CN106492875A - Prepare the method and the method for processing furfural waste-water of load nano-titanium dioxide/zinc oxide molecular sieves - Google Patents
Prepare the method and the method for processing furfural waste-water of load nano-titanium dioxide/zinc oxide molecular sieves Download PDFInfo
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- CN106492875A CN106492875A CN201610945161.7A CN201610945161A CN106492875A CN 106492875 A CN106492875 A CN 106492875A CN 201610945161 A CN201610945161 A CN 201610945161A CN 106492875 A CN106492875 A CN 106492875A
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- titanium dioxide
- zinc oxide
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims abstract description 130
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 88
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 74
- 239000002351 wastewater Substances 0.000 title claims abstract description 48
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229940055360 titanium dioxide / zinc oxide Drugs 0.000 title claims abstract description 35
- 239000000758 substrate Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052753 mercury Inorganic materials 0.000 claims abstract description 8
- 230000005855 radiation Effects 0.000 claims abstract description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 86
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 49
- 239000000843 powder Substances 0.000 claims description 46
- 239000011787 zinc oxide Substances 0.000 claims description 45
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000010881 fly ash Substances 0.000 claims description 36
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 30
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 24
- 239000000376 reactant Substances 0.000 claims description 21
- 239000005060 rubber Substances 0.000 claims description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000008236 heating water Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000012423 maintenance Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 24
- 238000006731 degradation reaction Methods 0.000 description 24
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000006303 photolysis reaction Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000007788 liquid Chemical class 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- XPCTZQVDEJYUGT-UHFFFAOYSA-N 3-hydroxy-2-methyl-4-pyrone Chemical compound CC=1OC=CC(=O)C=1O XPCTZQVDEJYUGT-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 heterocyclic aldehydes Chemical class 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 description 1
- HYMLWHLQFGRFIY-UHFFFAOYSA-N Maltol Natural products CC1OC=CC(=O)C1=O HYMLWHLQFGRFIY-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 239000010866 blackwater Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 229940093503 ethyl maltol Drugs 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229940043353 maltol Drugs 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical compound C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000002760 rocket fuel Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/7049—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The method and the method for processing furfural waste-water of load nano-titanium dioxide/zinc oxide molecular sieves is prepared, it is related to the preparation method of photochemical catalyst and the method for processing waste water.Environmental requirement is not reached the invention aims to solving existing single method and processing furfural waste-water, multiple method Combined Treatment furfural waste-waters cause equipment investment big, the problem that flow process is complicated, operation maintenance is difficult and cost of water treatment is high.Method：First, molecular sieve substrate is prepared；2nd, load, obtain load nano-titanium dioxide/zinc oxide molecular sieves.The method for processing furfural waste-water：Load nano-titanium dioxide/zinc oxide molecular sieves are added in furfural waste-water, then photocatalytic degradation are carried out with ultraviolet high voltage mercury lamp radiation under agitation, the water after being processed.Load nano-titanium dioxide/zinc oxide molecular sieves prepared by the present invention are applied to process furfural waste-water.
Description
Technical field
The present invention relates to the preparation method of photochemical catalyst and the method for processing waste water.
Background technology
Furfural is the heterocyclic aldehydes with double bond, and chemical property is active, in organic synthesis industry occupies critically important status.
Having many uses for furfural and its liquid derivative is general, and it in addition to being industrially used as selective solvent can be also used for synthesizing
In resin, plastics, fiber, rubber, medicine, agricultural chemicals, dyestuff and the department such as food industry, national defense industry.Such as in food industry
In, for synthesizing apple acid, maltol and ethylmaltol etc.；In the electronics industry, a series of insulating materials can be manufactured,
The glass-like carbon that furfural and acetone reaction can also be made in being applied to atomic energy and other sophisticated industries after adding curing agent；In state
In anti-industry, explosive, rocket fuel ignition additives, extractant of rocket container coatings etc. can be synthesized；In leather industry, can
Synthetic tanning material.Some cationic ion-exchange resins for being used for purified industrial black water are exactly that furfural is obtained with humic acid reaction
, in addition furfural is additionally operable to produce analytical chemistry reagent, antioxidant, anticorrosive, plastics and rubber anti-ageing agent etc..
As environmental protection pressure is increasing, the improvement of furfural waste-water has become the significant problem for being related to the sector existence.
