A waugh manganese molybdate containing dysprosium-isonicotinic acid and its preparation method and application

A technology of manganese molybdate and isonicotinic acid is applied in the field of preparation of polyoxomolybdate chemical materials, which can solve problems such as photocatalytic performance that have not yet been seen, achieve good photocatalytic degradation, simple preparation method and high yield Effect

CN106366102BInactive Publication Date: 2018-02-16HENAN UNIVERSITY
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2018-02-16
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention relates to a Waugh-type manganese molybdate containing dysprosium-isonicotinic acid, the chemical formula of which is: (NH4)3[Dy(Hina)2(H2O)6][MnIVMo9O32]·7H2O. The compound is prepared by reacting manganese acetate, dysprosium nitrate, isonicotinic acid, 30% hydrogen peroxide, glacial acetic acid and ammonium heptamolybdate under aqueous solution conditions. The preparation method is simple, easy to operate, low in cost, and the crystal grows quickly and produces The rate is higher. This experimental study found that this compound has a good photocatalytic degradation effect on azo fluorescent pink. This research result provides experimental basis for the application of polymolybdate in the field of photocatalytic degradation of organic dyes.
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Description

technical field

[0001] The invention belongs to the technical field of polymolybdate chemical material preparation, and in particular relates to a preparation method of Waugh-type manganese molybdate containing dysprosium-isonicotinic acid and its application in the photodegradation of organic dyes. The compound utilizes manganese acetate, Dysprosium nitrate, isonicotinic acid, 30% hydrogen peroxide, glacial acetic acid and ammonium heptamolybdate react in aqueous solution. Background technique

[0002] Polyacid compounds, also known as polyoxometalates, are composed of high-priced pre-transition metal ions (such as Mo Ⅵ , W Ⅵ , V Ⅴ ,Nd Ⅴ , Ta Ⅴ etc.) are highly polymerized with oxygen to form inorganic polymer clusters with a spatial network structure. Because of their oxygen-rich surfaces, controllable structure, size, compositional and structural diversity, and unique redox activities, they have attracted great attention in the fields of catalysis, fluorescence, magn...

Examples

Embodiment 1

[0036] A Waugh-type manganese molybdate containing dysprosium-isonicotinic acid, its chemical formula is: (NH 4 ) 3 [Dy(Hina) 2 (H 2 O) 6 ][Mn IV Mo 9 o 32 ]·7H 2 O.

[0037] The Waugh-type manganese molybdate contained in the above-mentioned dysprosium-isonicotinic acid is synthesized by a traditional aqueous solution method, and its preparation method specifically includes the following steps:

[0038]1) Prepare solution A: In a 25 mL beaker, dissolve ammonium heptamolybdate (2.002 g, 1.62 mmol) in distilled water with stirring and adjust its pH to 5.0 with glacial acetic acid, then add manganese acetate (0.120 g, 0.49mmol), isonicotinic acid (0.156 g, 1.27 mmol), dysprosium nitrate (0.120 g, 0.26 mmol) and 0.45 mL 30%H 2 o 2 , stirred at room temperature for 20 minutes to form a homogeneous mixed phase, then placed in a water bath at 90±2°C and heated for 1 hour, took it out and filtered it into a 50 mL beaker while it was hot to obtain solution A;

[0039] 2) Pr...

Embodiment 2

[0042] A Waugh-type manganese molybdate containing dysprosium-isonicotinic acid, its chemical formula is: (NH 4 ) 3 [Dy(Hina) 2 (H 2 O) 6 ][Mn IV Mo 9 o 32 ]·7H 2 O.

[0043] The Waugh-type manganese molybdate contained in the above-mentioned dysprosium-isonicotinic acid is synthesized by a traditional aqueous solution method, and its preparation method specifically includes the following steps:

[0044] 1) Prepare solution A: In a 25 mL beaker, dissolve ammonium heptamolybdate (2.002 g, 1.62 mmol) in distilled water with stirring and adjust its pH to 5.0 with glacial acetic acid, then add manganese acetate (0.120 g, 0.49mmol), isonicotinic acid (0.156 g, 1.27 mmol), dysprosium nitrate (0.120 g, 0.26 mmol) and 0.45 mL 30%H 2 o 2 , stirred at room temperature for 20 minutes to form a homogeneous mixed phase, then placed in a water bath at 90±2°C and heated for 1 hour, took it out and filtered it into a 50 mL beaker while it was hot to obtain solution A;

[0045] 2) P...

Embodiment 3

[0048] A Waugh-type manganese molybdate containing dysprosium-isonicotinic acid, its chemical formula is: (NH 4 ) 3 [Dy(Hina) 2 (H 2 O) 6 ][Mn IV Mo 9 o 32 ]·7H 2 O.

[0049] The Waugh-type manganese molybdate contained in the above-mentioned dysprosium-isonicotinic acid is synthesized by a traditional aqueous solution method, and its preparation method specifically includes the following steps:

[0050] 1) Prepare solution A: In a 25 mL beaker, dissolve ammonium heptamolybdate (2.002 g, 1.62 mmol) in distilled water with stirring and adjust its pH to 5.0 with glacial acetic acid, then add manganese acetate (0.120 g, 0.49mmol), isonicotinic acid (0.156 g, 1.27 mmol), dysprosium nitrate (0.120 g, 0.26 mmol) and 0.45 mL 30%H 2 o 2 , stirred at room temperature for 20 minutes to form a homogeneous mixed phase, then placed in a water bath at 90±2°C and heated for 1 hour, took it out and filtered it into a 50 mL beaker while it was hot to obtain solution A;

[0051] 2) P...