CN107159211A - A kind of preparation method of nanometer of UV Fenton composite - Google Patents
A kind of preparation method of nanometer of UV Fenton composite Download PDFInfo
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- CN107159211A CN107159211A CN201710548493.6A CN201710548493A CN107159211A CN 107159211 A CN107159211 A CN 107159211A CN 201710548493 A CN201710548493 A CN 201710548493A CN 107159211 A CN107159211 A CN 107159211A
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- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 29
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 16
- 238000005457 optimization Methods 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000011790 ferrous sulphate Substances 0.000 claims description 8
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 8
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 8
- 229920005610 lignin Polymers 0.000 claims description 8
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 8
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 12
- 239000010902 straw Substances 0.000 abstract description 12
- 240000008042 Zea mays Species 0.000 abstract description 11
- 235000002017 Zea mays subsp mays Nutrition 0.000 abstract description 11
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 abstract description 10
- 235000009973 maize Nutrition 0.000 abstract description 10
- 239000003054 catalyst Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000004064 recycling Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 231100000252 nontoxic Toxicity 0.000 abstract description 4
- 230000003000 nontoxic effect Effects 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 239000002028 Biomass Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 239000012153 distilled water Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 239000002243 precursor Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
- 229920002488 Hemicellulose Polymers 0.000 description 5
- 235000011054 acetic acid Nutrition 0.000 description 5
- 150000001243 acetic acids Chemical class 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005287 template synthesis Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 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
- B01J23/70—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
-
- B01J35/33—
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention discloses the preparation method of a kind of nanometer of UV Fenton composite, the present invention is that template prepares Fe using maize straw3O4/TiO2Composite, can both obtain the catalyst with porous hierarchy, and the recycling of straw biomass resource can be realized again, while obtained nanometer Fe3O4/TiO2Composite has good chemical stability, stronger Fenton-like catalytic capability and certain photo-catalysis capability, the features such as nano level catalyst is due to special surface nature and safety non-toxic, in addition, the material also has certain magnetic, recycling is convenient for, therefore its application in terms of catalytic degradation organic pollution is increasingly subject to the concern of people.
Description
Technical field
The present invention relates to field of nano material preparation, the preparation side of more particularly to a kind of nanometer UV-Fenton composite
Method.
Background technology
Biological template synthesis prepares nano material and enjoyed favor in recent years, is made by the use of natural biological structure as template
One new technology of standby special material structure, has the advantages that structure is efficient, environment-friendly, cheap.At present, conduct
The natural material that biological template is applied to material preparation has a lot, for example：Absorbent cotton, protein, butterfly's wing, timber, bagasse,
Leaf etc..Jilin Province can all produce substantial amounts of maize straw every year as the big province of corn planting, and these maize straws are usual
It can only be incinerated as agricultural residue, this not only pollutes atmospheric environment, and also results in the waste of resource.
TiO2With extremely stable physics and chemical property, good corrosion resistance, be insoluble in it is sour, nontoxic, inexpensive etc.
Advantage and be widely studied, on TiO2Most study is in photocatalysis field.Photocatalysis technology mainly uses ultraviolet light
Or visible light catalytic generation light induced electron and hole, reduction or oxidation degradation of contaminant using light induced electron or hole,
But the problem of still having inefficient when handling the pollutant relatively stablized only with photocatalysis method.With high-level oxidation technology
Continue to develop, the development of Fenton catalytic oxidation technologies is of increasing concern, and the technology is by light-catalyzed reaction and chemical senior oxygen
Change reaction to be combined, using the advantage of the two, substantially increase the efficiency of reaction, and mild condition, oxidability are strong, applicable
Scope is wide.
And existing Fenton material preparation methods are cumbersome, processing waste water removal efficiency is low, and catalyst reclaims difficult, and application
Condition is limited.
The content of the invention
Present invention aim to address above-mentioned existing Fenton material preparation methods are cumbersome, processing waste water removal efficiency is low,
Catalyst reclaims difficult, and application conditions it is limited the problems such as, and provide the preparation side of a kind of nanometer of UV-Fenton composite
Method.
The present invention is that template prepares Fe using maize straw3O4/TiO2Composite, can both have been obtained with porous layering
The catalyst of structure, can realize the recycling of straw biomass resource again, while obtained nanometer Fe3O4/TiO2Composite wood
Material has good chemical stability, stronger Fenton-like catalytic capability and certain photo-catalysis capability, nano level catalysis
The features such as agent is due to special surface nature and safety non-toxic, in addition, the material also has certain magnetic so that its
It is easy to recycling, therefore its application in terms of catalytic degradation organic pollution is increasingly subject to the concern of people.
