CN105949134A - 一种磺胺嘧啶铁钯纳米复合粒子及其制备方法 - Google Patents
一种磺胺嘧啶铁钯纳米复合粒子及其制备方法 Download PDFInfo
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- SEEPANYCNGTZFQ-UHFFFAOYSA-N sulfadiazine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CC=N1 SEEPANYCNGTZFQ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229960004306 sulfadiazine Drugs 0.000 title claims abstract description 53
- 239000002245 particle Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002114 nanocomposite Substances 0.000 title abstract 6
- SORXVYYPMXPIFD-UHFFFAOYSA-N iron palladium Chemical compound [Fe].[Pd] SORXVYYPMXPIFD-UHFFFAOYSA-N 0.000 title abstract 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 86
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000013110 organic ligand Substances 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 9
- 238000005859 coupling reaction Methods 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 239000003446 ligand Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 150000002505 iron Chemical class 0.000 claims description 12
- 150000002940 palladium Chemical class 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 10
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- 239000011203 carbon fibre reinforced carbon Substances 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
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- 238000006555 catalytic reaction Methods 0.000 abstract description 8
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- 229910052742 iron Inorganic materials 0.000 abstract description 3
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- 239000002184 metal Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract 1
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 230000000694 effects Effects 0.000 description 8
- 239000012046 mixed solvent Substances 0.000 description 6
- 239000011943 nanocatalyst Substances 0.000 description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 6
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
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- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
