CN104741068B - Bagasse synthesis perovskite LaCoO3The method of composite oxide material - Google Patents
Bagasse synthesis perovskite LaCoO3The method of composite oxide material Download PDFInfo
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- 241000609240 Ambelania acida Species 0.000 title claims abstract description 26
- 239000010905 bagasse Substances 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 17
- 230000015572 biosynthetic process Effects 0.000 title claims description 3
- 238000003786 synthesis reaction Methods 0.000 title description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract 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 abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 229910002254 LaCoO3 Inorganic materials 0.000 claims description 6
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims 1
- 238000000643 oven drying Methods 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000002028 Biomass Substances 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 238000009841 combustion method Methods 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 240000000111 Saccharum officinarum Species 0.000 abstract 1
- 235000007201 Saccharum officinarum Nutrition 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 229910001960 metal nitrate Inorganic materials 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002156 adsorbate Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 240000001972 Gardenia jasminoides Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
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Abstract
甘蔗渣合成钙钛矿LaCoO3复合氧化物材料的方法，涉及一种钙钛矿型复合氧化物材料。1)将硝酸镧与硝酸钴溶于水中形成混合溶液，再加入甘蔗渣，干燥后得干凝胶；2)将步骤1)得到的干凝胶引燃，得到黑色的前驱体粉末，在马弗炉中预分解后，煅烧，即得到钙钛矿LaCoO3复合氧化物材料。采用甘蔗渣直接与金属盐络合燃烧法，制备钙钛矿结构LaCoO3复合金属氧化物材料，工艺简单，成本低，是一种可再生生物质制备钙钛矿型纳米材料的新方法。A method for synthesizing a perovskite LaCoO composite oxide material from sugarcane bagasse relates to a perovskite type composite oxide material. 1) dissolving lanthanum nitrate and cobalt nitrate in water to form a mixed solution, then adding bagasse, and drying to obtain xerogel; 2) igniting the xerogel obtained in step 1) to obtain black precursor powder, and After pre-decomposition in the furnace, calcining, the perovskite LaCoO 3 composite oxide material is obtained. The complex combustion method of bagasse directly with metal salts is used to prepare perovskite-structured LaCoO 3 composite metal oxide materials. The process is simple and the cost is low. It is a new method for preparing perovskite-type nanomaterials from renewable biomass.
Description
技术领域technical field
本发明涉及一种钙钛矿型复合氧化物材料，尤其是涉及一种甘蔗渣合成钙钛矿LaCoO3复合氧化物材料的方法。The invention relates to a perovskite type composite oxide material, in particular to a method for synthesizing perovskite LaCoO3 composite oxide material from bagasse.
背景技术Background technique
生物质作为一种可再生的资源，在绿色化学合成方面越来越显现出重要性，近年来，生物质在绿色合成纳米材料方面也表现出独特的优势。从植物和微生物中提取的生物质含有丰富的活性官能团可以与金属离子发生还原作用。已经成功合成纳米银、纳米金、核壳结构的纳米材料。郑楠等利用生物质栀子合成多孔氧化铝(ZL201110399340.2)。最近有报道利用稻草秸杆制备二氧化硅杂化材料(Bioresource Technology 101(2010)8402–8405)。钙钛矿型复合氧化物LaCoO3具有优异的磁电性能，被广泛应用于燃料电池、传感器及多相催化等相关领域。常规的制备方法主要有燃烧法、固相法、柠檬酸络合法、溶胶凝胶法、水热法、模板法等。这些方法制备工艺复杂，成本较高。As a renewable resource, biomass has become more and more important in green chemical synthesis. In recent years, biomass has also shown unique advantages in green synthesis of nanomaterials. Biomass extracted from plants and microorganisms is rich in active functional groups that can undergo reduction with metal ions. Nano-silver, nano-gold, and core-shell nanomaterials have been successfully synthesized. Zheng Nan et al. synthesized porous alumina using biomass gardenia (ZL201110399340.2). Recently, it has been reported to use rice straw to prepare silica hybrid materials (Bioresource Technology 101 (2010) 8402–8405). Perovskite composite oxide LaCoO 3 has excellent magnetoelectric properties and is widely used in related fields such as fuel cells, sensors, and heterogeneous catalysis. Conventional preparation methods mainly include combustion method, solid phase method, citric acid complexation method, sol-gel method, hydrothermal method, template method, etc. These methods have complicated preparation process and high cost.
