CN102836728A - Preparation method of TiO2/schorlite/rare earth ion composite photo-catalytic material - Google Patents

Preparation method of TiO2/schorlite/rare earth ion composite photo-catalytic material Download PDF

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CN102836728A
CN102836728A CN 201210326321 CN201210326321A CN102836728A CN 102836728 A CN102836728 A CN 102836728A CN 201210326321 CN201210326321 CN 201210326321 CN 201210326321 A CN201210326321 A CN 201210326321A CN 102836728 A CN102836728 A CN 102836728A
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rare earth
schorl
earth ion
tio
preparation
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杜悦
黄朝晖
李妍
刘艳改
房明浩
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China University of Geosciences
China University of Geosciences Beijing
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China University of Geosciences Beijing
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Abstract

The invention relates to a preparation method of a TiO2/schorlite/rare earth ion composite photo-catalytic material, belonging to the technical field of preparation of photo-catalytic materials. TiO2 has the characteristics of stable chemical property, no toxicity, no pollution, wide application range and the like, and is the most common photo-catalyst in recent years. According to the preparation method, schorlite, tetrabutyl titanate and rare earth oxides (Nd2O3 and Gd2O3) are used as raw materials; and through component design, a series of TiO2/schorlite/rare earth ion (Nd<3+> and Gd<3+>) composite photo-catalytic materials are prepared by using a sol-gel method. Ground dry gel is calcined at a calcination temperature system of 500 DEG C, is cooled and is used for photo-catalytic degradation of various organic pollutants. Constituent phases of TiO2 in the TiO2/schorlite/rare earth ion (Nd<3+> and Gd<3+>) composite photo-catalytic material prepared by the invention are anatase phase and a small amount of rutile phase; the average particle diameter of the TiO2 is at nanoscale; and the degradation effect on methyl orange of the pollutants is obviously superior to that of pure TiO2. The preparation method of the TiO2/schorlite/rare earth ion composite photo-catalytic material has the prominent advantages of low cost, less energy consumption in a preparation process and the like.

Description

A kind of TiO 2The preparation method of/schorl/rare earth ion composite photocatalyst material
Technical field
The present invention relates to a kind of preparation TiO 2The method of/schorl/rare earth ion composite photocatalyst material, this material is used for organic pollutions such as photocatalytic degradation methyl orange, belongs to the catalysis material preparing technical field.
Background technology
Along with the continuous development of printing and dyeing industry, the discharge capacity of dyeing waste water is more and more, and its problem of environmental pollution is more and more serious, has caused people's attention gradually.Methyl orange waste water is one of important composition of dyeing waste water, and the research of handling to methyl orange in recent years gets more and more.Photocatalytic method is efficient because of having, environmental protection, do not produce advantage such as secondary pollution, becomes to have one of method of DEVELOPMENT PROSPECT most.
TiO 2Characteristics such as it is stable to have chemical property, nontoxic, pollution-free, applied widely.Compare TiO with photochemical catalysts such as sulfide, nitride 2Persistence organic pollutant removal effect to some difficult degradations is better, and anti-light and resistance to chemical corrosion are stronger, and stability is better, thereby becomes the most frequently used photochemical catalyst.Be used for light-catalysed TiO 2With anatase is main with rutile mutually mutually, wherein anatase phase TiO 2Photocatalysis performance best.But TiO 2Forbidden band broad (E=3.2eV) has only the ultraviolet light below the absorbing wavelength 387.5nm, could the excitation electron transition form light induced electron and hole, and light induced electron and hole be prone to compoundly, causes the photo-quantum efficiency reduction, thereby influences TiO 2Photocatalysis efficiency.The researcher is raising TiO both at home and abroad in recent years 2Photocatalysis performance adopt the whole bag of tricks that it is carried out modification, the result shows that the adding of tourmaline and rare earth element can effectively improve TiO 2Photo-quantum efficiency, thereby improve its photocatalysis performance.
The natural electric polarity of tourmaline makes it can spontaneously attract TiO 2In light induced electron, thereby avoided the compound again of light induced electron and hole effectively, improved photocatalytic quantum.And a small amount of doping of rare earth element can be at TiO 2The middle right shallow gesture in light induced electron-hole that forms is caught trap, prolongs the time of electronics and hole-recombination, and inhibition anatase rutile in opposite directions changes mutually.
