CN104556201B - A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex - Google Patents

A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex Download PDF

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CN104556201B
CN104556201B CN201510026316.2A CN201510026316A CN104556201B CN 104556201 B CN104556201 B CN 104556201B CN 201510026316 A CN201510026316 A CN 201510026316A CN 104556201 B CN104556201 B CN 104556201B
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microwave
complex
reaction
cuo nano
deionized water
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CN104556201A (en
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殷立雄
王菲菲
黄剑锋
孔新刚
张东东
柴思敏
韩鑫
裴宇梁
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Shaanxi University of Science and Technology
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Abstract

The open a kind of microwave-hydrothermal method that adopts of the present invention prepares Sm (OH) 3the method of/CuO nano-complex: by analytical pure Sm (NO 3) 36H 2o and Cu (NO 3) 23H 2o is dissolved in obtained solution A in deionized water with the mol ratio of 1:0.2 ~ 1:2; Adopt pH to 7 ~ 13 of analytical pure sodium hydrate regulator solution A, continue stirring 1 ~ 2h forming reactions precursor liquid; Reaction precursor liquid is poured in water heating kettle, puts into microwave hydrothermal reaction (MDS-10 type) after envelope still, at 100 ~ 200 DEG C, react 1 ~ 2h, after reaction terminates, naturally cool to room temperature; Product uses deionized water and dehydrated alcohol centrifuge washing 4 ~ 6 times successively, collects product vacuum-drying 0.5 ~ 2h at 60 ~ 80 DEG C, obtains Sm (OH) 3/ CuO nano-complex.Raw material of the present invention is easy to get and cost is low, and processing unit is simple, and energy consumption is low, and speed is fast.

