CN105032401A - Method for rapidly preparing snowflake cerium molybdate through microwave radiation - Google Patents
Method for rapidly preparing snowflake cerium molybdate through microwave radiation Download PDFInfo
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- CN105032401A CN105032401A CN201510551954.6A CN201510551954A CN105032401A CN 105032401 A CN105032401 A CN 105032401A CN 201510551954 A CN201510551954 A CN 201510551954A CN 105032401 A CN105032401 A CN 105032401A
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- molybdate
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Abstract
The invention discloses a method for rapidly preparing snowflake cerium molybdate through microwave radiation. The method comprises the following steps that 1, suspension liquid is prepared, wherein deionized water is used for preparing cerous nitrate and sodium molybdate mixed suspension liquid, the molar concentration ratio of Ce3+ to MoO42- is 2:3; 2, the pH is adjusted, wherein the pH of the suspension liquid is adjusted to range from 4.5 to 6.5; 3, a microwave heating reaction is carried out, wherein the suspension liquid is transferred to glassware and then placed in a microwave oven for a low-heat reaction for 20-40 min, and finally the snowflake cerium molybdate is obtained. No solvent or organic additive is adopted, and the reaction time is effectively shortened by the adoption of microwave heating; the method for rapidly preparing snowflake cerium molybdate through microwave radiation is simple in technology, short in reaction time and easy to control, and can prepare snowflake cerium molybdate in an environment-friendly mode.
Description
Technical field
The invention belongs to the processing preparation technology field of inorganic material and functional material, be specifically related to a kind of method that microwave prepares flakes cerous molybdate fast.
Background technology
Along with the fast development of dyestuff, weaving, printing industry, the application of dyestuff and dyestuff intermediate is ubiquitous, and these organic compounds are while increasing substantially people's quality of life, and its waste water produced causes serious environmental pollution.These waste water have the features such as concentration is high, colourity is dark, organic components is complicated, toxicity is large, biological degradability is poor, become one of key industry waste water of the large and refractory reason of discharge capacity.The method of current these waste water of process comprises Physical, chemical method, physico-chemical process and biochemical process etc., but the process of these methods to dyeing waste water is difficult to meet discharge standard.The photocatalytic oxidation degradation pollutant technology that development in recent years is got up receives much concern, the method technique is simple, energy consumption is low, reaction condition is gentle, organic pollution finally can be made to be converted into inorganic molecules and to reach inorganic permineralization, is comparatively applicable to carrying out advanced treating to industrial dye waste water.From domestic and international present Research, in all photochemical catalysts, conventional semiconductors Ti0
2(anatase) is widely used due to the reason such as non-toxic inexpensive and high activity, but due to Ti0
2very low to the utilization ratio of solar energy, usually need to excite with ultraviolet source, limit the application of its reality; And other nano materials are as ZnO, Fe
20
3deng due to shortcomings such as valence band current potential are lower, photostability is poor, also not satisfactory for photocatalysis to degrade organic matter effect.Therefore, develop low cost, the novel photocatalysis material of high catalytic activity has important theory significance and actual application value to environmental improvement.
Cerium has good catalytic activity, and the molybdenum-base oxide catalyst that to be a class important, cerium and molybdenum oxide is combined to be prepared into cerous molybdate new material be the better catalyst of a kind of catalytic performance.In addition, domestic and international many scholar's research show, cerium and cerium-containing compound are good water treatment absorbents, so cerous molybdate energy selective absorption and catalysis organic dyestuff under sunshine, be a kind of novel photochemical catalyst, in dye wastewater treatment, have potential application prospect.
At present, about preparation method's mainly solvent-thermal method of cerous molybdate, this method preparation process is normal with an organic solvent, and organic substance will be added make adjuvant, adding of these organic substances all may cause secondary pollution, also may affect the growth course of crystal, and its purity and performance are affected.In addition, this preparation method's operating process is too numerous and diverse, and the reaction time is long.Therefore, fault need research and develop a kind of cerous molybdate preparation method of short, environmental protection simple to operate, consuming time.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, provides a kind of microwave to prepare the method for flakes cerous molybdate fast, and to overcome, flower-shaped cerous molybdate preparation section is loaded down with trivial details, the reaction time long and the defect of environmental protection not.
For realizing above-mentioned technical problem, the present invention takes following technical scheme:
Microwave prepares a method for flakes cerous molybdate fast, with sodium molybdate and cerous nitrate for raw material, comprises following concrete steps:
(1) formulated suspension: the mixing suspension preparing cerous nitrate and sodium molybdate by deionized water, wherein Ce
3+/ MoO
4 2-molar concentration rate is 2:3;
(2) pH is regulated: pH to 4.5 ~ 6.5 regulating suspension;
(3) heating using microwave reaction: suspension is transferred to glassware, after being placed in the low fire reaction of micro-wave oven 20 ~ 40min, collecting solid and is flakes cerous molybdate.
Preferably, mixing suspension described in step (1) is first respectively with deionized water preparation cerous nitrate and sodium molybdate solution, then at room temperature both is mixed together rapidly.
