CN107149936A - A kind of CoFe2O4AgI composite photo-catalysts and preparation method thereof - Google Patents
A kind of CoFe2O4AgI composite photo-catalysts and preparation method thereof Download PDFInfo
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- CN107149936A CN107149936A CN201710229638.6A CN201710229638A CN107149936A CN 107149936 A CN107149936 A CN 107149936A CN 201710229638 A CN201710229638 A CN 201710229638A CN 107149936 A CN107149936 A CN 107149936A
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- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 35
- 239000010941 cobalt Substances 0.000 claims abstract description 35
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000006185 dispersion Substances 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 229910002518 CoFe2O4 Inorganic materials 0.000 claims abstract description 30
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 28
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 229910003321 CoFe Inorganic materials 0.000 claims abstract description 22
- 239000000725 suspension Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000008187 granular material Substances 0.000 claims abstract description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000002604 ultrasonography Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 abstract description 7
- 238000005406 washing Methods 0.000 abstract description 7
- 238000005286 illumination Methods 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract 1
- 229910021612 Silver iodide Inorganic materials 0.000 description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 32
- 229910001868 water Inorganic materials 0.000 description 31
- 239000003054 catalyst Substances 0.000 description 15
- 239000007787 solid Substances 0.000 description 15
- 230000015572 biosynthetic process Effects 0.000 description 11
- 238000001354 calcination Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 239000005457 ice water Substances 0.000 description 8
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 229940045105 silver iodide Drugs 0.000 description 6
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 5
- 229910002651 NO3 Inorganic materials 0.000 description 5
- 238000013019 agitation Methods 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910020598 Co Fe Inorganic materials 0.000 description 1
- 230000010748 Photoabsorption Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- MSFPLIAKTHOCQP-UHFFFAOYSA-M silver iodide Chemical compound I[Ag] MSFPLIAKTHOCQP-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/36—Organic compounds containing halogen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/38—Organic compounds containing nitrogen
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Abstract
The invention provides a kind of CoFe2O4AgI composite photo-catalysts and preparation method thereof, preparation process is as follows：Prepare ferrous acid cobalt granule；Ferrous acid cobalt granule is placed in ultrasonic disperse in EG, constant temperature stirring obtains the dispersion liquid A of cobalt ferrite；Silver nitrate is added in dispersion liquid A, ultrasound obtains being dissolved with the cobalt ferrite dispersion liquid B of silver nitrate；At a constant temperature, KI is dissolved in EG, stirring obtains solution C；Under conditions of constant temperature and uniform stirring, solution C is added dropwise in dispersion liquid B, continues stirring a period of time at a constant temperature, obtains suspension；Gained suspension is transferred in reactor, solvent thermal reaction is carried out, after completion of the reaction, by product cooling washing drying, CoFe is obtained2O4AgI composite photo-catalysts.CoFe prepared by the present invention2O4The preparation method of/AgI composites is simple and easy to apply, cost is low, its under visible light illumination 45min be that can reach 98% to the degradation rate of rhodamine B.
Description
Technical field
The present invention relates to catalysis material, a kind of visible light-responded CoFe is refered in particular to2O4- AgI compounded visible light photocatalysts
And preparation method thereof, belong to photocatalysis technology field in composite and environmental improvement.
Background technology
In the last few years, because problem of environmental pollution becomes increasingly conspicuous, attention of the people to global crisis is caused, and photocatalysis
Technology is a kind of environmentally friendly, low-cost type environmental improvement technology, therefore by extensive concern, so designing and developing high property
The visible light-responded catalysis material of energy is significant, and becomes the direction of photochemical catalyst development.