Description

A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex
[technical field]
The invention belongs to Nano semiconductor field of composite material preparation, be specifically related to one and prepare Sm (OH) 3the method of/CuO nano-complex.
[background technology]
Sm (OH) 3a kind of white powder, water insoluble, be soluble in mineral acid.Sm (OH) 3as typical rare earth metal hydroxide material, nano level Sm (OH) 3with the characteristic of rare earth and nano material, in multiple fields of the functional materialss such as high efficiency light-emitting device, magneticsubstance, catalytic material, there is potential using value.
As wide bandgap semiconductor, Sm (OH) 3corresponding lower to visible ray, can only utilize the light of below spectrum 390nm, only have 1% to the utilization ratio of sun power.
[summary of the invention]
A kind of microwave-hydrothermal method that adopts is the object of the present invention is to provide to prepare Sm (OH) 3the method of/CuO nano-complex, the reaction medium of the method is the aqueous solution, and security is high, and resultant velocity is fast, can control composite crystals pattern, prepared Sm (OH) 3uniform particle sizes, the good dispersity of/CuO nano-complex, there is better photocatalytic activity.
For achieving the above object, the technical solution used in the present invention is:
A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex, comprises the following steps:
1) by analytical pure Sm (NO 3) 36H 2o and Cu (NO 3) 23H 2o is with 1:(0.2 ~ 2) mol ratio to be dissolved in solvent obtained Sm 3+concentration is the solution A of 0.1 ~ 2mol/L;
2) pH to 7 ~ 13 of regulator solution A under magnetic stirring, continue stirring 1 ~ 2h forming reactions precursor liquid;
3) reaction precursor liquid is poured in microwave hydrothermal reaction kettle, put into microwave hydrothermal reaction after envelope still, at 100 ~ 200 DEG C, react 1 ~ 2h, after reaction terminates, naturally cool to room temperature;
4) product washing, drying, obtain Sm (OH) 3/ CuO nano-complex.
Described solvent is deionized water.
Step 2) middle employing analytical pure sodium hydroxide adjust ph.
Step 4) described washing, drying be specially: use deionized water and dehydrated alcohol centrifuge washing 4 ~ 6 times successively, be placed in 60 ~ 80 DEG C of electric vacunm drying case inner drying 0.5 ~ 2h.
Relative to prior art, the present invention has following beneficial effect:
The present invention prepares Sm (OH) with microwave-hydrothermal method 3/ CuO nano-complex, utilizes microwave to make its overall homogeneous heating to heating objects, the Sm (OH) of gained 3/ CuO nano-complex purity is high, and crystallinity is strong, pattern uniform, controllable and size uniform.The raw material of this reaction is easy to get and cost is low, and processing unit is simple, and energy consumption is low, and speed is fast, so very economical, practical, has good industrial prospect.
Sm (OH) prepared by microwave-hydrothermal method of the present invention 3/ CuO nano-complex, reaction medium is the aqueous solution, and security is high, and reaction raw materials is easy to get, and feasibility is strong, and processing unit is simple.Utilize microwave heating can make the overall homogeneous heating of object, resultant velocity is fast, obtained Sm (OH) 3/ CuO nano-complex; The present invention utilizes microwave to carry out heating to reactant and makes its overall thermally equivalent, and speed of response is fast, composite crystals morphology controllable, narrow diameter distribution.
The present invention is in order to improve Sm (OH) 3to the utilization ratio of sun power, compound is carried out to it, be effectively separated photoproduction electron-hole pair; CuO energy gap is narrower, with Sm (OH) 3form the utilization of heterojunction raising to sunlight, photocatalysis efficiency improves greatly.
[accompanying drawing explanation]
Fig. 1 is that the present invention is with Sm prepared by microwave hydrothermal (OH) 3the XRD figure of/CuO nano-complex.
[embodiment]
Embodiment 1:
1) by analytically pure Sm (NO 3) 36H 2o and Cu (NO 3) 23H 2o is dissolved in obtained Sm in 10ml deionized water with the mol ratio of 1:0.2 3+concentration is the solution A of 0.1mol/L;
2) adopt the pH to 7 of analytically pure sodium hydrate regulator solution A under magnetic stirring, continue to stir 1h forming reactions precursor liquid;
3) reaction precursor liquid being poured into deionized water is that the microwave hydrothermal of solvent is sent out and answered in still, puts into microwave hydrothermal reaction, hydro-thermal reaction 2h at 100 DEG C, naturally cool to room temperature after reaction terminates after envelope still;
4) product uses deionized water and dehydrated alcohol centrifuge washing 4 ~ 6 times successively, is placed in 60 DEG C of electric vacunm drying case inner drying 0.5h, obtains Sm (OH) 3/ CuO nano-complex.
Embodiment 2:
1) by analytically pure Sm (NO 3) 36H 2o and Cu (NO 3) 23H 2o is dissolved in obtained Sm in 10ml deionized water with the mol ratio of 1:0.5 3+concentration is the solution A of 2mol/L;
2) adopt the pH to 9 of analytically pure sodium hydrate regulator solution A under magnetic stirring, continue to stir 1h forming reactions precursor liquid;
3) reaction precursor liquid being poured into deionized water is in the microwave hydrothermal reaction kettle of solvent, puts into microwave hydrothermal reaction, hydro-thermal reaction 2h at 100 DEG C, naturally cool to room temperature after reaction terminates after envelope still;
4) product uses deionized water and dehydrated alcohol centrifuge washing 4 ~ 6 times successively, is placed in 70 DEG C of electric vacunm drying case inner drying 1h, obtains Sm (OH) 3/ CuO nano-complex.
Embodiment 3:
1) by analytically pure Sm (NO 3) 36H 2o and Cu (NO 3) 23H 2o is dissolved in obtained Sm in 10ml deionized water with the mol ratio of 1:0.8 3+concentration is the solution A of 0.5mol/L;
2) adopt the pH to 11 of analytically pure sodium hydrate regulator solution A under magnetic stirring, continue to stir 1.5h forming reactions precursor liquid;
3) reaction precursor liquid being poured into deionized water is in the microwave hydrothermal reaction kettle of solvent, puts into microwave hydrothermal reaction, hydro-thermal reaction 1.5h at 130 DEG C, naturally cool to room temperature after reaction terminates after envelope still;
4) product uses deionized water and dehydrated alcohol centrifuge washing 4 ~ 6 times successively, is placed in 80 DEG C of electric vacunm drying case inner drying 1h, obtains Sm (OH) 3/ CuO nano-complex.
Embodiment 4:
1) by analytically pure Sm (NO 3) 36H 2o and Cu (NO 3) 23H 2o is dissolved in obtained Sm in 10ml deionized water with the mol ratio of 1:1 3+concentration is the solution A of 1mol/L;
2) adopt the pH to 12 of analytically pure sodium hydrate regulator solution A under magnetic stirring, continue to stir 2h forming reactions precursor liquid;
3) reaction precursor liquid being poured into deionized water is in the microwave hydrothermal reaction kettle of solvent, puts into microwave hydrothermal reaction, hydro-thermal reaction 1h at 170 DEG C, naturally cool to room temperature after reaction terminates after envelope still;
4) product uses deionized water and dehydrated alcohol centrifuge washing 4 ~ 6 times successively, is placed in 80 DEG C of electric vacunm drying case inner drying 1h, obtains Sm (OH) 3/ CuO nano-complex.
Embodiment 5:
1) by analytically pure Sm (NO 3) 36H 2o and Cu (NO 3) 23H 2o is dissolved in obtained Sm in 10ml deionized water with the mol ratio of 1:2 3+concentration is the solution A of 1.5mol/L;
2) adopt the pH to 13 of analytically pure sodium hydrate regulator solution A under magnetic stirring, continue to stir 2h forming reactions precursor liquid;
3) reaction precursor liquid being poured into deionized water is in the microwave hydrothermal reaction kettle of solvent, puts into microwave hydrothermal reaction, hydro-thermal reaction 1h at 200 DEG C, naturally cool to room temperature after reaction terminates after envelope still;
4) product uses deionized water and dehydrated alcohol centrifuge washing 4 ~ 6 times successively, is placed in 80 DEG C of electric vacunm drying case inner drying 2h, obtains Sm (OH) 3/ CuO nano-complex.
Fig. 1 is that the present invention is with Sm prepared by microwave-hydrothermal method (OH) 3the XRD figure of/CuO nano-complex, as can be seen from the figure high, the good crystallinity of the purity of product, has good Research Prospects in degradation of organic substances environmental problem.In photo-catalytic degradation of methyl-orange, Sm (OH) 3/ CuO nano-complex shows good photocatalysis performance, after uv irradiating 45min, complete degraded to tropeolin-D, simple Sm (OH) 3but 120min and 100min is needed with CuO.

