CN106362734A - Preparation method for novel composite zinc oxide photocatalyst - Google Patents
Preparation method for novel composite zinc oxide photocatalyst Download PDFInfo
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- CN106362734A CN106362734A CN201610655254.6A CN201610655254A CN106362734A CN 106362734 A CN106362734 A CN 106362734A CN 201610655254 A CN201610655254 A CN 201610655254A CN 106362734 A CN106362734 A CN 106362734A
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- zinc oxide
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- photocatalyst
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 28
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 18
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims abstract description 16
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 15
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 15
- 239000011572 manganese Substances 0.000 claims abstract description 15
- 239000010445 mica Substances 0.000 claims abstract description 15
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 150000000703 Cerium Chemical class 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 5
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 4
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 9
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 2
- 239000002893 slag Substances 0.000 abstract 2
- RFVNOJDQRGSOEL-UHFFFAOYSA-N 2-hydroxyethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCO RFVNOJDQRGSOEL-UHFFFAOYSA-N 0.000 abstract 1
- 229940100242 glycol stearate Drugs 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- -1 DSSC Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- OSYLPIYJUCCMTQ-UHFFFAOYSA-N [O-][N+]([O-])=O.N.[Ce+3] Chemical compound [O-][N+]([O-])=O.N.[Ce+3] OSYLPIYJUCCMTQ-UHFFFAOYSA-N 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 208000017983 photosensitivity disease Diseases 0.000 description 1
- 231100000434 photosensitization Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method for a novel composite zinc oxide photocatalyst. The preparation method comprises the following steps: weighing raw materials consisting of, by weight, 40 to 60 parts of zinc nitrate hexahydrate, 8 to 12 parts of polyethylene glycol, 10 to 15 parts of thiourea, 6 to 10 parts of manganese slag. 2 to 3 parts of cerium salt and 10 to 15 parts of mica powder; adding zinc nitrate hexahydrate into an ultrasonic generator, adding absolute ethyl alcohol for dissolving, then adding a sodium hydroxide solution and carrying out an ultrasonic reaction so as to obtain a suspension A; adding thiourea into a stirrer and then adding a proper amount of water for dissolving so as to obtain a suspension B; pouring the suspension B into the ultrasonic generator filled with the suspension A, then adding polyethylene glycol stearate and carrying out an ultrasonic reaction so as to obtain a mixed solution; adding the mixed solution, manganese slag, cerium salt and mica powder into a ball mill, adding water and carrying out stirring so as to obtain paste; and carrying out washing, drying, grinding and roasting so as to obtain the photocatalyst. The preparation method has the advantages of wide sources of raw materials, low cost, simple preparation process, high production efficiency and low energy consumption; and the prepared photocatalyst has the advantages of good adsorption performance, high catalytic activity, high catalysis efficiency, etc.
Description
Technical field
The present invention relates to catalysis material technical field, specifically a kind of preparation side of NEW TYPE OF COMPOSITE photocatalyst of zinc oxide
Method.
Background technology
Since 21 century, the lifting with industrialization paces and the excessive use of natural resourcess, dirty along with various environment
Dye, energy scarcity problem constantly aggravate.Therefore, various pollutions are administered, the pressure finding new forms of energy to alleviate the earth is extremely urgent.
Photocatalysis technology is in wastewater treatment, gas purification, sterilization, antifouling, self-cleaning material, DSSC, cosmetic
The many such as product, gas sensor fields have a wide range of applications.Photocatalysis are can be produced under light excites based on semi-conducting material
Life has the light induced electron of strong reducing property and the fundamental characteristics in the hole with strong oxidizing property, and solid photocatalysts can absorb the sun
Water is become hydrogen by light with biomass decomposition, also the organic pollution in air and water body environment and inorganic pollution can be aoxidized or
Deoxidization, degradation is innocuous substance.Therefore, there is low energy consumption, environmental protection.
At present, the conductor photocatalysis material of domestic and international most study is mainly metal-oxide and sulfide, such as ti02,
W03, zno, fe203, cds etc..Zinc oxide (zno) due to low cost, preparation method is simple, pattern is easily controllable, photocatalysis
Functional the advantages of, will have good application prospect in Photocatalitic Technique of Semiconductor field.But zno is as photocatalyst
There is itself, the such as greater band gap (eg=3.4 ev) of ti02, ultraviolet light can only be absorbed, and ultraviolet light only accounts for solar energy
The 4% about of amount is very low to the utilization rate of sunlight.Also there is photo-generate electron-hole to multiple during its use simultaneously
Conjunction, photocatalysis quantum efficiency are low, so significantly limit its extensive application.Therefore, in order to reduce light induced electron and sky
Cave recombination probability, in recent years numerous researcheres take various methods: include noble metal loading, nonmetallic ion-doped, transition
Metal ion mixing, photosensitization of quasiconductor etc..Its granule of nano zine oxide is excessively trickle, be easy in use environment inactivation and
Cohesion, not free settling, lead to it to be difficult to separate, reclaim and reuse.For solving the above problems, increase its stability in use,
Nano zine oxide is carried on certain carrier, such as glass, silica gel, activated carbon etc., but these carriers have mechanical strength relatively
The limitation such as weak, chemical stability and heat stability difference.Therefore, how to improve the photocatalytic activity of photocatalyst and stability is to work as
Modern study hotspot.