Utilize sol-gel process to prepare TiO 2/ schorl/rare earth ion composite photocatalyst material is easy and simple to handle, and cost is low, and energy resource consumption is few.This material has overcome pure TiO simultaneously 2The shortcoming that photo-quantum efficiency is low has significantly improved TiO 2Photocatalytic degradation rate to organic pollution methyl orange.
Summary of the invention
TiO 2Characteristics such as it is stable to have chemical property, nontoxic, pollution-free, applied widely.And its persistence organic pollutant removal effect to some difficult degradations is superior to photochemical catalysts such as traditional sulfide, nitride.Therefore become widely used in recent years a kind of photochemical catalyst.The present invention is with schorl, butyl titanate and rare earth oxide (Nd 2O 3, Gd 2O 3) be primary raw material, adopt sol-gel process to prepare a series of schorl/TiO 2/ rare earth ion (Nd 3+, Gd 3+) composite photocatalyst material, can be applicable to handle the organic pollutions such as methyl orange in the dyeing and printing sewage.
The present invention relates to a kind of preparation TiO 2The new method of/schorl/rare earth ion composite photocatalyst material, this photocatalysis raw material is mainly used in photocatalysis degradation organic contaminant.It is characterized by: the present invention is with schorl, butyl titanate and rare earth oxide (Nd 2O 3, Gd 2O 3) be primary raw material, press different proportion and mix, utilize sol-gel process to prepare xerogel, 3h is calcined in levigate back under 500 ℃ of conditions, promptly get TiO 2/ schorl/rare earth ion catalysis material.The prepared TiO of the present invention 2TiO in/schorl/rare earth ion composite photocatalyst material 2Constituent be mainly anatase mutually mutually on a small quantity for the rutile phase.The mass percent of the addition of said schorl powder is 1～2%, said rare earth ion (Nd 3+, Gd 3+) mass percent of addition is 0.1～0.2%
Said schorl powder originates from the Lingshou County, Hebei province, and powder granularity is at 600 orders.Its chemical composition is B 2O 3: SiO 9.72%, 2: Fe 36.72%, 2O 3: Al 4.77%, 2O 3: 31.08%, MgO:8.71%, Na 2O:1.90%, CaO:1.4%, K 2O:0.48%, MnO:0.03%, Li 2O:0.008%.
Said butyl titanate raw material is usually commercially available raw material, and its purity requirement is greater than 99.5%.
Said rare earth oxide Nd 2O 3, Gd 2O 3For common marketable material, "dead", harmless to health.Its purity requirement is greater than 99.5%.
Said preparation process adopts sol-gel process, and gel process carries out under 40 ℃ magnetic agitation.Gel through drying oven at 80 ℃ of following grind into powders behind the dry 24h, again through chamber type electric resistance furnace at 500 ℃ of calcining 3h down, promptly get TiO after the cooling 2/ schorl/rare earth ion catalysis material.
The TiO that makes 2TiO in/schorl/rare earth ion composite photocatalyst material 2Constituent be mutually anatase mutually with rutile on a small quantity mutually, TiO 2Average grain diameter at nanoscale.The catalysis material that makes is used for organic pollutions such as photocatalytic degradation methyl orange, and effect obviously is superior to pure TiO 2, composite to the high degradation rate of methyl orange than pure TiO 2Improved about 26%.This TiO that the present invention relates to 2The preparation method of/schorl/rare earth ion composite photocatalyst material has outstanding advantages such as cost is low, preparation process consumed energy is few, and the photocatalysis of the composite photocatalyst material of preparing is effective.
The specific embodiment
Below in conjunction with embodiment technical scheme of the present invention is further specified:
The present invention prepares the composition of raw materials and the proportioning that adopt in the process and is respectively: the volume ratio of absolute ethyl alcohol and butyl titanate 1: 1, the schorl powder accounts for 1～2% of total batching mass fraction, rare earth oxide (Nd 2O 3, Gd 2O 3) account for total batching mass fraction O.1～0.2%.Wherein, schorl powder degree is 600 orders, and purity requirement is greater than 99.8%; Rare earth oxide (Nd 2O 3, Gd 2O 3) purity requirement is greater than 99.5%; The butyl titanate purity requirement is greater than 99.5%; The addition of hydrolysis inhibitor red fuming nitric acid (RFNA) is a 3/10ml butyl titanate.
