CN104437460B - The photochemical catalyst nano composite material prepared based on single-phase bismuth titanate - Google Patents

The photochemical catalyst nano composite material prepared based on single-phase bismuth titanate Download PDF

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CN104437460B
CN104437460B CN201410673747.3A CN201410673747A CN104437460B CN 104437460 B CN104437460 B CN 104437460B CN 201410673747 A CN201410673747 A CN 201410673747A CN 104437460 B CN104437460 B CN 104437460B
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bismuth
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tio
photochemical catalyst
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CN104437460A (en
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熊菊莲
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Jining High Tech Keda Technology Project Service Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts 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
    • B01J23/18Arsenic, antimony or bismuth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/396Distribution of the active metal ingredient
    • B01J35/399Distribution of the active metal ingredient homogeneously throughout the support particle

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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Abstract

The present invention is open a kind of based on single-phase bismuth titanate (Bi20TiO32) the photochemical catalyst nano composite material prepared, it is to prepare Bi by supercritical methanol technology20TiO32During add a small amount of Graphene and together react, make the Bi that reaction is formed20TiO32Being uniformly dispersed on graphene film, this is conducive to the diffusion of reactant and product, and then the raising of beneficially photocatalysis performance, and last fired crystallization forms Graphene Bi20TiO32Nano composite material.Preparation process reaction condition of the present invention is gentle, it is relatively low to realize cost, and the photocatalysis performance of the photochemical catalyst nano composite material prepared is better than single-phase bismuth titanate, and tool has a broad prospect of the use.

Description

The photochemical catalyst nano composite material prepared based on single-phase bismuth titanate
Technical field
The present invention relates to photocatalysis technology, especially relate to a kind of photocatalysis prepared based on single-phase bismuth titanate Agent nano composite material.
Background technology
Bi and Ti is because non-toxic inexpensive is referred to as " green metal ", Bi2Q3And TiQ2Compound can be formed many Plant the composite oxides of crystal phase structure.Bismuth titanates series is a kind of typical Aurivillius stratified material, it Crystal formation specifically include that Bi4Ti3O12、Bi2Ti2O7、Bi12TiO20、Bi20TiO32Deng.Study table Bright molecular formula is Bi20TiO32Single-phase bismuth titanate nano-material can be used as visible light-responded photocatalytic degradation Pollutant.
Bi20TiO32Being the one of the bismuth titanates series material with photocatalytic activity, it disclosure satisfy that at the sun Still there is under light this requirement of high photocatalysis performance, and this material itself is nontoxic, meets novel The requirement of environmentally friendly catalysis material.
But, single-phase Bi20TiO32Have the drawback that as photochemical catalyst
1, under general condition, single-phase Bi20TiO32Being in a kind of metastable state, it is only at titanium bismuth mixed oxidization Thing is to Bi2Ti2O7Occur during transformation of crystal, by consulting Bi2O3-TiO2The phasor of system understands, Bi under normal conditions20TiO32Being in metastable state, it is to be formed under conditions of temperature is less than 400 DEG C 's.Synthesis temperature in existing method is higher, due to single-phase Bi20TiO32Synthesis condition harshness and meta-stable thereof Property, at present in addition to high temperature quenching method, also do not have other synthesize in a mild condition have higher too The single-phase Bi of sun photocatalytic activity20TiO32The report of nano-photocatalyst material.
2, single-phase Bi20TiO32Nano-photocatalyst material is higher because of the recombination probability of photogenerated charge, causes its light Catalysis activity performance is the highest.To this end, improve the separative efficiency of bismuth titanates photo-generated carrier the most further And then improve its photocatalysis performance, it has also become currently one of technical barrier needing research badly.