Content of the invention
The present invention is directed to the problem that existing photocatalyst exists, and provides a kind of preparation of NEW TYPE OF COMPOSITE photocatalyst of zinc oxide
Method.The photocatalyst of this method preparation has that specific surface area is big, catalysis activity is high, catalytic efficiency high to the utilization rate of light source
Height, good stability, environment-protecting asepsis, low cost, the advantages of can repeatedly use.
In order to realize object above, the technical solution used in the present invention is as follows:
A kind of preparation method of NEW TYPE OF COMPOSITE photocatalyst of zinc oxide, comprises the following steps:
(1) weigh each raw material according to parts by weight: zinc nitrate hexahydrate 40-60 part, Polyethylene Glycol 8-12 part, thiourea 10-15 part,
Manganese mud 6-10 part, cerium salt 2-3 part and mica powder 10-15 part；
(2) zinc nitrate hexahydrate is added in ultrasonic generator, add dehydrated alcohol to be dissolved, be subsequently adding sodium hydroxide molten
Liquid adjusts ph to 12-13, continues ultrasonic 30-60min, obtain suspension a under frequency is for 40-60khz；
(3) thiourea is added in agitator, adding suitable quantity of water stirring makes it dissolve, and obtains suspension b；
(4) suspension b is poured in the supersonic generator equipped with suspension a, add Polyethylene Glycol, be 40- in frequency
Continue ultrasonic 30-60min under 60khz, obtain mixed liquor；
(5) mixed liquor, manganese mud, cerium salt and mica powder are added ball mill, add suitable quantity of water stirring, obtain pastel；
(6) first use distilled water wash pastel, then microwave drying 1-2h, the grinding after being dried at 100-120 DEG C by pastel
Become powder, place into muffle furnace roasting 3-5h at temperature is for 400-600 DEG C, obtain final product photocatalyst.
Preferably, the addition of the above dehydrated alcohol is 4-6 times of zinc nitrate hexahydrate weight.
Preferably, the concentration of the above sodium hydroxide solution is 1-5mol/l.
Preferably, the above cerium salt is one of cerous sulfate, cerous nitrate or ammonium ceric nitrate.
Preferably, the described stirring of above step (5) is stirring 30-60min under rotating speed is for 300-500r/min.
Preferably, the heating rate of the above roasting is 5-10 DEG C/min.
Preferably, the described grinding of above step (6) is to grind the material to particle diameter for 0.5-1.0mm.
Compared with prior art, advantages of the present invention and having the beneficial effect that
1st, the photocatalyst that the inventive method is obtained has larger specific surface area, good pore structure and more catalysis and lives
Property center, improve the absorption property of catalyst so that light induced electron and hole can efficiently separate, so improve catalyst
Activity and efficiency, expand the absorption in visible-range for the catalyst, greatly improve the utilization rate to sunlight for the catalyst.
2nd, the present invention, using Polyethylene Glycol as dispersant, can solve catalyst and be easy to inactivate and solidifying in use environment
Poly-, not free settling problem.
3rd, the present invention is using manganese mud and mica powder as carrier, catalyst performance can not only be made more stable it is easier to
Separate, reclaim and be used repeatedly moreover it is possible to improve absorption property and the photocatalysis performance of catalyst.
4th, the photocatalyst specific surface area of present invention preparation is 200-250m2/ g, to methylene blue in lower 1 hour of sunlight
Degradation rate reach more than 92%.
5th, the present invention has that raw material sources are extensive, with low cost, preparation process is simple, production efficiency high, energy consumption is low, reaction
Mild condition, environmental friendliness, absorption property are good, catalysis activity is high, high catalytic efficiency the advantages of, can efficiently under visible light exposure
Catalytic degradation wastewater organic pollutant, has good economic benefit, social benefit and ecological benefits, is more suitable for industrial life
Produce.
Specific embodiment
Below in conjunction with specific embodiment, this programme is further illustrated, but be not limited to protection scope of the present invention.