This preparation TiO that the present invention proposes 2The method of/schorl/rare earth ion composite photocatalyst material: at first get 100g schorl powder, place beaker, add the ultrasonic dispersion of deionized water 1h; The hydrochloric acid solution that behind the vavuum pump suction filtration, adds 1mol/L; Behind the ultrasonic dispersion 1h, leave standstill 24h, remove unnecessary hydrochloric acid; Repeatedly wash to neutrality with deionized water, put into the baking oven drying for standby.10mlTi (OC4H9) 4 is dissolved in the 10ml absolute ethyl alcohol, adds 3 red fuming nitric acid (RFNA)s with glue head dropper simultaneously, seal, at 40 ℃ of following vigorous stirring 30min, obtain clear solution 1. through magnetic stirring apparatus with preservative film.Rare earth oxide (Nd with certain mass 2O 3, Gd 2O 3) obtain the nitrate solution of rare earth with the dissolving of an amount of red fuming nitric acid (RFNA); This solution and 1.5ml deionized water, 15ml absolute ethyl alcohol, 1ml red fuming nitric acid (RFNA) are added in the separatory funnel jointly, obtain mixed solution 2., with the speed of 1/2s slowly be added drop-wise to solution 1. in; To delay hydrolysis rate; Avoid forming and reunite and deposition, vigorous stirring obtains vitreosol simultaneously.In gained colloidal sol, add pretreated schorl powder, behind magnetic force heating stirrer vigorous stirring 40min, ageing 24h obtains clear gel under the room temperature again.Clear gel except that after desolvating, grinds to form fine powder with the gained xerogel through oven drying (baking temperature is 80 ℃, and be 24h drying time), and calcining 3h under 500 ℃ promptly gets schorl/TiO again 2/ rare earth ion (Nd 3+, Gd 3+) composite photocatalyst material.
A kind of TiO 2Preparation technology's flow process of/schorl/rare earth ion composite photocatalyst material is: ageing → drying → calcining → TiO under raw material → pretreatment of raw material → batching batch mixing → magnetic agitation → room temperature 2/ schorl/rare earth ion catalysis material
Embodiment 1
Pretreatment of raw material:
The schorl powder is placed beaker, behind each 1h of the ultrasonic dispersion of the hydrochloric acid solution of deionized water and 1mol/L, leave standstill 24h, remove unnecessary hydrochloric acid, repeatedly wash to neutrality, put into the baking oven drying for standby with deionized water.
Raw material and proportioning: each 10ml of absolute ethyl alcohol and butyl titanate, the schorl powder accounts for 2% of total batching mass fraction, rare earth ion (Nd 3+, Gd 3+) account for 0.1% of total batching mass fraction.
The batching batch mixing:
Absolute ethyl alcohol and butyl titanate are packed in the beaker according to said ratio, add 3 red fuming nitric acid (RFNA)s with glue head dropper simultaneously, seal, at 40 ℃ of following vigorous stirring 30min, obtain clear solution 1. through magnetic stirring apparatus with preservative film.With 0.0369g (0.0364g) rare earth oxide Nd 2O 3(Gd 2O 3) obtain the nitrate solution of rare earth with the dissolving of an amount of red fuming nitric acid (RFNA); This solution and 1.5ml deionized water, 15ml absolute ethyl alcohol, 1ml red fuming nitric acid (RFNA) are added in the separatory funnel jointly, obtain mixed solution 2., with the speed of 1/2s slowly be added drop-wise to solution 1. in, vigorous stirring obtains vitreosol simultaneously.In gained colloidal sol, add pretreated schorl powder, again through magnetic force heating stirrer vigorous stirring 40min.
Ageing under the room temperature:
With the colloidal sol that stirs ageing 24h at room temperature, obtain clear gel.
Dry:
With clear gel with oven drying (baking temperature is 80 ℃, and be 24h drying time) remove desolvate after.
Calcining:
The gained xerogel is ground to form fine powder, and calcining 3h under 500 ℃ promptly gets schorl/TiO again 2/ rare earth ion (Nd 3+, Gd 3+) composite photocatalyst material.
Check: rare earth ion Nd 3+(Gd 3+) doping is 0.1%, the schorl doping is 2% TiO 2/ schorl/Nd 2O 3(Gd 2O 3) TiO in the composite photocatalyst material 2The thing phase composition be 86.15% (84.36%) anatase mutually with 13.85% (15.64%) rutile mutually, average grain diameter is 42.12nm (62.25nm), is 84.97% (98.67%) to the degradation rate of methyl orange.
