、碱金属、碱土金属和其它阳离子。
在一个或多个实施方式中,陶瓷颗粒的特征在于其算术平均粒径为约2微米至约45微米、在其它实施方式中约20微米至约150微米、在其它实施方式中约45微米至约2,000微米,在其它实施方式中约2微米至约2,000微米。
在一个或多个实施方式中,耐火基体成分可包括砖组合物。砖材料可包括例如粘土、含粘土的土壤、砂、混凝土及其混合物。
在一个或多个实施方式中,一种或多种耐火基体成分可包含低粘土、高氧化铝(alumina)组合物。在一个或多个实施方式中,基于耐火基体成分的总重量,低粘土、高氧化铝组合物可包含约0%至30%的粘土以及约100%至85%的氧化铝。
在一个或多个实施方式中,一种或多种耐火基体成分可包含高粘土、低氧化铝组合物。在一个或多个实施方式中,基于耐火基体成分的总重量,高粘土、低氧化铝组合物可包含约70%至100%的粘土以及约28%至45%的氧化铝。
在一个或多个实施方式中,一种或多种耐火基体成分可包含非粘土碱性砖组合物。在一个或多个实施方式中,基于耐火基体成分的总重量,非粘土碱性砖组合物可包含约0%至5%的粘土以及约95%至100%的金属氧化物,例如单独或组合的镁氧化物、铬氧化物、钙氧化物、白云石;或金属硅酸盐,例如硅酸锆。
在一个或多个实施方式中,一种或多种耐火基体成分可包含耐火粘土组合物。如本领域技术人员通常所知,耐火粘土通常可描述为由含有或不含有游离二氧化硅的水合硅酸铝(Al2O3·2SiO2·2H2O)组成的矿物骨料。在一个或多个实施方式中,基于耐火基体成分总重量,耐火粘土组合物可包含约20%至40%的Al2O3和约45%至65%的SiO2。
在一个或多个实施方式中,一种或多种耐火基体成分可以可挤出组合物为特征。在一个或多个实施方式中,一种或多种耐火基体成分可以可挤出氧化铝基组合物为特征。在一个或多个实施方式中,基于未烧陶瓷组合物的总重量,可挤出氧化铝基组合物可包含约0%至25%的单独或组合的粘土、金属氧化物和金属硅酸盐以及约75%至100%的氧化铝。
在一个或多个实施方式中,一种或多种耐火基体成分可包含高氧化铝粉末组合物。在一个或多个实施方式中,基于未烧陶瓷组合物的总重量,高氧化铝粉末组合物可包含约0%至25%的单独或组合的粘土、金属氧化物和金属硅酸盐以及约75%至100%的氧化铝。
未烧陶瓷组合物的其它成分
除了耐火基体成分、合成聚合物粘合剂和任选的水之外,本发明的未烧陶瓷组合物还可包含未烧陶瓷组合物中通常使用的其它成分。
在一个或多个实施方式中,未烧陶瓷组合物还包含一种或多种附加的粘合剂。合适的附加的粘合剂包括聚乙烯醇、改性玉米淀粉和糊精。
在一个或多个实施方式中,未烧陶瓷组合物还包含一种或多种附加的增塑剂。合适的附加的增塑剂是甲基纤维素。
在一个或多个实施方式中,未烧陶瓷组合物还包含一种或多种附加的润滑剂。合适的附加的润滑剂包括硬脂酸钠。
在一个或多个实施方式中,胶乳粘合剂为未烧陶瓷组合物提供合适的润滑性能、粘合及塑化性能,使得未烧陶瓷组合物可以不含或基本上不含附加的粘合剂、附加的增塑剂和附加的润滑剂。
未烧陶瓷成分含量
本领域技术人员理解,原始的合成胶乳的固体部分包括聚合物颗粒和胶乳中残余量的其它固体(例如表面活性剂)。因此,可参照胶乳固体,其包括胶乳的固体部分,而所述胶乳包含合成聚合物粘合剂。
在一个或多个实施方式中,基于胶乳固体和一种或多种耐火基体成分的总重量,本发明的未烧陶瓷组合物可包含约0.1wt.%至约1wt.%、在其它实施方式中约0.5wt.%至约5wt.%、在其它实施方式中约0.07wt.%至约3wt.%以及在其它实施方式中约0.1wt.%至约5wt.%的胶乳固体。就本说明书而言,胶乳固体和耐火基体成分可称为干的未烧陶瓷组合物。未烧陶瓷组合物和陶瓷生坯的成形方法
在一个或多个实施方式中,未烧陶瓷组合物可通过将耐火基体成分(即,陶瓷颗粒)与本文所述的合成胶乳合并而形成。在一个或多个实施方式中,这可产生陶瓷颗粒和胶乳聚合物的浆料。可对陶瓷颗粒和胶乳的混合物进行掺混,以将胶乳聚合物和/或陶瓷颗粒分布在整个组合物中。可以添加和掺混水以及其它任选组分。
在一个或多个实施方式中,通过合并陶瓷颗粒和胶乳所形成的组合物(例如,浆料)可被干燥以形成未烧陶瓷颗粒,所述未烧陶瓷颗粒可包含与来自胶乳的合成胶乳聚合物接触、或者被合成胶乳聚合物涂覆或部分涂覆的陶瓷颗粒。在一个或多个实施方式中,这些未烧陶瓷颗粒可通过浆料或其它载水(water-laden)组合物的喷雾干燥形成。
在一个或多个实施方式中,经干燥或未经干燥的未烧陶瓷组合物可成形为具有所需形状的陶瓷生坯。例如,浆料形式的未烧陶瓷组合物可同时(例如在模具中)经历成形和脱水以成形为陶瓷生坯。在其它实施方式中,可将未烧陶瓷颗粒(例如,通过喷雾干燥获得的未烧陶瓷颗粒)压制成所需形状以成形为陶瓷生坯。在一个或多个实施方式中,未烧陶瓷组合物可以是可挤出组合物的形式,所述可挤出组合物可以被挤出以成形为陶瓷生坯。在一个或多个实施方式中,未烧陶瓷组合物或未烧陶瓷颗粒可以可注射组合物提供,其可被注射模塑以成形为陶瓷生坯。
随后可对陶瓷生坯进行已知为烧结的剧烈热处理。烧结过程使得陶瓷生坯的胶乳粘合剂燃烧或蒸发,从而将陶瓷生坯转化为内聚烧成陶瓷产品。烧成陶瓷产品可具有整体或近乎整体的多晶陶瓷相。
