CN106660799A - 催化剂颗粒及其生产方法 - Google Patents
催化剂颗粒及其生产方法 Download PDFInfo
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- CN106660799A CN106660799A CN201580030524.8A CN201580030524A CN106660799A CN 106660799 A CN106660799 A CN 106660799A CN 201580030524 A CN201580030524 A CN 201580030524A CN 106660799 A CN106660799 A CN 106660799A
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Abstract
本发明公开了一种用于生产催化剂颗粒的方法。该方法包括:形成包含溶剂和含催化剂物质的材料的溶液,其中使含催化剂物质的材料溶解或乳化在溶剂中,雾化所形成的溶液以产生包含含催化剂物质的材料的液滴,和处理该液滴,以从该包含在液滴中的含催化剂物质的材料产生催化剂颗粒或中间体催化剂颗粒。本发明还公开了用于生产纳米材料的方法,用于生产催化剂颗粒的设备、催化剂颗粒和溶液液滴。
Description
发明领域
本发明涉及微米和纳米级颗粒及其生产方法。更具体地,本发明涉及催化剂颗粒及其制备方法。
背景技术
纳米材料包括广泛的结构和形态,包括膜、片(platelets)、球体和甚至更复杂的形状,例如纳米立方体、纳米锥和纳米星。许多这些纳米材料可以在涉及具有不同于目标纳米材料的给定组成的催化剂颗粒的催化反应中产生。这些催化产生的纳米材料的特殊子类是高纵横比分子结构(HARM),例如碳纳米管(CNT)、碳纳米芽(CNB)、银纳米线(AgNW)和其它纳米管,纳米线和纳米带型结构。基于HARM的透明和导电以及半导体的薄膜对于诸如晶体管、印刷电子、触摸屏、传感器、光子器件、用于太阳能电池的电极、闪电、感测和显示器件的许多应用是重要的。较厚和多孔的HARM膜也可用于例如燃料电池和水净化。对于透明电极应用,HARM薄膜相对于现有ITO薄层的主要优点是其改善的柔性,同时具有类似的透明度。碳供应也比铟供应更便宜和更容易获得。
本领域已知的催化剂生产方法通常包括用于气溶胶催化剂生产的物理气相成核和用于CVD催化剂生产的固溶体中的氧化物的还原。特别地,诸如已经包括预制的催化剂颗粒的溶液蒸发的方法已经用于生产气相中的催化剂颗粒。然而,本领域已知的方法产生具有通常不可预测的形状、尺寸和其它控制不良的性质的催化剂颗粒。本领域已知的催化剂颗粒包括镍、钴和铁颗粒。
发明概述
在该部分中,描述了权利要求中限定的本发明的主要实施方案,并且给出了某些定义。
根据本发明的第一方面,公开了一种用于生产催化剂颗粒的方法。该方法包括:形成包含溶剂和含催化剂物质的材料的溶液,其中使含催化剂物质的材料溶解或乳化在溶剂中,雾化(aerosolizing)所形成的溶液以产生包含含催化剂物质的材料的液滴,和处理该液滴,以从包含在液滴中的含催化剂物质的材料产生催化剂颗粒或中间体催化剂颗粒。
溶液在这里应理解为是指一种或多种成分的任何组合,其中至少一种成分是液体、凝胶、浆液或糊剂形式。根据本发明,溶剂包括将材料分散在液相中的材料。因此,包括在溶剂中的是例如乳化剂。