CN104624222B - Method for preparing CuO-TiO2/zeolite nanocomposite material for treating dye wastewater - Google Patents
Method for preparing CuO-TiO2/zeolite nanocomposite material for treating dye wastewater Download PDFInfo
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- CN104624222B CN104624222B CN201510040762.9A CN201510040762A CN104624222B CN 104624222 B CN104624222 B CN 104624222B CN 201510040762 A CN201510040762 A CN 201510040762A CN 104624222 B CN104624222 B CN 104624222B
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- tio
- zeolite
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- 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
Abstract
The invention belongs to the field of material preparation, and discloses a method for preparing a CuO-TiO2/zeolite nanocomposite material for treating dye wastewater. The method comprises the following steps: firstly pretreating with hydrochloric acid and calcining to obtain natural zeolite; mixing butyl titanate, anhydrous ethanol and diethanolamine according to a ratio of 3:10: 1 to prepare TiO2 sol, dispersing the natural zeolite in the TiO2 sol, heating in a water bath, stirring, drying, and calcining to obtain TiO2/zeolite; and finally preparing a Cu(NO3)2 solution with the concentration of 5mmol/L, uniformly dispersing TiO2/zeolite in the Cu(NO3)2 solution, stirring, drying, and calcining to obtain the CuO-TiO2/zeolite nanocomposite material. Therefore, the obtained CuO-TiO2/zeolite nanocomposite material has dye wastewater treatment efficiency of more than 90% after being measured by a UV-visible spectrophotometer under fluorescent illumination. The prepared CuO-TiO2/zeolite nanocomposite material is easily recycled, is good in adsorption and degradation performances and low in overall cost.
Description
Technical field
The invention belongs to field of material preparation, particularly for the nano-cu o-tio processing waste water from dyestuff2/ zeolite is combined
The preparation method of material.
Background technology
Textile industry is one of conventional industries of China, and it includes weaving, chemical fibre, clothes and printing and dyeing etc..Since 21 century,
The dyeing industry fast development of China, if but in its production process discharge waste water administer improper environment will be caused very tight
The pollution of weight.Dyeing waste water has the features such as organic pollution concentration is high, and alkalescence is big, colourity is deep.According to incompletely statistics, China's print
The discharge capacity of dye waste water is 300～4,000,000 m3/d.Now, feasible in the urgent need to textile printing and dyeing wastewater is proposed with one
Administer countermeasure.At present, the traditional handicraft processing dyeing waste water mainly has a flocculent precipitation, absorption method, biochemical process, electrochemical process,
Chemical oxidization method and photocatalytic method etc..
Photocatalytic method has a low energy consumption, non-secondary pollution, can permineralization organic matter the advantages of.Nanometer tio2Because it has
Photocatalytic activity is high, and stable chemical nature, the advantages of nontoxic, is widely used as semiconductor light-catalyst.By
In nanometer tio2Greater band gap, only under ultraviolet irradiation, valence-band electrons just can be excited to transit to conduction band, form photoproduction electricity
Son and hole, therefore, significantly limit tio2Application in field of environment engineering.However, the energy gap of cuo is 1.7ev,
Conduction level compares tio2Conduction level is more negative, by cuo and tio2It is combined, can be with excitation wavelength red shift to visible region.
Nano semiconductor photochemical catalyst is less due to particle diameter, easily reunites, and is difficult to place, adsorption capacity is not strong, limits
Its application in terms of wastewater treatment, however, support type semiconductor light-catalyst has easily separated, easy recovery, reusable
The advantages of.Conventional carrier has: activated carbon, glass fibre, clay, zeolite etc..Because zeolite has uniform pore passage structure, can
There is provided place for reaction, there is good ion exchange and absorption property simultaneously, single use tio can be made up2Deficiency,
Therefore, zeolite can become photochemical catalyst firmly load and homodisperse carrier.Natural zeolite is as a kind of nonmetallic mineral material
Material, quite enriches in the reserves of China, and it has relatively low cost and abundant reserves, so that natural zeolite is increasingly subject to
Pay attention to.
Content of the invention
The present invention is by nano-cu o and tio of good solar absorption2Composite load is on natural zeolite as a kind of semiconductor
Photochemical catalyst, same to tio2/ zeolite is compared, nano-cu o-tio2The effect of/zeolite adsorption degradation of dye waste water is more preferable.