The preparation method of a kind of nanometer of UV-Fenton composite, comprises the following steps：
First, the TiO of porous hierarchy2Preparation
1) the agricultural stalk peeling after dry-cure will have been shone, be cut into after sequin, stalk disk is extracted with ammonia extracting method,
6h is dried in 60 DEG C of baking ovens, using butyl titanate as titanium source, absolute ethyl alcohol is added, it is impregnated with processed stalk disk
In, it is caused in standing adsorption 24h under 60 DEG C of baking ovens；
2) by 60 DEG C of oven for drying of titanium source stalk disk after the completion of absorption, it is put into after 550 DEG C of pipe reaction stove calcination 4h,
Obtain porous hierarchy TiO2；
2nd, nanometer Fe3O4/TiO2The preparation of composite
Using ferrous iron, thiosulfate as raw material, according to last Fe3O4/TiO2Theoretical Mass ratio be 2:1 ratio adds
Enter the porous hierarchy TiO described in step one2, add after alkali lye, stirring and be put into 140 DEG C of high temperature oven reclaimed water heat seals
Into reaction 12h, by centrifugation, filtering, a nanometer UV-Fenton composites are obtained after drying；
As optimization, the ammonia extracting method described in step one is the ammoniacal liquor heating extracting stalk disk using 20% concentration,
Lignin therein and metallic element are removed；
As optimization, the TiO described in step one2For Detitanium-ore-type or rutile-type；
As optimization, the divalent iron salt described in step 2 is ferrous sulfate or frerrous chloride or ferrous nitrate；
As optimization, the thiosulfate described in step 2 is sodium thiosulfate or potassium thiosulfate；
As optimization, the aqueous slkali described in step 2 is sodium hydroxide solution or potassium hydroxide solution, dense
Degree is respectively 1mol/L.
Beneficial effects of the present invention：
Preparation technology of the present invention is simple, environment-friendly, and selected maize straw is supported as construction unit, it is suppressed that
Fe3O4Reunion, obtained nanometer Fe3O4/TiO2Composite has good chemical stability, stronger Fenton-like catalysis
Ability and certain photo-catalysis capability, nano level catalyst is due to special surface nature and safety non-toxic, the thing
Matter also has certain magnetic so that it is easy to recycling.
Brief description of the drawings
Fig. 1 is the nanometer Fe that embodiment 4 is prepared3O4/TiO2The SEM figures of composite.
Fig. 2 is the nanometer Fe that embodiment 4 is prepared3O4/TiO2The TEM figures of composite.
Fig. 3 is the nanometer Fe that embodiment 4 is prepared3O4/TiO2The XRD spectrum of composite.
Fig. 4 is the nanometer Fe that embodiment 4 is obtained3O4/TiO2The XPS figures of composite.
Fig. 5 is the nanometer Fe that embodiment 4 is prepared3O4/TiO2The SEM figures of composite.
Embodiment
The preparation method of a kind of nanometer of UV-Fenton composite, comprises the following steps：
First, the TiO of porous hierarchy2Preparation
1) the agricultural stalk peeling after dry-cure will have been shone, be cut into after sequin, stalk disk is extracted with ammonia extracting method,
6h is dried in 60 DEG C of baking ovens, using butyl titanate as titanium source, absolute ethyl alcohol is added, it is impregnated with processed stalk disk
In, it is caused in standing adsorption 24h under 60 DEG C of baking ovens；
2) by 60 DEG C of oven for drying of titanium source stalk disk after the completion of absorption, it is put into after 550 DEG C of pipe reaction stove calcination 4h,
Obtain porous hierarchy TiO2；
2nd, nanometer Fe3O4/TiO2The preparation of composite
Using ferrous iron, thiosulfate as raw material, according to last Fe3O4/TiO2Theoretical Mass ratio be 2:1 ratio adds
Enter the porous hierarchy TiO described in step one2, add after alkali lye, stirring and be put into 140 DEG C of high temperature oven reclaimed water heat seals
Into reaction 12h, by centrifugation, filtering, a nanometer UV-Fenton composites are obtained after drying；
As optimization, the ammonia extracting method described in step one is the ammoniacal liquor heating extracting stalk disk using 20% concentration,
Lignin therein and metallic element are removed；
As optimization, the TiO described in step one2For Detitanium-ore-type or rutile-type；
As optimization, the divalent iron salt described in step 2 is ferrous sulfate or frerrous chloride or ferrous nitrate；
As optimization, the thiosulfate described in step 2 is sodium thiosulfate or potassium thiosulfate；
As optimization, the aqueous slkali described in step 2 is sodium hydroxide solution or potassium hydroxide solution, dense
Degree is respectively 1mol/L.