Embodiment 1
A kind of preparation method of NEW TYPE OF COMPOSITE photocatalyst of zinc oxide, comprises the following steps:
(1) proportionally weigh each raw material: zinc nitrate hexahydrate 40g, Polyethylene Glycol 8g, thiourea 12g, manganese mud 7g, cerous nitrate
2g and mica powder 10g；
(2) zinc nitrate hexahydrate is added in ultrasonic generator, add 200ml dehydrated alcohol to be dissolved, be subsequently adding concentration
Sodium hydroxide solution for 1mol/l adjusts ph to 12, continues ultrasonic 60min, obtain suspension a under frequency is for 40khz；
(3) thiourea is added in agitator, adding the stirring of 100ml water makes it dissolve, and obtains suspension b；
(4) suspension b is poured in the supersonic generator equipped with suspension a, add Polyethylene Glycol, be 40khz in frequency
The ultrasonic 60min of lower continuation, obtains mixed liquor；
(5) mixed liquor, manganese mud, cerous nitrate and mica powder are added ball mill, add the stirring of 120ml water, obtain pastel；
(6) first use distilled water wash pastel, then by pastel at 100 DEG C microwave drying 2h, be dried after grind to form particle diameter
Powder for 0.5mm, places into muffle furnace roasting 5h at temperature is 400 DEG C, obtains final product photocatalyst.
Embodiment 2
A kind of preparation method of NEW TYPE OF COMPOSITE photocatalyst of zinc oxide, comprises the following steps:
(1) proportionally weigh each raw material: zinc nitrate hexahydrate 50g, Polyethylene Glycol 10g, thiourea 10g, manganese mud 6g, cerous sulfate
2g and mica powder 12g；
(2) zinc nitrate hexahydrate is added in ultrasonic generator, add 300ml dehydrated alcohol to be dissolved, be subsequently adding concentration
Sodium hydroxide solution for 2mol/l adjusts ph to 13, continues ultrasonic 45min, obtain suspension a under frequency is for 50khz；
(3) thiourea is added in agitator, adding the stirring of 100ml water makes it dissolve, and obtains suspension b；
(4) suspension b is poured in the supersonic generator equipped with suspension a, add Polyethylene Glycol, be 50khz in frequency
The ultrasonic 60min of lower continuation, obtains mixed liquor；
(5) mixed liquor, manganese mud, cerous nitrate and mica powder are added ball mill, add the stirring of 120ml water, obtain pastel；
(6) first use distilled water wash pastel, then by pastel at 120 DEG C microwave drying 1h, be dried after grind to form particle diameter
Powder for 0.5mm, places into muffle furnace roasting 4h at temperature is 500 DEG C, obtains final product photocatalyst.
Embodiment 3
A kind of preparation method of NEW TYPE OF COMPOSITE photocatalyst of zinc oxide, comprises the following steps:
(1) proportionally weigh each raw material: zinc nitrate hexahydrate 60g, Polyethylene Glycol 12g, thiourea 12g, manganese mud 10g, nitric acid
Cerium ammonium 3g and mica powder 15g；
(2) zinc nitrate hexahydrate is added in ultrasonic generator, add 400ml dehydrated alcohol to be dissolved, be subsequently adding concentration
Sodium hydroxide solution for 5mol/l adjusts ph to 13, continues ultrasonic 30min, obtain suspension a under frequency is for 60khz；
(3) thiourea is added in agitator, adding the stirring of 120ml water makes it dissolve, and obtains suspension b；
(4) suspension b is poured in the supersonic generator equipped with suspension a, add Polyethylene Glycol, be 60khz in frequency
The ultrasonic 30min of lower continuation, obtains mixed liquor；
(5) mixed liquor, manganese mud, cerous nitrate and mica powder are added ball mill, add the stirring of 150ml water, obtain pastel；
(6) first use distilled water wash pastel, then by pastel at 110 DEG C microwave drying 1.5h, be dried after grind granulating
Footpath is the powder of 1.0mm, places into muffle furnace roasting 3h at temperature is 600 DEG C, obtains final product photocatalyst.
Embodiment 4
A kind of preparation method of NEW TYPE OF COMPOSITE photocatalyst of zinc oxide, comprises the following steps:
(1) proportionally weigh each raw material: zinc nitrate hexahydrate 50g, Polyethylene Glycol 10g, thiourea 10g, manganese mud 6g, cerous sulfate
2g and mica powder 12g；
(2) zinc nitrate hexahydrate is added in ultrasonic generator, add 300ml dehydrated alcohol to be dissolved, be subsequently adding concentration
Sodium hydroxide solution for 2mol/l adjusts ph to 13, continues ultrasonic 45min, obtain suspension a under frequency is for 50khz；
(3) thiourea is added in agitator, adding the stirring of 100ml water makes it dissolve, and obtains suspension b；
(4) suspension b is poured in the supersonic generator equipped with suspension a, add Polyethylene Glycol, be 50khz in frequency
The ultrasonic 60min of lower continuation, obtains mixed liquor；
(5) mixed liquor, manganese mud, cerous nitrate and mica powder are added ball mill, add the stirring of 120ml water, obtain pastel；
(6) first use distilled water wash pastel, then by pastel at 120 DEG C microwave drying 1h, be dried after grind to form particle diameter
Powder for 0.5mm, places into muffle furnace roasting 4h at temperature is 500 DEG C, obtains final product photocatalyst.