Summary of the invention
For overcoming the defect of prior art, the present invention proposes a kind of based on single-phase bismuth titanate (Bi20TiO32) system Standby photochemical catalyst nano composite material, preparation process reaction condition is gentle, it is relatively low to realize cost, and system The photocatalysis performance of the standby photochemical catalyst nano composite material obtained is better than single-phase bismuth titanate (Bi20TiO32)。
The present invention adopts the following technical scheme that realization: a kind of photochemical catalyst prepared based on single-phase bismuth titanate is received Nano composite material, the nano combined material of this photochemical catalyst prepared by following steps:
Soluble bismuth salt being joined in carboxylic acid, making bismuth/carboxylic acid mol ratio is 1:50-70, and stirring is to bismuth salt Adding titanate esters after being completely dissolved, the mol ratio making titanium/bismuth is 1:8-13, adds structure directing agent, makes The mol ratio of bismuth/structure directing agent is 1:3-4.5, is stirring evenly and then adding into urea, make bismuth/urea mole Ratio is 1:0.5-3, obtains the first mixed solution;
Being injected in alcoholic solvent by first mixed solution, alcoholic solvent volume is 25-45mL every gram soluble bismuth salt Raw material, and in every 100ml alcoholic solvent, add the Graphene of 0.5~2g, it is transferred to high pressure after mixing anti- Answer in still, be passed through 8~12bar nitrogen, under it is protected, be heated to 200-250 DEG C keep 2-6h, make bismuth salt complete All-hydrolytic or alcoholysis, then open vent valve door row and go out the presoma that solvent obtains being dried;
Being washed repeatedly by ethanol and deionized water successively by presoma, at 300-400 DEG C, roasting is brilliant after drying Change 4-6h, cool down and i.e. obtain photochemical catalyst Graphene-Bi20TiO32Nano composite material.
Wherein, described soluble bismuth salt is bismuth nitrate or bismuth chloride.
Wherein, described titanate esters is butyl titanate or isopropyl titanate, or the arbitrary proportion of both mixes Compound.
Wherein, during described structure directing agent is the tert-butyl alcohol, phenmethylol, benzyl carbinol and p nitrobenzyl alcohol A kind of or the arbitrary proportion mixture of these four.
Wherein, the arbitrary proportion mixture of a kind of or these three during alcoholic solvent is methyl alcohol, ethanol and propyl alcohol.
Compared with prior art, there is advantages that
Photochemical catalyst nano composite material of the present invention is to prepare Bi by supercritical methanol technology20TiO32During add A small amount of Graphene together reacts, and makes the Bi that reaction is formed20TiO32It is uniformly dispersed on graphene film, this Be conducive to reactant and the diffusion of product, and then the raising of beneficially photocatalysis performance, last fired crystalline substance Change and form Graphene-Bi20TiO32Nano composite material.The photochemical catalyst Graphene prepared due to the present invention- Bi20TiO32Nano composite material has the biggest surface area and higher porosity, thus improves stone Ink alkene-Bi20TiO32The nano composite material pre-adsorption capacity to the contaminant molecule that is degraded, meanwhile, also shape Become the biggest diffusion admittance, can be with contaminant restraining to space during single or multiple recycles Blocking, it is to avoid Graphene-Bi20TiO32The inactivation of nano composite material, such that it is able to keep higher Photocatalytic activity and stability.It addition, Graphene-Bi20TiO32The photocatalysis performance of nano composite material carries High source efficiently separating and transmitting in photogenerated charge, by synthesizing single-phase Bi20TiO32During add A small amount of Graphene, thus react formation Graphene-Bi20TiO32Nano composite material, this Graphene- Bi20TiO32Nano composite material is at Graphene and Bi20TiO32Define closely-coupled boundary between the two Face, thus constructed the transmission of good electron propagation ducts, beneficially light induced electron, and then improve light The separative efficiency of raw carrier, thus compare single-phase Bi20TiO32There is more preferably photocatalysis performance.This Bright widen single-phase Bi20TiO32In the application of photocatalysis field, tool has a broad prospect of the use.
Accompanying drawing explanation
Fig. 1 is Bi20TiO32And Graphene-Bi20TiO32XRD schematic diagram.
Detailed description of the invention
The application indication single-phase bismuth titanate molecular formula i.e. is Bi20TiO32, therefore in the context of this application " single-phase bismuth titanate ", " the single-phase Bi mentioned20TiO32" and " Bi20TiO32" all implications are identical.
