CN109772348A - A kind of erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper and its preparation method and application - Google Patents
A kind of erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to catalysis material technical field, a kind of erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper and its preparation method and application are disclosed.The photochemical catalyst is prepared by following methods: (1) carrier of photocatalyst being put into acid solution and impregnated, then taken out and clean and dry, then high-temperature calcination is spare；(2) it is in batches dissolved in iron containing compounds, bismuth-containing compound, copper-containing compound in same nitric acid solution and containing erbium compound, obtains solution A；(3) continue that alkaline solution is added dropwise into solution A under stirring condition, until precipitating completely, forms colloid；(4) the calcined carrier of photocatalyst of step (1) high temperature is immersed in the colloid in step (3), taking-up is calcined under the high temperature conditions up to the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper.Gained catalyst of the invention is remarkably reinforced compared to pure bismuth ferrite photocatalysis performance, and catalyst is immobilized secured, not easily to fall off, and preparation process is simple, reproducible.
Description
Technical field
The invention belongs to catalysis material technical field, in particular to a kind of erbium-codoped bismuth ferrite photocatalysis of solid-carrying type copper
Agent and its preparation method and application.
Background technique
With the improvement of people's living standards, more and more people start to pay attention to environmental problem.Instantly, organic contamination is
In environmental problem one of the problem of most serious.In recent years, photochemical catalyst in terms of organic pollutant processing application at
For one of the hot spot of people's research.Bismuth ferrite is that one kind can be urged using the novel semi-conductor light that visible light carries out photocatalysis
Agent, and at room temperature with ferroelectricity and magnetic material, chemical property is stable and at low cost, before tempting application
Scape.But it causes catalytic efficiency not high since bismuth ferrite quantum yield is low and weak magnetic causes separating effect bad and restricts
Its application, therefore to its A have important show with B progress codopes to improve the performance of its optics, electricity and magnetics
Sincere justice.
Currently, photocatalysis oxidation technique is appointed in practical applications, there are some problems.Mainly photochemical catalyst is difficult to separate
Recycling, since most of used photochemical catalyst is powder to photocatalysis oxidation technique during handling organic pollutant,
It is easy to agglomerate in water, is not easily settled, easily causes photochemical catalyst to be lost, be unfavorable for the regeneration and recycling of photochemical catalyst.By light
The immobilized problem that can solve separation and recovery of catalyst hardly possible of catalyst, can also overcome suspended phase poor catalyst stability and easily in
The disadvantage of poison.Therefore, developing a kind of stabilization, efficient immobilization photochemical catalyst and carrying out the application of its photocatalysis oxidation technique is
The difficult point of the relevant technologies.It finds a kind of with multiple hole, the excellent load that large specific surface area, adsorption capacity is strong, chemical property is stable
Body, the shortcomings that can effectively solve photochemical catalyst.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of solid-carrying type copper
The preparation method of erbium-codoped bismuth ferrite photocatalyst.
Another object of the present invention is to provide the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper of above method preparation.
Still a further object of the present invention is to provide the above-mentioned erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper in the treatment of waste water
Application.
The purpose of the present invention is realized by following proposal:
A kind of preparation method of the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper, mainly comprises the steps that
(1) carrier of photocatalyst is put into dilute acidic solution under room temperature and is impregnated 1 hour, then taken out and clean and dry,
Final high temperature calcining, it is spare；
(2) by iron containing compounds, bismuth-containing compound, copper-containing compound and to be dissolved in containing erbium compound same nitric acid in batches molten
In liquid, solution A is obtained；
(3) continue that alkaline solution is added dropwise into solution A under stirring condition, until precipitating completely, forms colloid；
(4) the calcined carrier of photocatalyst of step (1) high temperature is immersed in the colloid in step (3), impregnates one section
Drying is taken out after time to immerse again, is taken out and is calcined under the high temperature conditions up to the erbium-codoped bismuth ferrite of solid-carrying type copper after being repeated several times
Photochemical catalyst.
Carrier of photocatalyst described in step (1) can be ceramic honey comb, foamed iron, foam copper, glass, magnesium alloy, aluminium
The carrier material commonly used in the art such as alloy, ceramic membrane；The acid solution be acetic acid, sulfuric acid, nitric acid, hydrochloric acid and its
One or more of his acidic aqueous solution, the acid solution concentration are 5wt%~15wt%.
High-temperature calcination described in step (1) refers in 200~800 DEG C of 0.5~4h of calcining.
Iron containing compounds described in step (2) are preferably ferric nitrate；The bismuth-containing compound is preferably bismuth nitrate；Institute
The copper-containing compound stated is preferably copper nitrate；Described is preferably erbium nitrate containing erbium compound.
The concentration of nitric acid solution described in step (2) is 0.01~6mol/L；Iron content chemical combination described in step (2)
Object, bismuth-containing compound, copper-containing compound and the dosage containing erbium compound are the erbium-codoped bismuth ferrite of copper formed in step (2)
Chemical formula metered proportions be Bi1-xErxFe1-yCuyO3(0 < x≤0.1,0 < y≤0.1).
Alkaline solution described in step (3) is sodium hydroxide solution, potassium hydroxide solution, ammonium hydroxide and other common alkali
Property solution；Stirring described in step (3) refers to that mixing speed is 300~1000r/min, dropwise addition described in step (3)
Preferably rate of addition is 1~2 drop/s.
Time of infusion described in step (4) refers to 0.5~1h of dipping；The drying refers at 60~100 DEG C
Dry 0.5~2h；The dipping refers to dipping 1~10 time for several times；
High-temperature calcination described in step (4) refers to 0.5~4h of calcining at 200~800 DEG C.