At present, there are electroosmose process, extraction-rectification method, bioanalysis, micro-electrolysis method, catalytic oxidation etc. to the method that furfural waste-water is administered,
As single processing method does not reach environmental requirement, existing mostly be several method Combined Treatment, this also causes equipment investment
Greatly, flow process is complicated, operation maintenance is difficult, cost of water treatment increases year by year.In recent years, nano-photo catalytic oxidation technology is due to its work
Skill is simple, small investment, high treating effect, illustrates fabulous application prospect in terms for the treatment of of Organic Wastewater.
With nano-TiO2For photochemical catalyst, the heterogeneous photocatalytic oxidation technology of ultraviolet light (UV) irradiation generation OH is because of which
There is energy-efficient, the nontoxic, non-secondary pollution of cleaning and process is simple, show as most in terms of Sewage advanced treatment
One of high-level oxidation technology of potentiality, the extensive attention for causing.There is scholar's research nano-TiO2Treatment by Photocatalysis Oxidation chaff
The effect of aldehyde waste water, it was demonstrated that nano-photo catalytic oxidation technology can be used for the improvement of furfural waste-water.It is reported that single UV/
TiO2Less high to furfural waste-water oxidation efficiency, and use TiO2Super fine (nano particle size) makees catalyst, to the process later stage
Catalyst immediately separation and recovery brings great inconvenience, and the recycling problem of conventional load limits the technology
Industrial applications.
Content of the invention
Environmental requirement is not reached the invention aims to solving existing single method and processing furfural waste-water, multiple method connection
Closing process furfural waste-water causes equipment investment big, the problem that flow process is complicated, operation maintenance is difficult and cost of water treatment is high, and provides
Prepare the method and the method for processing furfural waste-water of load nano-titanium dioxide/zinc oxide molecular sieves.
The method for preparing load nano-titanium dioxide/zinc oxide molecular sieves, is completed according to the following steps：
First, molecular sieve substrate is prepared：
1., flyash is placed in hydrochloric acid solution, then low whipping speed is 300r/min～1000r/min and 75 DEG C～85
Heating water bath 1.5h～3h at DEG C, then suction filtration is carried out, the solid matter that suction filtration is obtained is cleaned using distilled water, to cleaning
Liquid is neutrality, then under conditions of temperature is for 75 DEG C～90 DEG C dries 6h～9h, the flyash after being processed；
Step one 1. described in the volume ratio of quality and hydrochloric acid solution of flyash be 1g:(14mL～16mL)；
2. flyash, after the process for 1. obtaining step one, NaOH and sodium carbonate are well mixed, then are placed in temperature
Spend calcining 60min～80min in the Muffle furnace for 500 DEG C～600 DEG C；Obtain reactant；Reactant is added to absolute ethyl alcohol
In, then the absolute ethyl alcohol containing reactant is moved to reactor, by reactor temperature be heat at 90 DEG C～110 DEG C 10h～
14h, then 2h～4h is dried at 75 DEG C～90 DEG C after the material in reactor is taken out, obtain molecular sieve substrate；
Step one 2. described in process after the mass ratio of flyash and NaOH be 1:(1～1.5)；
Step one 2. described in process after the mass ratio of flyash and sodium carbonate be 1:(0.25～0.35)；
Step one 2. described in the volume ratio of quality and absolute ethyl alcohol of reactant be 1g:(10mL～12mL)；
2nd, load：Low whipping speed is by TiO under 300r/min～1000r/min2Powder, ZnO powder are added to anhydrous
In ethanol, stir, the molecular sieve substrate obtained in adding step one 2. is obtained containing TiO2/ ZnO powder and molecular sieve
The absolute ethyl alcohol of substrate；TiO will be contained2The absolute ethyl alcohol of/ZnO powder and molecular sieve substrate is in the perseverance that temperature is 30 DEG C～35 DEG C
Warm water bath is stirred and is volatilized to absolute ethyl alcohol completely, obtains powdered rubber；Powdered rubber is done in the case where temperature is for 90 DEG C～95 DEG C
Dry 3h～4h, then moves to temperature for roasting 3h～4h at 500 DEG C～550 DEG C, then is ground, obtain loading nanometer titanium dioxide
Titanium/zinc oxide molecular sieves；
TiO described in step 22The gross mass of powder and ZnO powder is 1g with the volume ratio of absolute ethyl alcohol:(10mL～
12mL)；
TiO described in step 22Powder is 1 with the mass ratio of ZnO powder:(1～1.1)；
TiO described in step 22Powder is 0.1 with the mass ratio of molecular sieve substrate:(1～1.1).
