CN114433068A - 一种a位阳离子调控性能的二元金属钒酸盐材料的制备及应用 - Google Patents
一种a位阳离子调控性能的二元金属钒酸盐材料的制备及应用 Download PDFInfo
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- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 30
- 239000002184 metal Substances 0.000 title claims abstract description 30
- 239000000463 material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 150000001768 cations Chemical class 0.000 title claims abstract description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 230000001699 photocatalysis Effects 0.000 claims abstract description 22
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 19
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 230000009467 reduction Effects 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 239000007790 solid phase Substances 0.000 claims abstract description 12
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
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- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- 238000001308 synthesis method Methods 0.000 claims abstract description 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims abstract description 3
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001429 cobalt ion Inorganic materials 0.000 claims abstract description 3
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 3
- 239000012535 impurity Substances 0.000 claims abstract description 3
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- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000012467 final product Substances 0.000 abstract description 3
- 239000004570 mortar (masonry) Substances 0.000 description 9
- 239000011941 photocatalyst Substances 0.000 description 8
- 229910005466 Ni2V2O7 Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910018039 Cu2V2O7 Inorganic materials 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910021276 Co2V2O7 Inorganic materials 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910007383 Zn2V2O7 Inorganic materials 0.000 description 3
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 150000004687 hexahydrates Chemical class 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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Abstract
一种A位阳离子调控性能的二元金属钒酸盐材料的制备方法,采用两步固相烧结的合成方法,1)所述二元金属钒酸盐指分子通式为A2V2O7,所述的A位金属离子为钴离子、镍离子、铜离子和锌离子;将含有偏钒酸铵和对应A位阳离子的化合物按照等摩尔比配制,研磨混合均匀。2)将步骤1)所得均匀混合物置于马弗炉中低温预处理120±20分钟,去除杂质。3)将步骤(2)所得混合物粉末再次研磨,再置于马弗炉高温反应120±20分钟,自然冷却至室温,得到所制备产物。最终所得产物应用于光催化二氧化碳还原。本发明的二元金属钒酸盐通过A位阳离子调控实现了不同的光催化性能,且具有制备方法简单,材料性能稳定的优点。
Description
技术领域
本发明涉及一种二元金属钒酸盐的制备方法和应用,并在光催化还原二氧化碳领域通过调控A位阳离子的元素种类改变性能。
背景技术
工业革命以来,化石能源的大量消耗不可避免地带来能源枯竭和二氧化碳的大量排放,对人类社会生活造成了不可避免的负面影响,能源危机和环境问题成为全球关注的热点。全球各国也纷纷实行能源结构转型,寻求新的可再生清洁能源,我国也于2020年9月首次提出了“碳达峰、碳中和”的战略目标,争取在2030跨年前达到二氧化碳排放量峰值,努力在2060年实现碳中和。在一系列的解决措施中,光催化技术因其独特的优势脱颖而出:它受自然界光合作用的启发,利用源源不断的太阳光能量将二氧化碳转化为具有附加价值的化学品,例如一氧化碳、甲烷、甲醇等,既能消耗二氧化碳,又能够将丰富的太阳能以化学能的形式储存起来。而这一过程,因为二氧化碳的的热力学稳定性和动力学惰性使转化极为困难,因此寻找一种合适光学催化剂能够提供足够的能量激发二氧化碳转化显得尤为重要。