A kind of nano-cu o-tio for processing waste water from dyestuff that the present invention provides2The preparation method of/Zeolite composite materials
As follows: to use salt low-kappa number first, through calcining to obtain natural zeolite；Then by butyl titanate, absolute ethyl alcohol, diethanol amine press 3:
The ratio of 10:1 is mixed with tio2Colloidal sol, natural zeolite is dispersed in tio2In colloidal sol, heating water bath stirs, after drying, through forging
Burning obtains tio2/ zeolite；Finally prepare the cu (no of 5mmol/l concentration3)2Solution, by tio2/ zeolite is dispersed in cu (no3)2
Stir in solution, after drying, obtain nano-cu o-tio through calcining2/ Zeolite composite materials.
Preferably, the present invention is used for processing the nano-cu o-tio of waste water from dyestuff2The preparation method tool of/Zeolite composite materials
Body is as follows:
(1) hydrochloric acid is mixed by the dilution proportion of 1:1 with distilled water, natural zeolite is added thereto, at 80 DEG C～90 DEG C
Heating stirring 4h～5h in water-bath, uses distilled water filtration washing, after being dried under the conditions of 90 DEG C, under the conditions of 500 DEG C～600 DEG C
Calcining obtains the zeolite 0.5g～1g handling well；
(2) by butyl titanate, absolute ethyl alcohol, diethanol amine is prepared containing 0.3mol～0.5mol in the ratio of 3:10:1
tio2Colloidal sol, 0.5g～1g natural zeolite good for above-mentioned pretreatment is put into the tio of the 25ml～50ml preparing2In colloidal sol, through 70
DEG C～90 DEG C of heating water baths stirring 2h～4h after, be dried under the conditions of 90 DEG C, after calcining under the conditions of 450 DEG C～650 DEG C, received
Rice tio2/ Zeolite composite materials；
(3) prepare the cu (no that 20ml～50ml concentration is 5mmol/l～25mmol/l3)2Solution, by 0.5g～1g nanometer
tio2/ Zeolite composite materials are dispersed in the cu (no of 20ml～50ml3)2In solution, stir 2h, use distilled water filtration washing, 90
It is dried under the conditions of DEG C, after calcining under the conditions of 400 DEG C～600 DEG C, obtain nano-cu o-tio2/ Zeolite composite materials.
The mechanism of action of the present invention is: energy is more than or equal to the photon of energy gap energy equivalence value, can be by conduction band
Electron excitation transit to valence band, positively charged hole is stayed on valence band, moves to the e of semiconductor surface-And h+With absorption
O2、h2o、oh-With generation redox reactions such as organic matters；But nanometer tio2Energy gap be 3.2ev, can only absorb
The ultraviolet light of below 380nm, relatively low to the utilization rate accounting for solar energy, available low-gap semiconductor is combined and can improve
ti02The visible light catalysis activity of catalyst system；When the energy of photon is not enough to excite ti02Electronics, and low-gap semiconductor
Valence-band electrons be stimulated transition when, e-Move to ti02Conduction band on, hole is stayed in narrow-band semiconductor valence band, realize photoproduction electricity
Efficiently separating of son-hole, suppresses the light rotten candle phenomenon of low-gap semiconductor.
Preferably, in described step (1), hydrochloric acid is mixed by the dilution proportion of 1:1 with distilled water, natural zeolite is added
Wherein, heating stirring 5h in 90 DEG C of water-baths.
Preferably, the tio in described step (2)2Colloidal sol, with butyl titanate, absolute ethyl alcohol, diethanol amine presses 3:10:1's
Ratio prepares the tio containing 0.5mol2Colloidal sol.
Preferably, the nano-cu o-tio in described step (3)2/ Zeolite composite materials, are tio2/ zeolite is in 600 DEG C of conditions
Lower calcining obtains.
The nano-cu o-tio that the present invention is obtained2/ Zeolite composite materials, evaluate its light using degraded methyl blue solution and urge
Change activity, weigh in 0.1g sample placement surface ware, after adding, in sample, the methylene blue solution that 20ml concentration is 10mg/l,
Surface plate is put irradiation 3h under fluorescent light, after ultra-violet and visible spectrophotometer test, it is to dye wastewater treatment efficiency
Reach more than 90%.