Embodiment 2
Pretreatment of raw material:
The schorl powder is placed beaker, behind each 1h of the ultrasonic dispersion of the hydrochloric acid solution of deionized water and 1mol/L, leave standstill 24h, remove unnecessary hydrochloric acid, repeatedly wash to neutrality, put into the baking oven drying for standby with deionized water.
Raw material and proportioning: each 10ml of absolute ethyl alcohol and butyl titanate, the schorl powder accounts for 2% of total batching mass fraction, rare earth ion (Nd 3+, Gd 3+) account for 0.15% of total batching mass fraction.
The batching batch mixing:
Absolute ethyl alcohol and butyl titanate are packed in the beaker according to said ratio, add 3 red fuming nitric acid (RFNA)s with glue head dropper simultaneously, seal, at 40 ℃ of following vigorous stirring 30min, obtain clear solution 1. through magnetic stirring apparatus with preservative film.With 0.0552g (0.0546g) rare earth oxide Nd 2O 3(Gd 2O 3) obtain the nitrate solution of rare earth with the dissolving of an amount of red fuming nitric acid (RFNA); This solution and 1.5ml deionized water, 15ml absolute ethyl alcohol, 1ml red fuming nitric acid (RFNA) are added in the separatory funnel jointly, obtain mixed solution 2., with the speed of 1/2s slowly be added drop-wise to solution 1. in, vigorous stirring obtains vitreosol simultaneously.In gained colloidal sol, add pretreated schorl powder, again through magnetic force heating stirrer vigorous stirring 40min.
Ageing under the room temperature:
With the colloidal sol that stirs ageing 24h at room temperature, obtain clear gel.
Dry:
With clear gel with oven drying (baking temperature is 80 ℃, and be 24h drying time) remove desolvate after.
Calcining:
The gained xerogel is ground to form fine powder, and calcining 3h under 500 ℃ promptly gets schorl/TiO again 2/ rare earth ion (Nd 3+, Gd 3+) composite photocatalyst material.
Check: rare earth ion Nd 3+(Gd 3+) doping is 0.15%, the schorl doping is 2% TiO 2/ schorl/Nd 2O 3(Gd 2O 3) TiO in the composite photocatalyst material 2The thing phase composition be 86.75% (84.13%) anatase mutually with 13.25% (15.87%) rutile mutually, average grain diameter is 42.54nm (62.12nm), is 94.84% (94.38%) to the degradation rate of methyl orange.
Embodiment 3
Pretreatment of raw material:
The schorl powder is placed beaker, behind each 1h of the ultrasonic dispersion of the hydrochloric acid solution of deionized water and 1mol/L, leave standstill 24h, remove unnecessary hydrochloric acid, repeatedly wash to neutrality, put into the baking oven drying for standby with deionized water.
Raw material and proportioning: each 10ml of absolute ethyl alcohol and butyl titanate, the schorl powder accounts for 2% of total batching mass fraction, rare earth ion (Nd 3+, Gd 3+) account for 0.2% of total batching mass fraction.
The batching batch mixing:
Absolute ethyl alcohol and butyl titanate are packed in the beaker according to said ratio, add 3 red fuming nitric acid (RFNA)s with glue head dropper simultaneously, seal, at 40 ℃ of following vigorous stirring 30min, obtain clear solution 1. through magnetic stirring apparatus with preservative film.With 0.0632g (0.0728g) rare earth oxide Nd 2O 3(Gd 2O 3) obtain the nitrate solution of rare earth with the dissolving of an amount of red fuming nitric acid (RFNA); This solution and 1.5ml deionized water, 15ml absolute ethyl alcohol, 1ml red fuming nitric acid (RFNA) are added in the separatory funnel jointly, obtain mixed solution 2., with the speed of 1/2s slowly be added drop-wise to solution 1. in, vigorous stirring obtains vitreosol simultaneously.In gained colloidal sol, add pretreated schorl powder, again through magnetic force heating stirrer vigorous stirring 40min.
Ageing under the room temperature:
With the colloidal sol that stirs ageing 24h at room temperature, obtain clear gel.
Dry:
With clear gel with oven drying (baking temperature is 80 ℃, and be 24h drying time) remove desolvate after.
Calcining:
The gained xerogel is ground to form fine powder, and calcining 3h under 500 ℃ promptly gets TiO again 2/ schorl/rare earth ion (Nd 3+, Gd 3+) composite photocatalyst material.
