CN104741068B

CN104741068B - Bagasse synthesis perovskite LaCoO3The method of composite oxide material

Info

Publication number: CN104741068B
Application number: CN201510180887.1A
Authority: CN
Inventors: 贾立山; 罗明萍; 凌枫; 潘欣伟
Original assignee: Xiamen University
Current assignee: Xiamen University
Priority date: 2015-04-16
Filing date: 2015-04-16
Publication date: 2017-06-23
Anticipated expiration: 2035-04-16
Also published as: CN104741068A

Abstract

Bagasse synthesis perovskite LaCoO₃The method of composite oxide material, is related to a kind of perovskite Composite Oxides Materials.1) by lanthanum nitrate and cobalt nitrate formation mixed solution soluble in water, bagasse is added, xerogel is obtained after drying；2) by step 1) xerogel that obtains ignites, and obtains the precursor powder of black, and after predecomposition in Muffle furnace, calcining obtains perovskite LaCoO₃Composite oxide material.Using bagasse directly with slaine complex-combustion, prepare perovskite structure LaCoO₃Composite metal oxide material, process is simple, low cost is a kind of new method that renewable biomass prepares calcium-titanium ore type nano material.

Description

Bagasse synthesis perovskite LaCoO3The method of composite oxide material

Technical field

The present invention relates to a kind of perovskite Composite Oxides Materials, perovskite is synthesized more particularly, to a kind of bagasse LaCoO₃The method of composite oxide material.

Background technology

Biomass increasingly show importance, in recent years as a kind of reproducible resource in terms of green chemical synthesis Come, biomass also show the advantage of uniqueness in terms of green syt nano material.The biology extracted from plant and microorganism Matter contains abundant active function groups can occur reduction with metal ion.Succeeded synthesizing nano-silver, nm of gold, core The nano material of shell structure.Zheng Nan etc. is using the synthesizing porous aluminum oxide of biomass cape jasmine (ZL201110399340.2).Have recently Report using straw straw prepare silicon dioxide hybrid materials (Bioresource Technology 101 (2010) 8402- 8405).Perovskite composite oxide LaCoO₃With excellent magnetic electricity performance, it is widely used in fuel cell, sensor And the association area such as heterogeneous catalysis.Conventional preparation method mainly has combustion method, solid phase method, citric acid complex method, collosol and gel Method, hydro-thermal method, template etc..These methods preparation technology is complicated, relatively costly.

The content of the invention

It is an object of the invention to provide a kind of bagasse synthesis perovskite LaCoO₃The method of composite oxide material.

The present invention is comprised the following steps：

1) by lanthanum nitrate and cobalt nitrate formation mixed solution soluble in water, bagasse is added, xerogel is obtained after drying；

2) by step 1) xerogel that obtains ignites, and obtains the precursor powder of black, after predecomposition in Muffle furnace, forge Burn, that is, obtain perovskite LaCoO₃Composite oxide material.

In step 1) in, the lanthanum nitrate can be 1: 1 with the mol ratio of cobalt nitrate, and the water can use deionized water；Institute The consumption for stating bagasse can be by mass percentage the 10%~40% of mixed solution；The dry temperature can be 80~100 DEG C, the dry time can be 12~24h；The bagasse can be using the bagasse discarded after squeezing the juice through washing, and 105 DEG C of baking ovens are done Dry to be crushed with pulverizer to after constant weight, it is the bagasse of 60~100 mesh to sieve.

In step 2) in, described igniting can be ignited using electric furnace；The temperature of the predecomposition can be 400 DEG C, predecomposition Time can be 2h；The temperature of the calcining can be 600~800 DEG C, and the time of calcining can be 4h.

Prepared perovskite LaCoO₃The specific surface area test of composite oxide material is as follows：Nano-perovskite material Specific surface area is tested and completed on the type Full-automatic physical chemical adsorption instruments of Micromeritics TriStar 3000.With High Purity Nitrogen It is adsorbate, is adsorbed in liquid nitrogen temperature (77K).Sample vacuumize process 5h at 150 DEG C before test, catalyst amount is about It is 0.1g.Specific surface area test uses multilayer physical adsorption process, i.e. BET equations.

The present invention using bagasse directly with slaine complex-combustion, prepare perovskite structure LaCoO₃Composition metal oxygen Compound material, process is simple, low cost is a kind of new method that renewable biomass prepares calcium-titanium ore type nano material.

Brief description of the drawings

Fig. 1 is LaCoO prepared by embodiment 1₃XRD.In Fig. 1, mark ◆ be LaCoO₃。

Fig. 2 is LaCoO prepared by embodiment 1₃Nano material scanning electron microscope sem figure.