溶剂可以选自例如以下组中:1,1,2-三氯三氟乙烷、1-丁醇、1-辛醇、1-氯丁烷、1,4-二噁烷、1,2-二氯乙烷、1,4-二噁烷、1-甲基-2-吡咯烷酮、1,2-二氯苯、2-丁醇、2,2,2-三氟乙醇、2-乙氧基乙基醚、2-甲氧基乙醇、2-甲氧基乙基乙酸酯、乙酸、乙酸酐、乙腈(MeCN)、丙酮、苯、乙酸丁酯、苄腈、四氯化碳、二硫化碳、氯仿、氯苯、柑橘萜烯、环戊烷、环己烷、二氯甲烷、二乙醚、二氯甲烷(DCM)、二乙基酮、二甲氧基乙烷、二甲基甲酰胺(DMF)、二甲亚砜、氧化氘丙酮、二乙胺、二乙二醇、二乙二醇二甲醚、二甲亚砜(DMSO)、二甲基甲酰胺(DMF)、乙醇、乙酸乙酯、乙二醇、甲酸、甘油、己烷、庚烷、六甲基磷酰三胺、六甲基磷酰胺、异丙醇(IPA)、异丁醇、异戊醇、间二甲苯、甲醇、甲基异丁基酮、甲基乙基酮、二氯甲烷、乙酸甲酯、硝基甲烷、正丁醇、正丙醇、硝基甲烷、N,N-二甲基乙酰胺、邻二甲苯、对二甲苯、戊烷、石油醚、石油醚、碳酸丙烯酯、吡啶、丙酸、四氢呋喃(THF)、甲苯、松节油、三乙胺、叔丁基甲基醚、叔丁醇、四氯乙烯和水。根据本发明,其它溶剂是可能的。
催化剂物质在这里被理解为广泛地涵盖气态、液态、固态或可用于催化纳米材料生长的任何其它形式的所有物质。实例包括但不限于诸如铁、镍、钼、钴、铂、铜、银或金的金属及其混合物或含有它们的化合物(例如碳化物、氮化物、氯化物、溴化物、硫酸盐、羰基化物和氧化物)。
所产生的催化剂可以处于中间体状态,即中间体催化剂颗粒。这是指这样的状态,其中颗粒基本上没有溶剂,但是还没有被催化活化。
根据一个实施方案,如果生产中间体催化剂颗粒,该方法还包括处理中间体催化剂颗粒以产生催化剂颗粒。
含催化剂物质的材料是指如下二者:含催化剂的材料和催化剂前体或催化剂源,并且在这里被理解为广泛地涵盖气态、液态、固态或任何其它形式的所有材料,当处理或加工时,其产生气态、液态或固态形式的催化剂材料,和/或催化剂颗粒或催化剂材料。此外,在其表面上具有表面活性剂以允许通过例如溶剂化或乳化而分散在溶剂中的催化剂材料和催化剂源在本文中被认为是根据本发明的含催化剂物质的材料,除非另有说明。
“材料溶解”是指材料或其离子扩散开(spread out)并被溶剂分子包围。
“乳化”在这里是指产生通常不混溶(不可混合或不可共混)的两种或更多种液体的混合物。
使形成的溶液雾化以产生液滴并处理该液滴以产生催化剂颗粒提供了控制所产生的催化剂颗粒的各种性质例如其尺寸、形状、形态和组成的技术效果。例如,如果需要更大的催化剂颗粒,则可以选择雾化参数,使得产生更大的液滴,其直接影响所得催化剂颗粒的尺寸。相反,如果需要较小的催化剂颗粒,则可以选择溶剂参数,使得每个液滴存在较少的催化剂材料,其直接影响所得催化剂颗粒的尺寸。
根据一个实施方案,所形成的溶液具有0.0001帕斯卡秒(Pa S)至10PaS,优选0.0001Pa S至1Pa S的粘度。在一些情况下,合适的粘度随雾化方法和优选的溶液液滴尺寸而变化。
如本领域技术人员所理解的,溶液可以具有超过上述范围的任何粘度。对于通过本发明所使用的装置来雾化的溶液而言,0.0001Pa S至10Pa S的粘度可以有利地低。
根据一个实施方案,溶液包含10-99.9重量%的溶剂,优选90-99重量%的溶剂。
根据一个实施方案,溶液包含0.01-50重量%的含催化剂物质的材料,优选0.1-4重量%的含催化剂物质的材料。
如本领域技术人员所理解的,溶液可以包括超过上述范围的任何重量百分比的溶剂和含催化剂物质的材料。
根据一个实施方案,该方法进一步包括添加助催化剂(promoter),以生产包含至少部分助催化剂的催化剂颗粒。
助催化剂在这里被理解为涵盖气态、液态、固态或任何其它形式的所有物质,其促进、加速或以其他方式增加或改善纳米材料的成核或生长速率或有助于控制待生产的纳米材料的一种或多种性质。助催化剂的实例包括但不限于硫、硒、碲、镓、锗、磷、铅、铋、氧、氢、氨、水、醇、硫醇、醚、硫醚、酯、硫酯、胺、酮、硫酮、醛、硫醛和二氧化碳。为了本发明的目的,助催化剂前体被认为是助催化剂。例如,在硫助催化剂(promoter sulfur)的情况下,作为硫助催化剂的前体或来源的化合物例如噻吩、二茂铁基硫化物、固体硫、二硫化碳、苯硫酚、苯并噻吩、二硫化二氢、二甲亚砜在此称为助催化剂。
