CN104477994A - 一种钽酸钠的制备方法 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- KVDJFAANUSOHTB-UHFFFAOYSA-N sodium;oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[Na+].[Ta+5] KVDJFAANUSOHTB-UHFFFAOYSA-N 0.000 title abstract 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 120
- 239000000047 product Substances 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 5
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 15
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- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
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- 238000010189 synthetic method Methods 0.000 description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- YECIFGHRMFEPJK-UHFFFAOYSA-N lidocaine hydrochloride monohydrate Chemical compound O.[Cl-].CC[NH+](CC)CC(=O)NC1=C(C)C=CC=C1C YECIFGHRMFEPJK-UHFFFAOYSA-N 0.000 description 1
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- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
- B01J2523/10—Constitutive chemical elements of heterogeneous catalysts of Group I (IA or IB) of the Periodic Table
- B01J2523/12—Sodium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
- B01J2523/50—Constitutive chemical elements of heterogeneous catalysts of Group V (VA or VB) of the Periodic Table
- B01J2523/57—Tantalum
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Abstract
本发明为一种钽酸钠的制备方法,该方法包括以下步骤:(1)将氢氧化钠和五氧化二钽混合后研磨,其中,摩尔比为NaOH:Ta2O5=2:1~8:1;(2)将步骤(1)中得到的混合物在500~800℃熔融反应1~10小时;(3)用去离子水和稀酸溶液清洗步骤(2)得到的反应产物,然后再50~180℃烘干即可以得到钽酸钠产物。本发明采用的氢氧化钠熔融法是一种简单、高效的NaTaO3合成方法,并且能够在较温和条件下制备掺杂量可精确控制的掺杂钽酸钠。
Description
技术领域
本发明涉及一种光催化剂的制备方法,具体为一种钽酸钠光催化剂的氢氧化钠熔融制备方法。
背景技术
随着社会与经济的高速发展,人类面临着严重的环境污染问题和能源危机。光催化剂被认为是解决这两种难题的关键材料,它既可以用来光催化裂解水制氢,又可以用来光催化降解有机染料。钽酸钠(NaTaO3)是一种性能优异的、紫外光激活的催化剂(H.Kato,A.Kudo,Cata.Lett.1999,58,153-155)。负载NiO的NaTaO3分解纯水制备H2和O2的量子效率达到20-28%(H.Kato,A.Kudo,J.Phys.Chem.B 2001,105,4285-4292)。掺杂被认为是一种有效地调节NaTaO3能带结构的方法,通过掺杂可以获得可见光响应的、高效率的催化剂。目前,单相和掺杂NaTaO3的合成方法主要有高温固相反应法、水热法和溶胶-凝胶法。其中,固相反应法通常以NaHCO3、Ta2O5为原料,经过1200℃、10h高温反应多次才能得到单相的NaTaO3(W.Lin,C.Cheng,C.Hu,H.Teng,Appl.Phys.Lett.2006,89,211904)。这种高温反应过程耗能、耗时,并且产物是催化效率较低的正交相NaTaO3。这种高温固相反应方法尤其不利于N掺杂NaTaO3的合成,因为作为N源的Ta3N5或者TaON通过在700℃即分解。