The method that furfural waste-water is processed using load nano-titanium dioxide/zinc oxide molecular sieves, is to complete according to the following steps
's：
Load nano-titanium dioxide/zinc oxide molecular sieves are added in furfural waste-water, then low whipping speed is 500r/
Photocatalytic degradation 30min～90min, the water after being processed is carried out under min～1000r/min and ultraviolet high voltage mercury lamp radiation；
In described furfural waste-water, furfural is 1 with the mass ratio of load nano-titanium dioxide/zinc oxide molecular sieves:1.
Advantages of the present invention：
First, TiO2Nano particle is belonged to ZnO, and relatively low with the compatibility processed between waste water, suspension is easily formed, no
Easily recycle, so, nano titanium oxide/zinc oxide is loaded on molecular sieve, beneficial to recycling or secondary utilization；
2nd, TiO2Itself is widely used in every field as photodissociation catalyst, but TiO2Can only be swashed by ultraviolet light
Send out, and the utilization rate to solar energy is very low and photo-quantum efficiency is relatively low, and ZnO can overcome the disadvantages that TiO just2This is not enough, therefore,
The two is mixed, is not only expanded the wave-length coverage of photodissociation, is also increased its degradation rate to furfuryl aldehyde solution, 30min is to degrade
Example, loads nano-TiO2Molecular sieve be 51.36% to the degradation rate of furfuryl aldehyde solution, load the molecular sieve of nano-ZnO to furfural
The degradation rate of solution is 52.8%, and the degradation rate of load nano-titanium dioxide/zinc oxide molecular sieves prepared by the present invention is
57.99%, the degradation rate relative to single load has significantly increase.
Load nano-titanium dioxide/zinc oxide molecular sieves prepared by the present invention are applied to process furfural waste-water.
Description of the drawings
Degradation rate curves of the Fig. 1 for furfural in furfural waste-water under different degradation times in embodiment one.
Specific embodiment
Specific embodiment one：Present embodiment is that the method for preparing load nano-titanium dioxide/zinc oxide molecular sieves is
Complete according to the following steps：
First, molecular sieve substrate is prepared：
1., flyash is placed in hydrochloric acid solution, then low whipping speed is 300r/min～1000r/min and 75 DEG C～85
Heating water bath 1.5h～3h at DEG C, then suction filtration is carried out, the solid matter that suction filtration is obtained is cleaned using distilled water, to cleaning
Liquid is neutrality, then under conditions of temperature is for 75 DEG C～90 DEG C dries 6h～9h, the flyash after being processed；
Step one 1. described in the volume ratio of quality and hydrochloric acid solution of flyash be 1g:(14mL～16mL)；
2. flyash, after the process for 1. obtaining step one, NaOH and sodium carbonate are well mixed, then are placed in temperature
Spend calcining 60min～80min in the Muffle furnace for 500 DEG C～600 DEG C；Obtain reactant；Reactant is added to absolute ethyl alcohol
In, then the absolute ethyl alcohol containing reactant is moved to reactor, by reactor temperature be heat at 90 DEG C～110 DEG C 10h～
14h, then 2h～4h is dried at 75 DEG C～90 DEG C after the material in reactor is taken out, obtain molecular sieve substrate；
Step one 2. described in process after the mass ratio of flyash and NaOH be 1:(1～1.5)；
Step one 2. described in process after the mass ratio of flyash and sodium carbonate be 1:(0.25～0.35)；
Step one 2. described in the volume ratio of quality and absolute ethyl alcohol of reactant be 1g:(10mL～12mL)；
2nd, load：Low whipping speed is by TiO under 300r/min～1000r/min2Powder, ZnO powder are added to anhydrous
In ethanol, stir, the molecular sieve substrate obtained in adding step one 2. is obtained containing TiO2/ ZnO powder and molecular sieve
The absolute ethyl alcohol of substrate；TiO will be contained2The absolute ethyl alcohol of/ZnO powder and molecular sieve substrate is in the perseverance that temperature is 30 DEG C～35 DEG C
Warm water bath is stirred and is volatilized to absolute ethyl alcohol completely, obtains powdered rubber；Powdered rubber is done in the case where temperature is for 90 DEG C～95 DEG C
Dry 3h～4h, then moves to temperature for roasting 3h～4h at 500 DEG C～550 DEG C, then is ground, obtain loading nanometer titanium dioxide
Titanium/zinc oxide molecular sieves；
TiO described in step 22The gross mass of powder and ZnO powder is 1g with the volume ratio of absolute ethyl alcohol:(10mL～
12mL)；
TiO described in step 22Powder is 1 with the mass ratio of ZnO powder:(1～1.1)；
TiO described in step 22Powder is 0.1 with the mass ratio of molecular sieve substrate:(1～1.1).