助催化剂可以加入溶液中,在雾化期间或之后引入,或在处理期间引入。根据本发明的一个实施方案,助催化剂在雾化之前存在于溶液中,尽管助催化剂可以在本方法的稍后阶段添加或引入。助催化剂存在于溶液中的技术效果在于,可更精确地控制其相对于溶剂和含催化剂物质的材料的浓度。
根据一个实施方案,雾化溶液以产生液滴是通过喷雾嘴雾化、空气辅助雾化(airassisted nebulization)、旋转盘雾化、加压液体雾化、电喷雾、振动孔雾化、超声、喷墨印刷、喷涂、旋转盘涂布和/或电喷雾离子化进行。如本领域技术人员所理解的,溶液可以通过根据本发明的其它方式进行雾化。
根据一个实施方案,处理液滴以产生催化剂颗粒是通过加热、蒸发、热分解、超声、辐照和/或化学反应进行。化学反应可包括添加试剂以在颗粒内部引起化学转化。化学反应或热分解也可用于从前体中释放材料。
根据一个实施方案,含催化剂物质的材料选自由有机金属化合物和金属有机化合物组成的组。根据本发明,其它的含催化剂物质的材料是可能的。含催化剂物质的材料在液滴处理期间例如通过化学反应或热分解可易于释放催化剂物质。
这些化合物的实例包括但不限于六羰基钼;二茂铁;五羰基铁;二茂镍;二茂钴;四羰基镍;碘(甲基)镁MeMgI;二乙基镁;有机镁化合物如碘(甲基)镁MeMgI、二乙基镁(Et2Mg);Grignard试剂;甲基钴胺素血红蛋白;肌红蛋白有机锂化合物例如正丁基锂(n-BuLi);有机锌化合物例如二乙基锌(Et2Zn)和氯(乙氧基羰基甲基)锌(ClZnCH2C(=O)OEt);和有机铜化合物例如二甲基铜酸锂(Li+[CuMe2]-);金属β-二酮化物;醇盐和二烷基酰胺;乙酰丙酮化物;金属醇盐;镧系元素;锕系元素和半金属;三乙基硼烷(Et3B)。
任何上述实施方案的方法可以用于纳米材料的催化合成。
根据本发明的第二方面,公开了一种方法。该方法包括:形成包含溶剂和含催化剂物质的材料的溶液,其中使含催化剂物质的材料溶解或乳化在溶剂中,雾化所形成的溶液以产生包含所述含催化剂物质的材料的液滴,和处理液滴,以从包含在液滴中的含催化剂物质的材料产生催化剂颗粒,引入纳米材料源,和从纳米材料源和至少一种催化剂颗粒合成纳米材料。
在本发明的一个实施方案中,溶剂可以用作纳米材料源。
在本发明的一个实施方案中,在纳米材料的成核和/或生长之前,溶剂基本上从催化剂颗粒或催化剂前体颗粒去除。
在本发明的一个实施方案中,催化剂颗粒含有一种或多种催化剂物质和一种或多种助催化剂。
纳米材料在本文中被认为是具有0.1至100nm的最小特征长度的任何材料。例如,在纳米管或纳米棒的情况下,特征尺寸是直径。
根据一个实施方案,该方法还包括将所形成的纳米材料沉积到基底上。
基底可以是例如石英、PC、PET、PE、硅、硅树脂或玻璃基底。
根据一个实施方案,纳米材料源是碳纳米材料源。
纳米材料源在此被理解为意指含有组成纳米材料的任何或所有化合物或元素的任何材料。在碳纳米材料的情况下,例如,纳米材料源包括碳和含碳化合物(包括一氧化碳、有机物和烃)。根据本发明,作为碳源,可以使用各种含碳前体。糖、淀粉和醇是根据本发明的可能的碳源。碳源包括但不限于气态碳化合物如甲烷、乙烷、丙烷、乙烯、乙炔以及液体挥发性碳源如苯、甲苯、二甲苯、三甲基苯、甲醇、乙醇和/或辛醇。一氧化碳气体单独或在氢气存在下也可用作碳源。饱和烃(例如CH4、C2H6、C3H8),具有从C2H2经由C2H4至C2H6的饱和碳键的芳族化合物的体系(苯C6H6,甲苯C6H5-CH3、邻二甲苯C6H4-(CH3)2、1,2,4-三甲基苯、C6H3-(CH3)3)苯、富勒烯分子也可以用作碳源。
包含碳的纳米材料涵盖宽范围的结构和形态,包括薄膜;片如石墨烯;球体或球状体(spheroids)如纳米洋葱,富勒烯和巴基球;纤维;管;棒和更复杂的形状,例如碳纳米树,纳米角,纳米带,纳米锥,石墨化的碳纳米管,碳纳米豆荚和多组分纳米材料例如碳氮纳米管和碳硼纳米管。