Embodiment 1：
First, the TiO of porous hierarchy2Preparation
The maize straw being collected into is removed the peel and is cut into the thick thin slices of 2mm, is dried, by dried stalk with 20% dilute ammonia
Water is stripped pretreatment, to remove the material such as the lignin of blocking channel, hemicellulose in stalk；By 50ml butyl titanates
Solution is dissolved in 150mL absolute ethyl alcohols, is added 1ml glacial acetic acids, is configured to precursor liquid；2g stalks are impregnated in 24h in precursor liquid
After be washed with deionized and dry for several times and in 60 DEG C of baking ovens, repeated impregnations/drying steps 2 times, finally 550 in tube furnace
DEG C high-temperature roasting 4h, heating rate is 2 DEG C/min, obtains the TiO with porous hierarchy2Sample；
2nd, nanometer Fe3O4/TiO2The preparation of composite
Weigh 1.39g ferrous sulfate and the water of 1.24g five and sodium thiosulfate is dissolved in 14ml distilled water, add 0.386g
The TiO prepared2Sample, weighs 0.4gNaOH solid dissolvings in 10ml distilled water, and two kinds of solution are mixed, and loads
In pyroreaction kettle, 12h is incubated in 140 DEG C of high temperature ovens, centrifuges, filter after taking-up, a nanometer UV- is obtained after drying
TiO in Fenton composites, composite2Content be 50%.
Embodiment 2：
First, the TiO of porous hierarchy2Preparation
The maize straw being collected into is removed the peel and is cut into the thick thin slices of 2mm, is dried, by dried stalk with 20% dilute ammonia
Water is stripped pretreatment, to remove the material such as the lignin of blocking channel, hemicellulose in stalk；By 50ml butyl titanates
Solution is dissolved in 150mL absolute ethyl alcohols, is added 1ml glacial acetic acids, is configured to precursor liquid；2g stalks are impregnated in 24h in precursor liquid
After be washed with deionized and dry for several times and in 60 DEG C of baking ovens, repeated impregnations/drying steps 2 times, finally 550 in tube furnace
DEG C high-temperature roasting 4h, heating rate is 2 DEG C/min, obtains the TiO with porous hierarchy2Sample；
2nd, nanometer Fe3O4/TiO2The preparation of composite
Weigh 1.39g ferrous sulfate and the water of 1.24g five and sodium thiosulfate is dissolved in 14ml distilled water, add 0.772g
The TiO prepared2Sample, weighs 0.4gNaOH solid dissolvings in 10ml distilled water, and two kinds of solution are mixed, and loads
In pyroreaction kettle, 12h is incubated in 140 DEG C of high temperature ovens, centrifuges, filter after taking-up, a nanometer UV- is obtained after drying
TiO in Fenton composites, composite2Content be 66.7%.
Embodiment 3：
First, the TiO of porous hierarchy2Preparation
The maize straw being collected into is removed the peel and is cut into the thick thin slices of 2mm, is dried, by dried stalk with 20% dilute ammonia
Water is stripped pretreatment, to remove the material such as the lignin of blocking channel, hemicellulose in stalk；By 50ml butyl titanates
Solution is dissolved in 150mL absolute ethyl alcohols, is added 1ml glacial acetic acids, is configured to precursor liquid；2g stalks are impregnated in 24h in precursor liquid
After be washed with deionized and dry for several times and in 60 DEG C of baking ovens, repeated impregnations/drying steps 2 times, finally 550 in tube furnace
DEG C high-temperature roasting 4h, heating rate is 2 DEG C/min, obtains the TiO with porous hierarchy2Sample；
2nd, nanometer Fe3O4/TiO2The preparation of composite
Weigh 1.39g ferrous sulfate and the water of 1.24g five and sodium thiosulfate is dissolved in 14ml distilled water, add 1.158g
The TiO prepared2Sample, weighs 0.4gNaOH solid dissolvings in 10ml distilled water, and two kinds of solution are mixed, and loads
In pyroreaction kettle, 12h is incubated in 140 DEG C of high temperature ovens, centrifuges, filter after taking-up, a nanometer UV- is obtained after drying
TiO in Fenton composites, composite2Content be 75%.