Silver iodide are a kind of new visible light-responded photochemical catalysts, under visible light illumination with excellent photocatalysis
Performance and can effectively degradable organic pollutant, show stronger photocatalytic activity；By the modification to silver iodide, improve
It is the further effective way for improving silver iodide photocatalytic activity in the absorption characteristic of visible region；Therefore, the present invention is provided
A kind of visible light-responded CoFe2O4The preparation method of-AgI composite visible light response catalysts, it is therefore an objective to pass through CoFe2O4's
Load can strengthen absorbability of the silver iodide to visible region energy, and then improve utilization rate of the catalyst to visible ray, finally
Reach the purpose for improving photocatalysis performance.
The content of the invention
It is an object of the invention to provide a kind of silver iodide composite visible light catalysis material with low cost, efficient and its
Preparation method, and solve that existing catalyst is not high to visible light utilization efficiency, stability is poor, to degradation of organic dyes inefficient etc.
Problem.
The present invention is achieved through the following technical solutions：
A kind of CoFe2O4- AgI composite photo-catalysts, the composite photo-catalyst is by CoFe2O4It is composited with AgI
, the CoFe2O4Mass fraction be 1~5%, by the CoFe2O4- AgI composite photo-catalysts are used for sieve to 10mg/L
Red bright B photocatalytic degradation, 98% has been reached in 45 minutes.
A kind of CoFe2O4The preparation method of-AgI composite photo-catalysts, step is as follows：
Step 1, prepare ferrous acid cobalt granule；
Step 2, ferrous acid cobalt granule is placed in ultrasonic disperse in EG, and stirred in water bath with thermostatic control (0-30 DEG C), obtain iron
The dispersion liquid A of sour cobalt；
Step 3, silver nitrate is added in dispersion liquid A, ultrasound obtains being dissolved with the cobalt ferrite dispersion liquid B of silver nitrate；
Step 4, under water bath with thermostatic control (0-30 DEG C), KI is dissolved in EG, stirring obtain solution C；
Step 5, under conditions of water bath with thermostatic control (0-30 DEG C) and uniform stirring, solution C is added dropwise to dispersion liquid B
In, continue stirring a period of time in water bath with thermostatic control (0-30 DEG C)；So that it forms good combination between cobalt ferrite
Power, obtains suspension；
Step 6, step 5 gained suspension is transferred in reactor, carries out solvent thermal reaction, after completion of the reaction, will produce
Thing cooling washing drying, obtains CoFe2O4- AgI composite photo-catalysts.
In step 2, in dispersion liquid A, the amount ratio of the cobalt ferrite and EG is 12~20mg：30mL, the constant temperature be 0~
30℃。
In step 3, in dispersion liquid B, silver nitrate and EG amount ratio are 0.4g：30mL；The silver nitrate ultrasonic time is
10~30 minutes, ultrasonic power was 90w, and mixing time is 20~60 minutes.
In step 4, in solution C, the concentration of the KI is 0.1g/mL, and the constant temperature is 0~30 DEG C, the mixing time
For 20-60 minutes.
In step 5, the solution C and dispersion liquid B volume ratio are 2~15, and the constant temperature is 0~30 DEG C, the stirring
Time is 30-120 minutes.
In step 6, the temperature of the solvent thermal reaction is 140 DEG C, and the time is 12h.
The present invention compared with prior art, its distinguishing feature：
Utilize CoFe2O4Silver iodide photocatalyst is modified, a kind of New Co Fe has been obtained2O4/ AgI composites,
Absorption characteristic of the silver iodide to visible ray is improved, secondly the CoFe prepared by the present invention2O4The preparation method of/AgI composites
It is simple and easy to apply, cost is low, its under visible light illumination 45min be that can reach 98% to the degradation rate of rhodamine B.