根据本发明的第三方面,公开了一种用于生产催化剂颗粒的设备。该设备包括:用于雾化包含溶剂和含催化剂物质的材料的溶液的装置,其中含催化剂物质的材料溶解或分散在溶剂中,以产生包含含催化剂物质的材料的液滴;以及用于处理液滴以从包含在液滴中的含催化剂物质的材料产生催化剂颗粒的装置。
在一个实施方案中,该设备还包括用于形成包含溶剂和含催化剂物质的材料的溶液的装置,其中含催化剂物质的材料溶解或分散在溶剂中。
在一个实施方案中,该设备还包括用于添加助催化剂以产生包含至少部分助催化剂的催化剂颗粒的装置。
根据一个实施方案,用于雾化溶液以产生液滴的装置包括用于喷雾嘴雾化、空气辅助雾化、旋转盘雾化、加压液体雾化、电喷雾、振动孔雾化、超声、喷墨印刷、喷涂、旋转盘涂布和/或电喷雾离子化的装置。
在一个实施方案中,用于处理液滴以产生催化剂颗粒的装置包括用于加热、蒸发、热分解、辐照、超声和/或化学反应的装置。
根据本发明的第四方面,公开了一种用于生产催化剂颗粒的溶液液滴。溶液液滴包含溶剂、含催化剂物质的材料和助催化剂。
根据本发明的第五方面,公开了一种用于生产催化剂颗粒的设备。该设备包括:气雾器,其用于雾化包含溶剂和含催化剂物质的材料的溶液,其中含催化剂物质的材料溶解或分散在溶剂中,以产生包含含催化剂物质的材料的液滴;和用于处理液滴以从包含在液滴中的含催化剂物质的材料产生催化剂颗粒的反应器。
在一个实施方案中,该设备还包括用于形成包含溶剂和含催化剂物质的材料的溶液的混合器或搅拌器,其中含催化剂物质的材料溶解或分散在溶剂中。
根据本发明的一个实施方案,溶液可含有试剂,其可与溶液的一种或多种组分发生化学或催化反应,以从含催化剂物质的材料中释放催化剂物质和/或产生或活化助催化剂。
活化在此理解为引起化学或物理变化,使得材料的预期效果被活化或物质被释放。实例包括从助催化剂前体(例如噻吩)中释放助催化剂(例如硫)。活化可以通过例如化学反应或热分解来实现。
气雾器也可以是磁性混合器或搅拌器、喷雾器(nebulizer)、液滴产生器或雾化器(atomizer)。
用于处理液滴的反应器可包括加热单元、UV处理单元、化学反应单元、超声单元、加压或减压单元、辐照单元或其组合。
根据本发明的第六方面,公开了催化剂颗粒。催化剂颗粒包含催化剂物质和至少一种助催化剂。助催化剂可选自由如下组成的组:硫、硒、碲、镓、锗、磷、铅、铋、氧、氢、氨、水、醇、硫醇、醚、硫醚、酯、硫酯、胺、酮、硫酮、醛、硫醛和二氧化碳。
催化剂颗粒可以是可用于合成的催化剂颗粒或中间体催化剂颗粒。
例如,在使用助催化剂生产催化剂颗粒之后,助催化剂可以保留在颗粒内部。当催化剂颗粒用于纳米材料合成时,包含催化剂物质和助催化剂的催化剂颗粒可以例如提供纳米材料在催化剂颗粒中的增加或降低的溶解度。在相同催化剂颗粒中提供催化剂物质和助催化剂的技术效果是改善的转化产率、生长速率和对纳米材料性质的控制。
在一个实施方案中,催化剂物质选自由如下组成的组:铁、镍、钴、铂、铜、银、金和其任意组合,以及包括这些物质中的至少一种的任何化合物。这样的化合物可包括碳化物、氮化物、氯化物、溴化物、硫酸盐、羰基化合物和氧化物。
在本发明的一个实施方案中,催化剂颗粒是固体。
附图说明
图1示出了根据本发明的一个实施方案的方法。
图2示出了根据本发明的一个实施方案的方法。
图3a和3b是根据一个实施方案的纳米材料的SEM和TEM图像。
图4是60个SWCNT的直径分布。
图5示出了根据一个实施方案的不同硫浓度的CNT的直径分布。
具体实施方案的详细描述
现在将参考本发明的实施方案,其示例在附图中示出。
