CN106994345B - A kind of particle self assembly TiO2/Fe2O3The preparation method of chain composite granule - Google Patents
A kind of particle self assembly TiO2/Fe2O3The preparation method of chain composite granule Download PDFInfo
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- CN106994345B CN106994345B CN201710361734.6A CN201710361734A CN106994345B CN 106994345 B CN106994345 B CN 106994345B CN 201710361734 A CN201710361734 A CN 201710361734A CN 106994345 B CN106994345 B CN 106994345B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000002245 particle Substances 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000008187 granular material Substances 0.000 title claims abstract description 17
- 238000001338 self-assembly Methods 0.000 title claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000004471 Glycine Substances 0.000 claims abstract description 16
- 235000019441 ethanol Nutrition 0.000 claims abstract description 16
- 239000010936 titanium Substances 0.000 claims abstract description 12
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 12
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical group [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 10
- 229960004756 ethanol Drugs 0.000 claims description 9
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical group [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000012805 post-processing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000004408 titanium dioxide Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 abstract description 3
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 13
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000002604 ultrasonography Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 150000001875 compounds Chemical group 0.000 description 3
- 238000000921 elemental analysis Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005308 ferrimagnetism Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/39—
Abstract
A kind of particle self assembly TiO2/Fe2O3The preparation method of chain composite granule is related to magnetic carrying of titanium dioxide preparation technical field.The present invention prepares particle self assembly TiO using titanium source, soluble ferric iron salt, glycine as reaction raw materials, by hydro-thermal reaction2/Fe2O3Chain composite granule.Titanium source is dissolved in ethyl alcohol, soluble ferric iron salt, glycine and water is then added, is transferred in reaction kettle after mixing and carries out hydrothermal synthesis reaction, obtained after post treatment after fully reacting.The present invention successfully obtains a kind of magnetic coupling chain material of titanium dichloride load by glycine biomolecule assisting alcohol-hydrothermal method.By serial experiment the result shows that can successfully prepare magnetic titanium dioxide nanometer chain composite granule as template and raw material by glycine, have the characteristics that narrower particle size distribution, topographic profile are uniform and controllable.
Description
Technical field
The present invention relates to magnetic carrying of titanium dioxide preparation technical fields, are specifically related to a kind of particle self assembly TiO2/Fe2O3
The preparation method of chain composite granule.
Background technique
In photocatalysis field, TiO2Photocatalytic activity is high, and chemical property stablizes (acid and alkali-resistance and chemical attack), visible
Light area can be made into white block or transparent membrane without absorption, and raw material sources are abundant, inexpensively, do not generate secondary pollution.But due to receiving
Rice TiO2Particle is subtle, is not easy precipitating and difficult recycling, and active ingredient loss is big, is unfavorable for the regeneration and recycling of catalyst.Therefore
Realize that this technology is applied to large-scale water process, it is necessary to the recycling for solving the problems, such as photochemical catalyst, it is magnetic herein by preparation
Photochemical catalyst facilitates using magnetic separation technique and recycles fastly, so that it had not only been able to maintain higher photocatalytic activity, but also can be repeatedly
Regeneration, therefore magnetic carrier is prepared a large amount of concerns.
There are many method for preparing magnetic carrying of titanium dioxide at present.Watson etc. has synthesized ferrimagnetism using liquid phase deposition
Material, and high-temperature process magnetic composite is had studied to TiO2The influence of light phase transfer and photocatalytic activity；Chen and Gao etc.
Report is led by the method preparation of sol-gel with magnetic γ-Fe respectively2O3As carrier TiO2Magnetic conduction photochemical catalyst, research report
When at road heat, when calcination temperature is more than 400 DEG C, γ-Fe2O3α-Fe can mutually be become rapidly2O3, to influence photocatalysis performance
And magnetic property；State university of communications Zhan Zongcheng et al. prepares Mn-Fe oxysome with chemical coprecipitation, and ethyl orthosilicate is precursor
Multiple coated Si O is carried out to it2, obtain fine and close SiO2The Mn-Fe oxysome soft magnetism carrier of protective layer.These report that majorities are all
Synthesize magnetic carrying of titanium dioxide receive, micron particles, synthesize particle self assembly TiO2/Fe2O3Chain composite granule rarely has report
Road.
It is raw material that the present invention, which mainly passes through ferrocene, glycine, water, ethyl alcohol and four fourth rouge of metatitanic acid, is obtained using hydro-thermal method
The TiO of particle self assembly2/Fe2O3Chain powder.