Brief description of the drawings
Fig. 1 is AgI, CoFe prepared by embodiment 12O4With 1% (3%, 5%, 10%) CoFe2O4/ AgI complex lights are urged
The XRD of agent；
Fig. 2 is the AgI and 1% (3%, 5%) CoFe prepared by embodiment 12O4The DRS figures of/AgI composite catalysts；
Fig. 3 is the AgI and 1% (3%, 5%) CoFe prepared by embodiment 12O4The impedance diagram of/AgI composite photo-catalysts；
Fig. 4 is (a) AgI (b) 1%CoFe prepared by embodiment 12O4/ AgI (c) 3%CoFe2O4/ AgI (d) 5%
CoFe2O4The SEM figures of/AgI composite catalysts；
Fig. 5 AgI and 1% (3%, 5%) CoFe2O4/ AgI composite photo-catalysts are under visible light illumination 10mg/ to concentration
L rhodamine B photocatalytic degradation curve map.
Embodiment
The following is several embodiments of the present invention, the present invention is further illustrated, but the present invention is not limited only to this.
Embodiment 1
The CoFe of nano particle is synthesized by hydro-thermal method and calcination method2O4, concrete operations are as follows：Measure 10mmol Fe
(NO3)3·9H2O and 5mmol Co (NO3)2·6H2O, which is placed in 100mL water, dissolves to obtain solution A, while by 15mmol C6H8O7·
H2O dissolves to obtain solution B in 100mL water, then solution A is added dropwise in solution B under the conditions of 60 DEG C of constant temperature, magnetic force is stirred
1-1.5h is mixed to forming uniform suspension C.Then suspension C is stood to layering, abandoning supernatant is washed with deionized
Solid formation is placed in 90 DEG C of baking ovens after solid formation to neutrality and keeps 24h, is then taken out from baking oven after obtained solid abrasive
Be put into crucible, be finally put into tube furnace be warming up to 500 DEG C calcining 2h obtain CoFe2O4Sample.
A certain amount of cobalt ferrite is placed in ultrasonic disperse 20min in 30ml EG, and stirred in ice-water bath (0 DEG C), is obtained
The dispersion liquid D of cobalt ferrite；0.4g silver nitrates are scattered in above-mentioned dispersion liquid mechanical agitation for a period of time after (30min), obtained
It is dissolved with the cobalt ferrite dispersion liquid E of silver nitrate；Simultaneously in (0 DEG C) bath of frozen water, 0.4g KIs are dissolved in 4ml EG and stirred
A period of time obtains solution F；Under conditions of 15 DEG C of water bath with thermostatic control and uniform stirring, the F solution prepared is added dropwise
Enter into E solution, continue the stirring 60min in ice-water bath (0 DEG C), gained suspension is then transferred to two 20mL reactors
In, reacted at 140 DEG C after 12h, product cooling washing is obtained into catalyst；The quality score of the cobalt ferrite and silver nitrate of generation
Wei 1:100,3:100,5:100；After the product of gained is dried, you can obtain described composite photo-catalyst, most it is ordered at last
Entitled 1%CoFe2O4/ AgI, 3%CoFe2O4/ AgI, 5%CoFe2O4/AgI。
The structure and composition of catalyst is determined using characterization methods such as XRD, XPS, SEM, TEM；The XRD of catalyst, DRS,
EIS, SEM are characterized as shown in Figure 1,2,3, 4；XRD results show the crystallinity of the composite catalyst of synthesis preferably, 3%CoFe2O4/
Only have AgI diffraction maximum and crystallinity preferable in AgI spectrograms, CoFe2O4Content is low without there is CoFe2O4Diffraction maximum；
DRS shows that composite has more preferable photo absorption performance than monomer；EIS results show that composite has lower resistance than monomer
It is anti-；SEM results show 3%AgI/CoFe2O4Compound have preferable pattern, CoFe2O4With the more well-regulated granulated in edge
Formula is present and well dispersed, and the SEM figures of composite are it can be seen that both can be effectively bonded together；
Fig. 5 is monomer AgI and 1% (3%, 5%) AgI/CoFe2O4The activity experiment of composite photocatalyst for degrading rhodamine B
Figure.It can be seen that 3%CoFe2O4/ AgI is in the RhB that 45min is removable 98%, hence it is evident that 84% higher than monomer AgI removes
Rate.