钒酸盐因为其多变价态、良好的抗光腐蚀性成为光学催化剂的研究对象之一,在引入过渡金属元素后,由于3d轨道的杂化和调控在可见光范围内表现出良好的光吸收能力,同时对于催化剂的能带位置也产生了显著的影响,是值得研究的课题。
发明内容
本发明的目的在于,提供一种A位阳离子调控性能的二元金属钒酸盐材料的制备和应用。
为实现上述目的,本发明采用的技术方案是:采用两步固相烧结的合成方法,包括以下步骤:
(1)所述二元金属钒酸盐指分子通式为A2V2O7,所述的A位金属离子为钴离子、镍离子、铜离子和锌离子;将含有偏钒酸铵和对应A位阳离子的化合物按照等摩尔比配制,研磨混合均匀。
(2)将步骤(1)所得均匀混合物置于马弗炉中低温预处理120±20分钟,去除杂质。
(3)将步骤(2)所得混合物粉末再次研磨,再置于马弗炉高温反应120±20分钟,自然冷却至室温,得到所制备产物。
(4)将步骤(3)最终所得产物应用于光催化二氧化碳还原;
A位金属离子来自于对应的A位金属的硝酸盐。
低温预处理的温度为350℃并保温120分钟,以4~10℃/min的升温速率达到低温预处理的温度。
钒酸钴的反应温度为800±20℃,钒酸镍的反应温度为800±20℃,钒酸铜的反应温度为500±20℃,钒酸锌的反应温度为600±20℃,升温速率均为5℃/min。
所述的方法得到的二元金属钒酸盐材料在光催化还原二氧化碳领域的应用。
二元金属钒酸盐指Co2V2O7、Ni2V2O7、Cu2V2O7或Zn2V2O7;将步骤(3)最终所得产物作为催化剂应用于光催化二氧化碳还原领域。
本发明的二元金属钒酸盐通过A位阳离子调控实现了不同的光催化性能,且具有制备方法简单,材料性能稳定的优点。
本发明的有益效果:经过两步固相烧结的合成方法制备了一系列二元金属钒酸盐光催化材料,并通过A位阳离子的调控实现了不同的光催化还原二氧化碳的性能,具有制备方法简单,稳定、选择性高的优点,为过渡金属元素在能带调控方面提供了参照。
附图说明
图1为两步固相烧结法所制备的二元金属钒酸盐光催化材料Ni2V2O7的X射线衍射图谱;
图2为两步固相烧结法所制备的二元金属钒酸盐光催化材料Ni2V2O7的扫描电镜照片;
图3为两步固相烧结法所制备的二元金属钒酸盐光催化材料Ni2V2O7的高分辨透射电镜照片;
图4为两步固相烧结法所制备的二元金属钒酸盐光催化材料Ni2V2O7的光催化还原二氧化碳性能测试。
具体实施方式
下面结合附图及具体实施例对本发明做进一步的详细描述。将硝酸钴、硝酸镍、硝酸铜和硝酸锌分别与偏钒酸铵按照等摩尔比放置在研钵中研磨,混合均匀后在空气中进行预处理,在350℃保温120分钟,自然降温后将预处理过的混合物粉末再次研磨,置于马弗炉中以对应的结晶温度反应120分钟即得所需产物。
实施例1
两步固相烧结制备二元金属钒酸盐光催化剂Ni2V2O7步骤如下:称量等摩尔比的偏钒酸铵和六水合硝酸钴,在研钵中充分混合后,放入马弗炉,在空气氛围中以5℃/min的升温速率升温到350℃并保温120分钟进行预处理。预处理过后的混合物再次在研钵中研磨,在马弗炉中以5℃/min的升温速率升温到800℃并保温120分钟进行反应,岁炉冷却至室温后取出样品,得到二元金属钒酸盐光催化剂Ni2V2O7。光催化还原二氧化碳性能测试见图4。
光催化二氧化碳测试条件:在反应装置中充入高纯二氧化碳,注射适量去离子水,使整个反应装置保持在常压状态,使用300W氙灯作为光源模拟日光,在可见光波长范围(>430nm)照射下进行光催化测试,间隔固定时间使用色谱测定主要产物CO的产量
实施例2
步固相烧结制备二元金属钒酸盐光催化剂Co2V2O7步骤如下:称量等摩尔比的偏钒酸铵和六水合硝酸钴,在研钵中充分混合后,放入马弗炉,在空气氛围中以5℃/min的升温速率升温到350℃并保温120分钟进行预处理。预处理过后的混合物再次在研钵中研磨,在马弗炉中以5℃/min的升温速率升温到800℃并保温130分钟进行反应,岁炉冷却至室温后取出样品,得到二元金属钒酸盐光催化剂Co2V2O7。光催化还原二氧化碳性能测试效果类似实施例1;
实施例3
两步固相烧结制备二元金属钒酸盐光催化剂Cu2V2O7步骤如下:称量等摩尔比的偏钒酸铵和六水合硝酸钴,在研钵中充分混合后,放入马弗炉,在空气氛围中以5℃/min的升温速率升温到350℃并保温120分钟进行预处理。预处理过后的混合物再次在研钵中研磨,在马弗炉中以5℃/min的升温速率升温到500℃并保温110分钟进行反应,随炉冷却至室温后取出样品,得到二元金属钒酸盐光催化剂Cu2V2O7。光催化还原二氧化碳性能测试效果类似实施例1;
实施例4
两步固相烧结制备二元金属钒酸盐光催化剂Zn2V2O7步骤如下:称量等摩尔比的偏钒酸铵和六水合硝酸钴,在研钵中充分混合后,放入马弗炉,在空气氛围中以5℃/min的升温速率升温到350℃并保温120分钟进行预处理。预处理过后的混合物再次在研钵中研磨,在马弗炉中以5℃/min的升温速率升温到600℃并保温125分钟进行反应,随炉冷却至室温后取出样品,得到二元金属钒酸盐光催化剂Zn2V2O7。光催化还原二氧化碳性能测试效果类似实施例1。测试方法相同,产物相同,但是最终性能结果对比为:Ni2V2O7>Co2V2O7>Zn2V2O7>Cu2V2O7。
以上实例将有助于相关领域的技术工作人员进一步理解本发明,但不以任何形式限制本发明。同时,这里指出对本领域的普通技术人员来说,本发明中最优的数据只针对本发明,在不脱离本发明构思的前提下,合理地若干调整和改进,都属于本发明的保护范围。
Claims (5)
1.一种A位阳离子调控性能的二元金属钒酸盐材料的制备方法,其特征在于,采用两步固相烧结的合成方法,包括以下步骤:
(1)所述二元金属钒酸盐指分子通式为A2V2O7,所述的A位金属离子为钴离子、镍离子、铜离子和锌离子;将含有偏钒酸铵和对应A位阳离子的化合物按照等摩尔比配制,研磨混合均匀;
(2)将步骤(1)所得均匀混合物置于马弗炉中低温预处理120±20分钟,去除杂质;
(3)将步骤(2)所得混合物粉末再次研磨,再置于马弗炉高温反应120±20分钟,自然冷却至室温,得到所制备产物。
2.根据权利要求1所述方法,其特征在于,A位金属离子来自于对应的A位金属的硝酸盐。
3.根据权利要求1所述方法,其特征在于,低温预处理的温度为350℃并保温120分钟,以4~10℃/min的升温速率达到低温预处理的温度。
4.根据权利要求1所述方法,其特征在于,钒酸钴的反应温度为800±20℃,钒酸镍的反应温度为800±20℃,钒酸铜的反应温度为500±20℃,钒酸锌的反应温度为600±20℃,升温速率均为5℃/min。
5.一种基于权利要求1-4任一所述的方法得到的二元金属钒酸盐材料在光催化还原二氧化碳领域的应用。
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