CN109305914A - 一种碳包覆过渡金属的纳米复合材料及其应用 - Google Patents
一种碳包覆过渡金属的纳米复合材料及其应用 Download PDFInfo
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- CN109305914A CN109305914A CN201810841571.6A CN201810841571A CN109305914A CN 109305914 A CN109305914 A CN 109305914A CN 201810841571 A CN201810841571 A CN 201810841571A CN 109305914 A CN109305914 A CN 109305914A
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- nanocomposite
- carbon
- transition metal
- coating
- nitrogen
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- 239000011248 coating agent Substances 0.000 title claims abstract description 68
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 51
- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 50
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 45
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002253 acid Substances 0.000 claims abstract description 30
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 30
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 29
- 239000001301 oxygen Substances 0.000 claims abstract description 29
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- 239000011148 porous material Substances 0.000 claims description 41
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 claims description 38
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- 239000002904 solvent Substances 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
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- 239000010949 copper Substances 0.000 claims description 8
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- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
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- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 2
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- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229940011182 cobalt acetate Drugs 0.000 description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
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- OUUQCZGPVNCOIJ-UHFFFAOYSA-N hydroperoxyl Chemical compound O[O] OUUQCZGPVNCOIJ-UHFFFAOYSA-N 0.000 description 1
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical compound [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1143—Making porous workpieces or articles involving an oxidation, reduction or reaction step
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/38—Removing components of undefined structure
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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Abstract
本发明提供一种碳包覆过渡金属的纳米复合材料及其应用,所述纳米复合材料含具有壳层和内核的核壳结构,所述壳层为掺杂氮和氧的石墨化碳层,所述内核为过渡金属纳米粒子,其中,所述复合材料的酸洗损失率≤10%。本发明的纳米复合材料具有严密包覆的石墨化碳层,通过这种严密包覆的纳米复合材料可以更好的保证内核过渡金属在制备和应用中损失率降低,从而更好的发挥纳米复合材料的作用并保证了纳米复合材料的安全性。本发明的碳包覆过渡金属的纳米复合材料制备方法简单,适用性广,作为催化剂催化效果佳,可用于各类加氢还原反应。
Description
技术领域
本发明涉及碳/金属复合材料领域,具体涉及一种碳包覆过渡金属的纳米复合材料及其应用。
背景技术
过渡金属纳米颗粒由于具有优异的光学、电学、磁学性能而受到广泛关注。但过渡金属纳米颗粒活性高,容易发生团聚或被氧化甚至在空气中燃烧,大大影响了这类材料的性能及其应用。与此同时,作为非金属材料,纳米碳材料具有耐酸碱腐蚀、化学性质稳定等优点。
近年来,纳米碳包覆金属复合材料成为了人们关注的热点。这类材料由单层至数层弯曲石墨化碳层为壳紧密包裹内核的金属纳米粒子,将金属纳米粒子与外界进行隔绝,大大提高了复合材料的稳定性。因此,这种独特的核壳结构纳米材料在催化材料、吸波材料、信息存储材料、磁光材料、生物医学材料,以及润滑油添加剂等领域有着广阔的应用前景。
目前已有通过碳材料包覆过渡金属的相关文献报道,但这类材料在实际应用中仍存在各种问题,例如传质效率不高、产率低、工艺复杂、碳包覆不良、使用时不稳定等问题,无法适用于工业化生产和应用。比如以金属-有机骨架化合物(MOF)为前驱体热解的方法,该方法需要在高温、高压下于溶剂中制得具有周期性结构的晶态固体材料(即MOF),通常制备MOFs的条件比较严格,所需配体价格昂贵,并且很难进行大量生产;此外,该方法制备的复合材料中对金属粒子的包覆不严密。又如CN 105032424A公开了一种用于芳香硝基化合物选择性氢化的催化剂,该文献包覆金属粒子的方法是pechini法(溶胶凝胶法),与MOF法类似,该方法也需要于溶剂中制得固体的配位聚合物,且该方法制备的复合材料中对金属粒子的包覆也不严密。
需注意的是,前述背景技术部分公开的信息仅用于加强对本发明的背景理解,因此它可以包括不构成对本领域普通技术人员已知的现有技术的信息。
发明内容
针对现有技术存在的问题,本发明提供一种碳包覆过渡金属的纳米复合材料,具有丰富的介孔结构,可提高传质效率并增加稳定性。
为了实现上述目的,本发明采用如下技术方案:
一种碳包覆过渡金属的纳米复合材料,所述复合材料含具有壳层和内核的核壳结构,所述壳层为掺杂氮和氧的石墨化碳层,所述内核为过渡金属纳米粒子,其中所述纳米复合材料的酸洗损失率≤10%。
在本发明的纳米复合材料的一个实施方式中,所述纳米复合材料为具有至少一个介孔分布峰的介孔材料。
在本发明的纳米复合材料的另一个实施方式中,所述纳米复合材料为具有大于一个的介孔分布峰的介孔材料,即具有两个或两个以上介孔分布峰的介孔材料。
在本发明的纳米复合材料的另一个实施方式中,纳米复合材料在2~5nm的孔径范围和6~16nm的孔径范围分别具有一个介孔分布峰。
在本发明的纳米复合材料的另一个实施方式中,所述介孔结构中孔径在2~5nm范围内的介孔体积占总孔体积的比例可以大于5%,比如10%~30%。
在本发明的纳米复合材料的另一个实施方式中,纳米复合材料中,介孔体积占总孔体积的比例大于50%,优选大于80%,更优选大于95%。
根据本发明的一个实施方式,其中所述复合材料中,介孔体积为0.05-1.25cm3/g,介孔体积也可以为0.10-0.40cm3/g。
在本发明的纳米复合材料的另一个实施方式中,以质量百分比计,所述纳米复合材料中的碳含量为15~60wt%,过渡金属含量为30~80wt%;优选地,所述纳米复合材料中的碳含量为30~60wt%,过渡金属含量为30~60wt%。
在本发明的纳米复合材料的另一个实施方式中,以质量百分比计,所述纳米复合材料中的氮和氧的总含量小于15%。
在本发明的纳米复合材料的另一个实施方式中,以质量百分比计,所述纳米复合材料中的氮的含量为2~8%。