The photocatalysis test of catalyst: below will be by commercial nano zinc oxide photocatalyst and various embodiments of the present invention system
Standby photocatalyst contrasts to the degradation rate of methylene blue, and measurement result is as shown in the table:
The photocatalyst of each embodiment preparation and nano zinc oxide photocatalyst are weighed 1g respectively, putting into 1l concentration is 20mg/l
Methylene blue simulated water sample, add in the reactor of quartzy interlayer, using 500 w xenon lamps as solar source, in rotating speed be
Under 500r/min, stirring radiation 1h, using the concentration of Water By High Performance Liquid sample Methylene Blue, calculates photocatalysis
Agent degradation rate.
As seen from table, the photocatalyst prepared by various embodiments of the present invention has higher photocatalytic activity, right under sunlight
The degradation rate of methylene blue all reaches more than 92%, significantly larger than presently commercially available product, has good market prospect.
Above content is it cannot be assumed that the present invention is embodied as being confined to these explanations, for the technical field of the invention
Those of ordinary skill for, under the premise of without departing from present inventive concept, some simple deduction or replace can also be made, all answer
When being considered as belonging to the scope of patent protection that the present invention is determined by claims of being submitted to.
Claims (7)
1. a kind of preparation method of NEW TYPE OF COMPOSITE photocatalyst of zinc oxide it is characterised in that: comprise the following steps:
(1) weigh each raw material according to parts by weight: zinc nitrate hexahydrate 40-60 part, Polyethylene Glycol 8-12 part, thiourea 10-15 part,
Manganese mud 6-10 part, cerium salt 2-3 part and mica powder 10-15 part；
(2) zinc nitrate hexahydrate is added in ultrasonic generator, add dehydrated alcohol to be dissolved, be subsequently adding sodium hydroxide molten
Liquid adjusts ph to 12-13, continues ultrasonic 30-60min, obtain suspension a under frequency is for 40-60khz；
(3) thiourea is added in agitator, adding suitable quantity of water stirring makes it dissolve, and obtains suspension b；
(4) suspension b is poured in the supersonic generator equipped with suspension a, add Polyethylene Glycol, be 40- in frequency
Continue ultrasonic 30-60min under 60khz, obtain mixed liquor；
(5) mixed liquor, manganese mud, cerium salt and mica powder are added ball mill, add suitable quantity of water stirring, obtain pastel；
(6) first use distilled water wash pastel, then microwave drying 1-2h, the grinding after being dried at 100-120 DEG C by pastel
Become powder, place into muffle furnace roasting 3-5h at temperature is for 400-600 DEG C, obtain final product photocatalyst.
2. according to claim 1 NEW TYPE OF COMPOSITE photocatalyst of zinc oxide preparation method it is characterised in that: described anhydrous second
The addition of alcohol is 4-6 times of zinc nitrate hexahydrate weight.
3. according to claim 1 NEW TYPE OF COMPOSITE photocatalyst of zinc oxide preparation method it is characterised in that: described hydroxide
The concentration of sodium solution is 1-5mol/l.
4. according to claim 1 NEW TYPE OF COMPOSITE photocatalyst of zinc oxide preparation method it is characterised in that: described cerium salt is
One of cerous sulfate, cerous nitrate or ammonium ceric nitrate.
5. according to claim 1 NEW TYPE OF COMPOSITE photocatalyst of zinc oxide preparation method it is characterised in that: step (5) institute
Stating stirring is stirring 30-60min under rotating speed is for 300-500r/min.
6. according to claim 1 NEW TYPE OF COMPOSITE photocatalyst of zinc oxide preparation method it is characterised in that: described roasting
Heating rate is 5-10 DEG C/min.
7. according to claim 1 NEW TYPE OF COMPOSITE photocatalyst of zinc oxide preparation method it is characterised in that: step (6) institute
Stating grinding is to grind the material to particle diameter for 0.5-1.0mm.
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| CN112385939A (en) * | 2020-10-27 | 2021-02-23 | 广州市宗仁鞋业有限公司 | Fashion shoe manufacturing process |
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| CN112385939A (en) * | 2020-10-27 | 2021-02-23 | 广州市宗仁鞋业有限公司 | Fashion shoe manufacturing process |
| CN112385939B (en) * | 2020-10-27 | 2022-04-05 | 广州市宗仁鞋业有限公司 | Fashion shoe manufacturing process |
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