发明内容Contents of the invention
本发明的目的在于提供一种甘蔗渣合成钙钛矿LaCoO3复合氧化物材料的方法。The object of the present invention is to provide a method for synthesizing perovskite LaCoO 3 composite oxide materials from bagasse.
本发明包括以下步骤：The present invention comprises the following steps:
1)将硝酸镧与硝酸钴溶于水中形成混合溶液，再加入甘蔗渣，干燥后得干凝胶；1) dissolving lanthanum nitrate and cobalt nitrate in water to form a mixed solution, then adding bagasse, and drying to obtain xerogel;
2)将步骤1)得到的干凝胶引燃，得到黑色的前驱体粉末，在马弗炉中预分解后，煅烧，即得到钙钛矿LaCoO3复合氧化物材料。2) Ignite the xerogel obtained in step 1) to obtain a black precursor powder, which is pre-decomposed in a muffle furnace and then calcined to obtain a perovskite LaCoO 3 composite oxide material.
在步骤1)中，所述硝酸镧与硝酸钴的摩尔比可为1∶1，所述水可采用去离子水；所述甘蔗渣的用量按质量百分比可为混合溶液的10％～40％；所述干燥的温度可为80～100℃，干燥的时间可为12～24h；所述甘蔗渣可采用榨汁后废弃的甘蔗渣经水洗，105℃烘箱干燥至恒重后用粉碎机粉碎，筛分为60～100目的甘蔗渣。In step 1), the molar ratio of the lanthanum nitrate and cobalt nitrate can be 1:1, and the water can be deionized water; the amount of the bagasse can be 10% to 40% of the mixed solution by mass percentage The drying temperature can be 80-100°C, and the drying time can be 12-24h; the bagasse can be washed with water after the juice is squeezed, dried in an oven at 105°C to constant weight, and crushed with a pulverizer , Screened into bagasse of 60-100 mesh.
在步骤2)中，所述引燃可采用电炉引燃；所述预分解的温度可为400℃，预分解的时间可为2h；所述煅烧的温度可为600～800℃，煅烧的时间可为4h。In step 2), the ignition can be ignited by an electric furnace; the pre-decomposition temperature can be 400°C, and the pre-decomposition time can be 2h; the calcination temperature can be 600-800°C, and the calcination time It can be 4h.
所制备的钙钛矿LaCoO3复合氧化物材料的比表面积测试如下：纳米钙钛矿材料的比表面积测试在Micromeritics TriStar 3000型全自动物理化学吸附仪上完成。以高纯氮为吸附质，于液氮温度(77K)进行吸附。测试前样品在150℃下抽真空处理5h，催化剂用量约为0.1g。比表面积测试采用的是多层物理吸附方法，即BET方程。The specific surface area test of the prepared perovskite LaCoO 3 composite oxide material is as follows: The specific surface area test of the nano perovskite material is completed on a Micromeritics TriStar 3000 automatic physical and chemical adsorption instrument. Using high-purity nitrogen as the adsorbate, the adsorption is carried out at liquid nitrogen temperature (77K). Before the test, the sample was vacuum treated at 150°C for 5 hours, and the catalyst dosage was about 0.1 g. The specific surface area test uses a multi-layer physical adsorption method, namely the BET equation.
本发明采用甘蔗渣直接与金属盐络合燃烧法，制备钙钛矿结构LaCoO3复合金属氧化物材料，工艺简单，成本低，是一种可再生生物质制备钙钛矿型纳米材料的新方法。The present invention adopts bagasse directly and metal salt complex combustion method to prepare perovskite structure LaCoO 3 composite metal oxide material, the process is simple, the cost is low, and it is a new method for preparing perovskite nanomaterials from renewable biomass .