The present invention proposes a kind of photochemical catalyst nano composite material prepared based on single-phase bismuth titanate, prepares Journey reaction condition is gentle, it is relatively low to realize cost, and the light of the photochemical catalyst nano composite material prepared Catalytic performance is better than single-phase bismuth titanate.
Photochemical catalyst nano composite material of the present invention is to prepare Bi by supercritical methanol technology20TiO32During add A small amount of Graphene together reacts, and makes the Bi that reaction is formed20TiO32It is uniformly dispersed on graphene film, this Be conducive to reactant and the diffusion of product, and then the raising of beneficially photocatalysis performance, last fired crystalline substance Change and form Graphene-Bi20TiO32Nano composite material.
It is prepared as follows:
1. the preparation of raw material: soluble bismuth salt joined in small-molecular-weight carboxylic acid, makes bismuth/carboxylic acid mol ratio For 1:50-70, it is stirred continuously to bismuth salt and is completely dissolved, then in solution, be added dropwise over titanate esters, make titanium/bismuth Mol ratio is 1:8-13, and the alcohol being added thereto to molecular weight after continuing to stir to clarify bigger is led as structure To agent, making bismuth/alcohol mol ratio is 1:3-4.5, can be added thereto to urea, make bismuth/urine after stirring Element mol ratio is 1:0.5-3, stirs to clarify transparent, obtains the first mixed solution;
2. supercritical reaction: step 1. gained the first mixed solution is injected into the alcoholic solvent of molecular weight In, solvent volume is 25-45mL every gram soluble bismuth salt raw material, and adds 0.5~2g in every 100ml solvent Graphene, be transferred to after mixing in autoclave, be passed through 8~12bar nitrogen, its protect under It is heated to 200-250 DEG C and keeps 2-6h, make bismuth salt complete hydrolysis or alcoholysis, then open vent valve door row and go out Solvent obtains the presoma being dried;
3. crystallization shapes: presoma step 2. prepared washs repeatedly by ethanol and deionized water successively, Dried roasting crystallization 4-6h at 300-400 DEG C, take out after being cooled to room temperature i.e. obtain photochemical catalyst Graphene- Bi20TiO32Nano composite material.
In above step, soluble bismuth salt is bismuth nitrate or bismuth chloride etc., and small-molecular-weight carboxylic acid is formic acid, second Acid or propionic acid etc., titanate esters is butyl titanate or isopropyl titanate etc., and the alcohol that molecular weight is bigger is tertiary fourth Alcohol, phenmethylol, benzyl carbinol or p nitrobenzyl alcohol etc., the alcohol of molecular weight is methyl alcohol, ethanol or third Alcohol etc..Wherein, small-molecular-weight carboxylic acid is primary solvent, and it can make titanate esters and the hydrolytic process of bismuth salt Slowing down and mutually suppress, make obtained solution-stabilized and clarify, the urea added can regulate product Pattern so that affect its photocatalysis performance.
Further, the photochemical catalyst Graphene-Bi that the inventive method prepares20TiO32Nano composite material, by Less in Graphene content, still keep single-phase Bi20TiO32Laminated structure with holes, use transmission electron microscope Observing visible chip size is 20-100nm, and sheet mesoporous is 8-10nm.
Embodiment 1
Weighing 8g bismuth nitrate and join in acetic acid, making bismuth/carboxylic acid mol ratio is 1:70, is stirred continuously to nitric acid Bismuth is added dropwise over butyl titanate after being completely dissolved the most wherein, and making titanium/bismuth mol ratio is 1:13, continues to stir Mixing to obtain injecting structure directed agents phenmethylol wherein after clarified solution, making bismuth/alcohol mol ratio is 1:4.5, the most backward Adding urea in above-mentioned solution, making bismuth/urea mol ratio is 1:3, then stirs to solution clear.Will Obtained solution is injected in 360mL alcohol solvent, after adding 1.8g Graphene, stirs 4 hours, mixed Move in autoclave after closing uniformly, under the protection of 12bar nitrogen, be heated to 250 DEG C keep 6h, make nitre Acid bismuth complete hydrolysis or alcoholysis, then open vent valve door row and go out the presoma that solvent obtains being dried, then will This presoma respectively washs 5 times by ethanol and deionized water successively, roasting crystallization 4h at 400 DEG C after drying, Photochemical catalyst Graphene-Bi is taken out to obtain after being cooled to room temperature20TiO32Nano composite material.