Present embodiment step one 1. described in flyash be commercial flyash.
The advantage of present embodiment：
First, TiO2Nano particle is belonged to ZnO, and relatively low with the compatibility processed between waste water, suspension is easily formed, no
Easily recycle, so, nano titanium oxide/zinc oxide is loaded on molecular sieve, beneficial to recycling or secondary utilization；
2nd, TiO2Itself is widely used in every field as photodissociation catalyst, but TiO2Can only be swashed by ultraviolet light
Send out, and the utilization rate to solar energy is very low and photo-quantum efficiency is relatively low, and ZnO can overcome the disadvantages that TiO just2This is not enough, therefore,
The two is mixed, is not only expanded the wave-length coverage of photodissociation, is also increased its degradation rate to furfuryl aldehyde solution, 30min is to degrade
Example, loads nano-TiO2Molecular sieve be 51.36% to the degradation rate of furfuryl aldehyde solution, load the molecular sieve of nano-ZnO to furfural
The degradation rate of solution is 52.8%, and the degradation rate of load nano-titanium dioxide/zinc oxide molecular sieves prepared by present embodiment
For 57.99%, the degradation rate relative to single load has significantly increase.
Load nano-titanium dioxide/zinc oxide molecular sieves prepared by present embodiment are applied to process furfural waste-water.
Specific embodiment two：Difference of the present embodiment from specific embodiment one is：Step one 1. described in
The concentration of hydrochloric acid solution is 10mol/L～12mol/L.Other are identical with specific embodiment one.
Specific embodiment three：Difference of the present embodiment from specific embodiment one or two is：Step one is 1. middle will
Flyash is placed in hydrochloric acid solution, then low whipping speed is heating water bath 2h at 500r/min～1000r/min and 80 DEG C, then is entered
Row suction filtration, is cleaned to the solid matter that suction filtration is obtained using distilled water, is neutrality to cleaning fluid, then is 80 DEG C in temperature
Under the conditions of dry 8h, the flyash after being processed.Other are identical with specific embodiment one or two.
Specific embodiment four：Difference of the present embodiment from one of specific embodiment one to three is：Step one is 2.
Flyash, NaOH and sodium carbonate after the middle process for 1. obtaining step one is well mixed, then is placed in temperature for 550 DEG C
Muffle furnace in calcine 70min；Obtain reactant；Reactant is added in absolute ethyl alcohol, then by containing the anhydrous of reactant
Ethanol moves to reactor, and reactor is heated 12h in the case where temperature is for 90 DEG C, then after the material in reactor is taken out at 80 DEG C
3h is dried, molecular sieve substrate is obtained.Other are identical with specific embodiment one to three.
Specific embodiment five：Difference of the present embodiment from one of specific embodiment one to four is：Step one is 2.
Described in process after the mass ratio of flyash and NaOH be 1:1.2.Other are identical with specific embodiment one to four.
Specific embodiment six：Difference of the present embodiment from one of specific embodiment one to five is：Step one is 2.
Described in process after the mass ratio of flyash and sodium carbonate be 1:0.3.Other are identical with specific embodiment one to five.
Specific embodiment seven：Difference of the present embodiment from one of specific embodiment one to six is：In step 2
Low whipping speed is by TiO under 1000r/min2Powder, ZnO powder are added in absolute ethyl alcohol, are stirred, and add step
One 2. in the molecular sieve substrate that obtains, obtain containing TiO2/ ZnO powder and the absolute ethyl alcohol of molecular sieve substrate；TiO will be contained2/
The absolute ethyl alcohol of ZnO powder and molecular sieve substrate is stirred in the thermostat water bath that temperature is 35 DEG C and is volatilized to absolute ethyl alcohol completely,
Obtain powdered rubber；Powdered rubber is dried 3h in the case where temperature is for 95 DEG C, temperature is then moved to for roasting 3h at 500 DEG C, then is carried out
Grinding, obtains load nano-titanium dioxide/zinc oxide molecular sieves.Other are identical with specific embodiment one to six.