Check: rare earth ion Nd 3+(Gd 3+) doping is 0.2%, the schorl doping is 2% TiO 2/ schorl/Nd 2O 3(Gd 2O 3) TiO in the composite photocatalyst material 2The thing phase composition be 86.71% (85.84%) anatase mutually with 13.29% (14.16%) rutile mutually, average grain diameter is 42.36nm (62.39nm), is 85.22% (86.72%) to the degradation rate of methyl orange.

Claims (6)

1. the present invention relates to a kind of preparation TiO 2The new method of/schorl/rare earth ion composite photocatalyst material, this photocatalysis raw material is mainly used in photocatalysis degradation organic contaminant, it is characterized by: the present invention is with schorl, butyl titanate and rare earth oxide (Nd 2O 3, Gd 2O 3) be primary raw material, press different proportion and mix, add red fuming nitric acid (RFNA) as hydrolysis inhibitor.Utilize sol-gel process to prepare xerogel, 3h is calcined in levigate back under 500 ℃ of conditions, promptly get TiO 2/ schorl/rare earth ion composite photocatalyst material, the prepared TiO of the present invention 2TiO in/schorl/rare earth ion composite photocatalyst material 2Constituent be mainly anatase mutually mutually on a small quantity for the rutile phase, the mass percent of the addition of said schorl powder is 1～2%, said rare earth ion (Nd 3+, Gd 3+) mass percent of addition is 0.1～0.2%.
2. a kind of preparation TiO according to claim 1 2The method of/schorl/rare earth ion composite photocatalyst material is characterized in that: said schorl powder originates from the Lingshou County, Hebei province, and powder granularity is at 600 orders; Its chemical composition is B 2O 3: SiO 9.72%, 2: Fe 36.72%, 2O 3: Al 4.77%, 2O 3: 31.08%, MgO:8.71%, Na 2O:1.90%, CaO:1.4%, K 2O:0.48%, MnO:0.03%, Li 2O:0.008%.
3. a kind of preparation TiO according to claim 1 2The method of/schorl/rare earth ion composite photocatalyst material is characterized in that: said butyl titanate raw material is common commercially available raw material, and its purity requirement is greater than 99.5%.
4. a kind of preparation TiO according to claim 1 2The method of/schorl/rare earth ion composite photocatalyst material is characterized in that: said rare earth oxide Nd 2O 3, Gd 2O 3Be common marketable material, its purity requirement is greater than 99.5%.
5. a kind of preparation TiO according to claim 1 2The method of/schorl/rare earth ion composite photocatalyst material; It is characterized in that: said preparation process adopts sol-gel process; Gel process carries out under 40 ℃ magnetic agitation; Gel through drying oven at 80 ℃ of following grind into powders behind the dry 24h, again through chamber type electric resistance furnace at 500 ℃ of calcining 3h down, promptly get TiO after the cooling 2/ schorl/rare earth ion composite photocatalyst material.
6. a kind of preparation TiO according to claim 1 2The method of/schorl/rare earth ion composite photocatalyst material is characterized in that: the catalysis material that makes is used for organic pollutions such as photocatalytic degradation methyl orange, and effect obviously is superior to pure TiO 2, composite to the high degradation rate of methyl orange than pure TiO 2Improved about 26%, this TiO that the present invention relates to 2The preparation method of/schorl/rare earth ion composite photocatalyst material has outstanding advantages such as cost is low, preparation process consumed energy is few, and the photocatalysis of the catalysis material of preparing is effective.
CN 201210326321 2012-09-06 2012-09-06 Preparation method of TiO2/schorlite/rare earth ion composite photo-catalytic material Pending CN102836728A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103641128A (en) * 2013-11-18 2014-03-19 江西理工大学 Sealed molten salt method used for changing surfaces of black tourmaline into red
CN110564051A (en) * 2019-08-07 2019-12-13 千年舟新材科技集团有限公司 negative ion functional PP decorative film and preparation method and application thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103641128A (en) * 2013-11-18 2014-03-19 江西理工大学 Sealed molten salt method used for changing surfaces of black tourmaline into red
CN103641128B (en) * 2013-11-18 2015-08-26 江西理工大学 A kind of aphrizite surface changes red closed system molten-salt growth method method
CN110564051A (en) * 2019-08-07 2019-12-13 千年舟新材科技集团有限公司 negative ion functional PP decorative film and preparation method and application thereof

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Application publication date: 20121226