Embodiment 2
The CoFe of nano particle is synthesized by hydro-thermal method and calcination method2O4, concrete operations are as follows：Measure 10mmol Fe
(NO3)3·9H2O and 5mmol Co (NO3)2·6H2O, which is placed in 100mL water, dissolves to obtain solution A, while by 15mmol C6H8O7·
H2O dissolves to obtain solution B in 100mL water, then solution A is added dropwise in solution B under the conditions of 60 DEG C of constant temperature, magnetic force is stirred
1-1.5h is mixed to forming uniform suspension C.Then suspension C is stood to layering, abandoning supernatant is washed with deionized
Solid formation is placed in 90 DEG C of baking ovens after solid formation to neutrality and keeps 24h, is then taken out from baking oven after obtained solid abrasive
Be put into crucible, be finally put into tube furnace be warming up to 500 DEG C calcining 2h obtain CoFe2O4Sample.
0.012g cobalt ferrite is placed in ultrasonic disperse 10min in 30ml EG, and stirred in ice-water bath (0 DEG C), is obtained
The dispersion liquid D of cobalt ferrite；0.4g silver nitrates are scattered in above-mentioned dispersion liquid mechanical agitation for a period of time after (30min), obtained
It is dissolved with the cobalt ferrite dispersion liquid E of silver nitrate；Simultaneously in (0 DEG C) bath of frozen water, 0.4g KIs are dissolved in 4ml EG and stirred
A period of time obtains solution F；Under conditions of 15 DEG C of water bath with thermostatic control and uniform stirring, the F solution prepared is added dropwise
Enter into E solution, continue the stirring 60min in ice-water bath (0 DEG C), gained suspension is then transferred to two 20mL reactors
In, reacted at 140 DEG C after 12h, product cooling washing is obtained into catalyst；The cobalt ferrite of generation and the mass ratio of silver nitrate are
3:100；The product of gained is washed and dried, you can described composite photo-catalyst is obtained, most it is named as 3%AgI/ at last
CoFe2O4.Under visible light illumination, 45min can remove 98.0% rhodamine B to the material.
Embodiment 3
The CoFe of nano particle is synthesized by hydro-thermal method and calcination method2O4, concrete operations are as follows：Measure 10mmol Fe
(NO3)3·9H2O and 5mmol Co (NO3)2·6H2O, which is placed in 100mL water, dissolves to obtain solution A, while by 15mmol C6H8O7·
H2O dissolves to obtain solution B in 100mL water, then solution A is added dropwise in solution B under the conditions of 60 DEG C of constant temperature, magnetic force is stirred
1-1.5h is mixed to forming uniform suspension C.Then suspension C is stood to layering, abandoning supernatant is washed with deionized
Solid formation is placed in 90 DEG C of baking ovens after solid formation to neutrality and keeps 24h, is then taken out from baking oven after obtained solid abrasive
Be put into crucible, be finally put into tube furnace be warming up to 500 DEG C calcining 2h obtain CoFe2O4Sample.