The invention has the benefit that the nano-cu o-tio that the present invention obtains2/ Zeolite composite materials, shine in fluorescent lamp
Penetrate down, after ultraviolet-visible spectrophotometer test, dye wastewater treatment efficiency is reached with more than 90%, and the nanometer prepared
cuo-tio2/ Zeolite composite materials are easily recycled, and absorption degradation performance is good, and integrated cost is low.
Brief description
Fig. 1 is the nano-cu o-tio of embodiment 1 gained2/ Zeolite composite materials are tested through ultraviolet-visible spectrophotometer
Result.
Fig. 2 is the nano-cu o-tio of embodiment 2 gained2/ Zeolite composite materials are tested through ultraviolet-visible spectrophotometer
Result.
Fig. 3 is the nano-cu o-tio of embodiment 3 gained2/ Zeolite composite materials are tested through ultraviolet-visible spectrophotometer
Result.
Specific embodiment
The following examples can make those skilled in the art be more completely understood by the present invention, but limits never in any form
The present invention.
Embodiment 1
The present invention is used for processing the nano-cu o-tio of waste water from dyestuff2The preparation method of/Zeolite composite materials is specific as follows:
(1) hydrochloric acid is mixed by the dilution proportion of 1:1 with distilled water, natural zeolite is added thereto, in 80 DEG C of water-baths
Heating stirring 4h, uses distilled water filtration washing, and after being dried under the conditions of 90 DEG C, calcining under the conditions of 500 DEG C obtains handling well
Zeolite 0.5g；
(2) butyl titanate, absolute ethyl alcohol are used, diethanol amine prepares tio containing 0.3mol in the ratio of 3:10:12Colloidal sol,
0.5g natural zeolite good for above-mentioned pretreatment is put into the tio of the 25ml preparing2In colloidal sol, stir 2h through 70 DEG C of heating water baths
Afterwards, it is dried under the conditions of 90 DEG C, after calcining under the conditions of 450 DEG C, obtain a nanometer tio2/ Zeolite composite materials；
(3) prepare the cu (no that 20ml concentration is 5mmol/l3)2Solution, by 0.5g nanometer tio2/ Zeolite composite materials divide
It is dispersed in the cu (no of 20ml3)2In solution, stir 2h, use distilled water filtration washing, be dried under the conditions of 90 DEG C, under the conditions of 400 DEG C
After calcining, obtain nano-cu o-tio2/ Zeolite composite materials.
The nano-cu o-tio that the present invention is obtained2/ Zeolite composite materials, evaluate its light using degraded methyl blue solution and urge
Change activity, weigh in 0.1g sample placement surface ware, after adding, in sample, the methylene blue solution that 20ml concentration is 10mg/l,
Surface plate is put irradiation 3h under fluorescent light, after ultra-violet and visible spectrophotometer test, it is to dye wastewater treatment efficiency
Reach 90%.Test result is as shown in Figure 1.
Embodiment 2
The present invention is used for processing the nano-cu o-tio of waste water from dyestuff2The preparation method of/Zeolite composite materials is specific as follows:
(1) hydrochloric acid is mixed by the dilution proportion of 1:1 with distilled water, natural zeolite is added thereto, in 85 DEG C of water-baths
Heating stirring 5h, uses distilled water filtration washing, and after being dried under the conditions of 90 DEG C, calcining under the conditions of 550 DEG C obtains handling well
Zeolite 1g；
(2) butyl titanate, absolute ethyl alcohol are used, diethanol amine prepares tio containing 0.4mol in the ratio of 3:10:12Colloidal sol,
1g natural zeolite good for above-mentioned pretreatment is put into the tio of the 40ml preparing2In colloidal sol, stir through 80 DEG C of heating water baths after 3h,
It is dried under the conditions of 90 DEG C, after calcining under the conditions of 550 DEG C, obtain a nanometer tio2/ Zeolite composite materials；
(3) prepare the cu (no that 20ml concentration is 15mmol/l3)2Solution, by 1g nanometer tio2/ Zeolite composite materials disperse
Cu (no in 20ml3)2In solution, stir 2h, use distilled water filtration washing, be dried under the conditions of 90 DEG C, forge under the conditions of 500 DEG C
After burning, obtain nano-cu o-tio2/ Zeolite composite materials.