烧成陶瓷产品的合适形式包括耐火砖、耐火板、陶瓷薄壁催化剂载体构件(例如,汽车催化转化器结构)、陶瓷支撑剂颗粒、催化剂载体和瓷砖。
未烧陶瓷组合物的性能
如本文所公开,本发明的胶乳粘合剂尤其可用于粘合未烧陶瓷组合物。未烧陶瓷组合物可通过其性能来表征。
在一个或多个实施方式中,未烧陶瓷组合物可由未烧断裂模量(Modulus ofRupture,MOR)表征。未烧MOR可通过三点弯曲试验的ASTM C674测定。在一个或多个实施方式中,未烧MOR可以为至少0.4磅力(lbf),在其它实施方式中,至少为0.45lbf,在其它实施方式中,至少为0.5lbf。
烧成陶瓷性能
在一个或多个实施方式中,烧成陶瓷产品可由烧成吸水率表征。将烧成样品放入沸水中2小时,接着浸泡24,可测定烧成吸水率。较低的吸水率表明:在使用中采用烧成陶瓷产品时,坯体更致密,被热金属或腐蚀性气体穿透的机会更小。
在一个或多个实施方式中,烧成陶瓷产品可通过烧成断裂模量(MOR)来表征。烧成MOR可通过三点弯曲试验的ASTM C674测定。
其它-整体耐火材料
在一个或多个实施方式中,本文所述的胶乳粘合剂可用作独立干式粘合剂(separate dry binder)的助流剂。许多传统的粘合剂以干式发货并且随后被水活化。在整体耐火材料(例如浇注料、喷补混合料和修补混合料)的制造中尤其如此。在一个或多个实施方式中,本文所述的胶乳粘合剂可用于水活化干式粘合剂。
工业实用性
在一个或多个实施方式中,本发明作为提供未烧陶瓷组合物具有工业实用性,其可特别用于制造烧成耐火陶瓷。
实施例
实施例1
使用通常已知为羧基化、非羟基官能化胶乳的胶乳来制备比较例1和比较例2样品。根据本发明的上述描述使用胶乳制备本发明实施例1样品,因此,可称之为使用了羧基化、羟基官能化的胶乳。详情示于表1。
所有陶瓷样品均按照本领域技术人员通常所知的方法制备,用于粉碎细料%试验和生坯强度试验。生坯强度按照ASTM C674进行。相对于胶乳粘合剂和一种或多种耐火基体成分(即,干的未烧陶瓷组合物),每个样品在不同的胶乳粘合剂wt.%下进行试验。该试验是在粘合剂干基的基础上,以轻质支撑剂(LWP)进行造粒试验。
表1
如下表2所示、并如图1进一步所示,相较于比较例1和比较例2,本发明实施例1具有更低的粉碎细料%和更高的生坯强度。
表2
实施例2
比较例样品包括商业上通常用作陶瓷粘合剂的某些材料以及其它对比材料。比较例包括:仅水、0.5wt.%PVA、1.0wt.%PVA、1wt.%改性玉米淀粉、2wt.%改性玉米淀粉、4wt.%改性玉米淀粉、0.5wt.%糊精。
根据本发明的上述描述,使用胶乳制备本发明实施例1样品。相对于胶乳粘合剂和一种或多种耐火基体成分(即,干的未烧陶瓷组合物),以0.2wt.%胶乳、0.3wt.%胶乳、0.5wt.%胶乳和1.0wt.%胶乳制备本发明实施例样品。
所有样品均按照本领域技术人员通常所知的方式制备,用于各自的试验。
粉碎细料%和生坯强度结果示于下表3中,并进一步示于图2中。生坯强度按照ASTM C674进行。
表3
挤出棒吸水率结果示于下表4和图3中。低吸水率是通过将烧成样品放在沸水中2小时、然后浸泡24来测定,这是用于确定样品孔隙率的标准试验。低吸水率表明:在使用中,坯体更致密,被热金属或腐蚀性气体穿透的机会更小。
表4
挤出棒的干燥收缩率和烧成收缩率结果示于下表5和图4中。在确定挤出颗粒填充时,未处理至干燥的烧成收缩率很重要。较低的值表明:干燥过程中用于收缩的孔隙小。更致密的干燥坯体也会带来较低的烧成收缩率。在两种情况下,低收缩率将会带来加工过程中的较少缺陷。
表5
压制棒烧成断裂模量(MOR)结果示于下表6和图5中。使用的压制压力分别为10,000psi和15,000psi。
表6
在不脱离本发明的范围和精神下,各种修改和变更对于本领域技术人员而言是显而易见的。本发明不应当受限于本文所述的示例性实施例。
Claims (16)
1.一种未烧陶瓷组合物,所述未烧陶瓷组合物包含:
i.陶瓷颗粒;
ii.合成聚合物粘合剂,所述合成聚合物粘合剂具有:
(a)来源于软单体的单体单元;
(b)来源于硬的非酸性单体的单体单元;
(c)来源于酸性单体的单体单元;和
(d)来源于羟基官能化单体的单体单元;以及,
iii.水。
2.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,所述合成聚合物粘合剂粘合所述陶瓷颗粒。
3.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,所述软单体为1,3-丁二烯。
4.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,所述硬的非酸性单体为苯乙烯。
5.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,所述酸性单体为衣康酸。
7.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,所述羟基官能化单体为丙烯酸羟乙酯。
8.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,所述合成聚合物粘合剂具有-15℃至60℃的Tg。
