CN109607477A - 一种La-Cu-Mn系储氧-释氧材料及其制备方法与应用 - Google Patents
一种La-Cu-Mn系储氧-释氧材料及其制备方法与应用 Download PDFInfo
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- QRSFFHRCBYCWBS-UHFFFAOYSA-N [O].[O] Chemical compound [O].[O] QRSFFHRCBYCWBS-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910017566 Cu-Mn Inorganic materials 0.000 title claims abstract description 38
- 229910017871 Cu—Mn Inorganic materials 0.000 title claims abstract description 38
- 238000003860 storage Methods 0.000 title claims abstract description 20
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- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 23
- 238000001354 calcination Methods 0.000 claims description 16
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 10
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- 239000010949 copper Substances 0.000 description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 9
- XQBXQQNSKADUDV-UHFFFAOYSA-N lanthanum;nitric acid Chemical compound [La].O[N+]([O-])=O XQBXQQNSKADUDV-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002328 LaMnO3 Inorganic materials 0.000 description 3
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- 238000003786 synthesis reaction Methods 0.000 description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 1
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Abstract
本发明公开一种La‑Cu‑Mn系储氧‑释氧材料及其制备方法与应用,属于材料技术领域;本发明La‑Cu‑Mn系储氧‑释氧材料化学通式为LaxCu1‑xMnO3‑δ,其中,0.1≤x≤0.95,0<δ<3;采用溶胶‑凝胶法制备La‑Cu‑Mn系储氧‑释氧材料。本发明的La‑Cu‑Mn系储氧‑释氧材料在化学链重整制氢反应中具有高反应活性和热稳定性,具有较高的产氢率、较好的抗积碳性能和高的CH4转化率。
Description
技术领域
本发明涉及一种La-Cu-Mn系储氧-释氧材料及其制备方法与应用,属于材料技术领域。
背景技术
氢是一种理想的洁净可再生能源,它具有高能量密度和零排放的优点。 地球上3/4的表面被海洋覆盖,资源丰富,是天然的氢矿。此外,氢在各行各业都得到了广泛应用,包括原油精炼、化学品生产、航空航天、金属冶炼、食品加工等。因此,氢是理想的燃料和能源载体。目前,已有多种技术被提出并应用于生产氢气,包括传统的水电解,蒸汽甲烷重整和化学链蒸汽重整。化学链蒸汽重整是洁净、高效的新一代制氢技术。
化学链蒸汽重整耦合了晶格氧部分氧化制合成气与分解水制氢的技术优势,反应过程分为两个部分。第一部分是用甲烷还原氧载体,获得H2/CO摩尔比为2.0的合成气;第二部分是以水蒸气为氧源对氧载体进行再生进而得到纯氢气。化学链蒸汽重整的一个关键挑战是选择具有合适性能的氧载体:更高的CH4转化率、H2产率、热稳定性和抗积碳性能。LaMnO3氧载体在化学链蒸汽重整过程中具有较高的产氢率和较好的抗积碳性能,但CH4转化率和热稳定性较差。