水热法是另一种较简便的NaTaO3纳米颗粒合成方法,研究者通常以Ta2O5和超浓的NaOH溶液([NaOH]≥10M)为原料,在反应釜中经过160~240℃反应12~48h制备具有立方体形貌的NaTaO3纳米颗粒(Y.He,Y.Zhu,N.Wu,J.SolidState Chem.2004,177,3868-3872;J.W.Liu,G.Chen,Z.H.Li,Int.J.Hydrogen Energy,2007,32,2269-2272)。但是,以水热法合成钽酸钠的过程中,反应在水溶液中进行,这样在合成金属离子掺杂的钽酸钠时,掺杂物质通常会溶于水中,不易控制最终产物中掺杂离子的含量。以溶胶-凝胶法制备NaTaO3时,虽然可以在较低的温度下合成单相NaTaO3,但需要采用价格昂贵的TaCl5或Ta(CH3CH2OH)5为钽源,因此这种合成路线的成本较高。因此,迄今为止单相和掺杂的NaTaO3的简易、高效、低成本的制备方法仍然是缺乏的。
发明内容
本发明针对当前制备钽酸钠技术中存在的不足,提供一种钽酸钠的制备方法,该方法采用NaOH熔融法能在较低温度下合成设计化学计量比的掺杂NaTaO3催化剂,不仅克服了固相反应合成NaTaO3时的高温、长时的缺点;而且能够较精确地控制合成的掺杂钽酸钠中掺杂离子的浓度。本发明采用氢氧化钠熔融法具有简单、反应条件温和、低成本的优点。
本发明的技术方案是:
一种钽酸钠的制备方法,该方法包括以下步骤:
(1)将氢氧化钠和五氧化二钽混合后研磨,其中,摩尔比为NaOH:Ta2O5=2:1~8:1;
(2)将步骤(1)中得到的混合物在空气气氛或者保护气氛中以每分钟1~30℃的速率升温至500~800℃,然后在该温度下熔融反应1~10小时,然后降温至室温得到反应产物,
(3)用稀酸溶液和去离子水清洗步骤(2)得到的反应产物,然后再50~180℃烘干即可以得到钽酸钠产物;
所述的稀酸溶液为稀硝酸、稀盐酸或者稀硫酸溶液。
其中,保护气氛为氮气、氩气或两者的混合气体。
本发明的有益效果是:
1.本发明采用的氢氧化钠熔融方法能在较温和的条件下合成了单相。如图1(b)所示,摩尔比为NaOH:Ta2O5=2.5:1混合原料经过500℃、3h的熔融反应就能够得到单相的NaTaO3。在以上合成反应过程中,NaOH既是反应物,又能在此反应温度下熔融,从而提供了液相反应介质。这一合成温度远低于固相反应法合成钽酸钠的温度(1200℃),反应时间也远远短于固相反应所需要的时间(12~36h);与水热反应相比,在本发明的合成方案所需要的设备简单,不需要水热反应中必需的水热釜;与溶胶-凝胶法相比,成本大大降低。因此,本发明采用的氢氧化钠熔融法是一种简单、高效的NaTaO3合成方法。
2.本发明采用的氢氧化钠熔融法能够在较温和条件下制备掺杂量可精确控制的掺杂钽酸钠。如图3所示是以化学式NaTa1-xMoxO3-xNx(x=0,0.01,0.03,0.05,0.1)为目标产物,以NaOH、Ta2O5、Ta3N5和(NH4)6Mo7O24·4H2O为原料(其中,NaOH和Ta2O5的摩尔比为NaOH:Ta2O5=2.5:1)在700℃的N2中反应3h得到产物的XRD图谱。制备的产物为单相的NaTaO3,没有其他杂质相产生。通过EDS图谱分析了制备产物的化学组成(图4),在制备的掺杂的NaTaO3中存在掺杂离子Mo和N。并且,产物中掺杂离子浓度随反应物中掺杂含量的提高而升高,与设计化学式的成分接近。
附图说明
下面结合附图和具体实施对本发明进一步说明。
图1为实例1~9中不同化学计量比和不同温度下合成样品的XRD图谱,其中,图1(a)不同摩尔比的NaOH/Ta2O5经过700℃、3h反应之后得到产物的XRD图谱;图1(b)摩尔比为NaOH:Ta2O5=2.5:1的混合物经过不同温度下3h反应之后得到产物的XRD图谱。
图2为实例6~9中摩尔比为NaOH:Ta2O5=2.5:1的混合物经过不同温度下3h反应之后得到产物的微观结构的扫描照片,图2(a)为500℃,图2(b)为600℃,图2(c)为700℃和图2(d)为800℃,反应气氛为空气。
图3为实例10~14中通过熔融法在700℃的N2中以NaOH,Ta2O5,Ta3N5,(NH4)6Mo7O24·4H2O为原料分别合成的NaTa1-xMoxO3-xNx(x=0,0.01,0.03,0.05和0.1产物的XRD图谱。
图4为实例13中通过熔融法合成的NaTa0.95Mo0.05O2.95N0.05产物EDS图谱。
具体实施方式
实施例1
(1)按照摩尔比NaOH:Ta2O5=2:1称取反应原料氢氧化钠和氧化钽,然后在玛瑙研钵中研磨20min以上,使原料混合均匀。将混合原料置于氧化铝坩埚中,在空气氛围下以每分钟20℃的速率升温至700℃,然后在空气中、700℃熔融反应3h,得到白色固体物质;
(2)将步骤(1)中得到的产物用稀硝酸(体积浓度为10%)溶液清洗4次,再用去离子水清洗4次,以去除多余的NaOH以及可能存在的铝离子。将清洗后得到的白色物质放入60℃的烘干箱中,保温12h,得到白色产物。
实施例2、3、4、5