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- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
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Abstract
本发明公开了一种磺胺嘧啶铁钯纳米复合粒子及其制备方法，本发明中将一定比例的两种金属盐溶液加入到含有的磺胺嘧啶有机配体中，在一定温度下水热反应，反应结束冷却至室温，过滤，干燥，制得相应的金属‑配体纳米复合粒子。制备过程简单，成本低，适合大量生产；通过控制反应物的用量、反应时间和反应温度，实现磺胺嘧啶铁钯纳米复合粒子粒径的大小及分散性的有效调控。本发明制备的磺胺嘧啶铁钯纳米复合粒子是一种含有铁和钯的功能化纳米粒子，性能稳定，可用于催化C‑C键偶联反应，催化效率高，产率可达95％以上。因此该磺胺嘧啶铁钯纳米复合粒子在催化领域具有广阔的应用前景。
Description
技术领域
本发明属于纳米材料催化领域，具体涉及到用于催化碳碳偶联反应的一种磺胺嘧啶铁钯纳米复合粒子及其制备方法。
背景技术
构成纳米材料的纳米粒子也叫超微颗粒，一般是指尺寸在1～100nm间的粒子，是处在原子簇和宏观物体交界的过渡区域，从通常的关于微观和宏观的观点看，这样的系统既非典型的微观系统亦非典型的宏观系统，是一种典型的介观系统，它具有表面效应、小尺寸效应和宏观量子隧道效应。当人们将宏观物体细分成超微颗粒(纳米级)后，它将显示出许多奇异的特性，即它的光学、热学、电学、磁学、力学以及化学方面的性质和大块固体时相比将会有显著的不同。如今，纳米颗粒的研究是一大热门，真正有意识的研究纳米粒子可追溯到20世纪30年代的日本的为了军事需要而开展的“沉烟试验”，到了20世纪60年代人们开始对分立的纳米粒子进行研究。1963年，Uyeda用气体蒸发冷凝法制的了金属纳米微粒，并对其进行了电镜和电子衍射研究。1984年德国萨尔兰大学(SaarlandUniversity)的Gleiter以及美国阿贡实验室的Siegal相继成功地制得了纯物质的纳米细粉。Gleiter在高真空的条件下将粒子直径为6nm的铁粒子原位加压成形，烧结得到了纳米微晶体块，从而使得纳米材料的研究进入了一个新阶段。
纳米材料研究的价值很高、深而广之，这里仅仅涉及其催化方面的作用。由于纳米微粒粒径小、比表面积大、表面原子数增多并且生成不饱键，这就使得纳米微粒具有高的表面活性。并且粒径越小，表面原子数所占比率越大；比表面积越大，表面粗糙度越大，增加了化学反应的接触面，使其具有优良的催化性能。纳米催化剂由于其高效的还原或氧化作用，在催化或光催化领域的应用非常广泛，与普通商用催化剂相比，表现出高活性和高选择性等优异的催化性能。在反应中，纳米催化剂的尺寸、形貌、表面性质等对其活性和选择性起到了关键的作用。纳米催化剂制备过程中的条件，如原料浓度、反应时间、反应温度、溶剂比例和表面活性剂等，对于控制制备纳米催化剂至关重要。目前，人们对各种纳米催化剂的制备和应用做了大量研究，取得了丰硕的成果，同时也提出了纳米催化剂在实际应用中出现的许多问题。本发明立足于绿色、廉价、简易、可工业化放大的制备方法，来获得磺胺嘧啶铁钯纳米粒子。
发明内容
本发明所要解决的技术问题是，针对现有技术的不足，提供一种制备过程简单且成本低的可作为高效催剂的磺胺嘧啶铁钯纳米复合粒子及其制备方法。
本发明为解决上述技术问题所采用的技术方案为：一种可作为高效催剂的磺胺嘧啶铁钯纳米粒子复合粒子的制备方法，包括以下步骤：
将磺胺嘧啶溶于适量的蒸馏水中，配制成有机配体溶液；
将铁盐溶于适量的弱酸性水中，配制成铁盐溶液；
将钯盐溶于适量的蒸馏水中，配制成钯盐溶液；
将上述铁盐溶液与钯盐溶液混合，形成混合溶液，将混合溶液快速加入到机配体溶液中，然后将含有铁盐、钯盐和磺胺嘧啶有机配体的溶液转移到有聚四氟乙烯内衬的不锈钢反应釜中，120～160℃水热反应12～24h，反应结束冷却至室温，过滤，干燥，即获得所述磺胺嘧啶铁钯纳米复合粒子材料。
所述铁盐、钯盐和磺胺嘧啶有机配体的溶液中，铁、钯与磺胺嘧啶物质的量之比为3：1：4～3：1：8。
优选的，所述铁盐为氯化铁和硝酸铁中的任意一种；
优选的，所述钯盐为氯化钯和醋酸钯中的任意一种；
优选的，所述磺胺嘧啶有机配体的物质的量浓度为2～4mmol/L。
本发明提供一种磺胺嘧啶铁钯纳米复合粒子，所述磺胺嘧啶铁钯纳米复合粒子是根据上述磺胺嘧啶铁钯纳米复合粒子的制备方法制备得到。
优选地，所述磺胺嘧啶铁钯纳米复合粒子作为高效催化剂，用于催化碳-碳键偶联反应。
与现有技术相比，本发明的优点如下：
(1)上述有机配体磺胺嘧啶具有不对称的独特的结构，同时含有氨基等吸电子基团，对配体电子的离域性产生独特的影响，从而对配体的电子层结构产生影响，因而形成的化合物具有独特的物理化学性质。