在本发明的纳米复合材料的另一个实施方式中,以质量百分比计,所述纳米复合材料中的氧的含量为3~9%。
根据本发明,所述纳米复合材料中,各组分的含量之和为100%。
在本发明的纳米复合材料的另一个实施方式中,所述石墨化碳层的厚度为0.3~6nm,优选为0.3~3nm。
在本发明的纳米复合材料的另一个实施方式中,所述核壳结构的粒径为1~200nm,优选为3~100nm,更优选为4~50nm。
在本发明的纳米复合材料的另一个实施方式中,所述过渡金属选自铁、钴、镍、铜和锌中的一种或多种,优选为镍。
在本发明的纳米复合材料的另一个实施方式中,所述过渡金属纳米粒子的晶格结构为面心立方晶格结构和/或密排六方晶格结构。
另一方面,本发明提供上述纳米复合材料作为催化剂在加氢还原反应中的应用。
在本发明的应用的一个实施方式中,所述加氢还原反应包括:将硝基苯与所述纳米复合材料在溶剂中混合,在氢气气氛下进行反应合成苯胺。
在本发明的应用的另一个实施方式中,所述硝基苯为取代硝基苯,取代基选自C1-20的烷基、环烷基、芳基。
在本发明的应用的另一个实施方式中,所述纳米复合材料占所述硝基苯的质量百分比为1%-50%,优选5-30%。
在本发明的应用的另一个实施方式中,所述加氢还原反应一般在60-120℃下进行,所述氢气的压力一般为0.5-2MPa。
在本发明的应用的另一个实施方式中,所述溶剂选自醇类、醚类和水中的一种或多种。
本发明的有益效果在于:
本发明的碳包覆过渡金属的纳米复合材料,具有严密包覆的石墨化碳层结构,没有可使反应物接近过渡金属中心的孔道或缺陷,使内核的过渡金属材料十分稳定,不自燃,耐酸腐蚀,危险性低,适合保存与运输,从而保证了纳米复合材料使用的安全性。该严密包覆的纳米复合材料可作为催化剂应用于各类加氢还原反应,例如催化还原硝基苯为苯胺。作为催化材料时,具有重复性良好、高活性、高选择性等优点,适用于大规模工业化生产。
附图说明
附图是用来提供对本发明的进一步理解,并且构成说明书的一部分,与下面的具体实施方式一起应用于解释本发明,但并不构成对本发明的限制。在附图中:
图1示出了实施例1所制备的氮氧掺杂碳包覆镍纳米复合材料具有磁性的照片示意图;
图2为实施例1所制备的氮氧掺杂碳包覆镍纳米复合材料的TEM图;
图3为实施例1所制备的氮氧掺杂碳包覆镍纳米复合材料的XRD图;
图4a为实施例1所制备的氮氧掺杂碳包覆镍纳米复合材料的N2吸附-脱附等温线;
图4b为实施例1所制备的氮氧掺杂碳包覆镍纳米复合材料的BJH孔径分布曲线。
图5a是实施例1所制备的氮氧掺杂碳包覆镍纳米复合材料的XPS图;
图5b是实施例1所制备的氮氧掺杂碳包覆镍纳米复合材料的XPS中的Ni 2p谱图;
图5c是实施例1所制备的氮氧掺杂碳包覆镍纳米复合材料的XPS中的O 1s分峰结果;
图6是实施例2所制备的氮氧掺杂碳包覆镍纳米复合材料的TEM图;
图7是实施例2所制备的氮氧掺杂碳包覆镍纳米复合材料的XRD图;
图8是实施例2所制备的氮氧掺杂碳包覆镍纳米复合材料的BJH孔径分布曲线;
图9是实施例3所制备的氮氧掺杂碳包覆钴纳米复合材料的TEM图;
图10是实施例3所制备的氮氧掺杂碳包覆钴纳米复合材料的XRD图;
图11是实施例3所制备的氮氧掺杂碳包覆钴纳米复合材料的BJH孔径分布曲线;
图12是实施例4所制备的固体前驱体的XRD图;
图13是实施例4所制备的氮氧掺杂碳包覆镍钴纳米复合材料的TEM图;
图14是实施例4所制备的氮氧掺杂碳包覆镍钴纳米复合材料的XRD图;
图15是实施例4所制备的氮氧掺杂碳包覆镍钴纳米复合材料的BJH孔径分布曲线;
图16是对比例1所制备的材料的XRD图。
具体实施方式
以下结合附图通过具体的实施例对本发明作出进一步的详细描述,应当理解的是,此处所描述的具体实施方式仅用于说明和解释本发明,但不以任何方式限制本发明。
本发明中,除了明确说明的内容之外,未提到的任何事宜或事项均直接适用本领域已知的那些而无需进行任何改变。而且,本文描述的任何实施方式均可以与本文描述的一种或多种其他实施方式自由结合,由此形成的技术方案或技术思想均视为本发明原始公开或原始记载的一部分,而不应被视为是本文未曾披露或预期过的新内容,除非本领域技术人员认为该结合明显不合理。
本发明所公开的所有特征可以任意组合,这些组合应被理解为本发明所公开或记载的内容,除非本领域技术人员认为该组合明显不合理。本说明书所公开的数值点,不仅包括实施例中具体公开的数值点,还包括说明书中各数值范围的端点,这些数值点所任意组合的范围都应被视为本发明已公开或记载的范围。
在此未直接定义的任何术语应当被理解为具有与它们在本发明技术领域中通常所理解的相关联的含义。如贯穿本说明书使用的下面术语除非另外说明,应当理解为具有下面含义。
术语
术语“石墨化碳层”是指在高分辨透射电镜下可明显观察到层状结构的碳结构,而非无定型结构,且层间距为0.34nm。该石墨化碳层包覆过渡金属纳米粒子后形成的纳米复合材料呈球形或类球形。
术语“介孔”定义为孔径在2~50nm范围的孔。孔径小于2nm的孔定义为微孔,大于50nm的孔定义为大孔。