图1示出了根据本发明的一个实施方案的方法。在图1所示的实施方案中,该方法开始于形成包含溶剂和含催化剂物质的材料的溶液,如步骤101所示。可将溶剂和催化剂源(含催化剂物质的材料)加入到混合器102中以形成溶液。将催化剂源溶解、乳化或以其它方式分散在溶剂中,然后继续该方法。溶剂可以是例如水、甲苯、乙醇或允许催化剂源分散的任何其它合适的材料;并且例如催化剂源可以是诸如二茂铁等化合物。溶液可以具有0.0001Pa S至10Pa S,优选0.0001Pa S至1Pa S的粘度。这样的粘度可允许溶液有效雾化。溶液可包含10-99.9重量%的溶剂,优选90-99.9重量%的溶剂。其还可具有0.001-90重量%的催化剂源,优选0.01-50重量%的催化剂源,更优选0.1-5重量%的催化剂源。可提供上述比例范围以用于不同条件下的有效的催化剂材料的生产。
然后将溶液雾化以产生包含催化剂源的液滴103。这可以例如通过喷雾嘴雾化、空气辅助雾化或雾化来完成。根据雾化条件,包含催化剂源的液滴103可以具有不同的尺寸。它们也可以具有尺寸的分布。优选地,液滴尺寸分布的标准偏差低于5,更优选低于3,更优选低于2,更优选低于1.5%。在一个实施方案中,气溶胶尺寸分布是单分散的。
在本发明的一个实施方案中,在没有液滴或颗粒聚集或凝聚的情况下,每个溶液液滴均产生催化剂颗粒。反应器条件如温度、溶液、碳源和载气进料速率、溶剂、含催化剂物质的材料、溶液中助催化剂的重量分数、湍流水平、反应器构造或几何形状、液滴或催化剂颗粒的分类或预分类、液滴或催化剂颗粒的负载和压力都可以变化,以使导致聚集和凝聚的气相中的碰撞最小化。根据本发明,其它控制碰撞的装置是可能的。
在一个实施方案中,液滴103被处理以产生催化剂颗粒104。这可以例如通过加热、蒸发、热分解、超声、辐照和/或化学反应来进行。在处理期间,溶剂可以从液滴103蒸发。催化剂颗粒104由催化剂源产生,即催化剂物质从含催化剂物质的材料中释放并且形成催化剂颗粒。
在替代实施方案中,催化剂物质不能从含催化剂物质的材料中完全释放,并且形成了中间体催化剂颗粒106。在这种情况下,除去溶剂,但是催化剂材料不能从含催化剂物质的材料中释放。中间体颗粒106可以被进一步处理以从含催化剂物质的材料中释放催化剂物质。以这种方式,也可以形成催化剂颗粒104。
该方法还可以包括添加助催化剂105的任选步骤,如虚线箭头所示。助催化剂105可在催化剂颗粒生产期间的任何时刻引入,即加入到混合器102中的溶液中,在雾化期间或在处理期间引入。当所产生的催化剂颗粒用于生产纳米材料时,助催化剂可以增加或改善纳米材料的生长速率,或者有助于控制待生产的纳米材料的一种或多种性质。助催化剂的实例是噻吩。
在一个实施方案中,助催化剂材料不从助催化剂前体释放,并形成中间体助催化剂颗粒(图1中未示出)。
纳米材料的生产速率、质量控制和产率随材料转化效率和催化剂颗粒的均匀性和组成而变化。由于纳米材料的某些性质取决于在合成期间其催化剂颗粒的性质,因此通过该方法产生的纳米材料可具有可控的性质。例如,在诸如CNT和CNB的HARM的情况下,纳米材料的直径与催化剂直径直接相关。
因此,通过上述方法生产的催化剂颗粒103的尺寸和其它性质可以通过选择不同的雾化和处理技术以及条件来控制。由于催化剂颗粒不是由预制的催化剂材料生产,而是由溶解,乳化或以其它方式分散在溶剂中的催化剂源产生,因此它们的性质不依赖于预制材料的性质,并且可以选择条件,使得在气相中产生之前,它们不可能发生聚集。
图2示出了根据本发明的一个实施方案的合成纳米材料的方法。该方法类似于图1所示的方法,可以开始于形成包含溶剂和催化剂源的溶液201,该催化剂源溶解、乳化或以其它方式分布在其中。然后将溶液201雾化以产生包含催化剂源的液滴202,然后处理液滴并产生催化剂颗粒。此后,合成纳米材料204。纳米材料可以是碳纳米材料,例如碳纳米管或碳纳米芽(如图2所示)。
对于纳米材料204的合成,需要引入纳米材料源205,如图2中的箭头所示。纳米材料源205可在该方法期间的任何点引入,并且在图2所示的实施例中,其在纳米材料204的合成期间引入。在碳纳米材料的情况下,纳米材料源205可以包括碳和含碳化合物,包括一氧化碳、碳水化合物和烃。溶剂也可以充当纳米材料源(例如一旦溶剂基本上从液滴中蒸发)。