附图说明Description of drawings
图1为实施例1制备的LaCoO3XRD图。在图1中，标记◆为LaCoO3。FIG. 1 is the XRD pattern of LaCoO 3 prepared in Example 1. In FIG. 1 , the mark ◆ is LaCoO 3 .
图2为实施例1制备的LaCoO3纳米材料扫描电镜SEM图。FIG. 2 is a scanning electron microscope SEM image of the LaCoO 3 nanomaterial prepared in Example 1.
具体实施方式detailed description
实施例1Example 1
LaCoO3制备：按硝酸镧∶硝酸钴摩尔比为1∶1。分别取0.04mol的金属硝酸盐溶于0.1L去离子水，加入相对于LaCoO3的质量百分比为10％的60目的甘蔗渣。搅拌均匀，于80℃干燥24h，用电炉加热到燃烧，得到的前驱体粉末，经过400℃焙烧2h进一步分解，再经800℃焙烧4h得到纳米钙钛矿材料LaCoO3。LaCoO 3 preparation: according to the molar ratio of lanthanum nitrate: cobalt nitrate is 1:1. 0.04 mol of metal nitrate was dissolved in 0.1 L of deionized water, and 60-mesh bagasse with a mass percentage of 10% relative to LaCoO 3 was added. Stir evenly, dry at 80°C for 24 hours, and heat to burn in an electric furnace. The obtained precursor powder is further decomposed after roasting at 400°C for 2 hours, and then roasted at 800°C for 4 hours to obtain the nano perovskite material LaCoO 3 .
比表面积测试在Micromeritics TriStar 3000型全自动物理化学吸附仪上进行。以高纯氮为吸附质，于液氮温度(77K)进行吸附。称量约0.1g样品，压片，测试前样品在150℃下抽真空处理5h。比表面积为6.97m2/g。The specific surface area test was carried out on a Micromeritics TriStar 3000 automatic physical and chemical adsorption instrument. Using high-purity nitrogen as the adsorbate, the adsorption is carried out at liquid nitrogen temperature (77K). Weigh about 0.1 g of the sample, press it into tablets, and vacuumize the sample at 150°C for 5 hours before testing. The specific surface area is 6.97m 2 /g.
实施例2Example 2
LaCoO3制备：按硝酸镧∶硝酸钴摩尔比为1∶1。分别取0.04mol的金属硝酸盐溶于0.1L去离子水，加入相对于LaCoO3的质量百分比为15％的80目的甘蔗渣。搅拌均匀，于100℃干燥12h，用电炉加热到燃烧，得到的前驱体粉末，经过400℃焙烧2h进一步分解，再经700℃焙烧4h，得到纳米钙钛矿材料LaCoO3，其比表面积为6.72m2/g。LaCoO 3 preparation: according to the molar ratio of lanthanum nitrate: cobalt nitrate is 1:1. 0.04 mol of metal nitrate was dissolved in 0.1 L of deionized water, and 80-mesh bagasse with a mass percentage of 15% relative to LaCoO 3 was added. Stir evenly, dry at 100°C for 12 hours, and heat to burn in an electric furnace. The obtained precursor powder is further decomposed after roasting at 400°C for 2 hours, and then roasted at 700°C for 4 hours to obtain the nano-perovskite material LaCoO 3 , which has a specific surface area of 6.72 m 2 /g.