术语“介孔材料”定义为包含介孔孔道结构的多孔材料。
术语“碳包覆率”反映过渡金属被石墨化碳层有效包覆的比例,可通过高分辨透射电镜(HRTEM)的分析结果和催化氧化反应的实验结果表征。
术语“碳包覆严密程度”反映过渡金属被石墨化碳层与外部环境隔绝的比例,可通过高分辨透射电镜(HRTEM)的分析结果、过渡金属含量分析结果和酸洗实验结果表征。
术语“掺杂氮和氧的石墨化碳层”中的“氮”是指氮元素,“氧”是指氧元素,其中“氧含量”是指氧元素的含量,具体是指,在碳包覆纳米复合材料制备过程中,形成石墨化碳层中含有以各种形式存在的氧元素,所述“氧含量”为所有形式的氧元素的总含量,同理,“氮含量”是指氮元素的含量,即所有形式的氮元素的总含量。
术语“介孔分布峰”是指根据Barrett-Joyner-Halenda(BJH)方法对脱附曲线进行计算得到的孔分布曲线上的介孔分布峰。
术语“酸处理”是指在制备碳包覆过渡金属的纳米复合材料时对高温热解步骤后生成的产物所进行的处理方式,是制备复合材料中的步骤。
术语“酸洗损失率”是指制备完成的碳包覆过渡金属的纳米复合材料产品经酸洗后过渡金属的损失比例。其反映了石墨化碳层对过渡金属包覆的严密程度。如果石墨化碳层对过渡金属包覆不严密,则在酸处理后,内核的过渡金属会被酸溶解从而流失。酸洗损失率越大,表明石墨化碳层对过渡金属包覆的严密程度越低,反之,酸洗损失率越小,表明石墨化碳层对过渡金属包覆的严密程度越高。本发明中定义酸洗损失率≤10%为“严密包覆”的核壳结构的纳米复合材料。
所述的“酸洗损失率”按以下方式测量并计算:
按20mL硫酸水溶液(1mol/L)投加1g样品的比例,在90℃下对样品处理8h,然后用去离子水洗涤至中性,干燥后称重、分析,按下式计算酸洗损失率。酸洗损失率=[1-(酸洗后复合材料中过渡金属的质量分数×酸洗后复合材料的质量)÷(待酸洗复合材料中过渡金属的质量分数×待酸洗复合材料的质量)]×100%。
试剂、仪器与测试
如无特殊说明,本发明所采用试剂均为分析纯,所用试剂均为市售可得,例如购自西格玛奥德里奇(Sigma-Aldrich)。
本发明所采用XRD衍射仪的型号为XRD-6000型X射线粉末衍射仪(日本岛津),XRD测试条件为:Cu靶,Kα射线(波长λ=0.154nm),管电压为40kV,管电流为200mA,扫描速度为10°(2θ)/min。
本发明所采用高分辨透射电镜(HRTEM)的型号为JEM-2100(HRTEM)(日本电子株式会社),高分辨透射电镜测试条件为:加速电压为200kV。
本发明所采用X射线光电子能谱分析仪(XPS)为VG Scientifc公司生产配备有Avantage V5.926软件的ESCALab220i-XL型射线电子能谱仪,X射线光电子能谱分析测试条件为:激发源为单色化A1KαX射线,功率为330W,分析测试时基础真空为3×10-9mbar。另外。电子结合能用C1s峰(284.6eV)校正,后期分峰处理软件为XPSPEAK。
碳(C)、氢(H)、氧(O)、氮(N)四种元素的分析在Elementar Micro Cube元素分析仪上进行,具体操作方法和条件如下:样品在锡杯中称量1mg~2mg,放入自动进样盘,通过球阀进入燃烧管燃烧,燃烧温度为1000℃(为了去除进样时大气干扰,采用氦气吹扫),然后用还原铜对燃烧后的气体进行还原,形成氮气、二氧化碳和水。混合气体通过三根解吸柱进行分离,依次进TCD检测器检测。氧元素的分析是利用高温分解,在碳催化剂的作用下,将样品中的氧转化为CO,然后采用TCD检测CO。由于本发明的复合材料中仅含有碳、氢、氧、氮和金属元素,因此由碳、氢、氧、氮四种元素的总含量即可知金属元素的总含量。
不同金属元素之间的比例由X射线荧光光谱分析仪(XRF)测定,由已知的碳、氢、氧、氮四种元素总含量,算出不同金属元素在复合材料中的含量。本发明所采用X射线荧光光谱分析仪(XRF)的型号为Rigaku 3013X射线荧光光谱仪,X射线荧光光谱分析测试条件为:扫描时间为100s,气氛为空气。
BET测试方法:本发明中,样品的孔结构性质由Quantachrome AS-6B型分析仪测定,催化剂的比表面积和孔体积由Brunauer-Emmett-Taller(BET)方法得到,孔分布曲线根据Barrett-Joyner-Halenda(BJH)方法对脱附曲线进行计算得到。
本发明中,碳包覆过渡金属纳米粒子的平均粒径由XRD图分峰后,由谢乐公式:D=kγ/(B cosθ)计算得到。其中k为Scherrer常数,k=0.89;B为半高宽;θ为衍射角,单位弧度;γ为x射线波长,0.154054nm。
本发明所提供的碳包覆过渡金属的纳米复合材料含具有壳层和内核的核壳结构,壳层为掺杂氮和氧的石墨化碳层,内核为过渡金属纳米粒子,其中纳米复合材料的酸洗损失率≤10%。