(2)由于上述磺胺嘧啶电子的离域性强且具有不对称性，可以和铁离子和钯离子在不同方向进行配位，形成磺胺嘧啶铁钯纳米复合粒子。此纳米粒子性能稳定，在催化碳-碳键偶联反应中，显示了较高的反应活性，产率可达95％以上。
(3)上述磺胺嘧啶铁钯纳米复合粒子制备过程简单，成本低，适合大量生产。
(4)本发明通过选用两种不同的金属盐，控制反应时间、反应温度，实现磺胺嘧啶铁钯纳米复合粒子粒径的大小及分散性的有效调控，获得粒径不同的磺胺嘧啶铁钯纳米复合粒子，其在催化领域有广阔的应用前景。
附图说明
图1为本发明磺胺嘧啶铁钯纳米复合粒子材料的扫描电镜图。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1
称取3mmol的Fe(NO3)3·9H2O溶于15mL pH为5的水溶液中，将1mmol的PaCl2溶于和10mL的蒸馏水中，将铁和钯的溶液混合，形成混合溶液；称取4mmol的磺胺嘧啶溶于20mL蒸馏水中，在搅拌状态下，将铁和钯的溶液混合快速加入到磺胺嘧啶溶液中，然后将含有铁、钯和磺胺嘧啶配体的溶液转移到有聚四氟乙烯内衬的不锈钢反应釜中，120℃水热反应24h，反应结束冷却至室温，过滤，干燥，即获得所述磺胺嘧啶铁钯纳米复合粒子材料。用扫描电镜观察所得纳米复合粒子的形貌，如图1所示。
实施例2
称取3mmol的FeCl3溶于15mL pH为5的水溶液中，将1mmol的PaCl2溶于和10mL的蒸馏水中，将铁和钯的溶液混合，形成混合溶液；称取8mmol的磺胺嘧啶溶于20mL蒸馏水中，在搅拌状态下，将铁和钯的溶液混合快速加入到磺胺嘧啶溶液中，然后将含有铁、钯和磺胺嘧啶配体的溶液转移到有聚四氟乙烯内衬的不锈钢反应釜中，160℃水热反应12h，反应结束冷却至室温，过滤，干燥，即获得所述磺胺嘧啶铁钯纳米复合粒子材料。
实施例3
称取3mmol的Fe(NO3)3·9H2O溶于15mL pH为5的水溶液中，将1mmol的醋酸钯溶于和10mL的蒸馏水中，将铁和钯的溶液混合，形成混合溶液；称取6mmol的磺胺嘧啶溶于20mL蒸馏水中，在搅拌状态下，将铁和钯的溶液混合快速加入到磺胺嘧啶溶液中，然后将含有铁、钯和磺胺嘧啶配体的溶液转移到有聚四氟乙烯内衬的不锈钢反应釜中，140℃水热反应20h，反应结束冷却至室温，过滤，干燥，即获得所述磺胺嘧啶铁钯纳米复合粒子材料。
以实施例1，实施例2和实施例3制备的磺胺嘧啶铁钯纳米复合粒子为例，进行催化反应：
使用实施例1制备的磺胺嘧啶铁钯纳米复合粒子作为催化剂进行催化反应，反应条件为：将1.0mmol对碘苯乙醚、1.2mmol对甲基苯硼酸和3.0mmol K2CO3，在空气氛围中于H2O/EtOH混合溶剂中反应，该混合溶剂由3mL水和4mL乙醇组成，反应温度为90℃，反应时间为8h，采用柱色谱法分离产物，产率为99％。反应方程式如下：
使用实施例2制备的磺胺嘧啶铁钯纳米复合粒子作为催化剂进行催化反应，反应条件为：将1.0mmol对溴苯甲醚、1.2mmol对甲基苯硼酸和3.0mmol K2CO3，在空气氛围中于H2O/EtOH混合溶剂中反应，该混合溶剂由3mL水和4mL乙醇组成，反应温度为90℃，反应时间为8h，采用柱色谱法分离产物，产率为97％。反应方程式如下：
使用实施例3制备的磺胺嘧啶铁钯纳米复合粒子作为催化剂进行催化反应，反应条件为：将1.0mmol对碘苯乙醚、1.2mmol苯硼酸和3.0mmol K2CO3，在空气氛围中于H2O/EtOH混合溶剂中反应，该混合溶剂由3mL水和4mL乙醇组成，反应温度为90℃，反应时间为8h，采用柱色谱法分离产物，产率为98％。该反应方程式如下：
Claims (3)
1.一种磺胺嘧啶铁钯纳米复合粒子的制备方法，其特征在于所述制备方法包括以下步骤：
将磺胺嘧啶溶于适量的蒸馏水中，配制成有机配体溶液；
将铁盐溶于适量的pH为5的弱酸性水中，配制成铁盐溶液；
将钯盐溶于适量的蒸馏水中，配制成钯盐溶液；
将上述铁盐溶液与钯盐溶液混合，形成混合溶液，将混合溶液快速加入到机配体溶液中，然后将含有铁盐、钯盐和磺胺嘧啶有机配体的溶液转移到有聚四氟乙烯内衬的不锈钢反应釜中，120～160℃水热反应12～24h，反应结束冷却至室温，过滤，干燥，即获得所述磺胺嘧啶铁钯纳米复合粒子材料；
所述铁盐、钯盐和磺胺嘧啶有机配体的溶液中，铁、钯与磺胺嘧啶物质的量之比为3：1：4～3：1：8；
所述铁盐为氯化铁和硝酸铁中的任意一种；
所述钯盐为氯化钯和醋酸钯中的任意一种；
所述磺胺嘧啶有机配体的物质的量浓度为2～4mmol/L。
2.一种磺胺嘧啶铁钯纳米复合粒子，其特征在于，所述磺胺嘧啶铁钯纳米复合粒子根据权利要求1所述的磺胺嘧啶铁钯纳米复合粒子的制备方法制备得到。
3.一种如权利要求2所述的磺胺嘧啶铁钯纳米复合粒子，其特征在于，所述磺胺嘧啶铁钯纳米复合粒子作为高效催化剂，用于催化碳-碳键偶联反应。
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