0.02g cobalt ferrite is placed in ultrasonic disperse 40min in 30ml EG, and stirred in water bath with thermostatic control (30 DEG C), is obtained
To the dispersion liquid D of cobalt ferrite；0.4g silver nitrates are scattered in above-mentioned dispersion liquid mechanical agitation for a period of time after (30min), obtained
To the cobalt ferrite dispersion liquid E for being dissolved with silver nitrate；Simultaneously in water bath with thermostatic control (30 DEG C), 0.4g KIs are dissolved in 4ml EG
Stirring a period of time obtains solution F；Under conditions of 30 DEG C of water bath with thermostatic control and uniform stirring, by the F solution prepared by
It is added dropwise in E solution, continues the stirring 60min in water bath with thermostatic control (30 DEG C), gained suspension is then transferred to two
In 20mL reactors, reacted at 140 DEG C after 12h, product cooling washing is obtained into catalyst；The cobalt ferrite and silver nitrate of generation
Mass ratio be 5:100；After the product of gained is dried, you can obtain described composite photo-catalyst, most it is named as 5% at last
CoFe2O4/AgI。
Embodiment 4
The CoFe of nano particle is synthesized by hydro-thermal method and calcination method2O4, concrete operations are as follows：Measure 10mmol Fe
(NO3)3·9H2O and 5mmol Co (NO3)2·6H2O, which is placed in 100mL water, dissolves to obtain solution A, while by 15mmol C6H8O7·
H2O dissolves in 100mL water obtains solution B, then solution A is added dropwise in solution B under the conditions of 60 DEG C of constant temperature, magnetic force
1-1.5h is to forming uniform suspension C for stirring.Then suspension C is stood to layering, abandoning supernatant is washed with deionized water
Wash that solid formation is placed in 90 DEG C of baking ovens after solid formation to neutrality and keep 24h, obtained solid abrasive is then taken out from baking oven
After be put into crucible, be finally put into tube furnace be warming up to 550 DEG C calcining 2h obtain CoFe2O4Sample.
0.004g cobalt ferrite is placed in ultrasonic disperse 60min in 30ml EG, and stirred in ice-water bath (0 DEG C), is obtained
The dispersion liquid D of cobalt ferrite；0.4g silver nitrates are scattered in above-mentioned dispersion liquid mechanical agitation for a period of time after (30min), obtained
It is dissolved with the cobalt ferrite dispersion liquid E of silver nitrate；Simultaneously in (0 DEG C) bath of frozen water, 0.4g KIs are dissolved in 4ml EG and stirred
A period of time obtains solution F；Under conditions of 15 DEG C of water bath with thermostatic control and uniform stirring, the F solution prepared is added dropwise
Enter into E solution, continue the stirring 60min in ice-water bath (0 DEG C), gained suspension is then transferred to two 20mL reactors
In, reacted at 140 DEG C after 12h, product cooling washing is obtained into catalyst；The cobalt ferrite of generation and the mass ratio of silver nitrate are
1:100；After the product of gained is dried, you can obtain described composite photo-catalyst, most it is named as 1%CoFe at last2O4/
AgI。
Embodiment 5
The CoFe of nano particle is synthesized by hydro-thermal method and calcination method2O4, concrete operations are as follows：Measure 10mmol Fe
(NO3)3·9H2O and 5mmol Co (NO3)2·6H2O, which is placed in 100mL water, dissolves to obtain solution A, while by 15mmol C6H8O7·
H2O dissolves to obtain solution B in 100mL water, then solution A is added dropwise in solution B under the conditions of 60 DEG C of constant temperature, magnetic force is stirred
1-1.5h is mixed to forming uniform suspension C.Then suspension C is stood to layering, abandoning supernatant is washed with deionized
Solid formation is placed in 90 DEG C of baking ovens after solid formation to neutrality and keeps 24h, is then taken out from baking oven after obtained solid abrasive
Be put into crucible, be finally put into tube furnace be warming up to 500 DEG C calcining 2h obtain CoFe2O4Sample.
0.004g cobalt ferrite is placed in ultrasonic disperse 10min in 30ml EG, and stirred in ice-water bath (60 DEG C), is obtained
To the dispersion liquid D of cobalt ferrite；0.4g silver nitrates are scattered in above-mentioned dispersion liquid mechanical agitation for a period of time after (30min), obtained
To the cobalt ferrite dispersion liquid E for being dissolved with silver nitrate；Simultaneously in (0 DEG C) bath of frozen water, 0.4g KIs are dissolved in 4ml EG and stirred
Mix and obtain solution F for a period of time；Under conditions of 15 DEG C of water bath with thermostatic control and uniform stirring, by the F solution prepared dropwise
It is added in E solution, continues the stirring 60min in ice-water bath (0 DEG C), gained suspension is then transferred to two 20mL reactions
In kettle, reacted at 140 DEG C after 12h, product cooling washing is obtained into catalyst；The cobalt ferrite of generation and the mass ratio of silver nitrate
For 1:100；After the product of gained is dried, you can obtain described composite photo-catalyst, most it is named as 1%CoFe at last2O4/
AgI。
The ultrasonic disperse time is 10-30 minutes in the step 1, and ultrasonic power is 90w, and mixing time is 30-60 minutes.