Specific embodiment

Embodiment 1

LaCoO₃Prepare：By lanthanum nitrate: cobalt nitrate mol ratio is 1: 1.The metal nitrate for taking 0.04mol respectively is dissolved in 0.1L deionized waters, add relative to LaCoO₃Mass percent be 10% 60 mesh bagasse.Stir, in 80 DEG C 24h is dried, with heating by electric cooker to burning, the precursor powder for obtaining further is decomposed by 400 DEG C of roasting 2h, then through 800 DEG C Roasting 4h obtains nano-perovskite material LaCoO₃。

Specific surface area test is carried out on the type Full-automatic physical chemical adsorption instruments of Micromeritics TriStar 3000. With High Purity Nitrogen as adsorbate, adsorbed in liquid nitrogen temperature (77K).About 0.1g samples are weighed, compressing tablet tests preceding sample 150 Vacuumize process 5h at DEG C.Specific surface area is 6.97m²/g。

Embodiment 2

LaCoO₃Prepare：By lanthanum nitrate: cobalt nitrate mol ratio is 1: 1.The metal nitrate for taking 0.04mol respectively is dissolved in 0.1L deionized waters, add relative to LaCoO₃Mass percent be 15% 80 mesh bagasse.Stir, in 100 DEG C 12h is dried, with heating by electric cooker to burning, the precursor powder for obtaining further is decomposed by 400 DEG C of roasting 2h, then through 700 DEG C roasting 4h, obtain nano-perovskite material LaCoO₃, its specific surface area is 6.72m²/g。

Embodiment 3

LaCoO₃Prepare：By lanthanum nitrate: cobalt nitrate mol ratio is 1: 1.The metal nitrate for taking 0.04mol respectively is dissolved in 0.1L deionized waters, add relative to LaCoO₃Mass percent be 10% 100 mesh bagasse.Stir, in 90 DEG C 16h is dried, with heating by electric cooker to burning, the precursor powder for obtaining further is decomposed by 400 DEG C of roasting 2h, then through 600 DEG C roasting 4h, obtain nano-perovskite material LaCoO₃, its specific surface area is 11.72m²/g。

Embodiment 4

LaCoO₃Prepare：By lanthanum nitrate: cobalt nitrate mol ratio is 1: 1.The metal nitrate for taking 0.04mol respectively is dissolved in 0.1L deionized waters, add relative to LaCoO₃Mass percent be 20% 100 mesh bagasse.Stir, in 85 DEG C 18h is dried, with heating by electric cooker to burning, the precursor powder for obtaining further is decomposed by 400 DEG C of roasting 2h, then through 700 DEG C roasting 4h, the nano-perovskite material LaCoO for obtaining₃, its specific surface area is 8.00m²/g。

Embodiment 5

LaCoO₃Prepare：By lanthanum nitrate: cobalt nitrate mol ratio is 1: 1.The metal nitrate for taking 0.04mol respectively is dissolved in 0.1L deionized waters, add relative to LaCoO₃Mass percent be 30% 80 mesh bagasse.Stir, in 80 DEG C 20h is dried, with heating by electric cooker to burning, the precursor powder for obtaining further is decomposed by 400 DEG C of roasting 2h, then through 700 DEG C Roasting 4h, obtains nano-perovskite material LaCoO₃, its specific surface area is 9.65m²/g。

Embodiment 6

LaCoO₃Prepare：By lanthanum nitrate: cobalt nitrate mol ratio is 1: 1.The metal nitrate for taking 0.04mol respectively is dissolved in 0.1L deionized waters, add relative to LaCoO₃Mass percent be 40% 60 mesh bagasse.Stir, in 95 DEG C 12h is dried, with heating by electric cooker to burning, the precursor powder for obtaining further is decomposed by 400 DEG C of roasting 2h, then through 750 DEG C Roasting 4h, obtains nano-perovskite material LaCoO₃, its specific surface area is 8.11m²/g。

Claims

1. bagasse synthesizes perovskite LaCoO₃The method of composite oxide material, it is characterised in that comprise the following steps：

1) by lanthanum nitrate and cobalt nitrate formation mixed solution soluble in water, bagasse is added, xerogel is obtained after drying；The nitre Sour lanthanum is 1: 1 with the mol ratio of cobalt nitrate；The consumption of the bagasse is by mass percentage the 10%~40% of mixed solution；

The bagasse, through washing, is crushed after 105 DEG C of oven drying to constant weights using the bagasse discarded after squeezing the juice with pulverizer, It is the bagasse of 60~100 mesh to sieve；

2) by step 1) xerogel that obtains ignites, and obtains the precursor powder of black, after predecomposition in Muffle furnace, calcining, Obtain perovskite LaCoO₃Composite oxide material；

Described igniting is ignited using electric furnace；

The temperature of the calcining is 600~800 DEG C, and the time of calcining is 4h.

2. bagasse as claimed in claim 1 synthesizes perovskite LaCoO₃The method of composite oxide material, it is characterised in that in step It is rapid 1) in, the water uses deionized water.

3. bagasse as claimed in claim 1 synthesizes perovskite LaCoO₃The method of composite oxide material, it is characterised in that in step It is rapid 1) in, the dry temperature be 80~100 DEG C, the dry time be 12~24h.

4. bagasse as claimed in claim 1 synthesizes perovskite LaCoO₃The method of composite oxide material, it is characterised in that in step It is rapid 2) in, the temperature of the predecomposition is 400 DEG C, and the time of predecomposition is 2h.