Specific embodiment eight：Present embodiment is：Furfural is processed using load nano-titanium dioxide/zinc oxide molecular sieves
The method of waste water is completed according to the following steps：
Load nano-titanium dioxide/zinc oxide molecular sieves are added in furfural waste-water, then low whipping speed is 500r/
Photocatalytic degradation 30min～90min, the water after being processed is carried out under min～1000r/min and ultraviolet high voltage mercury lamp radiation；
In described furfural waste-water, furfural is 1 with the mass ratio of load nano-titanium dioxide/zinc oxide molecular sieves:1.
Specific embodiment nine：Difference of the present embodiment from specific embodiment eight is：In described furfural waste-water
The concentration of furfural is 1g/L～2g/L.Other are identical with specific embodiment eight.
Specific embodiment ten：Difference of the present embodiment from specific embodiment eight or nine is：Described ultraviolet height
The ultraviolet light intensity of pressure mercury lamp irradiation is 170uW/cm2～250uW/cm2.Other are identical with specific embodiment eight or nine.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：The method for preparing load nano-titanium dioxide/zinc oxide molecular sieves, is completed according to the following steps：
First, molecular sieve substrate is prepared：
1., flyash is placed in hydrochloric acid solution, then low whipping speed be 500r/min and 80 DEG C at heating water bath 2h, then
Suction filtration is carried out, the solid matter that suction filtration is obtained is cleaned using distilled water, be neutrality to cleaning fluid, then be 80 DEG C in temperature
Under conditions of dry 8h, the flyash after being processed；
Step one 1. described in the volume ratio of quality and hydrochloric acid solution of flyash be 1g:15mL；
2. flyash, after the process for 1. obtaining step one, NaOH and sodium carbonate are well mixed, then are placed in temperature
Spend calcining 70min in the Muffle furnace for 550 DEG C；Obtain reactant；Reactant is added in absolute ethyl alcohol, then will be containing reaction
The absolute ethyl alcohol of thing moves to reactor, reactor is heated in the case where temperature is for 100 DEG C 12h, then the material in reactor is taken out
3h is dried at 85 DEG C afterwards, molecular sieve substrate is obtained；
Step one 2. described in process after the mass ratio of flyash and NaOH be 1:1.2；
Step one 2. described in process after the mass ratio of flyash and sodium carbonate be 1:0.3；
Step one 2. described in the volume ratio of quality and absolute ethyl alcohol of reactant be 1g:10mL；
2nd, load：Low whipping speed is by TiO under 500r/min2Powder, ZnO powder are added in absolute ethyl alcohol, stirring
Uniformly, the molecular sieve substrate obtained in adding step one 2., obtains containing TiO2/ ZnO powder and molecular sieve substrate anhydrous
Ethanol；TiO will be contained2The absolute ethyl alcohol of/ZnO powder and molecular sieve substrate is stirred to nothing in the thermostat water bath that temperature is 35 DEG C
Water-ethanol volatilizees completely, obtains powdered rubber；Powdered rubber is dried 3h in the case where temperature is for 95 DEG C, temperature is then moved to for 500 DEG C
Lower roasting 3h, then be ground, obtain load nano-titanium dioxide/zinc oxide molecular sieves；
TiO described in step 22The gross mass of powder and ZnO powder is 1g with the volume ratio of absolute ethyl alcohol:10mL；
TiO described in step 22Powder is 1 with the mass ratio of ZnO powder:1；
TiO described in step 22Powder is 0.1 with the mass ratio of molecular sieve substrate:1.
Embodiment two：The load nano-titanium dioxide prepared using embodiment one/zinc oxide molecular sieves process furfural waste-water
Method, complete according to the following steps：
50mg load nano-titanium dioxides/zinc oxide molecular sieves are added in 50mL furfural waste-waters, then low whipping speed
For carrying out photocatalytic degradation 30min～90min, the water after being processed under 800r/min and ultraviolet high voltage mercury lamp radiation；Described
Furfural waste-water in the mass ratio of furfural and load nano-titanium dioxide/zinc oxide molecular sieves be 1:1；In described furfural waste-water
The concentration of furfural is 1g/L；The ultraviolet light intensity of described ultraviolet high voltage mercury lamp radiation is 200uW/cm2.