The mixing time of the step 2 is 30-60 minutes.
Mixing time in the step 3 is 50-100 minutes.
Claims (7)
1. a kind of CoFe2O4- AgI composite photo-catalysts, it is characterised in that the composite photo-catalyst is by CoFe2O4It is multiple with AgI
Close, the CoFe2O4Mass fraction be 1~5%, by the CoFe2O4- AgI composite photo-catalysts be used for pair
The photocatalytic degradation of 10mg/L rhodamine B, 98% has been reached in 45 minutes.
2. a kind of CoFe as claimed in claim 12O4The preparation method of-AgI composite photo-catalysts, it is characterised in that step is such as
Under：
Step 1, prepare ferrous acid cobalt granule；
Step 2, ferrous acid cobalt granule is placed in ultrasonic disperse in EG, constant temperature stirring obtains the dispersion liquid A of cobalt ferrite；
Step 3, silver nitrate is added in dispersion liquid A, ultrasound obtains being dissolved with the cobalt ferrite dispersion liquid B of silver nitrate；
Step 4, at a constant temperature, KI is dissolved in EG, and stirring obtains solution C；
Step 5, under conditions of constant temperature and uniform stirring, solution C is added dropwise in dispersion liquid B, continue at a constant temperature
Stirring a period of time, obtain suspension；
Step 6, step 5 gained suspension is transferred in reactor, carries out solvent thermal reaction, it is after completion of the reaction, product is cold
But drying is washed, CoFe is obtained2O4- AgI composite photo-catalysts.
3. a kind of CoFe as claimed in claim 22O4The preparation method of-AgI composite photo-catalysts, it is characterised in that step 2
In, in dispersion liquid A, the amount ratio of the cobalt ferrite and EG is 12~20mg：30mL, the constant temperature is 0~30 DEG C.
4. a kind of CoFe as claimed in claim 22O4The preparation method of-AgI composite photo-catalysts, it is characterised in that step 3
In, in dispersion liquid B, silver nitrate and EG amount ratio are 0.4g：30mL；The silver nitrate ultrasonic time is 10~30 minutes, is surpassed
Acoustical power is 90w, and mixing time is 20~60 minutes.
5. a kind of CoFe as claimed in claim 22O4The preparation method of-AgI composite photo-catalysts, it is characterised in that step 4
In, in solution C, the concentration of the KI is 0.1g/mL, and the constant temperature is 0~30 DEG C, and the mixing time is 20-60 minutes.
6. a kind of CoFe as claimed in claim 22O4The preparation method of-AgI composite photo-catalysts, it is characterised in that step 5
In, the solution C and dispersion liquid B volume ratio are 2~15, and the constant temperature is 0~30 DEG C, and the mixing time is 30-120 points
Clock.
7. a kind of CoFe as claimed in claim 22O4The preparation method of-AgI composite photo-catalysts, it is characterised in that step 6
In, the temperature of the solvent thermal reaction is 140 DEG C, and the time is 12h.
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| CN111701604A (en) * | 2020-06-10 | 2020-09-25 | 河南理工大学 | Preparation method of silver iodide-silver oxide-bismuth oxyhalide-cobalt ferrite magnetic visible-light-driven photocatalyst |
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| CN111701604A (en) * | 2020-06-10 | 2020-09-25 | 河南理工大学 | Preparation method of silver iodide-silver oxide-bismuth oxyhalide-cobalt ferrite magnetic visible-light-driven photocatalyst |
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