Preferably, the raw material of pH is regulated to be NaOH and salpeter solution described in step (2).
Preferably, described in step (2), the pH of suspension is 4.7.
Preferably, step (3) described glassware is glass evaporating dish.
Preferably, the low fire reaction time of micro-wave oven described in step (3) is 35min.
The present invention also provides a kind of flakes cerous molybdate prepared according to said method, is prepared from by following steps:
(1) formulated suspension: the mixing suspension preparing cerous nitrate and sodium molybdate by deionized water, wherein Ce
3+/ MoO
4 2-molar concentration rate is 2:3;
(2) pH is regulated: pH to 4.5 ~ 6.5 regulating suspension;
(3) heating using microwave reaction: suspension is transferred to glassware, namely obtains product after being placed in the low fire reaction of micro-wave oven 20 ~ 40min.
Preferably, described alabastrine structure is assembled by tiny thin slice.
Compared with prior art, the present invention achieves following beneficial effect and is: first, and the present invention does not use any organic solvent or organic additive, avoids the secondary pollution that may bring, and also make the product purity that obtains high, output is large.Secondly, the present invention adopts the mode of microwave to heat, and significantly accelerates reaction speed, greatly saves the reaction time, and experiment easily controls.In addition, the present invention uses raw material components few, and conditions of mixture ratios is easy-regulating more, and preparation technology is simple, with low cost.
Accompanying drawing explanation
The x-ray diffraction pattern of the flakes cerous molybdate that Fig. 1 obtains for the embodiment of the present invention 1.
The flakes cerous molybdate field emission scanning electron microscope photo that Fig. 2 obtains for the embodiment of the present invention 1.
The flakes cerous molybdate field emission scanning electron microscope photo that Fig. 3 obtains for the embodiment of the present invention 2.
The flakes cerous molybdate field emission scanning electron microscope photo that Fig. 4 obtains for the embodiment of the present invention 3.
The flakes cerous molybdate field emission scanning electron microscope photo that Fig. 5 obtains for the embodiment of the present invention 4.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is further described in detail.
Embodiment 1
Microwave prepares a method for flakes cerous molybdate fast, with sodium molybdate and cerous nitrate for raw material, comprises following concrete steps: (1) formulated suspension: with the mixing suspension of deionized water preparation 20mL cerous nitrate and sodium molybdate, wherein Ce
3+/ MoO
4 2-molar concentration rate is 2:3; (2) pH is regulated: the pH to 4.5 regulating suspension with NaOH and salpeter solution; (3) heating using microwave reaction: suspension is transferred to glassware, after being placed in micro-wave oven low fire reaction 20min, collecting solid and is flakes cerous molybdate.Products therefrom deionized water and absolute ethanol washing, dry 6h at 80 DEG C, carries out test and characterize.Fig. 1 is the XRD collection of illustrative plates of products therefrom, proves that products therefrom is Ce
2(MoO
4)
34.5H
2o; Fig. 2 is the field emission scanning electron microscope photo of product, and display product is the flakes structure that tiny thin slice is self-assembled into.
Embodiment 2
Microwave prepares a method for flakes cerous molybdate fast, with sodium molybdate and cerous nitrate for raw material, comprises following concrete steps: (1) formulated suspension: with the mixing suspension of deionized water preparation 20mL cerous nitrate and sodium molybdate, wherein Ce
3+/ MoO
4 2-molar concentration rate is 2:3; (2) pH is regulated: the pH to 6.5 regulating suspension with NaOH and salpeter solution; (3) heating using microwave reaction: suspension is transferred to glassware, after being placed in micro-wave oven low fire reaction 40min, collecting solid and is flakes cerous molybdate.Products therefrom deionized water and absolute ethanol washing, dry 6h at 80 DEG C, and Fig. 3 is the field emission scanning electron microscope photo of product, and display product is the flakes structure that tiny thin slice is self-assembled into.
Embodiment 3
Microwave prepares a method for flakes cerous molybdate fast, with sodium molybdate and cerous nitrate for raw material, comprises following concrete steps: (1) formulated suspension: with the mixing suspension of deionized water preparation 20mL cerous nitrate and sodium molybdate, wherein Ce
3+/ MoO
4 2-molar concentration rate is 2:3; (2) pH is regulated: the pH to 5 regulating suspension with NaOH and salpeter solution; (3) heating using microwave reaction: suspension is transferred to glassware, after being placed in micro-wave oven low fire reaction 30min, collecting solid and is flakes cerous molybdate.Products therefrom deionized water and absolute ethanol washing, dry 6h at 80 DEG C, and Fig. 4 is the field emission scanning electron microscope photo of product, and display product is the flakes structure that tiny thin slice is self-assembled into.