Every one section of reaction time, the water after 5mL is processed is taken, the water after applying aqueous filter membrane to obtain clarifying treatment is used in combination
Ultraviolet specrophotometer, determines its absorbance under the wavelength of 510nm, and calculates its degradation rate, as shown in Figure 1；Fig. 1 is real
Apply in example one the degradation rate curve of furfural in furfural waste-water under different degradation times；
From fig. 1, it can be seen that in embodiment one, when degradation time is 30min, the load nanometer two prepared using embodiment one
Titanium oxide/zinc oxide molecular sieves process furfural waste-water, and in furfural waste-water, the degradation efficiency of furfural is 57.99%, works as degradation time
For 60min when, in furfural waste-water the degradation efficiency of furfural be 60.99%, when degradation time be 90min when, chaff in furfural waste-water
The degradation efficiency of aldehyde is 67.55%.
By taking the 30min that degrades as an example, nano-TiO is individually loaded2Molecular sieve (described independent load nano-TiO2Molecule
TiO in sieve2Powder is 0.2 with the mass ratio of molecular sieve substrate:1；) it is 51.36% to the degradation rate of furfuryl aldehyde solution, individually load
(in the molecular sieve of described independent load nano-ZnO, ZnO powder with the mass ratio of molecular sieve substrate is the molecular sieve of nano-ZnO
0.2:1；) it is 52.8% to the degradation rate of furfuryl aldehyde solution, therefore, the method for furfural waste-water is processed in embodiment one compared with prior art
The method of middle single treatment furfural waste-water improves a lot, and the degradation efficiency of furfural is improved.
Claims (10)
1. the method for preparing load nano-titanium dioxide/zinc oxide molecular sieves, it is characterised in that prepare load nano-titanium dioxide/
The method of zinc oxide molecular sieves is completed according to the following steps：
First, molecular sieve substrate is prepared：
1., flyash is placed in hydrochloric acid solution, then low whipping speed is at 300r/min～1000r/min and 75 DEG C～85 DEG C
Heating water bath 1.5h～3h, then suction filtration is carried out, the solid matter that suction filtration is obtained is cleaned using distilled water, to cleaning fluid be
Neutrality, then 6h～9h, the flyash after being processed is dried under conditions of temperature is for 75 DEG C～90 DEG C；
Step one 1. described in the volume ratio of quality and hydrochloric acid solution of flyash be 1g:(14mL～16mL)；
2. flyash, after the process for 1. obtaining step one, NaOH and sodium carbonate are well mixed, then are placed in temperature and are
60min～80min is calcined in 500 DEG C～600 DEG C of Muffle furnace；Obtain reactant；Reactant is added in absolute ethyl alcohol, then
Absolute ethyl alcohol containing reactant is moved to reactor, reactor is heated 10h～14h in the case where temperature is for 90 DEG C～110 DEG C, then
2h～4h is dried at 75 DEG C～90 DEG C after material in reactor is taken out, molecular sieve substrate is obtained；
Step one 2. described in process after the mass ratio of flyash and NaOH be 1:(1～1.5)；
Step one 2. described in process after the mass ratio of flyash and sodium carbonate be 1:(0.25～0.35)；
Step one 2. described in the volume ratio of quality and absolute ethyl alcohol of reactant be 1g:(10mL～12mL)；
2nd, load：Low whipping speed is by TiO under 300r/min～1000r/min2Powder, ZnO powder are added to absolute ethyl alcohol
In, stirring, the molecular sieve substrate obtained in adding step one 2. is obtained containing TiO2/ ZnO powder and molecular sieve substrate
Absolute ethyl alcohol；TiO will be contained2The absolute ethyl alcohol of/ZnO powder and molecular sieve substrate is in the thermostatted water that temperature is 30 DEG C～35 DEG C
Bath is stirred and is volatilized to absolute ethyl alcohol completely, obtains powdered rubber；Powdered rubber is dried 3h in the case where temperature is for 90 DEG C～95 DEG C
～4h, then moves to temperature for roasting 3h～4h at 500 DEG C～550 DEG C, then is ground, obtain load nano-titanium dioxide/oxygen
Change Zn molecular sieve；
TiO described in step 22The gross mass of powder and ZnO powder is 1g with the volume ratio of absolute ethyl alcohol:(10mL～
12mL)；
TiO described in step 22Powder is 1 with the mass ratio of ZnO powder:(1～1.1)；
TiO described in step 22Powder is 0.1 with the mass ratio of molecular sieve substrate:(1～1.1).