Summary of the invention
For presently, there are above-mentioned technical problem, the present invention provides a kind of simple process, it is at low cost, be suitble to industrialization
The particle self assembly TiO of large-scale production2/Fe2O3The preparation method of chain composite granule.
To achieve the goals above, the technical scheme adopted by the invention is as follows: a kind of particle self assembly TiO2/Fe2O3Chain
The preparation method of composite granule prepares particle certainly by hydro-thermal reaction using titanium source, soluble ferric iron salt, glycine as reaction raw materials
Assemble TiO2/Fe2O3Chain composite granule.
As the preferred technical solution of the present invention, titanium source is dissolved in ethyl alcohol, soluble ferric iron salt, glycine is then added
And water, it is transferred in reaction kettle after mixing and carries out hydrothermal synthesis reaction, obtain particle after fully reacting after post treatment from group
Fill TiO2/Fe2O3Chain composite granule.
As present invention further optimization technical solution, titanium source is butyl titanate, soluble ferric iron salt be ferrocene or
Its derivative.Molar ratio between butyl titanate, ferrocene and glycine is 0.5~1:3.5~4.5:8~12, metatitanic acid four
The molar concentration of butyl titanate is 0.05~0.1mol/L in butyl ester/ethanol system, the volume ratio of ethyl alcohol and water is 1.5~
2.5:1.The hydrothermal synthesis reaction time is 12~36h, and reaction temperature is 160~200 DEG C.Post-processing is the powder that will be generated after reaction
End is centrifuged with centrifuge, and with dehydrated alcohol and deionized water, alternately powder after washing for several times, is put into constant temperature and done by washing respectively
Dry 4~10h in dry case, drying temperature are 30~60 DEG C.
The present invention successfully obtains a kind of magnetism of titanium dichloride load by glycine biomolecule assisting alcohol-hydrothermal method
Compound chain material.By serial experiment the result shows that can successfully prepare magnetic dioxy as template and raw material by glycine
Change titanium nanometer chain composite granule, has the characteristics that narrower particle size distribution, topographic profile are uniform and controllable.
Compared with prior art, the invention has the following advantages that
1) it is presoma that, the present invention, which is realized using glycine and ferrocene, and hydro-thermal method quickly obtains titanium dichloride load
Magnetic coupling chain material.Simple process, entire preparation system be easy building, easy to operate, condition is easily-controllable, it is low in cost,
Product composition it is easily-controllable, product is evenly distributed, it is not easy to reunite, be suitable for large-scale industrial production.
2), the present invention is not add other auxiliary during the preparation process as reactant using conventional soluble molysite
The by-product of substance, generation is few, and environmental pollution is smaller, is a kind of environment-friendly type synthesis technology.
3), product prepared by the present invention has many advantages, such as that photocatalytic activity is high, carries out separation easily to be recycled, and energy is wide
It is general to apply in fields such as sewage treatment, sterilizings.
Detailed description of the invention
With reference to embodiments with attached drawing to particle self assembly TiO of the invention2/Fe2O3The preparation side of chain composite granule
Method, which is made, to be discussed further.
Fig. 1 is the FE-SEM figure of 1 products therefrom of embodiment (a, b respectively indicate low, high magnification).
Fig. 2 is the FE-SEM figure of 2 products therefrom of embodiment (a, b respectively indicate low, high magnification).
Fig. 3 is the FE-SEM figure of 3 products therefrom of embodiment (a, b, c respectively indicate basic, normal, high multiplying power).
Fig. 4 is elemental analysis (EDS) figure of 3 products therefrom of embodiment.
Specific embodiment
Embodiment 1: partial size is the particle self assembly Fe of 50nm2O3Chain powder.
(1) first with second alcohol and water the instrument clean to be used one time, then pass through electronics day with 50mL small beaker
The flat ferrocene for weighing 4mmoL, 10mmoL glycine weigh 10mL ethyl alcohol with graduated cylinder, and 5mL water is added in small beaker, are formed
Solution A；It is placed on magnetic stirring apparatus after being stirred about 1h, forms solution B.
(2) mixed liquor after stirring is transferred in 25mL reaction kettle washed in advance；Reaction kettle is covered and is put into constant temperature air blast
In drying box, setting temperature is 180 DEG C, reacts 36h；To after reaction, take out reaction kettle, the powder generated after reaction is used
Centrifuge centrifugation, and alternately washed for several times with dehydrated alcohol and deionized water respectively, then 60 DEG C of dry 6h obtain yellow Fe2O3Powder
End.
