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Microwave hydrothermal preparation method for combination of collosol and gelatin of lanthanum cuprate nanocrystalline

A microwave hydrothermal and nanocrystalline technology, applied in copper compounds, nanotechnology, chemical instruments and methods, etc., can solve the problems of easy sintering, long reaction period, poor safety performance, etc., and achieve short preparation period and complete morphology. , good crystallization effect

Active Publication Date: 2013-10-09
山东格新精工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, these methods have their own shortcomings. For example, in order to obtain a high-purity target product in the solid-state reaction method, the reactant powder should be fine enough, and it needs to be roasted at high temperature for a long time and repeatedly ground, which is time-consuming. , and there are more impurity phases in the product; for the self-propagating combustion method, the combustion reaction is very violent, the combustion temperature is high, the reaction process is fast, it is not easy to control, the product is easy to sinter, and there is a high possibility of non-equilibrium phase in the product or metastable phase; for the hydrothermal method, the safety performance is poor and the reaction cycle is long

Method used

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  • Microwave hydrothermal preparation method for combination of collosol and gelatin of lanthanum cuprate nanocrystalline
  • Microwave hydrothermal preparation method for combination of collosol and gelatin of lanthanum cuprate nanocrystalline

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Effect test

Embodiment 1

[0017] 1) Analytical pure La(NO 3 ) 3 ·6H 2 O and Cu(NO 3 ) 3 ·3H 2 O was dissolved in deionized water, and the total metal ion concentration was prepared as solution A of 0.9mol / L;

[0018] 2) According to the molar ratio of the sum of citric acid and metal ions being 1.5:1, add citric acid to solution A, adjust pH=1.8 with urea and stir to form blue transparent sol B;

[0019] 3) Then use a sprayer to spray sol B into liquid nitrogen for freeze-drying. After the frozen material is separated from liquid nitrogen, put it into a sublimation drying device for drying treatment to obtain precursor C;

[0020] 4) Precursor C is ground and placed in a muffle furnace, heated from room temperature to 550 °C at a heating rate of 5 °C / min, kept for 2 hours, cooled to room temperature with the furnace, and ground into powder with a mortar to obtain La 2 CuO 4 Nanocrystalline.

[0021] Depend on figure 1 It can be seen that the product is a single-phase La 2 CuO 4 ,Depend on ...

Embodiment 2

[0023] 1) Analytical pure La(NO 3 ) 3 ·6H 2 O and Cu(NO 3 ) 3 ·3H 2 O is dissolved in deionized water, and the total metal ion concentration is prepared as solution A of 0.3mol / L;

[0024] 2) Add citric acid to solution A at a molar ratio of 0.8:1 to the sum of citric acid and metal ions, then adjust pH=2.0 with urea and stir to form a blue transparent sol B;

[0025] 3) Then spray sol B into liquid nitrogen with a sprayer, freeze-dry, adjust pH=2.8 with urea after cooling citric acid and stir to form blue transparent sol B;

[0026] 3) Then use a sprayer to spray sol B into liquid nitrogen for freeze-drying. After the frozen material is separated from liquid nitrogen, put it into a sublimation drying device for drying treatment to obtain precursor C;

[0027] 4) Precursor C is ground and placed in a muffle furnace, heated from room temperature to 700 °C at a heating rate of 8 °C / min, kept for 0.5 h, cooled to room temperature with the furnace, and ground into powder wit...

Embodiment 5

[0029] 1) Analytical pure La(NO 3 ) 3 ·6H 2 O and Cu(NO 3 ) 3 ·3H 2 O was dissolved in deionized water, and the total metal ion concentration was prepared into a solution A of 2.0mol / L;

[0030] 2) According to the molar ratio of the sum of citric acid and metal ions being 1.8:1, add citric acid to solution A, adjust pH=2.6 with urea and stir to form blue transparent sol B;

[0031] 3) Then use a sprayer to spray sol B into liquid nitrogen for freeze-drying. After the frozen material is separated from liquid nitrogen, put it into a sublimation drying device for drying treatment to obtain precursor C;

[0032] 4) Precursor C is ground and placed in a muffle furnace, heated from room temperature to 450 °C at a heating rate of 6 °C / min, kept for 3 hours, cooled to room temperature with the furnace, and ground into powder with a mortar to obtain La2 CuO 4 Nanocrystalline.

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Abstract

A microwave hydrothermal preparation method for the combination of collosol and gelatin of lanthanum cuprate nanocrystalline comprises the following steps: La (NO3) 3 6H2O and Cu(NO3) 3 3H2O are dissolved into deionized water to obtain a solution A; after citric acid is added into the solution A, the pH value is adjusted to be 1.4 to 2.8 by using urea, so as to obtain a collosol B; the collosol B is sprayed into liquid nitrogen through a sprayer so as to achieve freeze drying, and after being seperated from each other, frozen material and the liquid nitrogen are placed into a sublimation drying device for drying treatment to obtain a precursor C; and after being ground, the precursor C is placed into a muffle furnace for calcination and then ground into powder through a mortar, namely La2CuO4 nanocrystalline is obtained. In the invention, nanometer La2CuO4 powder is prepared through a vacuum freeze-drying method, since freeze drying is adopted for the preparation technology, the prepared La2CuO4 nanocrystalline is excellent, has a complete appearance, and is good in repeatability, the process is simple, the preparation period is shorter, and the La2CuO4 nanocrystalline is suitable for mass production.

Description

technical field [0001] The invention belongs to a catalyst preparation method, in particular to a sol-gel combined microwave hydrothermal preparation method of lanthanum cuprate nanocrystals. Background technique [0002] Because of its low carbon content, natural gas produces greenhouse gas CO when burned. 2 The amount is less, becoming a more ideal fuel. However, high temperature combustion of natural gas produces a large amount of NO X , discharged into the atmosphere will seriously pollute the environment. With the help of the catalyst, natural gas can be burned at a lower temperature, thereby avoiding the N in the air due to high temperature 2 Oxidation to NO X , to achieve high-efficiency combustion of natural gas and ultra-low emission processes. Therefore, catalytic oxidation is an environmentally friendly green technology with good application prospects. The traditional catalysts used for methane oxidation are supported noble metals. Although they have excellen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G3/00B82Y40/00
Inventor 黄剑锋李意峰孙莹曹丽云吴建鹏
Owner 山东格新精工有限公司