本发明的纳米复合材料是一种由“被石墨化碳层严密包覆(不与外界接触)的过渡金属纳米颗粒”和具有介孔结构的碳材料构成的复合材料。这种严密包覆的复合材料较非严密包覆的复合材料而言,可以更好的保证内核过渡金属在制备和应用中损失率降低,从而更好的发挥复合材料的作用。此外,本领域通常认为催化加氢反应的活性中心是过渡金属,不管催化剂的具体结构如何,必须能使反应物与金属中心接触。而本发明的被石墨化碳层严密包覆的过渡金属纳米复合材料,仍具有极佳的催化加氢还原有机化合物的能力,进一步证明了石墨化碳层包裹过渡金属内核的严密性对其催化性能十分重要,过渡金属在此起到了不可或缺的修饰作用。
在一些实施例中,纳米复合材料为具有至少一个介孔分布峰的介孔材料,介孔孔结构有利于提高材料的传质效率。具体而言,该纳米复合材料在根据Barrett-Joyner-Halenda(BJH)方法对脱附曲线进行计算得到的孔分布曲线上,至少具有一个介孔分布峰。在一些实施例中,单批次制造的复合材料,在介孔范围内有两个分布峰;如将多批次制造的复合材料混合,则在介孔范围内可以有更多的分布峰。当纳米复合材料具有不同孔径范围的多级介孔结构时,可以使其表现出更独特的性能,且多级介孔结构可适用的应用范围更广。
在一些实施例中,介孔结构在2~7nm和8~20nm的介孔范围分别具有一个介孔分布峰。丰富的介孔结构有利于反应物和产物的扩散,可在纳米复合材料作为催化材料时提高其传质效率,十分有利于其催化性能的发挥。此外,还可通过多批次制造的复合材料混合在介孔孔径范围内获得更多的分布峰。
在一些实施例中,孔径在2~7nm范围内的介孔体积占总孔体积的比例大于5%,通过控制介孔体积占总孔体积的比例,使该复合材料具有丰富的介孔孔结构,可以保证传质效率更高。
在一些实施例中,其介孔体积可以为0.05-1.25cm3/g,也可以为0.10-0.40cm3/g。
在一些实施例中,以质量百分比计,所述纳米复合材料中的碳含量为15~60wt%,过渡金属含量为30~80wt%,。
本发明的纳米复合材料在石墨化碳层中掺杂有氧和氮。氧含量可以通过在制造过程中额外引入含氧化合物,比如多元醇来调节。氮含量可以通过在制造过程中额外引入含氮化合物来调节。通过调节纳米复合材料中的氧含量和氮含量,可以调节石墨化碳层的催化性能,使其适用于催化不同的反应。在一些实施例中,以质量百分比计,该纳米复合材料中,氧含量为0.1~10wt%,氧含量为0.1~12wt%,此外,还含有少量的氢,氢含量为:0.2~2%。
本发明的纳米复合材料中,各组分的含量之和为100%。
在一些实施例中,石墨化碳层的厚度为0.3~6.0nm,优选为0.3~3nm。在一些实施例中,核壳结构的粒径为1~200nm,优选为3~100nm,更优选为4~50nm。
在一些实施例中,过渡金属选自铁(Fe)、钴(Co)、镍(Ni)、铜(Cu)和锌(Zn)中的一种或多种,优选为镍(Ni)。
在本发明的纳米复合材料的另一个实施方式中,过渡金属纳米粒子的晶格结构为面心立方晶格结构(fcc)和/或密排六方晶格结构(hcp),即可只存在面心立方晶格结构,还可同时存在面心立方晶格结构和密排六方晶格结构。
在一些实施例中,上述碳包覆过渡金属的纳米复合材料通过如下方法制备:
将过渡金属盐、“多元有机羧酸和含氮化合物,或者含氮的有机多元羧酸”以及其他有机化合物在溶剂中混合形成均相溶液,然后除去溶剂,从而形成含过渡金属的水溶性混合物;
将水溶性混合物在惰性气氛保护下高温热解;
将经过高温热解的产物用酸处理,得到碳包覆过渡金属的纳米复合材料。
具体地,制备方法中所提及的水溶性混合物是指将过渡金属盐、“多元有机羧酸和含氮化合物,或者含氮的有机多元羧酸”及除前者外的其它有机化合物在水、乙醇等中溶解成均相溶液,然后直接蒸发除去水分得到含过渡金属的水溶性混合物。蒸发水分的温度和工艺可以采用任意可行的现有技术,例如,在80-120℃下喷雾干燥,或在烘箱中干燥。
在一些实施例中,制备中所用到的有机多元羧酸包括但不限于柠檬酸。过渡金属盐为可溶性盐,包括但不限于醋酸盐。含氮化合物包括但不限于六亚甲基四胺等。其它有机化合物包括但不限于有机多元醇。
在一些实施例中,高温热解步骤中的惰性气氛采用氮气或氩气保护,其中热解过程包括升温段和恒温段,升温段的升温速率为0.5~10℃/min,优选2.5~10℃/min;恒温段的温度为400~1300℃,优选500~800℃;恒温时间为20~600min,优选30~300min。
在一些实施例中,过渡金属盐、多元有机羧酸、含氮化合物和其它有机化合物的质量比为1:0.5~10:0.5~10:0~10,优选1:1~3:1~3:0~3,即可以完全不加入其它有机化合物。
一些实施例中,所述酸处理中优选用非氧化性强酸处理,所述非氧化性强酸包括但不限于氢氟酸、盐酸、硝酸和硫酸中的一种或其任意的组合,优选盐酸和/或硫酸。
在一些实施例中,酸处理的条件为:在30℃~100℃之间处理1h以上,优选在60℃~100℃之间处理1h~20h,更优选在70℃~90℃之间处理1h~10h。
相比现有技术而言,本发明的纳米复合材料的制备简单高效,高温热解前驱体直接由过渡金属盐与多元有机羧酸和含氮化合物在水溶液中直接反应制备,前驱体过渡金属的原子利用率可达100%,克服了现有技术制备金属有机骨架结构前驱体需要使用高温高压反应釜自组装、大量浪费碳源前驱体、有机溶剂、提纯步骤繁琐等缺点。