发明内容
针对现有技术存在的问题,本发明提供一种La-Cu-Mn系储氧-释氧材料及其制备方法与应用,本发明La-Cu-Mn系储氧-释氧材料在化学链重整制氢反应中具有高反应活性和热稳定性。
一种La-Cu-Mn系储氧-释氧材料,化学通式为LaxCu1-xMnO3-δ,其中,0.1≤x≤0.95,0<δ<3。
La-Cu-Mn系储氧-释氧材料的制备方法,包括以下步骤:
(1)将硝酸镧、硝酸铜、硝酸锰和柠檬酸加入到去离子水中得到混合溶液A;
(2)将步骤(1)所得混合溶液A温度为30~100℃条件下搅拌1~10h得到溶胶B;
(3)将步骤(2)得到的溶胶B置于温度为60~200℃条件下恒温处理8~36h得到凝胶C;
(4)将凝胶C置于温度为200~600℃条件下进行一次高温恒温煅烧1~3.5h,再置于温度为700~1000℃条件下进行二次高温恒温煅烧1.5~4h得到La-Cu-Mn系储氧-释氧材料;
所述步骤(1)中硝酸镧、硝酸铜、硝酸锰和柠檬酸的摩尔比为x:(1-x):1:(0.1~10),0.1≤x≤0.95,混合溶液A中硝酸锰的浓度为0.1~2mol/L;
La-Cu-Mn系储氧-释氧材料作为化学链重整制氢反应的氧载体。
本发明的有益效果:
(1)本发明制备出了La-Cu-Mn系储氧-释氧材料在化学链重整制氢反应中具有高反应活性和热稳定性,具有较高的产氢率和较好的抗积碳性能和高的CH4转化率;
(2)本发明将Cu负载于LaMnO3载体上,获得了高反应活性和热稳定性的化学链重整制氢氧载体,并证实了Cu与LaMnO3载体在甲烷活化、氧离子扩散、抗积碳和水分子解离等方面存在协同作用。
具体实施方式
下面结合实施例对本发明作进一步详细说明,但本发明保护范围不局限于所述内容。
实施例1:本实施例La-Cu-Mn系储氧-释氧材料为La0.8Cu0.2MnO3-δ,其中0<δ<3;
La-Cu-Mn系储氧-释氧材料的制备方法,包括以下步骤:
(1)将硝酸镧、硝酸铜、硝酸锰和柠檬酸加入到去离子水中得到混合溶液A;其中硝酸镧、硝酸铜、硝酸锰和柠檬酸的摩尔比为0.8:0.2:1:0.1,混合溶液A中硝酸锰的浓度为0.1mol/L;
(2)将步骤(1)所得混合溶液A温度为30℃条件下搅拌10h得到溶胶B;
(3)将步骤(2)得到的溶胶B置于温度为60℃条件下恒温处理36h得到凝胶C;
(4)将凝胶C置于温度为200℃条件下进行一次高温恒温煅烧3.5h,再置于温度为700℃条件下进行二次高温恒温煅烧4h得到La-Cu-Mn系储氧-释氧材料La0.8Cu0.2MnO3-δ。
实施例2:本实施例La-Cu-Mn系储氧-释氧材料为La0.3Cu0.7MnO3-δ,其中0<δ<3;
La-Cu-Mn系储氧-释氧材料的制备方法,包括以下步骤:
(1)将硝酸镧、硝酸铜、硝酸锰和柠檬酸加入到去离子水中得到混合溶液A;其中硝酸镧、硝酸铜、硝酸锰和柠檬酸的摩尔比为0.3:0.7:1:10,混合溶液A中硝酸锰的浓度为2mol/L;
(2)将步骤(1)所得混合溶液A温度为100℃条件下搅拌1h得到溶胶B;
(3)将步骤(2)得到的溶胶B置于温度为200℃条件下恒温处理8h得到凝胶C;
(4)将凝胶C置于温度为600℃条件下进行一次高温恒温煅烧1h,再置于温度为1000℃条件下进行二次高温恒温煅烧1.5h得到La-Cu-Mn系储氧-释氧材料La0.3Cu0.7MnO3-δ。
实施例3:本实施例La-Cu-Mn系储氧-释氧材料为La0.7Cu0.3MnO3-δ,其中0<δ<3;
La-Cu-Mn系储氧-释氧材料的制备方法,包括以下步骤:
(1)将硝酸镧、硝酸铜、硝酸锰和柠檬酸加入到去离子水中得到混合溶液A;其中硝酸镧、硝酸铜、硝酸锰和柠檬酸的摩尔比为0.7:0.3:1:8,混合溶液A中硝酸锰的浓度为1.6mol/L;
(2)将步骤(1)所得混合溶液A温度为85℃条件下搅拌2h得到溶胶B;
(3)将步骤(2)得到的溶胶B置于温度为180℃条件下恒温处理12h得到凝胶C;
(4)将凝胶C置于温度为500℃条件下进行一次高温恒温煅烧1.5h,再置于温度为950℃条件下进行二次高温恒温煅烧2h得到La-Cu-Mn系储氧-释氧材料La0.7Cu0.3MnO3-δ。
实施例4:本实施例La-Cu-Mn系储氧-释氧材料为La0.6Cu0.4MnO3-δ,其中0<δ<3;
La-Cu-Mn系储氧-释氧材料的制备方法,包括以下步骤:
(1)将硝酸镧、硝酸铜、硝酸锰和柠檬酸加入到去离子水中得到混合溶液A;其中硝酸镧、硝酸铜、硝酸锰和柠檬酸的摩尔比为0.6:0.4:1:6,混合溶液A中硝酸锰的浓度为1.2mol/L;