2. the method for preparing load nano-titanium dioxide/zinc oxide molecular sieves according to claim 1, it is characterised in that step
Rapid one 1. described in hydrochloric acid solution concentration be 10mol/L～12mol/L.
3. the method for preparing load nano-titanium dioxide/zinc oxide molecular sieves according to claim 1, it is characterised in that step
Rapid one 1. in flyash is placed in hydrochloric acid solution, then low whipping speed be 500r/min～1000r/min and 80 DEG C at water-bath
Heating 2h, then is carried out suction filtration, the solid matter that suction filtration is obtained is cleaned using distilled water, is neutrality to cleaning fluid, then
Temperature is drying 8h, the flyash after being processed under conditions of 80 DEG C.
4. the method for preparing load nano-titanium dioxide/zinc oxide molecular sieves according to claim 1, it is characterised in that step
Rapid one 2. in flyash after the process that 1. obtains step one, NaOH and sodium carbonate be well mixed, then be placed in temperature and be
70min is calcined in 550 DEG C of Muffle furnace；Obtain reactant；Reactant is added in absolute ethyl alcohol, then by containing reactant
Absolute ethyl alcohol moves to reactor, and reactor is heated 12h in the case where temperature is for 90 DEG C, then 80 after the material in reactor is taken out
3h is dried at DEG C, molecular sieve substrate is obtained.
5. the method for preparing load nano-titanium dioxide/zinc oxide molecular sieves according to claim 1, it is characterised in that step
Rapid one 2. described in process after the mass ratio of flyash and NaOH be 1:1.2.
6. the method for preparing load nano-titanium dioxide/zinc oxide molecular sieves according to claim 1, it is characterised in that step
Rapid one 2. described in process after the mass ratio of flyash and sodium carbonate be 1:0.3.
7. the method for preparing load nano-titanium dioxide/zinc oxide molecular sieves according to claim 1, it is characterised in that step
In rapid two, low whipping speed is by TiO under 1000r/min2Powder, ZnO powder are added in absolute ethyl alcohol, are stirred, then plus
The molecular sieve substrate obtained in entering step one 2., obtains containing TiO2/ ZnO powder and the absolute ethyl alcohol of molecular sieve substrate；To contain
There is TiO2The absolute ethyl alcohol of/ZnO powder and molecular sieve substrate stirs complete to absolute ethyl alcohol in the thermostat water bath that temperature is 35 DEG C
Full volatilization, obtains powdered rubber；Powdered rubber is dried 3h in the case where temperature is for 95 DEG C, temperature is then moved to for roasting 3h at 500 DEG C,
It is ground again, obtains load nano-titanium dioxide/zinc oxide molecular sieves.
8. the method that the load nano-titanium dioxide/zinc oxide molecular sieves for being prepared using such as claim 1 process furfural waste-water, its
The method for being characterized by load nano-titanium dioxide/zinc oxide molecular sieves process furfural waste-water is to complete according to the following steps
's：
Load nano-titanium dioxide/zinc oxide molecular sieves are added in furfural waste-water, then low whipping speed be 500r/min～
Photocatalytic degradation 30min～90min, the water after being processed is carried out under 1000r/min and ultraviolet high voltage mercury lamp radiation；Described
In furfural waste-water, furfural is 1 with the mass ratio of load nano-titanium dioxide/zinc oxide molecular sieves:1.
9. the method that utilization load nano-titanium dioxide according to claim 8/zinc oxide molecular sieves process furfural waste-water,
It is characterized in that the concentration of furfural is 1g/L～2g/L in described furfural waste-water.
10. utilization load nano-titanium dioxide according to claim 8/zinc oxide molecular sieves process the side of furfural waste-water
Method, it is characterised in that the ultraviolet light intensity of described ultraviolet high voltage mercury lamp radiation is 170uW/cm2～250uW/cm2.
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