Embodiment 4
Microwave prepares a method for flakes cerous molybdate fast, with sodium molybdate, cerous nitrate raw material, comprises concrete following steps: (1) is by 0.43422g cerous nitrate (Ce (NO
3)
3﹒ 6H
2o) be dissolved in 10ml deionized water, wiring solution-forming A; (2) by 0.36294g sodium molybdate (Na
2moO
4﹒ 2H
2o) be dissolved in 10ml deionized water, wiring solution-forming B; (3) by above-mentioned joined solution A and solution B at room temperature rapidly mix and blend make suspension, after NaOH and nitric acid regulation system pH=4.7, suspension is transferred in glass evaporating dish, be placed in micro-wave oven again, low fire reaction 35min, finally collect gained solid product, with deionized water and absolute ethanol washing, at 80 DEG C, dry 6h.Fig. 5 is the field emission scanning electron microscope photo of product, and display product is the flakes structure that tiny thin slice is self-assembled into.
It should be noted last that, above detailed description of the invention is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (8)
1. microwave prepares a method for flakes cerous molybdate fast, it is characterized in that: with sodium molybdate and cerous nitrate for raw material, comprise following concrete steps:
(1) formulated suspension: the mixing suspension preparing cerous nitrate and sodium molybdate by deionized water, wherein Ce
3+/ MoO
4 2-molar concentration rate is 2:3;
(2) pH is regulated: pH to 4.5 ~ 6.5 regulating suspension;
(3) heating using microwave reaction: suspension is transferred to glassware, after being placed in the low fire reaction of micro-wave oven 20 ~ 40min, collecting solid and is flakes cerous molybdate.
2. microwave according to claim 1 prepares the method for flakes cerous molybdate fast, it is characterized in that: mixing suspension described in step (1) is first respectively with deionized water preparation cerous nitrate and sodium molybdate solution, then at room temperature both is mixed together rapidly.
3. microwave according to claim 1 prepares the method for flakes cerous molybdate fast, it is characterized in that: regulate the raw material of pH to be NaOH and salpeter solution described in step (2).
4. microwave according to claim 1 prepares the method for flakes cerous molybdate fast, it is characterized in that: described in step (2), the pH of suspension is 4.7.
5. microwave according to claim 1 prepares the method for flakes cerous molybdate fast, it is characterized in that: step (3) described glassware is glass evaporating dish.
6. microwave according to claim 1 prepares the method for flakes cerous molybdate fast, it is characterized in that: the low fire reaction time of micro-wave oven described in step (3) is 35min.
7., according to a flakes cerous molybdate prepared by claim 1 ~ 6 either method, it is characterized in that being prepared from by following steps:
(1) formulated suspension: the mixing suspension preparing cerous nitrate and sodium molybdate by deionized water, wherein Ce
3+/ MoO
4 2-molar concentration rate is 2:3;
(2) pH is regulated: pH to 4.5 ~ 6.5 regulating suspension;
(3) heating using microwave reaction: suspension is transferred to glassware, namely obtains product after being placed in the low fire reaction of micro-wave oven 20 ~ 40min.
8. flakes cerous molybdate according to claim 7, is characterized in that: described flakes structure is assembled by tiny thin slice.
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| CN201510551954.6A CN105032401A (en) | 2015-08-31 | 2015-08-31 | Method for rapidly preparing snowflake cerium molybdate through microwave radiation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108190957A (en) * | 2018-03-18 | 2018-06-22 | 中船重工黄冈贵金属有限公司 | A kind of preparation method of flower-shaped cerous molybdate sodium nanometer rods cluster |
| EP4183429A4 (en) * | 2020-07-15 | 2024-09-04 | Tokyo Inst Tech | Complex oxide ceramic, functional material, and article |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3302994A (en) * | 1960-10-27 | 1967-02-07 | Ronson Corp | Process producing cerium molybdate, tungstate and vanadate |
| CN102351248A (en) * | 2011-09-13 | 2012-02-15 | 武汉理工大学 | Method for synthesizing cerium molybdate material |
-
2015
- 2015-08-31 CN CN201510551954.6A patent/CN105032401A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3302994A (en) * | 1960-10-27 | 1967-02-07 | Ronson Corp | Process producing cerium molybdate, tungstate and vanadate |
| CN102351248A (en) * | 2011-09-13 | 2012-02-15 | 武汉理工大学 | Method for synthesizing cerium molybdate material |
Non-Patent Citations (3)
| Title |
|---|
| MINGYAN DONG, ET AL: "Synthesis of Cerium Molybdate Hierarchical Architectures and Their Novel Photocatalytic and Adsorption Performances", 《CRYST. GROWTH DES.》 * |
| YANEE KEEREETA, ET AL: "Effects of solution pH and processing cycle on nanostructured La2(MoO4)3 produced by cyclic microwave radiation", 《CURRENT APPLIED PHYSICS》 * |
| 石晓波，等: "Ce2Mo3O12超微粒子的制备及催化性能", 《化学研究》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108190957A (en) * | 2018-03-18 | 2018-06-22 | 中船重工黄冈贵金属有限公司 | A kind of preparation method of flower-shaped cerous molybdate sodium nanometer rods cluster |
| EP4183429A4 (en) * | 2020-07-15 | 2024-09-04 | Tokyo Inst Tech | Complex oxide ceramic, functional material, and article |
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Application publication date: 20151111 |