(2)将步骤(1)所得混合溶液A温度为70℃条件下搅拌4h得到溶胶B;
(3)将步骤(2)得到的溶胶B置于温度为150℃条件下恒温处理18h得到凝胶C;
(4)将凝胶C置于温度为400℃条件下进行一次高温恒温煅烧2h,再置于温度为900℃条件下进行二次高温恒温煅烧2.5h得到La-Cu-Mn系储氧-释氧材料La0.6Cu0.4MnO3-δ。
实施例5:本实施例La-Cu-Mn系储氧-释氧材料为La0.5Cu0.5MnO3-δ,其中0<δ<3;
La-Cu-Mn系储氧-释氧材料的制备方法,包括以下步骤:
(1)将硝酸镧、硝酸铜、硝酸锰和柠檬酸加入到去离子水中得到混合溶液A;其中硝酸镧、硝酸铜、硝酸锰和柠檬酸的摩尔比为0.5:0.5:1:4,混合溶液A中硝酸锰的浓度为0.8mol/L;
(2)将步骤(1)所得混合溶液A温度为55℃条件下搅拌6h得到溶胶B;
(3)将步骤(2)得到的溶胶B置于温度为120℃条件下恒温处理24h得到凝胶C;
(4)将凝胶C置于温度为350℃条件下进行一次高温恒温煅烧2.5h,再置于温度为850℃条件下进行二次高温恒温煅烧3h得到La-Cu-Mn系储氧-释氧材料La0.5Cu0.5MnO3-δ。
实施例6:本实施例La-Cu-Mn系储氧-释氧材料为La0.4Cu0.6MnO3-δ,其中0<δ<3;
La-Cu-Mn系储氧-释氧材料的制备方法,包括以下步骤:
(1)将硝酸镧、硝酸铜、硝酸锰和柠檬酸加入到去离子水中得到混合溶液A;其中硝酸镧、硝酸铜、硝酸锰和柠檬酸的摩尔比为0.4:0.6:1:2,混合溶液A中硝酸锰的浓度为0.4mol/L;
(2)将步骤(1)所得混合溶液A温度为40℃条件下搅拌8h得到溶胶B;
(3)将步骤(2)得到的溶胶B置于温度为80℃条件下恒温处理30h得到凝胶C;
(4)将凝胶C置于温度为300℃条件下进行一次高温恒温煅烧3h,再置于温度为750℃条件下进行二次高温恒温煅烧3.5h得到La-Cu-Mn系储氧-释氧材料La0.4Cu0.6MnO3-δ。
对比例:
采用溶胶-凝胶法制备LaMnO3储氧-释氧材料。
实施例7:实施例1~6的LaxCu1-xMnO3-δ(x=0.1~0.95)储氧-释氧材料和对比例的LaMnO3经压片过筛后,制得粒度为20~40目的粉体,在红外烟气分析仪上进行活性评价。分别取1.8g实施例1~6的LaxCu1-xMnO3-δ(x=0.1~0.95)储氧-释氧材料和对比例的LaMnO3造粒后的样品装入石英管中部,将石英管中部放置于反应器中部。实验时,通入N2排空反应系统中的空气,将反应器匀速升温至温度为830℃,在温度为830℃下通入5%CH4/N2混合气反应30min,储氧-释氧材料释放氧,CH4从中得到氧后产生合成气(CO和H2),再在温度为830℃下通入水蒸气,储氧-释氧材料从水蒸气中获得氧后产生纯氢气,红外烟气分析仪的检测系统在线检测每个反应阶段各种气体的含量;性能评价结果见表1:
表1
氢气产率是以储氧-释氧材料的总质量为基础进行计算的(水蒸气过量),即每千克储氧-释氧材料还原水蒸气可以生成氢气的物质的量;
积碳率是计算有多少甲烷裂解积碳;
甲烷转化率、氢气产率和积碳率是反应30min的平均值。
Claims (4)
1.一种La-Cu-Mn系储氧-释氧材料,其特征在于:该La-Cu-Mn系储氧-释氧材料化学通式为LaxCu1-xMnO3-δ,其中,0.1≤x≤0.95,0<δ<3。
2.权利要求1所述的La-Cu-Mn系储氧-释氧材料的制备方法,其特征在于,包括以下步骤:
(1)将硝酸镧、硝酸铜、硝酸锰和柠檬酸加入到去离子水中得到混合溶液A;
(2)将步骤(1)所得混合溶液A温度为30~100℃条件下搅拌1~10h得到溶胶B;
(3)将步骤(2)得到的溶胶B置于温度为60~200℃条件下恒温处理8~36h得到凝胶C;
(4)将凝胶C置于温度为200~600℃条件下进行一次高温恒温煅烧1~3.5h,再置于温度为700~1000℃条件下进行二次高温恒温煅烧1.5~4h得到La-Cu-Mn系储氧-释氧材料。
3.根据权利要求2所述的La-Cu-Mn系储氧-释氧材料的制备方法,其特征在于:步骤(1)中硝酸镧、硝酸铜、硝酸锰和柠檬酸的摩尔比为x:(1-x):1:(0.1~10),0.1≤x≤0.95;混合溶液A中硝酸锰的浓度为0.1~2mol/L。
4.权利要求1所述La-Cu-Mn系储氧-释氧材料作为化学链重整制氢反应的氧载体。
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