也可以在图2所示的方法期间的任何时刻添加助催化剂。助催化剂可以帮助和加速纳米材料204的合成,或提供对于纳米材料204的某些性质的控制。
根据本发明,催化剂物质、含催化剂物质的材料或助催化剂可通过溶剂化、乳化、通过使用表面活性剂或通过任何其它使其分散的方式分散在溶剂中。
在本发明的一个实施方案中,在纳米材料从催化剂颗粒成核或催化合成之前,可以例如通过蒸发或化学反应除去溶剂,使得一种或多种催化剂物质、含催化剂物质的材料和如果存在的助催化剂不再处于溶液中、不再乳化或以其它方式分散在溶剂中。因此,催化剂可以是固体、液体或熔融状态。根据本发明,该颗粒可以例如通过添加能量或通过化学反应来进一步处理,以从助催化剂前体中释放催化剂物质和/或助催化剂,从而使得它们被活化。
根据本发明的一个实施方案,可以将液体、固体或熔融的催化剂颗粒以中间体状态(即处于基本上没有溶剂但在活化以用于催化之前的状态)存储,以用于随后分散在气溶胶反应器中或沉积在用于纳米材料的表面支持生长的基底上。
根据本发明的一个实施方案,将液体、固体或熔融的最终催化剂颗粒或中间体催化剂颗粒储存在基底上或储存在二次溶液中,其中它们例如通过表面活性剂分散,随后雾化成纳米材料合成反应器或涂覆在基底上。
在本发明的一个实施方案中,催化剂颗粒或中间体催化剂颗粒在用于生产纳米材料的载气中时立即使用;或者在用于生产催化剂颗粒的载气中时进行进一步处理(当在用于生产纳米材料的载气中时,其立即使用),因此,该催化剂颗粒或中间体催化剂颗粒不被收集并存储在用于随后使用的基底上或溶液中。
合成的纳米材料204可以随后沉积到基底(未示出)上。
实施例
在本发明的一个实施方案中,将催化剂前体材料(二茂铁)和助催化剂(噻吩)溶解在溶剂(甲苯)中以形成液体原料(包括溶剂和催化剂源的溶液),其然后通过氮气(载气)射流进行雾化,以产生气溶胶液滴。在该实施例中,甲苯也是纳米材料(在这种情况下为碳)源。将该气溶胶通过不锈钢管以高的第二助催化剂(氢气(H2))流速(8lpm)连续送入反应器中。引入其它气态反应物(碳源乙烯(C2H4)和二氧化碳(CO2)),并根据需要与气流混合。气体反应物流通过质量流量控制器进行测量和控制。根据本发明的实施方案,其它纳米材料源、溶剂、助催化剂、载气、反应器材料和构造以及流速是可能的。
通过调节液滴(在该实施例中,通过二茂铁的热分解),然后在炉中生长铁原子团簇,获得催化剂颗粒(在这种情况下为铁,尽管根据本发明可能有其它催化剂颗粒)。根据本发明,用于生产催化剂颗粒和其它催化剂材料和前体的装置是可能的。反应器是直径为5cm的石英管,其通过具有60cm长的热区的拼合管炉进行加热。根据本发明,其它反应器材料、用于引入能量的装置和几何形状是可能的。
然后在包括1100℃的各种温度下进行CNT(碳纳米管)合成。尽管根据本发明,其它压力和流动条件(例如湍流或过渡流)是可能的,但是在大气压下在反应器内的层流条件下进行该合成。根据本发明,任何其它压力都是可能的。在反应器出口通过直径为11cm的硝化纤维素过滤器(Millipore,0.45μm的直径孔)收集CNT。根据本发明,其它收集装置是可能的,包括直接热泳、惯性、重力和电泳沉积。在反应器中的停留时间为约2秒。根据本发明,其它停留时间是可能的,只要允许足够的时间用于生长并且限制碳源的聚集或耗尽。
