CN102910679A

CN102910679A - Preparation method of nano manganese oxide

Info

Publication number: CN102910679A
Application number: CN2012103816652A
Authority: CN
Inventors: 王翀; 丁纯梅; 唐定兴
Original assignee: Anhui Polytechnic University
Current assignee: Anhui Polytechnic University
Priority date: 2012-10-10
Filing date: 2012-10-10
Publication date: 2013-02-06

Abstract

The invention discloses a preparation method of nano manganese oxide. The method comprises the following steps: ascorbic acid is added into acetum, and then the nano manganese oxide is obtained after the ascorbic acid and the acetum are stirred, mixed to be uniform, dried and roasted; the concentration of manganese acetate solution is 20 to 50 percent, the mol ratio of the ascorbic acid to manganese is (0.5 to 3):1, the stirring temperature is 40 to 80 DEG C, and vaporizing solvent is kept within the temperature range; the drying temperature is 110 DEG C; and the roasting temperature is 320 to 450 DEG C, and the roasting time is 2 to 10 hours. The method has the advantages that the production process flow is simple, material is common and easily available, and the particle size of obtained manganese oxide powder is smaller than 100nm.

Description

A kind of preparation method of nanostructured manganese oxide compound

Technical field

The present invention relates to a kind of preparation method of Mn oxide.

Background technology

Manganese material has widely purposes at the electronic energy source domain.For example, Mn ₃O ₄Powder and take the Mn-Zn ferrite soft magnetic material as raw material preparation, be applied in the electronic industry; Catalyzer take manganese as main active component can be used for nitrogen oxides reduction, nitro-compound and elimination carbon monoxide etc.The industrial main method for preparing the manganese powder body, a kind of is the oxyhydroxide of at high temperature calcining various manganese, nitrate, vitriol, carbonate etc., and the temperature of reaction that needs in this method is high, and energy consumption is large, and the particle that obtains the manganese oxide powder is thick; Also having a kind of method is metal M n method, claim again electrolytic metal Mn suspension oxidation style or electrolytic metal Mn bubble method, it is as raw material take the electrolytic metal Mn sheet, this method complex process equipment, the energy consumption of reaction needed is high, production cost is relatively more expensive, and the granular size of product manganese oxide also is difficult to control with distributing.

The preparation method who seeks the Ultra-fine Manganese that a kind of production technique is simple, cost is low is the present technical issues that need to address.

Summary of the invention

For solving the technical problem that exists in the prior art, the invention provides a kind of preparation method of Mn oxide, the technological process of production is simple, and raw material is common to be easy to get.

The preparation method who the purpose of this invention is to provide a kind of nanostructured manganese oxide compound.

Comprise following steps:

After the adding xitix mixed in the manganese acetate salts solution, evaporating solvent made described Mn oxide after oven dry, the roasting;

Described manganese acetate concentration of salt solution is 20～50%, and the mol ratio of described xitix and manganese is (0.5～3): 1, preferred (1～2): 1.

Described whipping temp is 40～80 ℃, and keeps evaporating solvent in this temperature range;

Described bake out temperature is 110 ℃;

Described maturing temperature is 320～450 ℃, and roasting time is 2～10 hours;

The grain diameter of the Mn oxide that makes is less than 100 nm.

Mn oxide powder preparation method of the present invention has following characteristics:

1, preparation technology's flow process is simple, and raw material is common to be easy to get, and energy consumption is low, is fit to scale operation;

The particle of the oxide powder of the manganese that 2, obtains is in 100 nanoscale scopes.

Description of drawings

The SEM Electronic Speculum figure of Fig. 1 embodiment 1

Embodiment

Below in conjunction with embodiment, further specify the present invention, but be not limited to these embodiment.