Claims (2)

1. one kind adopts microwave-hydrothermal method to prepare Sm (OH) 3the method of/CuO nano-complex, is characterized in that, comprises the following steps:
1) by analytical pure Sm (NO 3) 36H 2o and Cu (NO 3) 23H 2o is with 1:(0.2 ~ 2) mol ratio to be dissolved in solvent obtained Sm 3+concentration is the solution A of 0.1 ~ 2mol/L;
2) pH to 7 ~ 13 of regulator solution A under magnetic stirring, continue stirring 1 ~ 2h forming reactions precursor liquid;
3) reaction precursor liquid is poured in microwave hydrothermal reaction kettle, put into microwave hydrothermal reaction after envelope still, at 100 ~ 200 DEG C, react 1 ~ 2h, after reaction terminates, naturally cool to room temperature;
4) product washing, drying, obtain Sm (OH) 3/ CuO nano-complex;
Described solvent is deionized water;
Step 2) middle employing analytical pure sodium hydroxide adjust ph.
2. microwave-hydrothermal method according to claim 1 prepares Sm (OH) 3the method of/CuO nano-complex: it is characterized in that: step 4) described washing, drying be specially: use deionized water and dehydrated alcohol centrifuge washing 4 ~ 6 times successively, be placed in 60 ~ 80 DEG C of electric vacunm drying case inner drying 0.5 ~ 2h.
CN201510026316.2A 2015-01-19 2015-01-19 A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex Active CN104556201B (en)

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CN105642323B (en) * 2016-01-12 2018-02-23 陕西科技大学 One kind prepares Sm (OH) using in situ deposition method3/AgPO4The method of nano-complex
CN110152665B (en) * 2019-05-29 2022-02-15 湖南人文科技学院 CuO/Cu2Preparation method of O/Cu ternary composite material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101494170A (en) * 2009-02-19 2009-07-29 陕西科技大学 Method for preparing Sm2O3 film by microwave assisted hydrothermal process
CN102139197A (en) * 2010-01-29 2011-08-03 张颖 Method for preparing modified micro granules
CN104030335A (en) * 2014-06-20 2014-09-10 陕西科技大学 Method for preparing Sm(OH)3/ZnO nano-composite by using homogeneous hydrothermal method
CN104071821A (en) * 2014-06-20 2014-10-01 陕西科技大学 Method for preparing Sm(OH)3/ZnO composite film by using homogeneous hydrothermal method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101494170A (en) * 2009-02-19 2009-07-29 陕西科技大学 Method for preparing Sm2O3 film by microwave assisted hydrothermal process
CN102139197A (en) * 2010-01-29 2011-08-03 张颖 Method for preparing modified micro granules
CN103418316A (en) * 2010-01-29 2013-12-04 张颖 Preparation method of modified micro-granules
CN104030335A (en) * 2014-06-20 2014-09-10 陕西科技大学 Method for preparing Sm(OH)3/ZnO nano-composite by using homogeneous hydrothermal method
CN104071821A (en) * 2014-06-20 2014-10-01 陕西科技大学 Method for preparing Sm(OH)3/ZnO composite film by using homogeneous hydrothermal method

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