使用静电微分迁移率分析仪(TSI model 3071)和冷凝颗粒计数器(TSImodel3775)测量气溶胶数量大小分布。为了测量CNT薄膜的光吸收光谱和透射率(在550nm测量),将CNT从硝化纤维素过滤器转移到1mm厚的石英基底(Finnish玻璃),并且通过UV-vis-NIR吸收光谱仪(Perkin-ElmerLambda 950)记录光谱。对于TEM观察,通过将CNT放置在反应器出口处的收集过滤器上来使CNT直接沉积在铜TEM网格(Agar Scientific莱西碳网)上。使用双像差校正JEOL JEM-2200FS记录高分辨率TEM图像。SEM图像通过Zeiss Sigma VP显微镜记录。用HORIBA Jobin Yvon LabRAM HR800光谱仪和633nm HeNe激光器记录拉曼光谱。用4点线性探针(Jandel 4点探针,Jandel Engineering Ltd)测量薄层电阻(sheetresistance)。
由雾化器产生的包含催化剂源的气溶胶液滴具有72.4nm的几何平均直径和1.7的对数标准偏差。在该实施方案的优选操作中,气溶胶颗粒前体液滴由雾化器形成,但是可以采用本领域已知的从原料生成气溶胶的其它方法。雾化器允许生成具有明确的尺寸分布和浓度的气溶胶,其可以通过改变雾化氮气流来调节。
在示例性的实施方案中,用于合成的温度设定为1100℃。在该温度下,膜容易从过滤器上剥离,并且该膜通过干转移技术成功地转移到聚对苯二甲酸乙二醇酯(PET)、玻璃和石英基底上。SEM(图3a)和TEM(图3b)图像显示长的CNT和干净的网络。
在CNT壁上仅观察到少量副产物。通过60个SWCNT(单壁碳纳米管)的直径测量获得的直径分布示于图4。由这些测量计算的平均直径为2.1nm。
原料用0.5重量%至4重量%的浓度的二茂铁制备,并且在所尝试的最低二茂铁浓度(原料中0.5重量%的二茂铁)下获得了CNT膜的良好光电性能。当二茂铁浓度增加时,具有一定透射率的CNT膜的合成速率增加,但是薄层电阻也增加。选择0.5重量%的二茂铁浓度用于示例性实施方案的其余部分。
将噻吩作为含硫的助催化剂引入至反应器中以用于CNT生长。在液体原料中进行具有不同噻吩浓度的各种合成:硫与铁的摩尔比(S/Fe)为0至4:1。为了研究硫浓度变化对直径分布的影响,使用允许直接估计整体CNT直径分布的光吸收光谱法。观察到硫略微改变了CNT直径分布。进行直径分布的高斯拟合以获得不同硫浓度的CNT的平均直径(图5)。随着S/Fe原子比从1:1增加到4:1,直径从1.9增加到2.3nm。
通过制备具有不同乙烯流量(4sccm至100sccm)作为碳源的各种CNT样品,研究了乙烯浓度的影响。由于CNT在反应器出口处的收集时间对于所有样品都是相同的,可以观察到向反应器中引入更多的乙烯增加了合成的产率,并且还略微降低了CNT的直径分布。
对于技术人员显而易见的是,随着技术的进步,本发明的基本思想可以以各种方式实现。因此,本发明及其实施方案不限于上述示例;并且其可在权利要求的范围内变化。
Claims (24)
1.一种用于生产催化剂颗粒的方法,其特征在于,所述方法包括:
形成包含溶剂和含催化剂物质的材料的溶液,其中使所述含催化剂物质的材料溶解或乳化在所述溶剂中,
雾化所形成的溶液以产生包含含催化剂物质的材料的液滴,和
处理所述液滴,以从包含在液滴中的所述含催化剂物质的材料产生催化剂颗粒或中间体催化剂颗粒。
2.根据权利要求1所述的方法,其中产生了中间体催化剂颗粒,所述方法还包括:处理所述中间体催化剂颗粒以产生催化剂颗粒。
3.根据权利要求1和2中任一项所述的方法,其中所形成的溶液具有0.0001帕斯卡秒至10帕斯卡秒,优选0.0001帕斯卡秒至1帕斯卡秒的粘度。
4.根据权利要求1至3中任一项所述的方法,其中所述溶液包含10-99.9重量%的溶剂,优选90-99.9重量%的溶剂。
5.根据权利要求1至4中任一项所述的方法,其中所述溶液包含0.01-50重量%的含催化剂物质的材料,优选0.1-4重量%的含催化剂物质的材料。
6.根据权利要求1至5中任一项所述的方法,其中所述方法还包括添加助催化剂,以产生包含至少部分助催化剂的催化剂颗粒。
7.根据权利要求6所述的方法,其中将所述助催化剂添加至包含溶剂和含催化剂物质的材料的溶液中。