9.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,基于所述合成聚合物粘合剂的总重量,所述来源于软单体的单体单元以约15wt.%至约45wt.%的量存在。
10.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,基于所述合成聚合物粘合剂的总重量,所述来源于硬的非酸性单体的单体单元以45wt.%至85wt.%的量存在。
11.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,基于所述合成聚合物粘合剂的总重量,所述来源于酸性单体的单体单元以0.1wt.%至12wt.%的量存在。
12.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,基于所述合成聚合物粘合剂的总重量,所述来源于羟基官能化单体的单体单元以0.1wt.%至8wt.%的量存在。
13.如上述权利要求中任一项所述的未烧陶瓷组合物,其中,基于所述合成聚合物粘合剂和所述陶瓷颗粒的总重量,所述合成聚合物粘合剂以约0.1wt.%至约5wt.%的量存在。
14.如上述权利要求中任一项所述的未烧陶瓷组合物,所述合成聚合物粘合剂来源于具有算术平均粒径为50nm至350nm的聚合物颗粒的胶乳。
15.一种由上述权利要求中任一项所述的未烧陶瓷组合物制成的烧成陶瓷产品。
16.一种制造陶瓷产品的方法,所述方法包括以下步骤:
i.将陶瓷颗粒与水性乳液掺混,从而形成未烧陶瓷组合物,所述水性乳液包含水和聚合物颗粒,所述聚合物颗粒具有:
(a)来源于至少一种软单体的单体单元;
(b)来源于至少一种硬的非酸性单体的单体单元;
(c)来源于至少一种酸性单体的单体单元;和
(d)来源于至少一种羟基官能化单体的单体单元;
ii.将所述未烧陶瓷组合物成形为陶瓷生坯;以及,
iii.烧结所述陶瓷生坯。
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PCT/US2020/051752 WO2021055928A1 (en) | 2019-09-20 | 2020-09-21 | Green compositions for making refractory ceramic |
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2020
- 2020-09-21 BR BR112022004991A patent/BR112022004991A2/pt not_active Application Discontinuation
- 2020-09-21 CN CN202080065529.5A patent/CN114423724A/zh active Pending
- 2020-09-21 WO PCT/US2020/051752 patent/WO2021055928A1/en unknown
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- 2020-09-21 JP JP2022517808A patent/JP2022548380A/ja active Pending
- 2020-09-21 EP EP20786646.8A patent/EP4031510A1/en active Pending
- 2020-09-21 US US17/762,066 patent/US20220371965A1/en active Pending
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GB2167741A (en) * | 1984-10-16 | 1986-06-04 | Mitsui Toatsu Chemicals | Ceramics-forming composition |
US5057360A (en) * | 1987-10-23 | 1991-10-15 | Nippon Shokubai Kagaku Kogyo Co., Ltd. | Ceramic green sheet |
DE19811008C1 (de) * | 1998-03-13 | 2000-01-20 | Univ Bayreuth | Schlickerzusammensetzung und Verfahren zur Herstellung maschinell bearbeitbarer keramischer Grünkörper sowie damit hergestellter Grünkörper |
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KR20220062648A (ko) | 2022-05-17 |
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US20220371965A1 (en) | 2022-11-24 |
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