Fig. 1 is the FE-SEM figure of 1 products therefrom of embodiment (a, b respectively indicate low, high magnification).Obtained by known to Fig. 1 a
Fe2O3Morphology microstructure is uniform, is in chain structure, is assembled by tiny particle, average particle size 50nm, and crystallinity
It is good；The particle surface obtained known to FE-SEM Fig. 1 b of high power is smooth, is in small club shaped structure.
Embodiment 2: partial size is the particle self assembly Fe of 200nm2O3Chain powder.
(1) first with second alcohol and water the instrument clean to be used one time, then pass through electronics day with 50mL small beaker
The flat ferrocene for weighing 4mmoL, 10mmoL glycine weigh 12mL ethyl alcohol with graduated cylinder, and 3mL water is added in small beaker, are formed
Solution A；It is placed on magnetic stirring apparatus after being stirred about 1h, forms solution B.
(2) mixed liquor after stirring is transferred in 25mL reaction kettle washed in advance；Reaction kettle is covered and is put into constant temperature air blast
In drying box, setting temperature is 180 DEG C, reacts 36h；To after reaction, take out reaction kettle, the powder generated after reaction is used
Centrifuge centrifugation, and alternately washed for several times with dehydrated alcohol and deionized water respectively, then 60 DEG C of dry 6h obtain yellow Fe2O3Powder
End.
Fig. 2 is the FE-SEM figure of 2 products therefrom of embodiment (a, b respectively indicate low, high magnification).Obtained by known to Fig. 2 a
Fe2O3Morphology microstructure is less uniform, and particle dispersion is bad, varies, but particle is in coccoid average particle size
200nm, and good crystallinity；The most of particle obtained known to FE-SEM Fig. 2 b of high power is spherical in rule, and most of
Rough is assembled by more tiny nano particle.
Embodiment 3: partial size is the particle self assembly Fe of 50nm2O3/TiO2Compound chain powder
(1) first with second alcohol and water the instrument clean to be used one time, the titanium of 0.224g is weighed by electronic balance
Sour four fourth rouge (attention tries not to encounter water) are put into 50mL small beaker, are then weighed 10mL ethyl alcohol with graduated cylinder and are poured into small burning
In cup, it is put into ultrasound 5min in ultrasonic cleaner, forms solution A；Then 4mmol ferrocene is weighed, 10mmol glycine,
5mL water is added thereto, and forms solution B；Solution B is finally placed on magnetic stirring apparatus and is stirred general 1h formation solution C.
(2) mixed liquor after ultrasound is transferred in 25mL reaction kettle washed in advance, reaction kettle is covered and is put into constant temperature air blast
In drying box, setting temperature is 180 DEG C, reacts 36h；To after reaction, take out reaction kettle, the powder generated after reaction is used
Centrifuge centrifugation, and with dehydrated alcohol and deionized water, alternately powder after washing for several times, is put into thermostatic drying chamber by washing respectively
In, setting temperature is 40 DEG C, and dry 6h obtains dried powder.
Fig. 3 is the FE-SEM figure of 3 products therefrom of embodiment (a, b, c respectively indicate basic, normal, high multiplying power).From Fig. 3 a
Obtained Fe2O3/TiO2Composite granule pattern is uniform, and particle dispersion is preferable, be in chain structure, average grain diameter 50nm,
And good crystallinity；Schemed by the FE-SEM of middle and high multiplying power it is found that Fe2O3/TiO2The chain structure of composite granule is by more tiny
Nano particle assembles.Fig. 4 is elemental analysis (EDS) figure of 3 products therefrom of embodiment, and the product obtained as seen from Figure 4 is all
Be particle assembling chain structure, and by elemental analysis (EDS) know obtained chain product be by Fe, Ti and O this
What three kinds of elements were constituted, Cu comes from the substrate for doing scanning electron microscope.
Embodiment 4: particle self assembly Fe2O3/TiO2The preparation of compound chain powder
(1) first with second alcohol and water the instrument clean to be used one time, the titanium of 0.169g is weighed by electronic balance
Sour four fourth rouge (attention tries not to encounter water) are put into 50mL small beaker, are then weighed 10mL ethyl alcohol with graduated cylinder and are poured into small burning
In cup, it is put into ultrasound 5min in ultrasonic cleaner, forms solution A；Then 3.5mmol ferrocene, the sweet ammonia of 12mmol are weighed
Acid, 6.5mL water are added thereto, and form solution B；Solution B is finally placed on magnetic stirring apparatus and is stirred general 1h formation solution
C。
(2) mixed liquor after ultrasound is transferred in 25mL reaction kettle washed in advance, reaction kettle is covered and is put into constant temperature air blast
In drying box, setting temperature is 200 DEG C, reacts 12h；To after reaction, take out reaction kettle, the powder generated after reaction is used
Centrifuge centrifugation, and with dehydrated alcohol and deionized water, alternately powder after washing for several times, is put into thermostatic drying chamber by washing respectively
In, setting temperature is 60 DEG C, and dry 4h obtains dried powder.
Embodiment 5: particle self assembly Fe2O3/TiO2The preparation of compound chain powder
(1) first with second alcohol and water the instrument clean to be used one time, the titanium of 0.3424g is weighed by electronic balance
Sour four fourth rouge (attention tries not to encounter water) are put into 50mL small beaker, are then weighed 10mL ethyl alcohol with graduated cylinder and are poured into small burning
In cup, it is put into ultrasound 5min in ultrasonic cleaner, forms solution A；Then 4.5mmol ferrocene, the sweet ammonia of 8mmol are weighed
Acid, 4mL water are added thereto, and form solution B；Solution B is finally placed on magnetic stirring apparatus and is stirred general 1h formation solution C.
(2) mixed liquor after ultrasound is transferred in 25mL reaction kettle washed in advance, reaction kettle is covered and is put into constant temperature air blast
In drying box, setting temperature is 160 DEG C, reacts 30h；To after reaction, take out reaction kettle, the powder generated after reaction is used
Centrifuge centrifugation, and with dehydrated alcohol and deionized water, alternately powder after washing for several times, is put into thermostatic drying chamber by washing respectively
In, setting temperature is 30 DEG C, and dry 10h obtains dried powder.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (3)
1. a kind of particle self assembly TiO2/Fe2O3The preparation method of chain composite granule, which is characterized in that titanium source is dissolved in second
In alcohol, soluble ferric iron salt, glycine and water is then added, is transferred in reaction kettle after mixing and carries out hydrothermal synthesis reaction, instead
Particle self assembly TiO is obtained after post treatment after answering completely2/Fe2O3Chain composite granule；
Titanium source is butyl titanate, and soluble ferric iron salt is ferrocene or derivatives thereof；
Molar ratio between butyl titanate, ferrocene and glycine is 0.5~1: 3.5~4.5: 8~12, butyl titanate/
The molar concentration of butyl titanate is 0.05~0.1mol/L in ethanol system, and the volume ratio of ethyl alcohol and water is 1.5~2.5: 1；
The hydrothermal synthesis reaction time is 12~36h, and reaction temperature is 160~200 DEG C.
2. preparation method as described in claim 1, which is characterized in that post-processing is the powder centrifuge that will be generated after reaction
Centrifugation, and with dehydrated alcohol and deionized water, alternately washing for several times, powder after washing is put into thermostatic drying chamber dry respectively.
3. preparation method as claimed in claim 2, which is characterized in that drying time is 4~10h in thermostatic drying chamber, dry
Temperature is 30~60 DEG C.
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| CN107961803B (en) * | 2017-12-12 | 2020-10-09 | 北京众智创新科技开发有限公司 | Organic-inorganic composite photocatalyst for purifying environmental pollution |
| CN107983353B (en) * | 2017-12-22 | 2020-05-01 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | TiO 22-Fe2O3Preparation method and application of composite powder |
| CN108525665A (en) * | 2018-04-08 | 2018-09-14 | 合肥学院 | A kind of mesoporous γ-Fe2O3/TiO2The preparation method of the difunctional complex microsphere of magnetic/catalysis |
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| CN106517353A (en) * | 2016-11-02 | 2017-03-22 | 绥化学院 | Preparation method of alpha-Fe2O3/TiO2 nano-composite gas sensing material |
| CN108525665A (en) * | 2018-04-08 | 2018-09-14 | 合肥学院 | A kind of mesoporous γ-Fe2O3/TiO2The preparation method of the difunctional complex microsphere of magnetic/catalysis |
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| CN102824884A (en) * | 2012-05-14 | 2012-12-19 | 无锡润鹏复合新材料有限公司 | TiO2/Fe2O3 composite hollow microsphere and preparation method thereof |
| CN106517353A (en) * | 2016-11-02 | 2017-03-22 | 绥化学院 | Preparation method of alpha-Fe2O3/TiO2 nano-composite gas sensing material |
| CN108525665A (en) * | 2018-04-08 | 2018-09-14 | 合肥学院 | A kind of mesoporous γ-Fe2O3/TiO2The preparation method of the difunctional complex microsphere of magnetic/catalysis |
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