Embodiment 2
Weighing 8g bismuth nitrate and join in acetic acid, making bismuth/carboxylic acid mol ratio is 1:50, is stirred continuously to nitre Acid bismuth is added dropwise over butyl titanate after being completely dissolved the most wherein, and making titanium/bismuth mol ratio is 1:8, continues Stirring to obtain injecting structure directed agents phenmethylol wherein after clarified solution, making bismuth/alcohol mol ratio is 1:3, the most backward Adding urea in above-mentioned solution, making bismuth/urea mol ratio is 1:0.5, then stirs to solution clear. Obtained solution is injected in 200mL alcohol solvent, after adding 1g Graphene, stirs 2 hours, mixed Move in autoclave after closing uniformly, under the protection of 8bar nitrogen, be heated to 250 DEG C keep 6h, make nitre Acid bismuth complete hydrolysis or alcoholysis, then open vent valve door row and go out the presoma that solvent obtains being dried, then will This presoma respectively washs 5 times by ethanol and deionized water successively, roasting crystallization 6h at 300 DEG C after drying, Photochemical catalyst Graphene-Bi is taken out to obtain after being cooled to room temperature20TiO32Nano composite material.
Embodiment 3
Weighing 8g bismuth nitrate and join in acetic acid, making bismuth/carboxylic acid mol ratio is 1:65, is stirred continuously to nitre Acid bismuth is added dropwise over butyl titanate after being completely dissolved the most wherein, and making titanium/bismuth mol ratio is 1:12, continues Stirring to obtain injecting structure directed agents phenmethylol wherein after clarified solution, making bismuth/alcohol mol ratio is 1:4, the most backward Adding urea in above-mentioned solution, making bismuth/urea mol ratio is 1:0.8, then stirs to solution clear. Obtained solution is injected in 260mL alcohol solvent, after adding 2.4g Graphene, stirs 4 hours, Move in autoclave after mixing, under the protection of 12bar nitrogen, be heated to 200 DEG C keep 6h, make Bismuth nitrate complete hydrolysis or alcoholysis, then open vent valve door row and go out the presoma that solvent obtains being dried, then This presoma is respectively washed 5 times by ethanol and deionized water successively, roasting crystallization 5h at 400 DEG C after drying, Photochemical catalyst Graphene-Bi is taken out to obtain after being cooled to room temperature20TiO32Nano composite material.
From the Bi of Fig. 120TiO32And Graphene-Bi20TiO32XRD schematic diagram it can be seen that can become Merit realize titanium ion and bismuth ion to metastable state bismuth titanates (Bi20TiO32) conversion.Additionally, can from Fig. 1 Know, Graphene-Bi20TiO32Composite maintains metastable state bismuth titanates (Bi20TiO32) crystal structure; Owing in complex, Graphene content is relatively low, the compound of a certain amount of Graphene does not affects metastable state metatitanic acid Bismuth (Bi20TiO32) crystal structure.
Weigh the catalyst Graphene-Bi of the above-mentioned preparation of 0.1g20TiO32, disperseed the 1 of fourth 100ml ×10-5In the beaker (250ml) of M methyl orange solution, magnetic agitation 60min under dark condition so that it is Suction-desorption equilibrium can be reached, after tool balance, this system is put into sun-drenched also side, at the sun The catalytic degradation of methyl orange is carried out under light direct irradiation.Every certain reaction time, take 5ml reactant liquor, And separated by supercentrifuge, take out supernatant.Centrifugate is examined via ultraviolet-visible spectrophotometer Survey, and the change observing about maximum absorption peak intensity at 464nm speculates the dense of methyl orange degradation Degree change.Test result indicate that, the Graphene-Bi of the present invention20TiO32Photocatalytic activity is far above Bi20TiO32And commercialization P25 (titanium dioxide).Graphene-Bi20TiO32Catalyst at 75 minutes degradation rates is 98%;Bi20TiO32Light urges agent to be 72% at 75 minutes degradation rates, degradable, needs about 2.5 hours; And P25 only degraded 57% when 75 minutes, degradable, need 3.5 hours.