本发明还提供上述纳米复合材料作为催化剂在加氢还原反应中的应用。例如:采用本发明的复合材料将硝基苯通过催化加氢还原为苯胺。现有技术中用于催化硝基苯加氢反应的催化剂以铂(Pt)、钯(Pd)和铑(Rh)等贵金属催化剂及铜(Cu)、镍(Ni)、铅(Zn)、钼(Mo)等非贵金属催化剂为主。雷尼Ni催化剂由于价格便宜且催化活性相对较高,是目前工业化催化硝基苯类化合物加氢还原生产苯胺类化合物使用最普遍的催化剂,然而仍具有很多缺点,例如,骨架镍在空气中极易着火,无法保存;加氢车间存在氢气,极易发生***;反应副产物量较大,产品收率低且催化活性较低等等。本发明的碳包覆过渡金属的纳米复合材料通过石墨化碳层严密包覆过渡金属内核,保证了其使用和运输过程中的安全性。此外,如上所述,石墨化碳层具有极佳的催化加氢还原有机化合物的能力,有利于进一步提高该复合材料的催化性能。
在一些实施例中,加氢还原反应包括:将硝基苯与纳米复合材料在溶剂中混合,在氢气气氛下进行反应合成苯胺。
在一些实施例中,硝基苯为取代硝基苯,取代基选自C1-20的烷基、环烷基、芳基。
在一些实施例中,纳米复合材料占硝基苯的质量百分比为1%-50%,优选5-30%。
在一些实施例中,加氢还原反应一般在60-120℃下进行,氢气的压力一般为0.5-2MPa。
在一些实施例中,溶剂选自醇类、醚类和水中的一种或多种。
本发明的碳包覆过渡金属的纳米复合材料作为催化材料时,具有重复性良好、高活性、高选择性等优点,适用于大规模工业化生产。
实施例
制备例1
(1)称取10g醋酸镍、10g柠檬酸、20g六亚甲基四胺,将它们加入到含有30mL去离子水的烧杯中,在70℃下搅拌得到均相溶液,并继续加热蒸干得到固体。
(2)将步骤(1)得到的前驱体置于瓷舟内,然后将瓷舟置于管式炉的恒温区,通入氮气,流量100mL/min,并以5℃/min的速率升温至650℃,恒温2h后停止加热,在氮气气氛下冷却至室温,得到碳包覆镍纳米材料
(3)将步骤(2)得到的材料加入100mL10%的盐酸中,在回流温度下处理12h,然后用去离子水将样品洗涤至中性,干燥。如图1所示,将该纳米复合材料置于水中成悬浮液,在容器外侧放置一块磁铁,一段时间后该纳米复合材料均被吸引到磁铁一侧,可见该纳米复合材料具有磁性。该材料中所含元素的质量百分含量列于表1中。
材料的表征:该材料的TEM图如图2所示,可看出,该材料为含有碳包覆金属核壳结构的纳米复合材料,在镍纳米颗粒的外层包裹着具有一定石墨化程度的碳层,形成完整的核壳结构。碳包覆镍的纳米材料的X射线衍射谱图如图3所示,可看出,在该材料的衍射图中存在对应于石墨碳的衍射峰(2θ角为25.97°)和fcc Ni的衍射峰(2θ角为44.47°、51.34°和76.26°),由谢乐公式计算出该碳包覆镍纳米粒子的平均粒径为8.1nm。
BET测试表明,该材料的比表面积为200m2/g,孔体积为0.204cm3/g,其中介孔体积为0.201cm3/g,占总孔体积的98.6%;其中2-5nm的孔体积为0.0245cm3/g,占总孔体积的12.0%。图4a和图4b为该材料的N2吸附-脱附等温线及BJH孔径分布曲线,可以看出,所述复合材料在3.79nm和10.01nm处存在两个介孔分布峰。
该纳米复合材料的X射线光电子能谱(XPS)如图5a-图5c所示,从图5a可以看到明显存在C、O、N和Ni的XPS峰,证明了N、O元素的有效掺杂。从图5b可以看出,其中Ni价态为0价。从图5c可以看出,该复合纳米材料中的O不存在金属-氧(M-O)键,只存在羧基氧、羰基氧和羟基氧,充分证明了这种核壳结构有效的将高活性的Ni纳米粒子与空气隔绝,核壳结构完整。
按术语部分所述方法测量、计算,本制备例制得的复合材料的酸洗损失率为0。在术语部分所述方法的基础上,继续增加酸洗时间,酸洗损失率基本保持不变。
制备例2
(1)称取10g醋酸镍、20g柠檬酸、20g六亚甲基四胺,将它们加入到含有100mL去离子水的烧杯中,在80℃下搅拌得到均相溶液,并继续加热蒸干得到固体。
(2)将步骤(1)得到的前驱体置于瓷舟内,然后将瓷舟置于管式炉的恒温区,通入氮气,流量150mL/min,并以5℃/min的速率升温至600℃,恒温2h后停止加热,在氮气气氛下冷却至室温,得到碳包覆纳米材料。
(3)将步骤(2)得到的材料加入80mL 10%的盐酸中,在回流温度下处理10h,然后用去离子水将样品洗涤至中性,干燥。经元素分析仪和X射线荧光光谱分析仪(XRF)测定后,该材料中所含元素的质量百分含量列于表1中。