8.根据权利要求1至7中任一项所述的方法,其中雾化溶液以产生液滴的步骤是通过喷雾嘴雾化、空气辅助雾化、旋转盘雾化、加压液体雾化、电喷雾、振动孔雾化、超声、喷墨印刷、喷涂、旋转盘涂布和/或电喷雾离子化进行的。
9.根据权利要求1至8中任一项所述的方法,其中处理所述液滴以产生催化剂颗粒是通过加热、蒸发、热分解、超声、辐照和/或化学反应进行的。
10.根据权利要求1至9中任一项所述的方法,其中所述含催化剂物质的材料选自由有机金属化合物和金属有机化合物组成的组。
11.权利要求1至10中任一项所述的方法在纳米材料的催化合成中的用途。
12.一种用于生产纳米材料的方法,其特征在于,所述方法包括:
形成包含溶剂和含催化剂物质的材料的溶液,其中所述含催化剂物质的材料溶解或乳化在所述溶剂中,
雾化所形成的溶液以产生包含所述含催化剂物质的材料的液滴,和
处理所述液滴,以从包含在液滴中的所述含催化剂物质的材料产生催化剂颗粒,
引入纳米材料源,和
从纳米材料源和至少一种催化剂颗粒合成纳米材料。
13.根据权利要求12所述的方法,其中所述方法还包括将所形成的纳米材料沉积到基底上。
14.根据权利要求12和13中任一项所述的方法,其中所述纳米材料源是碳纳米材料源。
15.一种用于生产催化剂颗粒的设备,其特征在于,所述设备包括:
用于雾化包含溶剂和含催化剂物质的材料的溶液的装置,其中所述含催化剂物质的材料溶解或分散在所述溶剂中,以产生包含含催化剂物质的材料的液滴,
用于处理液滴以从包含在液滴中的含催化剂物质的材料产生催化剂颗粒或中间体催化剂颗粒的装置。
16.根据权利要求15所述的设备,其还包括用于形成包含溶剂和含催化剂物质的材料的溶液的装置,其中所述含催化剂物质的材料溶解或分散在所述溶剂中。
17.根据权利要求15和16中任一项所述的设备,其中所述设备包括用于添加助催化剂以产生包含至少部分助催化剂的催化剂颗粒的装置。
18.根据权利要求15至17中任一项所述的设备,其中用于雾化所述溶液以产生液滴的装置包括用于喷雾嘴雾化、空气辅助雾化、旋转盘雾化、加压液体雾化、电喷雾、振动孔雾化、超声、喷墨印刷、喷涂、旋转盘涂布和/或电喷雾离子化的装置。
19.根据权利要求15至18中任一项所述的设备,其中用于处理所述液滴以产生催化剂颗粒的装置包括用于加热、蒸发、热分解、辐照、超声和/或化学反应的装置。
20.一种用于生产催化剂颗粒的溶液液滴,所述催化剂颗粒包含溶剂、含催化剂物质的材料和助催化剂。
21.根据权利要求20所述的溶液液滴,其中所述催化剂物质选自由如下组成的组:铁、镍、钴、铂、铜、银、金和其任意组合,以及包含这些物质中的至少一种的任何化合物。
22.一种催化剂颗粒,其特征在于,所述催化剂颗粒包含催化剂物质和至少一种助催化剂。
23.根据权利要求22所述的催化剂颗粒,其中所述助催化剂选自由如下组成的组:硫、硒、碲、镓、锗、磷、铅、铋、氧、氢、氨、水、醇、硫醇、醚、硫醚、酯、硫酯、胺、酮、硫酮、醛、硫醛和二氧化碳。
24.根据权利要求23所述的催化剂颗粒,其中所述催化剂物质、所述含催化剂物质的材料和所述助催化剂处于固体、液体或熔融状态。
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CN112225198A (zh) * | 2020-11-03 | 2021-01-15 | 宁波埃氪新材料科技有限公司 | 一种汽车锂电池用的尺寸可调控碳纳米管合成方法及其制成的碳纳米管催化剂、碳纳米管 |
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CN110813295B (zh) * | 2018-08-13 | 2023-04-11 | 中国石油化工股份有限公司 | 浆态床加氢催化剂的制备方法及应用 |
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