Embodiment 4：
First, the TiO of porous hierarchy2Preparation
Refer to shown in Fig. 1, Fig. 2, Fig. 3, Fig. 4 and Fig. 5, the maize straw being collected into removed the peel and is cut into the thick thin slices of 2mm,
Dry, dried stalk is stripped pretreatment with 20% weak aqua ammonia, with remove the lignin of blocking channel in stalk,
The materials such as hemicellulose；50ml solution of tetrabutyl titanate is dissolved in 150mL absolute ethyl alcohols, 1ml glacial acetic acids are added, before being configured to
Drive liquid；2g stalks are impregnated in precursor liquid after 24h and is washed with deionized for several times and is dried in 60 DEG C of baking ovens, repeat to soak
Stain/drying steps 2 times, last 550 DEG C of high-temperature roasting 4h in tube furnace, heating rate is 2 DEG C/min, is obtained with porous point
The TiO of Rotating fields2Sample；
2nd, nanometer Fe3O4/TiO2The preparation of composite
Weigh 1.39g ferrous sulfate and the water of 1.24g five and sodium thiosulfate is dissolved in 14ml distilled water, add 1.544g
The TiO prepared2Sample, weighs 0.4gNaOH solid dissolvings in 10ml distilled water, and two kinds of solution are mixed, and loads
In pyroreaction kettle, 12h is incubated in 140 DEG C of high temperature ovens, centrifuges, filter after taking-up, a nanometer UV- is obtained after drying
TiO in Fenton composites, composite2Content be 80%；
Embodiment 5：
First, the TiO of porous hierarchy2Preparation
The maize straw being collected into is removed the peel and is cut into the thick thin slices of 2mm, is dried, by dried stalk with 20% dilute ammonia
Water is stripped pretreatment, to remove the material such as the lignin of blocking channel, hemicellulose in stalk；By 50ml butyl titanates
Solution is dissolved in 150mL absolute ethyl alcohols, is added 1ml glacial acetic acids, is configured to precursor liquid；2g stalks are impregnated in 24h in precursor liquid
After be washed with deionized and dry for several times and in 60 DEG C of baking ovens, repeated impregnations/drying steps 2 times, finally 550 in tube furnace
DEG C high-temperature roasting 4h, heating rate is 2 DEG C/min, obtains the TiO with porous hierarchy2Sample；
2nd, nanometer Fe3O4/TiO2The preparation of composite
Weigh 1.39g ferrous sulfate and the water of 1.24g five and sodium thiosulfate is dissolved in 14ml distilled water, add 1.930g
The TiO prepared2Sample, weighs 0.4gNaOH solid dissolvings in 10ml distilled water, and two kinds of solution are mixed, and loads
In pyroreaction kettle, 12h is incubated in 140 DEG C of high temperature ovens, centrifuges, filter after taking-up, a nanometer UV- is obtained after drying
TiO in Fenton composites, composite2Content be 83.3%.
Claims (1)
1. the preparation method of a kind of nanometer of UV-Fenton composite, comprises the following steps：
First, the TiO of porous hierarchy2Preparation
1) the agricultural stalk peeling after dry-cure will have been shone, be cut into after sequin, stalk disk has been extracted with ammonia extracting method, at 60 DEG C
6h is dried in baking oven, using butyl titanate as titanium source, absolute ethyl alcohol is added, with processed stalk disk dipping wherein,
It is caused in standing adsorption 24h under 60 DEG C of baking ovens；
2) by 60 DEG C of oven for drying of titanium source stalk disk after the completion of absorption, it is put into after 550 DEG C of pipe reaction stove calcination 4h, obtains
Porous hierarchy TiO2；
2nd, nanometer Fe3O4/TiO2The preparation of composite
Using ferrous iron, thiosulfate as raw material, according to last Fe3O4/TiO2Theoretical Mass ratio be 2:1 ratio adds step
Porous hierarchy TiO described in rapid one2, add after alkali lye, stirring that to be put into Hydrothermal Synthesiss in 140 DEG C of high temperature ovens anti-
12h is answered, by centrifugation, filtering, a nanometer UV-Fenton composites are obtained after drying；
As optimization, the ammonia extracting method described in step one is the ammoniacal liquor heating extracting stalk disk using 20% concentration, by it
In lignin and metallic element remove；
As optimization, the TiO described in step one2For Detitanium-ore-type or rutile-type；
As optimization, the divalent iron salt described in step 2 is ferrous sulfate or frerrous chloride or ferrous nitrate；
As optimization, the thiosulfate described in step 2 is sodium thiosulfate or potassium thiosulfate；
As optimization, the aqueous slkali described in step 2 is sodium hydroxide solution or potassium hydroxide solution, and concentration is respectively 1mol/
L。
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| CN111760569A (en) * | 2020-07-08 | 2020-10-13 | 合肥工业大学 | Composite photo-Fenton catalyst, preparation method and application |
| CN113135631A (en) * | 2021-05-28 | 2021-07-20 | 杭州绿夏环境科技有限公司 | Wastewater treatment method with low sludge yield based on multidimensional catalytic oxidation process |
| CN114177909A (en) * | 2021-11-26 | 2022-03-15 | 福建师范大学 | Magnesium-coconut shell carbon-ferroferric oxide composite material and preparation method thereof |
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