其他步骤同实施例1,不同之处为将步骤(1)中反应物的摩尔比NaOH:Ta2O5由2:1分别变为8:1、10:1、15:1和20:1。
以上实施例采用X射线衍射仪(XRD)对制备产物的物相组成进行分析,结果如图1(a)所示。当NaOH和Ta2O5的摩尔比为2:1至8:1时,在700℃反应3h可以得到单相的NaTaO3产物;当NaOH和Ta2O5的摩尔比高于10:1时,得到的是非晶相的NaTaO3。因此,采用氢氧化钠熔融法合成NaTaO3时,原料的摩尔比应为NaOH:Ta2O5=2:1~8:1。
实施例6
(1)按照摩尔比NaOH:Ta2O5=2.5:1称取原料氢氧化钠和氧化钽,然后在玛瑙研钵中混合均匀,于氧化铝坩埚中在500℃的空气中反应3h,得到白色固体物质;
(2)同实施例1的步骤(2)。
实施例7、8、9
其他步骤同实施例6,不同之处为将步骤(1)中反应温度由500℃分别变为600、700和800℃。
图1(b)摩尔比NaOH:Ta2O5=2.5:1的混合原料在不同温度下熔融反应得到产物的XRD图谱。在500℃熔融反应3h就可以得到单相的NaTaO3,随着反应温度逐渐升高至800℃,得到的单相NaTaO3产物的X射线衍射峰的半峰宽逐渐变窄,表明随着温度升高产物的结晶度增大。图2是以上不同温度反应得到产物的微观结构的扫描照片。在500和600℃熔融反应产物具有不规则的片状结构;当反应温度升高到700℃时,产物中出现立方颗粒形貌;当反应温度进一步升高到800℃时,反应产物具有规则的立方体或者产物体形貌,产物的尺寸分布在100~300nm之间。
实施例10
(1)按照设计的化学式NaTa1-xMoxO3-xNx(x=0.01,即设计的化学式为NaTa0.99Mo0.01O2.99N0.01)称取NaOH、Ta2O5、(NH4)6Mo7O24·4H2O和Ta3N5原料,其中NaOH和Ta2O5的摩尔比为2.5:1,Mo和N的掺杂量为x=0.01。将原料在玛瑙研钵中混合均匀,然后放入氧化铝坩埚中,在700℃的N2中反应3h,得到不同颜色的反应产物;
(2)将步骤(1)中得到的产物用稀硝酸和去离子水反复清洗8次以上,然后在60℃的烘干箱中干燥得到产物。
实施例11、12、13、14
其他步骤同实施例10,不同之处为将步骤(1)中掺杂量x=0.01改为x=0,0.03,0.05和0.1。随着Mo和N掺杂量的升高,得到掺杂NaTaO3样品的颜色逐渐由白色变为浅绿色和灰绿色,即样品颜色随掺杂浓度的增大而逐渐加深,这也说明了产物中掺杂物质浓度的变化。
如图3所示,当掺杂含量x≤0.05时,得到了单相的NaTaO3样品,并没有其他杂质相出现。在NaTa0.95Mo0.05O2.95N0.05样品EDS图谱中(图4),可以观察到明显的属于Mo和N的特征峰存在,说明掺杂的Mo和N进入到了NaTaO3的晶格位置。进一步的EDS分析结果表明,当x=0.01,0.03,0.05和0.1时,制备不同掺杂量的NaTaO3:Mo,N样品的化学式分别为NaTa0.998Mo0.007O2.986N0.009,NaTa0.984Mo0.027O2.965N0.027,NaTa0.962Mo0.045O2.943N0.048和NaTa0.917Mo0.076O2.898N0.083,实际产物的化学计量比基本与设计的化学计量比相近,微小的偏差可能是由EDS测试误差导致的。
实施例15、16
将实施例8(原料摩尔比NaOH:Ta2O5=2.5:1,反应温度为700℃)步骤(1)中的熔融反应时间分别改为1和10h,其他各项操作均与实施例8相同,得到产物同实施例8。
实施例17
将实施例8(原料摩尔比NaOH:Ta2O5=2.5:1,反应温度为700℃)步骤(1)中的反应气氛改为氩气,其他各项操作均与实施例8相同,得到产物同实施例8。
实施例18、19
将实施例8(原料摩尔比NaOH:Ta2O5=2.5:1,反应温度为700℃)步骤(2)中的烘干温度改为50和180℃,其他各项操作均与实施例8相同,得到产物同实施例8。
实施例21、22
将实施例8(原料摩尔比NaOH:Ta2O5=2.5:1,反应温度为700℃)步骤(2)中的稀硝酸溶液分别改为体积浓度为10%的稀盐酸和稀硫酸溶液,其他各项操作均与实施例8相同,得到产物同实施例8。
本发明未尽事宜为公知技术。
Claims (2)
1.一种钽酸钠的制备方法,其特征为该方法包括以下步骤:
(1)将氢氧化钠和五氧化二钽混合后研磨,其中,摩尔比为NaOH:Ta2O5=2:1~8:1;
(2)将步骤(1)中得到的混合物在空气气氛或者保护气氛中以每分钟1~30℃的速率升温至500~800℃,然后在该温度下熔融反应1~10小时,然后降温至室温得到反应产物,
(3)用稀酸溶液和去离子水清洗步骤(2)得到的反应产物,然后再50~180℃烘干即可以得到钽酸钠产物;
所述的稀酸溶液为稀硝酸、稀盐酸或者稀硫酸溶液。
2.如权利要求1所述的钽酸钠的制备方法,其特征为保护气氛为氮气、氩气或两者的混合气体。
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