实施例3Example 3
LaCoO3制备：按硝酸镧∶硝酸钴摩尔比为1∶1。分别取0.04mol的金属硝酸盐溶于0.1L去离子水，加入相对于LaCoO3的质量百分比为10％的100目的甘蔗渣。搅拌均匀，于90℃干燥16h，用电炉加热到燃烧，得到的前驱体粉末，经过400℃焙烧2h进一步分解，再经600℃焙烧4h，得到纳米钙钛矿材料LaCoO3，其比表面积为11.72m2/g。LaCoO 3 preparation: according to the molar ratio of lanthanum nitrate: cobalt nitrate is 1:1. 0.04 mol of metal nitrate was dissolved in 0.1 L of deionized water, and 100-mesh bagasse was added with a mass percentage of 10% relative to LaCoO 3 . Stir evenly, dry at 90°C for 16 hours, and heat to burn in an electric furnace. The obtained precursor powder is further decomposed after roasting at 400°C for 2 hours, and then roasted at 600°C for 4 hours to obtain the nano-perovskite material LaCoO 3 , which has a specific surface area of 11.72 m 2 /g.
实施例4Example 4
LaCoO3制备：按硝酸镧∶硝酸钴摩尔比为1∶1。分别取0.04mol的金属硝酸盐溶于0.1L去离子水，加入相对于LaCoO3的质量百分比为20％的100目的甘蔗渣。搅拌均匀，于85℃干燥18h，用电炉加热到燃烧，得到的前驱体粉末，经过400℃焙烧2h进一步分解，再经700℃焙烧4h，得到的纳米钙钛矿材料LaCoO3，其比表面积为8.00m2/g。LaCoO 3 preparation: according to the molar ratio of lanthanum nitrate: cobalt nitrate is 1:1. 0.04 mol of metal nitrate was dissolved in 0.1 L of deionized water, and 100-mesh bagasse with a mass percentage of 20% relative to LaCoO 3 was added. Stir evenly, dry at 85°C for 18 hours, and heat to burn in an electric furnace. The obtained precursor powder is further decomposed after roasting at 400°C for 2 hours, and then roasted at 700°C for 4 hours. The obtained nano-perovskite material LaCoO 3 has a specific surface area of 8.00 m 2 /g.
实施例5Example 5
LaCoO3制备：按硝酸镧∶硝酸钴摩尔比为1∶1。分别取0.04mol的金属硝酸盐溶于0.1L去离子水，加入相对于LaCoO3的质量百分比为30％的80目的甘蔗渣。搅拌均匀，于80℃干燥20h，用电炉加热到燃烧，得到的前驱体粉末，经过400℃焙烧2h进一步分解，再经700℃焙烧4h，得到纳米钙钛矿材料LaCoO3，其比表面积为9.65m2/g。LaCoO 3 preparation: according to the molar ratio of lanthanum nitrate: cobalt nitrate is 1:1. 0.04 mol of metal nitrate was dissolved in 0.1 L of deionized water, and 80-mesh bagasse with a mass percentage of 30% relative to LaCoO 3 was added. Stir evenly, dry at 80°C for 20 hours, and heat it to burn in an electric furnace. The obtained precursor powder is further decomposed after roasting at 400°C for 2 hours, and then roasted at 700°C for 4 hours to obtain the nano-perovskite material LaCoO 3 with a specific surface area of 9.65 m 2 /g.
实施例6Example 6
LaCoO3制备：按硝酸镧∶硝酸钴摩尔比为1∶1。分别取0.04mol的金属硝酸盐溶于0.1L去离子水，加入相对于LaCoO3的质量百分比为40％的60目的甘蔗渣。搅拌均匀，于95℃干燥12h，用电炉加热到燃烧，得到的前驱体粉末，经过400℃焙烧2h进一步分解，再经750℃焙烧4h，得到纳米钙钛矿材料LaCoO3，其比表面积为8.11m2/g。LaCoO 3 preparation: according to the molar ratio of lanthanum nitrate: cobalt nitrate is 1:1. 0.04 mol of metal nitrate was dissolved in 0.1 L of deionized water, and 60-mesh bagasse with a mass percentage of 40% relative to LaCoO 3 was added. Stir evenly, dry at 95°C for 12 hours, and heat to burn in an electric furnace. The obtained precursor powder is further decomposed after roasting at 400°C for 2 hours, and then roasted at 750°C for 4 hours to obtain the nano-perovskite material LaCoO 3 , which has a specific surface area of 8.11 m 2 /g.
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