Use reagent to be commercially available chemical reagent in the embodiment of the invention;

The test of carrying out:

SEM: scanning electron microscope (Hitachi SU8020,15kv)

Embodiment 1

Take by weighing manganese acetate (Mn (CH ₃COO) ₂4H ₂O, AR, molecular weight (245.10), 24.5 gram (0.1 mol) is dissolved in the 62 gram deionized waters it, forms 20% manganese acetate solution, after in water-bath, being heated to 40 ℃, to wherein adding 8.81 gram xitix particles (0.05 mol), stirring it is dissolved in the manganese acetate solution, is denoted as A1.

Improve bath temperature to 50 ℃, A1 forms B1 in wherein placing 8 hours.

B1 is put into baking oven, put into retort furnace 110 ℃ of lower bakings after 4 hours, after 4 hours, form C1 320 ℃ of lower roastings.C1 is carried out the analytical test of SEM, the crystalline form that obtains and particle size the results are shown in Table 1.

Embodiment 2

Take by weighing manganese acetate (Mn (CH ₃COO) ₂4H ₂O, AR) 24.5 grams (0.1 mol), it is dissolved in the 62 gram deionized waters, form 20% manganese acetate solution, in water-bath, be heated to 40 ℃ after, to wherein adding 52.8 gram xitix particles (0.3 mol), stirring is dissolved in the manganese acetate solution it, is denoted as A2.

Improve bath temperature to 60 ℃, A2 forms B2 in wherein placing 8 hours.

B2 is put into baking oven, put into retort furnace 110 ℃ of lower bakings after 4 hours, after 2 hours, form C2 350 ℃ of lower roastings.C2 is carried out the analytical test of SEM, the crystalline form that obtains and particle size the results are shown in Table 1.

Embodiment 3

Take by weighing manganese acetate (Mn (CH ₃COO) ₂4H ₂O, AR) 24.5 grams (0.1 mol), it is dissolved in the 62 gram deionized waters, form 20% manganese acetate solution, in water-bath, be heated to 40 ℃ after, to wherein adding 35.2 gram xitix particles (0.2 mol), stirring is dissolved in the manganese acetate solution it, is denoted as A3.

Improve bath temperature to 50 ℃, A3 forms B3 in wherein placing 8 hours.

B3 is put into baking oven, put into retort furnace 110 ℃ of lower bakings after 4 hours, after 4 hours, form C3 450 ℃ of lower roastings.C3 is advanced the analytical test of SEM, the crystalline form that obtains and particle size the results are shown in Table 1.

Embodiment 4

Take by weighing manganese acetate (Mn (CH ₃COO) ₂4H ₂O, AR) 24.5 grams (0.1 mol), it is dissolved in the 62 gram deionized waters, form 20% manganese acetate solution, in water-bath, be heated to 40 ℃ after, to wherein adding 17.6 gram xitix (0.1 mol), stirring is dissolved in the manganese acetate solution it, is denoted as A4.

Improve bath temperature to 50 ℃, A4 forms B4 in wherein placing 8 hours.

B4 is put into baking oven, put into retort furnace 110 ℃ of lower bakings after 4 hours, after 2 hours, form C4 400 ℃ of lower roastings.C4 is carried out the analytical test of SEM, the crystalline form that obtains and particle size the results are shown in Table 1.

The particle size SEM result of gained Mn oxide among each embodiment of table 1

?	Manganese acetate	Xitix	Mol ratio	Calcination process	Grain size
						Embodiment 1	0.1mol	0.05mol	0.5	320℃ 4h	45 nm
Embodiment 2	0.1mol	0.3mol	3	350℃ 2h	65 nm
						Embodiment 3	0.1mol	0.2mol	2	450℃ 4h	80nm
Embodiment 4	0.1mol	0.1mol	1	400℃ 2h	70 nm

Claims

1. the preparation method of a nanostructured manganese oxide compound comprises following steps:

After the adding xitix mixed in the manganese acetate salts solution, oven dry, roasting made the nanostructured manganese oxide compound;

The mol ratio of xitix and manganese is (0.5 ~ 3): 1;

Described whipping temp is 60～70 ℃, and keeps evaporating solvent in this temperature range;

Described bake out temperature is 110 ℃;

Described maturing temperature is 320～450 ℃, and roasting time is 2～10 hours.