The nano-cu o-tio that the present invention is obtained2/ Zeolite composite materials, evaluate its light using degraded methyl blue solution and urge
Change activity, weigh in 0.1g sample placement surface ware, after adding, in sample, the methylene blue solution that 20ml concentration is 10mg/l,
Surface plate is put irradiation 3h under fluorescent light, after ultra-violet and visible spectrophotometer test, it is to dye wastewater treatment efficiency
Reach 91%.Test result is as shown in Figure 2.
Embodiment 3
The present invention is used for processing the nano-cu o-tio of waste water from dyestuff2The preparation method of/Zeolite composite materials is specific as follows:
(1) hydrochloric acid is mixed by the dilution proportion of 1:1 with distilled water, natural zeolite is added thereto, in 90 DEG C of water-baths
Heating stirring 5h, uses distilled water filtration washing, and after being dried under the conditions of 90 DEG C, calcining under the conditions of 600 DEG C obtains handling well
Zeolite 1g；
(2) butyl titanate, absolute ethyl alcohol are used, diethanol amine prepares tio containing 0.5mol in the ratio of 3:10:12Colloidal sol,
1g natural zeolite good for above-mentioned pretreatment is put into the tio of the 50ml preparing2In colloidal sol, stir through 90 DEG C of heating water baths after 4h,
It is dried under the conditions of 90 DEG C, after calcining under the conditions of 650 DEG C, obtain a nanometer tio2/ Zeolite composite materials；
(3) prepare the cu (no that 50ml concentration is 25mmol/l3)2Solution, by 1g nanometer tio2/ Zeolite composite materials disperse
Cu (no in 50ml3)2In solution, stir 2h, use distilled water filtration washing, be dried under the conditions of 90 DEG C, forge under the conditions of 600 DEG C
After burning, obtain nano-cu o-tio2/ Zeolite composite materials.
The nano-cu o-tio that the present invention is obtained2/ Zeolite composite materials, evaluate its light using degraded methyl blue solution and urge
Change activity, weigh in 0.1g sample placement surface ware, after adding, in sample, the methylene blue solution that 20ml concentration is 10mg/l,
Surface plate is put irradiation 3h under fluorescent light, after ultra-violet and visible spectrophotometer test, it is to dye wastewater treatment efficiency
Reach 93%.Test result is as shown in Figure 3.
Contrast test: first, hydrochloric acid is mixed by the dilution proportion of 1:1 with distilled water, natural zeolite is added thereto,
Heating stirring 5h in 90 DEG C of water-baths, uses distilled water filtration washing, is dried under the conditions of 90 DEG C, after calcining, obtains under the conditions of 500 DEG C
The zeolite handled well；Then butyl titanate, absolute ethyl alcohol are used, diethanol amine prepares 0.5mol tio in the ratio of 3:10:12
Colloidal sol, and the above-mentioned tio preparing put into by the natural zeolite that 1g is pre-processed2In colloidal sol, heating stirring in 90 DEG C of water-baths,
It is dried under the conditions of 90 DEG C, after 550 DEG C of degree calcinings, obtain a nanometer tio2/ Zeolite composite materials.
Experimental data contrasts:
| Waste water treatment efficiency | |
| Embodiment 1 | 90% |
| Embodiment 2 | 91% |
| Embodiment 3 | 93% |
| tio2/ zeolite | 79% |
Upper table for this experiment with the conditions of degradation efficiency contrast it can be seen that nano-cu o-tio2/ Zeolite composite materials
Treatment effeciency be significantly larger than tio2The treatment effeciency of/zeolite.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, the change or replacement that can readily occur in,
All should be included within the scope of the present invention.Therefore, protection scope of the present invention should be with scope of the claims
It is defined.