It addition, photochemical catalyst Graphene-Bi prepared by the present invention20TiO32Also have and preferably reuse spy Property.
Photochemical catalyst Graphene-the Bi prepared due to the present invention20TiO32Nano composite material has the biggest Surface area and higher porosity, thus improve Graphene-Bi20TiO32Nano composite material is to being dropped Solve the pre-adsorption capacity of contaminant molecule, meanwhile, also form the biggest diffusion admittance, at single or many During secondary recycling can be with the contaminant restraining blocking to space, it is to avoid Graphene-Bi20TiO32Receive The inactivation of nano composite material, such that it is able to keep higher photocatalytic activity and stability.It addition, graphite Alkene-Bi20TiO32The photocatalysis performance raising of nano composite material comes from efficiently separating and passing of photogenerated charge Defeated, by synthesizing Bi after adding a small amount of Graphene20TiO32, thus form Graphene-Bi20TiO32Nanometer is multiple Condensation material, this Graphene-Bi20TiO32Nano composite material is at Graphene and Bi20TiO32Formed between the two Closely-coupled interface, thus constructed the biography of good electron propagation ducts, beneficially light induced electron Defeated, and then the separative efficiency of raising photo-generated carrier, thus compare Bi20TiO32There is more preferably photocatalysis Performance.The present invention has widened Bi20TiO32In the application of photocatalysis field, tool has a broad prospect of the use.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this Any amendment, equivalent and the improvement etc. made within the spirit of invention and principle, should be included in this Within the protection domain of invention.

Claims (5)

1. the photochemical catalyst nano composite material prepared based on single-phase bismuth titanate, it is characterised in that this light is urged The nano combined material of agent is prepared by following steps:
Soluble bismuth salt being joined in carboxylic acid, making bismuth/carboxylic acid mol ratio is 1:50-70, and stirring is to bismuth salt Adding titanate esters after being completely dissolved, the mol ratio making titanium/bismuth is 1:8-13, adds structure directing agent, makes The mol ratio of bismuth/structure directing agent is 1:3-4.5, is stirring evenly and then adding into urea, make bismuth/urea mole Ratio is 1:0.5-3, obtains the first mixed solution;
Being injected in alcoholic solvent by first mixed solution, alcoholic solvent volume is 25-45mL every gram soluble bismuth salt Raw material, and in every 100ml alcoholic solvent, add the Graphene of 0.5~2g, it is transferred to high pressure after mixing anti- Answer in still, be passed through 8~12bar nitrogen, under it is protected, be heated to 200-250 DEG C keep 2-6h, make bismuth salt complete All-hydrolytic or alcoholysis, then open vent valve door row and go out the presoma that solvent obtains being dried;
Being washed repeatedly by ethanol and deionized water successively by presoma, at 300-400 DEG C, roasting is brilliant after drying Change 4-6h, cool down and i.e. obtain photochemical catalyst Graphene-Bi20TiO32Nano composite material.
The photochemical catalyst nano composite material prepared based on single-phase bismuth titanate the most according to claim 1, It is characterized in that, described soluble bismuth salt is bismuth nitrate or bismuth chloride.
The photochemical catalyst nano composite material prepared based on single-phase bismuth titanate the most according to claim 1, It is characterized in that, described titanate esters is butyl titanate or isopropyl titanate, or the arbitrary proportion of both Mixture.
The photochemical catalyst nano composite material prepared based on single-phase bismuth titanate the most according to claim 1, It is characterized in that, described structure directing agent is in the tert-butyl alcohol, phenmethylol, benzyl carbinol and p nitrobenzyl alcohol A kind of or arbitrary proportion mixture of these four.
The photochemical catalyst nano composite material prepared based on single-phase bismuth titanate the most according to claim 1, It is characterized in that, alcoholic solvent is the arbitrary proportion mixing of a kind of or these three in methyl alcohol, ethanol and propyl alcohol Thing.
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CN201610514932.7A CN106179313A (en) 2014-11-20 2014-11-20 The photocatalyst nano composite material prepared based on single-phase bismuth titanate
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