CN104556201A - Method for preparing Sm(OH3)3/CuO nano composite by microwave-hydrothermal process - Google Patents

Method for preparing Sm(OH3)3/CuO nano composite by microwave-hydrothermal process Download PDF

Info

Publication number
CN104556201A
CN104556201A CN201510026316.2A CN201510026316A CN104556201A CN 104556201 A CN104556201 A CN 104556201A CN 201510026316 A CN201510026316 A CN 201510026316A CN 104556201 A CN104556201 A CN 104556201A
Authority
CN
China
Prior art keywords
microwave
cuo nano
hydrothermal
complex
reaction
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201510026316.2A
Other languages
Chinese (zh)
Other versions
CN104556201B (en
Inventor
殷立雄
王菲菲
黄剑锋
孔新刚
张东东
柴思敏
韩鑫
裴宇梁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201510026316.2A priority Critical patent/CN104556201B/en
Publication of CN104556201A publication Critical patent/CN104556201A/en
Application granted granted Critical
Publication of CN104556201B publication Critical patent/CN104556201B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention discloses a method for preparing a Sm(OH3)3/CuO nano composite by a microwave-hydrothermal process, which comprises the following steps: dissolving analytically pure Sm(NO3)3.6H2O and Cu(NO3)2.3H2O in a mole ratio of 1:0.2-1:2 in deionized water to obtain a solution A: regulating the pH value of the solution A to 7-13 by using analytically pure sodium hydroxide, and continuing stirring for 1-2 hours to form a reaction precursor solution; pouring the reaction precursor solution into a hydrothermal kettle, sealing the kettle, putting in a microwave-hydrothermal reaction instrument (MDS-10), reacting at 100-200 DEG C for 1-2 hours, and after the reaction finishes, naturally cooling to room temperature; and carrying out centrifuge washing on the product sequentially with deionized water and anhydrous ethanol 4-6 times, and carrying out vacuum drying on the collected product at 60-80 DEG C for 0.5-2 hours, thereby obtaining the Sm(OH3)3/CuO nano composite. The method has the advantages of accessible raw materials, low cost, simple technological equipment, low energy consumption and high speed.

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 (4)

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.
2. microwave-hydrothermal method according to claim 1 prepares Sm (OH) 3the method of/CuO nano-complex: it is characterized in that: described solvent is deionized water.
3. microwave-hydrothermal method according to claim 1 prepares Sm (OH) 3the method of/CuO nano-complex: it is characterized in that: step 2) middle employing analytical pure sodium hydroxide adjust ph.
4. 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)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510026316.2A CN104556201B (en) 2015-01-19 2015-01-19 A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510026316.2A CN104556201B (en) 2015-01-19 2015-01-19 A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex

Publications (2)

Publication Number Publication Date
CN104556201A true CN104556201A (en) 2015-04-29
CN104556201B CN104556201B (en) 2016-03-30

Family

ID=53073406

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510026316.2A Active CN104556201B (en) 2015-01-19 2015-01-19 A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex

Country Status (1)

Country Link
CN (1) CN104556201B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105642323A (en) * 2016-01-12 2016-06-08 陕西科技大学 Method for preparing Sm(OH)3/AgPO4 nanocomposite by virtue of in-situ deposition method
CN110152665A (en) * 2019-05-29 2019-08-23 湖南人文科技学院 CuO/Cu2The preparation method of O/Cu trielement 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

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105642323A (en) * 2016-01-12 2016-06-08 陕西科技大学 Method for preparing Sm(OH)3/AgPO4 nanocomposite by virtue of in-situ deposition method
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
CN110152665A (en) * 2019-05-29 2019-08-23 湖南人文科技学院 CuO/Cu2The preparation method of O/Cu trielement composite material
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

Also Published As

Publication number Publication date
CN104556201B (en) 2016-03-30

Similar Documents

Publication Publication Date Title
CN103482671B (en) Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode
CN104030335A (en) Method for preparing Sm(OH)3/ZnO nano-composite by using homogeneous hydrothermal method
CN112875755B (en) Preparation method of bismuth tungstate nano powder
CN103878011A (en) Method for synthesizing GaN: ZnO solid solution photocatalyst
CN105645469A (en) Nano rodlike lanthanum titanate powder and preparation method thereof
CN108101119B (en) Preparation method of iron oxide nanosheet material
CN103623799A (en) Preparation method of titanium dioxide mesoporous microspheres
CN102951686A (en) Preparation method for granular manganese tungstate nanocrystals
CN105366714A (en) Synthetic method of stannic oxide nanoflower array
CN102432056B (en) Method for preparing Sm2O3 nano crystals by solvent thermal method
CN105731518B (en) Normal-temperature crystallization preparation method of octahedron cuprous oxide crystal
CN104556201B (en) A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex
CN104117366A (en) ZnO/ZnSe heterogeneous nanometer array structure material, preparation method and application of ZnO/ZnSe heterogeneous nanometer array structure material
CN104402065A (en) Preparation method of spheroidic CoS2 nanometer powder
CN104556194A (en) Method for preparing hollow tubular Sm(OH3)3/ZnO nano composite by low-temperature water bath process
CN103754935A (en) Method for synthesizing lead molybdate tower crystal at room temperature
CN103611527A (en) Visible-light response Ce doped Bi2WO6 microcrystal, preparation method and application thereof
CN102951685A (en) Preparation method of rod-like manganese tungstate microcrystal
CN105498814A (en) Preparation method of lanthanum doped bismuth phosphate photocatalyst
CN103433036B (en) A kind of catalysis material Ag/AgMO 2and preparation method thereof
CN105056947B (en) One kind prepares AgO/Sm (OH) using two-step method3The method of/ZnO nano compound
CN102583525B (en) Preparation method of rutile titanium dioxide mesomorphic crystal
CN104528814A (en) Preparation method and product of CaTi2O4(OH)4 diamond nanosheet with lamellar structure
CN104556210B (en) A kind of employing hot two-step method of microwave-assisted solvent prepares Sm2sn2o7/ SnO2the method of nano-complex
CN103482672B (en) Preparation method of hexagonal-prism-shaped Sm(OH)3 nanocrystalline

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant