CN110465294A - Nanoscale Iron/mesoporous (001) face is compound-flower pattern crystal cladded type TiO2The preparation method of monocrystalline - Google Patents
Nanoscale Iron/mesoporous (001) face is compound-flower pattern crystal cladded type TiO2The preparation method of monocrystalline Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 239000013078 crystal Substances 0.000 title claims abstract description 76
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000000926 separation method Methods 0.000 claims abstract description 15
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007791 liquid phase Substances 0.000 claims abstract description 7
- 230000009467 reduction Effects 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 60
- 239000000243 solution Substances 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 229910052757 nitrogen Inorganic materials 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 26
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- 230000001376 precipitating effect Effects 0.000 claims description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000012279 sodium borohydride Substances 0.000 claims description 12
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 12
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000011737 fluorine Substances 0.000 claims description 10
- 229910052731 fluorine Inorganic materials 0.000 claims description 10
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 claims description 10
- 238000003760 magnetic stirring Methods 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 239000013049 sediment Substances 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 239000010935 stainless steel Substances 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 229910052603 melanterite Inorganic materials 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 5
- 230000002045 lasting effect Effects 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000005284 excitation Effects 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 238000011160 research Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 2
- 210000003850 cellular structure Anatomy 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005067 remediation Methods 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- -1 is centrifugated Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 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
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Abstract
The present invention provides a kind of Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2Monocrystalline, preparation method includes the following steps: mesoporous (001) face-flower pattern crystal cladded type TiO2The preparation of monocrystalline, Nanoscale Iron/mesoporous (001) face be compound-flower pattern crystal cladded type TiO2The preparation of monocrystalline.The present invention prepares mesoporous (001) face-flower pattern crystal cladded type TiO using-two one-step hydrothermal of Template-free method2Monocrystalline, this method effectively reduce pore-creating cost, avoid the releasing process of subsequent complexity.Meso-hole structure and flower pattern crystal morphology are effectively increased specific surface area and the photocatalytic activity site of monocrystalline.By liquid phase reduction (001) face mesoporous middle in-situ preparation Nanoscale Iron crystal grain be made high catalytic activity Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2Monocrystalline；The aerial stability of Nanoscale Iron and inoxidizability are not only effectively improved, so that Nanoscale Iron crystal grain more refines uniformly, the reuniting effect of Nanoscale Iron crystal grain is greatly inhibited, increases the active site of nano-iron material.Meanwhile Nanoscale Iron can promote excitation state TiO2The separation of monocrystalline photo-generate electron-hole enhances photoelectric effect, promotes the raising of photocatalytic activity.
Description
Technical field
It is that a kind of Nanoscale Iron/mesoporous (001) face is multiple the present invention relates to inorganic functional material and fine chemistry industry technology of preparing
Conjunction-flower pattern crystal cladded type TiO2The preparation method of monocrystalline.
Background technique
In conductor photocatalysis material synthesis and Applied research fields, anatase titanium dioxide TiO2Mono-crystalline structures are with its excellent boundary
The advantages such as (crystalline substance) face effect, quick charge transfer efficiency and high activity (001) face have attracted lot of domestic and foreign scholar extensive
Research enthusiasm.However, the anatase titanium dioxide TiO prepared using conventional hydrothermal method2Larger (the micron order of the size of monocrystalline；1 μm -3 μm),
Thus cause its specific surface area lower, photocatalytic activity site is less.To obtain more bigger serface and higher active rutile titania
Type TiO2Monocrystalline, many researchs are developed using reducing single crystal size as starting point with nano-scale dimension (10nm -30nm)
TiO2Monocrystalline.But due to nanoscale effect, so that nanometer-size die usually all has easy to reunite, bad dispersibility defect.It is many
Well known, in the synthesis of catalysis material, meso-hole structure and fold pattern are also to improve its specific surface area, increase active site
Another path of Research.
Mesoporous TiO2Monocrystalline is keeping anatase titanium dioxide TiO2Three-dimensional meso-hole structure is had both on the basis of monocrystalline inherent characteristic, makes it
Specific surface area is bigger, and active site is more, and dielectric property is more excellent.Substrate diffusion, contracting are accelerated during light-catalyzed reaction
The short reaction time and promote electric charge transfer.Currently, being directed to the preparation method of meso-hole structure, generallys use template agent method and carry out structure
It builds.But there is synthesis cost high (synthesis process needs a large amount of template) and work using the method for the synthesising mesoporous monocrystalline of template
The problems such as skill very complicated (template is injected into mould and the subsequent removal of template).In addition to this, the concentration of template, dispersion
Property and compatibility have a very big impact the formation of meso-hole structure, and subsequent template removal process easily leads to cellular structure
Collapsing and destruction.Research is thought, can reduce conjunction using each component interaction property in synthetic system to construct meso-hole structure
At cost, avoid that pore-forming caused by template agent method is unstable, givey disadvantage.
Nanoscale Iron is as a kind of emerging environment remediation engineering material, and which are mainly applied to the reparations of soil and underground water.
The key property that there is Nanoscale Iron common Zero-valent Iron not have, such as: large specific surface area, chemical activity is high, reproducibility is strong, absorption
Ability is strong etc..But due to the high activity that Nanoscale Iron itself has, keep its property stable in the air very poor, contact oxygen after easily by
Oxidation even spontaneous combustion, and due to its nano-scale, keep its easy to reunite, dispersibility is poor in aqueous medium, to limit nanometer
Application of the iron material in practical water treatment technology.Research is thought, Nanoscale Iron is carried on the load that size is larger and property is stable
On body, the composite nano iron material that can keep stablizing and have good dispersion in water solution and separation property in air is prepared
Material, to promoting application of the Nanoscale Iron in environment remediation to have important practical significance and application value.
Summary of the invention
It is above-mentioned to solve the problems, such as, the purpose of the present invention is to provide a kind of Nanoscale Iron/mesoporous (001) face it is compound-
Flower pattern crystal cladded type TiO2The preparation method of monocrystalline, with mesoporous (001) face-flower pattern crystal cladded type TiO2Monocrystalline is carrier, benefit
With its unique meso-hole structure, photoelectric characteristic and chemical property stablize the advantages that, by Nanoscale Iron crystal grain be combined to its it is mesoporous in, system
Standby highlight catalytic active out, excellent photoelectric characteristic can keep stablizing in air, be not easy to be oxidized and have good separation characteristic
Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2Monocrystalline.
To achieve the above object, the technical solution adopted by the present invention is that provide a kind of Nanoscale Iron/mesoporous (001) face it is compound-
Flower pattern crystal cladded type TiO2The preparation method of monocrystalline, method includes the following steps:
The preparation of (1) 0.02 mol/L titanium tetrafluoride solution
At a temperature of 15 DEG C -35 DEG C, 2.478g titanium tetrafluoride is dissolved in the hydrochloric acid solution that 1L concentration is 2 mol/L and obtains pH
=2 concentration are the titanium tetrafluoride solution of 0.02 mol/L；
(2) mesoporous (001) face-flower pattern crystal cladded type TiO2The preparation of monocrystalline
First one-step hydrothermal: by the hydrofluoric acid of the 0.02 mol/L titanium tetrafluoride solution of 50ml-70ml and 0.05 ml-0.1 ml
(mass fraction 40%) is added in 100 ml polytetrafluoroethyllining lining stainless steel autoclaves；It is placed in 180 DEG C of constant temperature in Muffle furnace
6h-8h obtains white solid particle after cooling, precipitating, filtering, 3-5 time wash with distilled water, centrifuge separation, it is dry after i.e. system
Obtain sample X；
Second one-step hydrothermal: by the sample X of 0.5g-1g, the 0.02 mol/L titanium tetrafluoride solution of 50 ml and 10ml-20ml
Isopropanol is added in 100 ml polytetrafluoroethyllining lining stainless steel autoclaves, is placed in 180 DEG C of constant temperature 10h- in Muffle furnace
12h obtains white solid particle after cooling, precipitating, filtering, and 3-5 time wash with distilled water, centrifuge separation, obtain after drying
Sample Y；
Surface fluorine removal and isopropoxy: sample Y obtained is placed in Muffle furnace at 500 DEG C and calcines 90 min-100min, is gone
Except surface fluorine and isopropoxy, mesoporous (001) face-flower pattern crystal cladded type TiO is obtained after cooling2Monocrystalline；
(3) Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2The preparation of monocrystalline
Using liquid phase reduction: to FeSO4Ethanol-water solution system, using be added dropwise strong reductant KBH4Or NaBH4To Fe2+
It carries out restoring obtained Nanoscale Iron crystal grain；
Prepare raw material: FeSO4·7H2O, above-mentioned acquired mesoporous (001) face-flower pattern crystal cladded type TiO2Monocrystalline, NaBH4
Or KBH4, distilled water, dehydrated alcohol, NaOH, nitrogen；
By above-mentioned mesoporous (001) face-flower pattern crystal cladded type TiO obtained of 0.5g-2.0g2The dehydrated alcohol of monocrystalline, 50ml
It is 0.2mol/L FeSO with 100ml concentration4·7H2O aqueous solution is placed in three-necked flask, and sealing is labeled as component A；By component A
It is placed on magnetic stirring apparatus, 10min nitrogen protection is first passed through into three-necked flask, later on magnetic agitation is simultaneously super to component A
Sound disperses 30min, is uniformly mixed component A；After 30min, 20min is staticly settled to component A, removes supernatant, is centrifugated,
Solid sediment is obtained, to obtaining sample M after solid sediment vacuum drying, nitrogen protection is sealed under oxygen free condition,
It is spare；
Prepare the NaBH that 100ml concentration is 0.4mol/L4Or KBH4Solution, and adjusting pH with NaOH is 9-10, and alkalescent is made
NaBH4Or KBH4Solution is labeled as B component；
The dehydrated alcohol of above-mentioned sample M and 60ml is placed in three-necked flask, is sealed and placed on magnetic stirring apparatus, then in nitrogen
It is uniformly mixed under the protection of gas atmosphere, is labeled as component C；The B component of preparation is added dropwise in component C dropwise, rate of addition is
45-60 drop/min, after being added dropwise, lasting stirring and nitrogen protection 40min stand 30min, and filtering obtains black precipitate
Black matrix precipitating particle is washed 3-5 times with dehydrated alcohol, the black precipitate particle after washing is placed in a vacuum drying oven by particle
3h-5h is dried, Nanoscale Iron/mesoporous (001) face for obtaining black is compound-flower pattern crystal cladded type TiO2Monocrystalline, nitrogen protection,
It is sealed under anaerobic.
Effect of the invention: 1, Nanoscale Iron of the present invention/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2Monocrystalline exists
On the basis of keeping Nanoscale Iron high activity, by Nanoscale Iron grain dispersion in mesoporous, its aerial stabilization is not only increased
Property and inoxidizability, and the reuniting effect of Nanoscale Iron is greatly inhibited, increase the active site of Nanoscale Iron.
2, Nanoscale Iron of the present invention/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2Nanoscale Iron crystal grain in monocrystalline exists
It can not only promote the separation of photo-generate electron-hole in light-catalyzed reaction, enhance TiO2The photoelectric effect of monocrystalline, and can extend
TiO2Spectral response range, promote to generate more hydroxyl radical free radicals, improve photocatalytic activity.
3, Nanoscale Iron of the present invention/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2The particle size range of monocrystalline be 3 μm-
5 μm, (001) face it is mesoporous in compound Nanoscale Iron particle size range be 30 nm -50nm, specific surface area is up to 450 m2/g -
650 m2/g。
4, in mesoporous (001) face-flower pattern crystal cladded type TiO2- two step hydro-thermal of Template-free method is used during single crystal preparation
Method manufactures meso-hole structure and flower pattern crystal simultaneously, not only reduces pore-creating cost, and effectively avoids subsequent very complicated
Knockout course, solve the problems, such as tunnel collapse caused by template agent removing process, greatly ensure that cellular structure and bone
The integrality of frame.
5, the Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2Monocrystalline does not glue in liquid phase reaction course
It pays in reactor surface, which can be recycled using miillpore filter (0.22 μm -0.45 μm), the rate of recovery, and will not up to 100%
Cause fouling membrane.
Detailed description of the invention
Fig. 1 be Nanoscale Iron of the present invention/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2The structural simulation figure of monocrystalline.
Fig. 2 be Nanoscale Iron of the present invention/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2The SEM of monocrystalline schemes.
Specific embodiment
In conjunction with the following example it is compound to Nanoscale Iron of the present invention/mesoporous (001) face-flower pattern crystal cladded type TiO2Monocrystalline
Preparation method is illustrated.
1 Nanoscale Iron load capacity of embodiment be 30% Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2It is single
Brilliant preparation
The preparation of (1) 0.02 mol/L titanium tetrafluoride solution
At a temperature of 15 DEG C -35 DEG C, 2.478g titanium tetrafluoride is dissolved in the hydrochloric acid solution that 1L concentration is 2 mol/L and obtains pH
=2 concentration are the titanium tetrafluoride solution of 0.02 mol/L；
(2) mesoporous (001) face-flower pattern crystal cladded type TiO2The preparation of monocrystalline
First one-step hydrothermal: by the 0.02 mol/L titanium tetrafluoride solution of 70ml and the hydrofluoric acid (mass fraction of 0.07 ml
40%) it is added in 100 ml polytetrafluoroethyllining lining stainless steel autoclaves；180 DEG C of constant temperature 7h in Muffle furnace are placed in, cool down,
Obtain white solid particle after precipitating, filtering, 4 times wash with distilled water, centrifuge separation, it is dry after obtain sample X；
Second one-step hydrothermal: the isopropanol of the sample X of 0.8g, the 0.02 mol/L titanium tetrafluoride solution of 50 ml and 20ml are added
Enter into 100 ml polytetrafluoroethyllining lining stainless steel autoclaves, is placed in Muffle furnace 180 DEG C of constant temperature 12h, it is cooling, heavy
Form sediment, obtain white solid particle after filtering, 4 times wash with distilled water, centrifuge separation, it is dry after obtain sample Y；
Surface fluorine removal and isopropoxy: sample Y obtained being placed in Muffle furnace at 500 DEG C and calcines 90 min, removes surface
Fluorine and isopropoxy obtain mesoporous (001) face-flower pattern crystal cladded type TiO after cooling2Monocrystalline；
(3) Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2The preparation of monocrystalline
Using liquid phase reduction: to FeSO4Ethanol-water solution system, using be added dropwise strong reductant KBH4Or NaBH4To Fe2+
It carries out restoring obtained Nanoscale Iron crystal grain；
Prepare raw material: FeSO4·7H2O, above-mentioned acquired mesoporous (001) face-flower pattern crystal cladded type TiO2Monocrystalline, NaBH4
Or KBH4, distilled water, dehydrated alcohol, NaOH, nitrogen；
By above-mentioned mesoporous (001) face-flower pattern crystal cladded type TiO obtained of 0.8g2Monocrystalline, 50ml dehydrated alcohol with
100ml concentration is 0.2mol/L FeSO4·7H2O aqueous solution is placed in three-necked flask, and sealing is labeled as component A；Component A is set
In on magnetic stirring apparatus, being first passed through 10min nitrogen protection into three-necked flask, later on magnetic agitation is simultaneously ultrasonic to component A
Disperse 30min, is uniformly mixed component A；After 30min, 20min is staticly settled to component A, removes supernatant, it is heavy to obtain solid
Starch is centrifugated solid sediment, obtains sample M after vacuum drying, nitrogen protection, is sealed under oxygen free condition,
It is spare；
Prepare the NaBH that 100ml concentration is 0.4mol/L4Or KBH4Solution, and adjusting pH with NaOH is 9, and alkalescent NaBH is made4
Or KBH4Solution is labeled as B component；
The dehydrated alcohol of above-mentioned sample M and 60ml is placed in three-necked flask, is sealed and placed on magnetic stirring apparatus, then in nitrogen
It is uniformly mixed under the protection of gas atmosphere, is labeled as component C；The B component of preparation is added dropwise in component C dropwise, rate of addition is
50 drops/min, after being added dropwise, lasting stirring and nitrogen protection 40min stand 30min, and filtering obtains black precipitate
Black matrix precipitating particle is washed 4 times with dehydrated alcohol, the black precipitate particle after washing is placed in a vacuum drying oven drying by grain
5h, obtain black Nanoscale Iron load capacity be 30% Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2It is single
Crystalline substance, nitrogen protection are sealed under anaerobic.
2 Nanoscale Iron load capacity of embodiment be 50% Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2It is single
Brilliant preparation
The preparation of (1) 0.02 mol/L titanium tetrafluoride solution
At a temperature of 15 DEG C -35 DEG C, 2.478g titanium tetrafluoride is dissolved in the hydrochloric acid solution that 1L concentration is 2 mol/L and obtains pH
=2 concentration are the titanium tetrafluoride solution of 0.02 mol/L；
(2) mesoporous (001) face-flower pattern crystal cladded type TiO2The preparation of monocrystalline
First one-step hydrothermal: by the 0.02 mol/L titanium tetrafluoride solution of 70ml and the hydrofluoric acid (mass fraction of 0.07 ml
40%) it is added in 100 ml polytetrafluoroethyllining lining stainless steel autoclaves；180 DEG C of constant temperature 7h in Muffle furnace are placed in, cool down,
Obtain white solid particle after precipitating, filtering, 4 times wash with distilled water, centrifuge separation, it is dry after obtain sample X；
Second one-step hydrothermal: the isopropanol of the sample X of 0.8g, the 0.02 mol/L titanium tetrafluoride solution of 50 ml and 20ml are added
Enter into 100 ml polytetrafluoroethyllining lining stainless steel autoclaves, is placed in Muffle furnace 180 DEG C of constant temperature 12h, it is cooling, heavy
Form sediment, obtain white solid particle after filtering, 4 times wash with distilled water, centrifuge separation, it is dry after obtain sample Y；
Surface fluorine removal and isopropoxy: sample Y obtained being placed in Muffle furnace at 500 DEG C and calcines 90 min, removes surface
Fluorine and isopropoxy obtain mesoporous (001) face-flower pattern crystal cladded type TiO after cooling2Monocrystalline；
(3) Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2The preparation of monocrystalline
Using liquid phase reduction: to FeSO4Ethanol-water solution system, using be added dropwise strong reductant KBH4Or NaBH4To Fe2+
It carries out restoring obtained Nanoscale Iron crystal grain；
Prepare raw material: FeSO4·7H2O, above-mentioned acquired mesoporous (001) face-flower pattern crystal cladded type TiO2Monocrystalline, NaBH4
Or KBH4, distilled water, dehydrated alcohol, NaOH, nitrogen；
By above-mentioned mesoporous (001) face-flower pattern crystal cladded type TiO obtained of 0.8g2Monocrystalline, 50ml dehydrated alcohol with
100ml concentration is 0.6mol/L FeSO4·7H2O aqueous solution is placed in three-necked flask, and sealing is labeled as component A；Component A is set
In on magnetic stirring apparatus, being first passed through 10min nitrogen protection into three-necked flask, later on magnetic agitation is simultaneously ultrasonic to component A
Disperse 30min, is uniformly mixed component A；After 30min, 20min is staticly settled to component A, removes supernatant, it is heavy to obtain solid
Starch is centrifugated solid sediment, obtains sample M after vacuum drying, nitrogen protection, is sealed under oxygen free condition,
It is spare；
Prepare the NaBH that 100ml concentration is 0.4mol/L4Or KBH4Solution, and adjusting pH with NaOH is 9, and alkalescent NaBH is made4
Or KBH4Solution is labeled as B component；
The dehydrated alcohol of above-mentioned sample M and 60ml is placed in three-necked flask, is sealed and placed on magnetic stirring apparatus, then in nitrogen
It is uniformly mixed under the protection of gas atmosphere, is labeled as component C；The B component of preparation is added dropwise in component C dropwise, rate of addition is
50 drops/min, after being added dropwise, lasting stirring and nitrogen protection 40min stand 30min, and filtering obtains black precipitate
Black matrix precipitating particle is washed 4 times with dehydrated alcohol, the black precipitate particle after washing is placed in a vacuum drying oven drying by grain
5h, obtain black Nanoscale Iron load capacity be 50% Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2It is single
Crystalline substance, nitrogen protection are sealed under anaerobic.
3 Nanoscale Iron load capacity of embodiment be 80% Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2It is single
Brilliant preparation
The preparation of (1) 0.02 mol/L titanium tetrafluoride solution
At a temperature of 15 DEG C -35 DEG C, 2.478g titanium tetrafluoride is dissolved in the hydrochloric acid solution that 1L concentration is 2 mol/L and obtains pH
=2 concentration are the titanium tetrafluoride solution of 0.02 mol/L；
(2) mesoporous (001) face-flower pattern crystal cladded type TiO2The preparation of monocrystalline
First one-step hydrothermal: by the 0.02 mol/L titanium tetrafluoride solution of 70ml and the hydrofluoric acid (mass fraction of 0.07 ml
40%) it is added in 100 ml polytetrafluoroethyllining lining stainless steel autoclaves；180 DEG C of constant temperature 7h in Muffle furnace are placed in, cool down,
Obtain white solid particle after precipitating, filtering, 4 times wash with distilled water, centrifuge separation, it is dry after obtain sample X；
Second one-step hydrothermal: the isopropanol of the sample X of 0.8g, the 0.02 mol/L titanium tetrafluoride solution of 50 ml and 20ml are added
Enter into 100 ml polytetrafluoroethyllining lining stainless steel autoclaves, is placed in Muffle furnace 180 DEG C of constant temperature 12h, it is cooling, heavy
Form sediment, obtain white solid particle after filtering, 4 times wash with distilled water, centrifuge separation, it is dry after obtain sample Y；
Surface fluorine removal and isopropoxy: sample Y obtained being placed in Muffle furnace at 500 DEG C and calcines 90 min, removes surface
Fluorine and isopropoxy obtain mesoporous (001) face-flower pattern crystal cladded type TiO after cooling2Monocrystalline；
(3) Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2The preparation of monocrystalline
Using liquid phase reduction: to FeSO4Ethanol-water solution system, using be added dropwise strong reductant KBH4Or NaBH4To Fe2+
It carries out restoring obtained Nanoscale Iron crystal grain；
Prepare raw material: FeSO4·7H2O, above-mentioned acquired mesoporous (001) face-flower pattern crystal cladded type TiO2Monocrystalline, NaBH4
Or KBH4, distilled water, dehydrated alcohol, NaOH, nitrogen；
By above-mentioned mesoporous (001) face-flower pattern crystal cladded type TiO obtained of 0.8g2Monocrystalline, 50ml dehydrated alcohol with
100ml concentration is 2mol/L FeSO4·7H2O aqueous solution is placed in three-necked flask, and sealing is labeled as component A；Component A is placed in
On magnetic stirring apparatus, 10min nitrogen protection is first passed through into three-necked flask, later on magnetic agitation simultaneously divides component A ultrasound
30min is dissipated, component A is uniformly mixed；After 30min, 20min is staticly settled to component A, removes supernatant, obtains solid precipitating
Object is centrifugated solid sediment, obtains sample M after vacuum drying, nitrogen protection, is sealed under oxygen free condition, standby
With；
Prepare the NaBH that 100ml concentration is 0.4mol/L4Or KBH4Solution, and adjusting pH with NaOH is 9, and alkalescent NaBH is made4
Or KBH4Solution is labeled as B component；
The dehydrated alcohol of above-mentioned sample M and 60ml is placed in three-necked flask, is sealed and placed on magnetic stirring apparatus, then in nitrogen
It is uniformly mixed under the protection of gas atmosphere, is labeled as component C；The B component of preparation is added dropwise in component C dropwise, rate of addition is
50 drops/min, after being added dropwise, lasting stirring and nitrogen protection 40min stand 30min, and filtering obtains black precipitate
Black matrix precipitating particle is washed 4 times with dehydrated alcohol, the black precipitate particle after washing is placed in a vacuum drying oven drying by grain
5h, obtain black Nanoscale Iron load capacity be 80% Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2It is single
Crystalline substance, nitrogen protection are sealed under anaerobic.
Claims (4)
- A kind of Nanoscale Iron/mesoporous 1. (001) face is compound-flower pattern crystal cladded type TiO2The preparation method of monocrystalline, this method include with Lower step:The preparation of (1) 0.02 mol/L titanium tetrafluoride solutionAt a temperature of 15 DEG C -35 DEG C, 2.478g titanium tetrafluoride is dissolved in the hydrochloric acid solution that 1L concentration is 2 mol/L and obtains pH =2 concentration are the titanium tetrafluoride solution of 0.02 mol/L；(2) mesoporous (001) face-flower pattern crystal cladded type TiO2The preparation of monocrystallineFirst one-step hydrothermal: by the hydrofluoric acid of the 0.02 mol/L titanium tetrafluoride solution of 50ml-70ml and 0.05 ml-0.1 ml (mass fraction 40%) is added in 100 ml polytetrafluoroethyllining lining stainless steel autoclaves；It is placed in 180 DEG C of constant temperature in Muffle furnace 6h-8h obtains white solid particle after cooling, precipitating, filtering, 3-5 time wash with distilled water, centrifuge separation, it is dry after i.e. system Obtain sample X；Second one-step hydrothermal: by the sample X of 0.5g-1g, the 0.02 mol/L titanium tetrafluoride solution of 50 ml and 10ml-20ml Isopropanol is added in 100 ml polytetrafluoroethyllining lining stainless steel autoclaves, is placed in 180 DEG C of constant temperature 10h- in Muffle furnace 12h obtains white solid particle after cooling, precipitating, filtering, and 3-5 time wash with distilled water, centrifuge separation, obtain after drying Sample Y；Surface fluorine removal and isopropoxy: sample Y obtained is placed in Muffle furnace at 500 DEG C and calcines 90 min-100min, is gone Except surface fluorine and isopropoxy, mesoporous (001) face-flower pattern crystal cladded type TiO is obtained after cooling2Monocrystalline；(3) Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2The preparation of monocrystallineUsing liquid phase reduction: to FeSO4Ethanol-water solution system, using be added dropwise strong reductant KBH4Or NaBH4To Fe2+Into Row, which restores, is made Nanoscale Iron crystal grain；Prepare raw material: FeSO4·7H2O, above-mentioned acquired mesoporous (001) face-flower pattern crystal cladded type TiO2Monocrystalline, NaBH4 Or KBH4, distilled water, dehydrated alcohol, NaOH, nitrogen；By above-mentioned mesoporous (001) face-flower pattern crystal cladded type TiO obtained of 0.5g-2.0g2Monocrystalline, 50ml dehydrated alcohol with 100ml concentration is 0.2mol/L FeSO4·7H2O aqueous solution is placed in three-necked flask, and sealing is labeled as component A；Component A is set In on magnetic stirring apparatus, being first passed through 10min nitrogen protection into three-necked flask, later on magnetic agitation is simultaneously ultrasonic to component A Disperse 30min, is uniformly mixed component A；After 30min, 20min is staticly settled to component A, removes supernatant, centrifuge separation obtains Solid sediment, to obtaining sample M after solid sediment vacuum drying, nitrogen protection is sealed under oxygen free condition, standby With；Prepare the NaBH that 100ml concentration is 0.4mol/L4Or KBH4Solution, and adjusting pH with NaOH is 9-10, and alkalescent is made NaBH4Or KBH4Solution is labeled as B component；The dehydrated alcohol of above-mentioned sample M and 60ml is placed in three-necked flask, is sealed and placed on magnetic stirring apparatus, then in nitrogen It is uniformly mixed under the protection of gas atmosphere, is labeled as component C；The B component of preparation is added dropwise in component C dropwise, rate of addition is 45-60 drop/min, after being added dropwise, lasting stirring and nitrogen protection 40min stand 30min, and filtering obtains black precipitate Black matrix precipitating particle is washed 3-5 times with dehydrated alcohol, the black precipitate particle after washing is placed in a vacuum drying oven by particle 3h-5h is dried, Nanoscale Iron/mesoporous (001) face for obtaining black is compound-flower pattern crystal cladded type TiO2Monocrystalline, nitrogen protection, It is sealed under anaerobic.
- Nanoscale Iron according to claim 1/mesoporous 2. (001) face is compound-flower pattern crystal cladded type TiO2The preparation side of monocrystalline Method, it is characterized in that: mesoporous (001) face of described being made-flower pattern crystal cladded type TiO2The method of monocrystalline is-two step of Template-free method Hydro-thermal method, this method make the action characteristic of crystal face by control hydrofluoric acid and isopropanol in the case where template is not used Hole not only reduces pore-creating cost, and effectively avoids the knockout course of subsequent very complicated, solves template agent removing Caused by process the problem of tunnel collapse.
- Nanoscale Iron according to claim 1/mesoporous 3. (001) face is compound-flower pattern crystal cladded type TiO2The preparation side of monocrystalline Method, it is characterized in that: the obtained Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2(001) face of monocrystalline is Meso-hole structure, (100) face and (010) face are coated by flower pattern crystal.
- Nanoscale Iron according to claim 1/mesoporous 4. (001) face is compound-flower pattern crystal cladded type TiO2The preparation side of monocrystalline Method, it is characterized in that: the obtained Nanoscale Iron/mesoporous (001) face it is compound-flower pattern crystal cladded type TiO2The particle size range of monocrystalline is 3 μm -5 μm, (001) face it is mesoporous in compound Nanoscale Iron particle size range be 30 nm -50nm, specific surface area is 450 m2/g- 650 m2/g。
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