材料的特征:该纳米复合材料的TEM图如图6所示,该纳米复合材料含有以纳米金属镍为核,具有一定石墨化的碳为壳的纳米粒子;该材料的X射线衍射谱图如图7所示,在该材料的XRD衍射图中存在对应于碳的衍射峰(2θ角为26.1°)、fcc Ni的衍射峰(44.6°、51.8°和76.4°)和hcp Ni的衍射峰(2θ角为41.7°、44.6°、47.6°和62.4°),由谢乐公式计算出该碳包覆镍纳米粒子的平均粒径为34.5nm;BET测试表明,该材料的比表面积为183m2/g,孔体积为0.278cm3/g,其中介孔体积为0.276cm3/g,占总孔体积的99.3%;其中2-5nm的孔体积为0.0646cm3/g,占总孔体积的23.2%。图8为该材料的BJH孔径分布曲线,可以看出,该复合材料在3.83nm和9.97nm处存在两个介孔分布峰。
按术语部分所述方法测量、计算,本制备例制得的复合材料的酸洗损失率为0。在术语部分所述方法的基础上,继续增加酸洗时间,酸洗损失率基本保持不变。
制备例3
(1)称取10g醋酸钴,10g柠檬酸、20g六亚甲基四胺,将它们加入到含有150mL去离子水的烧杯中,在60℃下搅拌得到均相溶液,并继续加热蒸干得到固体。
(2)将步骤(1)得到的前驱体粉末置于瓷舟内,然后将瓷舟置于管式炉的恒温区,通入氮气,流量100mL/min,并以5℃/min的速率升温至700℃,恒温1h后停止加热,在氮气气氛下冷却至室温,得到碳包覆纳米材料。
(3)将步骤(2)得到的材料加入80mL 10%的盐酸中,在回流温度下处理6h,然后用去离子水将样品洗涤至中性,干燥。经元素分析仪和X射线荧光光谱分析仪(XRF)测定,该纳米复合材料中所含元素的质量百分含量列于表1中。
材料的特征:该纳米复合材料的TEM图如图9所示,该纳米复合材料含有以纳米金属钴为核,具有一定石墨化的碳为壳的纳米粒子;该材料的X射线衍射谱图如图10所示,在该材料的XRD衍射图中存在对应于碳的衍射峰(2θ角为25.96°)、fcc Co的衍射峰(44.4°),由谢乐公式计算出该碳包覆钴纳米粒子的平均粒径为14.2nm;BET测试表明,该材料的比表面积为256m2/g,孔体积为0.244cm3/g,其中介孔体积为0.244cm3/g,占总孔体积的100%;其中2-5nm的孔体积为0.073cm3/g,占总孔体积的29.9%。图11为该材料的BJH孔径分布曲线,可以看出,该复合材料在3.66nm和13.52nm处存在两个介孔分布峰。
按术语部分所述方法测量、计算,本制备例制得的复合材料的酸洗损失率为7%。在术语部分所述方法的基础上,继续增加酸洗时间,酸洗损失率基本保持不变。
制备例4
(1)称取10g醋酸镍、10g醋酸钴,20g柠檬酸和10g六亚甲基四胺,将它们加入到含有150mL去离子水的烧杯中,在60℃搅拌反应24h后继续加热蒸干得到固体。该固体前驱体的X射线衍射谱图如图12所示。
(2)将步骤(1)得到的前驱体粉末置于瓷舟内,然后将瓷舟置于管式炉的恒温区,通入氮气,流量100mL/min,并以4℃/min的速率升温至600℃,恒温2h后停止加热,在氮气气氛下冷却至室温,得到碳包覆纳米材料。
(3)将步骤(2)得到的材料加入80mL 10%的盐酸中,在回流温度下处理4h,然后用去离子水将样品洗涤至中性,干燥。经元素分析仪和X射线荧光光谱分析仪(XRF)测定,该纳米复合材料中所含元素的质量百分含量列于表1中。
材料的特征:该纳米复合材料的TEM图如图13所示,该纳米复合材料含有以纳米金属镍和钴为核,具有一定石墨化的碳为壳的纳米粒子;该材料的X射线衍射谱图如图14所示,在该材料的XRD衍射图中存在对应于碳的衍射峰(2θ角为26.2°)和fcc Ni或Co的衍射峰(44.5°、51.7°和76.1°),由谢乐公式计算出该碳包覆镍钴纳米粒子的平均粒径为13.4nm;BET测试表明,该材料的比表面积为324m2/g,孔体积为0.389cm3/g,其中介孔体积为0.389cm3/g,占总孔体积的100%;其中2-5nm的孔体积为0.048cm3/g,占总孔体积的12.3%。图15为该材料的BJH孔径分布曲线,可以看出,该复合材料在3.74nm和6.59nm处存在两个介孔分布峰。
按术语部分所述方法测量、计算,本制备例制得的复合材料的酸洗损失率为4%。在术语部分所述方法的基础上,继续增加酸洗时间,酸洗损失率基本保持不变。
表1
制备例 | 碳,wt% | 氢,wt% | 氮,wt% | 氧,wt% | 镍,wt% | 钴,wt% |
制备例1 | 47.55 | 1.33 | 4.27 | 4.84 | 42.01 | _ |
制备例2 | 48.57 | 1.35 | 4.61 | 5.79 | 39.68 | _ |
制备例3 | 52.02 | 1.44 | 6.48 | 7.56 | _ | 32.5_ |
制备例4 | 42.68 | 1.82 | 3.27 | 7.51 | 24.27 | 20.45 |
对比例1
将10g醋酸镍固体置于瓷舟内,然后将瓷舟置于管式炉的恒温区,通入流量为150mL/min的氮气,并以5℃/min的速率升温至600℃,恒温2h后停止加热,并在氮气气氛下冷却至室温,得到样品材料。经元素分析仪和X射线荧光光谱分析仪(XRF)测定,该复合材料中所含元素的质量百分含量为:碳1.34%,氢0.32%,氧0.18%,镍98.16%。该纳米复合材料的X射线衍射谱图如图16所示,可看出,在该材料的衍射图中存在对应于fcc Ni的衍射峰(44.2°、51.6°和76.2°)。