Claims (4)
1. a kind of nano-cu o tio for processing waste water from dyestuff2The preparation method of/Zeolite composite materials it is characterised in that: tool
Preparation comprises the steps:
(1) hydrochloric acid is mixed by the dilution proportion of 1:1 with distilled water, natural zeolite is added thereto, in 80 DEG C～90 DEG C water-baths
Middle heating stirring 4h～5h, uses distilled water filtration washing, after being dried, calcines under the conditions of 500 DEG C～600 DEG C under the conditions of 90 DEG C
Obtain the zeolite 0.5g～1g handling well；
(2) by butyl titanate, absolute ethyl alcohol, diethanol amine is prepared containing 0.3mol～0.5mol by the volume ratio of 3:10:1
tio2Colloidal sol, 0.5g～1g natural zeolite good for above-mentioned pretreatment is put into the tio of the 25ml～50ml preparing2In colloidal sol, through 70
DEG C～90 DEG C of heating water baths stirring 2h～4h after, be dried under the conditions of 90 DEG C, after calcining under the conditions of 450 DEG C～650 DEG C, received
Rice tio2/ Zeolite composite materials；
(3) prepare the cu (no that 20ml～50ml concentration is 5mmol/l～25mmol/l3)2Solution, by 0.5g～1g nanometer tio2/
Zeolite composite materials are dispersed in the cu (no of 20ml～50ml3)2In solution, stir 2h, use distilled water filtration washing, in 90 DEG C of bars
It is dried under part, after calcining under the conditions of 400 DEG C～600 DEG C, obtain nano-cu o tio2/ Zeolite composite materials.
2. the nano-cu o tio for processing waste water from dyestuff according to claim 12The preparation side of/Zeolite composite materials
Method it is characterised in that: in described step (1), hydrochloric acid is mixed by the dilution proportion of 1:1 with distilled water, natural zeolite is added it
In, heating stirring 5h in 90 DEG C of water-baths.
3. the nano-cu o tio for processing waste water from dyestuff according to claim 12The preparation side of/Zeolite composite materials
Method it is characterised in that: the tio in described step (2)2Colloidal sol, with butyl titanate, absolute ethyl alcohol, diethanol amine presses 3:10:1's
Ratio prepares the tio containing 0.5mol2Colloidal sol.
4. the nano-cu o tio for processing waste water from dyestuff according to claim 12The preparation side of/Zeolite composite materials
Method it is characterised in that: the nano-cu o tio in described step (3)2/ Zeolite composite materials, are tio2/ zeolite is in 600 DEG C of conditions
Lower calcining obtains.
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| CN105233828A (en) * | 2015-11-04 | 2016-01-13 | 河海大学 | Recoverable titanium dioxide photocatalyst capable of quickly degrading high-concentration bisphenol A waste water as well as preparation method and application thereof |
| CN106076398A (en) * | 2016-06-06 | 2016-11-09 | 同济大学 | A kind of silver TiO2the preparation method of nano cupric oxide modified zeolite composite photo-catalyst |
| CN106179460A (en) * | 2016-07-06 | 2016-12-07 | 上海应用技术学院 | A kind of nanometer CuO/TiO2the preparation method of/Fe modified zeolite composite photo-catalyst |
| CN106799254B (en) * | 2016-12-23 | 2019-05-14 | 同济大学 | A kind of nanometer of Cu2O/Ag/TiO2The preparation method of zeolite compound photocatalyst |
| CN106853373B (en) * | 2016-12-23 | 2019-05-14 | 同济大学 | A kind of nanometer of Cu2O/Ag/TiO2The preparation method of iron modified zeolite composite photo-catalyst |
| CN107583455A (en) * | 2017-09-27 | 2018-01-16 | 湖北工业大学 | A kind of purification of air zeolite/TiO2/SrTiO3The preparation method of composite |
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| KR20030076931A (en) * | 2003-03-11 | 2003-09-29 | 이경주 | Sop system |
| CN100411730C (en) * | 2006-05-22 | 2008-08-20 | 苏州科技学院 | Zeolite based nano-titanium dioxide double function material and its prepn. method |
| CN101108335A (en) * | 2007-07-17 | 2008-01-23 | 延安大学 | Active clay loaded nano TiO2 compound photocatalysis material and method of manufacturing the same |
| CN101780416B (en) * | 2010-01-27 | 2012-07-25 | 石家庄经济学院 | Iron and chrome co-doped nano titanium dioxide/zeolite compound photocatalyst and preparation method thereof |
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