按术语部分所述方法测量、计算,本对比例制得的复合材料的酸洗损失率为100%。
实施例1
将制备例1所得纳米复合材料作为催化剂用于硝基苯加氢制备苯胺,具体的实验步骤为:
将0.1g纳米复合材料、1.97g硝基苯,100mL乙醇加入反应釜中,通H2置换反应釜3次后,通H2使反应釜内压力为3MPa,搅拌升温,升温至预定反应温度60℃,反应预定时间3小时后停止加热,降至室温,排压,开反应釜取产物苯胺进行色谱分析。通过以下公式计算反应物转化率及目的产物选择性:
转化率=已反应的反应物质量/反应物加入量×100%
选择性=目的产物质量/反应生成物质量×100%
经分析后,得硝基苯转化率为100%,苯胺选择性为99.3%。
实施例2
将制备例1所得纳米复合材料作为催化剂用于硝基苯加氢制备苯胺,具体的实验步骤为:
将0.1g纳米复合材料、0.49g硝基苯,30mL乙醇加入反应釜中,通H2置换反应釜3次后,通H2使反应釜内压力为0.5MPa,搅拌升温,升温至预定反应温度120℃,反应预定时间0.5小时后停止加热,降至室温,排压,开反应釜取产物苯胺进行色谱分析。通过实施例1所列公式计算反应物转化率及目的产物选择性:
经分析后,得硝基苯转化率为100%,苯胺选择性为99.6%。
实施例3
将制备例1所得纳米复合材料作为催化剂用于硝基苯加氢制备苯胺,具体的实验步骤为:
将0.1g纳米复合材料、0.33g硝基苯,30mL乙醇加入反应釜中,通H2置换反应釜3次后,通H2使反应釜内压力为1MPa,搅拌升温,升温至预定反应温度60℃,反应预定时间2小时后停止加热,降至室温,排压,开反应釜取产物苯胺进行色谱分析。通过实施例1所列公式计算反应物转化率及目的产物选择性:
经分析后,得硝基苯转化率为100%,苯胺选择性为99.9%。
实施例4
将制备例2所得纳米复合材料作为催化剂用于硝基苯加氢制备苯胺,具体的实验步骤为:
将0.1g纳米复合材料、0.66g硝基苯,50mL乙醇加入反应釜中,通H2置换反应釜3次后,通H2使反应釜内压力为1MPa,搅拌升温,升温至预定反应温度100℃,反应预定时间1小时后停止加热,降至室温,排压,开反应釜取产物苯胺进行色谱分析。通过实施例1所列公式计算反应物转化率及目的产物选择性:
经分析后,得硝基苯转化率为100%,苯胺选择性为99.7%。
由以上实验数据可知,本发明提供的碳包金属复合材料能够应用于硝基苯加氢制备苯胺反应中,且具有良好的转化率和选择性。
本领域技术人员应当注意的是,本发明所描述的实施方式仅仅是示范性的,可在本发明的范围内作出各种其他替换、改变和改进。因而,本发明不限于上述实施方式,而仅由权利要求限定。
Claims (16)
1.一种碳包覆过渡金属的纳米复合材料,所述纳米复合材料含具有壳层和内核的核壳结构,所述壳层为掺杂氮和氧的石墨化碳层,所述内核为过渡金属纳米粒子,其中,所述纳米复合材料的酸洗损失率≤10%。
2.根据权利要求1所述的纳米复合材料,其中所述纳米复合材料为具有至少一个介孔分布峰的介孔材料。
3.根据权利要求2所述的纳米复合材料,其中所述纳米复合材料为具有两个或两个以上介孔分布峰的介孔材料。
4.根据权利要求1至3中任一项所述的纳米复合材料,其中所述介孔材料中介孔体积占总孔体积的比例大于50%,优选大于80%。
5.根据权利要求1所述的纳米复合材料,其中以质量百分比计,所述纳米复合材料中的碳含量为15~60wt%,过渡金属含量为30~80wt%。
6.根据权利要求1所述的纳米复合材料,其中以质量百分比计,所述纳米复合材料中的氮和氧的总含量小于15%。
7.根据权利要求1所述的纳米复合材料,其中所述石墨化碳层的厚度为0.3~6nm,优选为0.3~3nm。
8.根据权利要求1所述的纳米复合材料,其中所述核壳结构的粒径为1~200nm,3~100nm,优选为4~50nm。
9.根据权利要求1至8中任一项所述的纳米复合材料,其中所述过渡金属选自铁、钴、镍、铜和锌中的一种或多种,优选为镍。
10.根据权利要求9所述的纳米复合材料,其中所述过渡金属纳米粒子的晶格结构为面心立方晶格结构和/或密排六方晶格结构。
11.根据权利要求1-10中任一项所述的纳米复合材料作为催化剂在加氢还原反应中的应用。
12.根据权利要求11所述的应用,其中所述加氢还原反应包括:
将硝基苯与所述纳米复合材料在溶剂中混合,在氢气气氛下进行反应合成苯胺。
13.根据权利要求12所述的应用,其中所述硝基苯为取代硝基苯,取代基选自C1-20的烷基、环烷基、芳基。
14.根据权利要求12所述的应用,其中所述纳米复合材料占所述硝基苯的质量百分比为1%-50%,优选5-30%。
15.根据权利要求12所述的应用,其中所述加氢还原反应在60-120℃下进行,所述氢气的压力为0.5-2MPa。
16.根据权利要求12至15中任一项所述的应用,其中所述溶剂选自醇类、醚类和水中的一种或多种。
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