A kind of erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper prepared by the above method.
Application of the above-mentioned erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper in waste water treatment is preferably dropped in photocatalysis
Solution is containing the application in aniline waste water.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
The present invention by iron containing compounds, bismuth-containing compound, copper-containing compound and containing erbium compound prepares to form colloid, passes through
The method calcined enters copper erbium co-doped in bismuth ferrite after dipping colloid, and is covered on carrier and obtains that homogeneity is good, urges
Change the high solid-carrying type photocatalyst material of activity, gained catalyst is remarkably reinforced compared to pure bismuth ferrite photocatalysis performance, catalyst
It is immobilized secured, not easily to fall off；Carrier can choose the strong material of multiple hole, large specific surface area, adsorption capacity, increase photocatalysis
Reaction site improves photocatalysis efficiency.And preparation process of the present invention is simple, it is reproducible.
Detailed description of the invention
Fig. 1 is embodiment 1, the photochemical catalyst prepared in comparative example 1 and 2 to the degradation curve figure of aniline.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1
Ceramic honey comb sample is put into 10% dilute nitric acid solution and is impregnated 1 hour, is rinsed after taking-up with deionized water, so
80 DEG C drying 2 hours in baking oven are placed on, 300 DEG C of Muffle furnace is put into and calcines 3 hours, it is spare.Prepare the nitric acid solution of 2mol/L
20mL, according to Bi0.95Er0.05Fe0.95Cu0.05O3Chemical formula metering ratio ferric nitrate, bismuth nitrate, copper nitrate and erbium nitrate are dissolved in
In the nitric acid solution；It is straight that sodium hydroxide solution is slowly added dropwise into above-mentioned nitric acid solution under the lasting stirring of 700r/min
Completely to precipitating, colloid is formed；Spare ceramic honey comb is immersed in the colloid again, dipping takes out after 0.5 hour and is placed in baking oven
In 80 DEG C drying 0.5 hour, dry 0.5 hour after then impregnating 0.5 hour again, be so repeated 8 times, then ceramic honey comb is put
Enter 600 DEG C of Muffle furnace to calcine 1 hour, obtain the erbium-codoped bismuth ferrite photocatalyst of the immobilized copper of ceramic honey comb, photochemical catalyst is negative
Carrying capacity is 25.5%, and 90 minutes degradation rates to aniline sewage are 97.5%.
Embodiment 2:
Ceramic honey comb sample is put into 10% dilution heat of sulfuric acid and is impregnated 1 hour, is rinsed after taking-up with deionized water, so
80 DEG C drying 2 hours in baking oven are placed on, 800 DEG C of Muffle furnace is put into and calcines 0.5 hour, it is spare.Prepare the nitric acid of 0.5mol/L
Solution 20mL, according to Bi0.9Er0.1Fe0.95Cu0.05O3Chemical formula metering than by ferric nitrate, bismuth nitrate, copper nitrate and erbium nitrate
It is dissolved in the nitric acid solution；Ammonium hydroxide is slowly added dropwise into above-mentioned nitric acid solution under the lasting stirring of 700r/min until heavy
It forms sediment completely, forms colloid；Spare ceramic honey comb is immersed in the colloid again, dipping takes out be placed in baking oven 80 DEG C after forty minutes
It is 0.5 hour dry, it then impregnates and dries 0.5 hour after forty minutes again, be so repeated 6 times, then ceramic honey comb is put into Muffle
800 DEG C of furnace are calcined 0.5 hour, and the erbium-codoped bismuth ferrite photocatalyst of the immobilized copper of ceramic honey comb, photocatalyst amount are obtained
It is 22.8%, 90 minutes degradation rates to aniline sewage are 92.8%.
Embodiment 3:
Foam copper sample is put into 10% hydrochloric acid solution and is impregnated 1 hour, is rinsed after taking-up with deionized water, is then set
80 DEG C drying 2 hours in baking oven are put into 600 DEG C of Muffle furnace and calcine 1 hour, spare.The nitric acid solution 20mL of 1mol/L is prepared,
According to Bi0.95Er0.05Fe0.9Cu0.1O3Chemical formula metering than ferric nitrate, bismuth nitrate, copper nitrate and erbium nitrate be dissolved in the nitric acid
In solution；Potassium hydroxide solution is slowly added dropwise into above-mentioned nitric acid solution under the lasting stirring of 700r/min until precipitating
Completely, colloid is formed；Spare foam copper is immersed in the colloid again, dipping takes out after 50 minutes and is placed in 80 DEG C of dryings in baking oven
It is 0.5 hour, 0.5 hour dry after then impregnating 50 minutes again, it is so repeated 4 times, then foam copper is put into 500 DEG C of Muffle furnace
Calcining 2 hours, obtains the erbium-codoped bismuth ferrite photocatalyst of the immobilized copper of foam copper, and photocatalyst amount is 18.6%, 90
Minute is 85.6% to the degradation rate of aniline sewage.
Embodiment 4:
Foam copper sample is put into 10% dilute nitric acid solution and is impregnated 1 hour, is rinsed after taking-up with deionized water, then
80 DEG C drying 2 hours in baking oven are placed in, 500 DEG C of Muffle furnace is put into and calcines 2 hours, it is spare.Prepare the nitric acid solution of 3mol/L
20mL, according to Bi0.9Er0.1Fe0.9Cu0.1O3Chemical formula metering than ferric nitrate, bismuth nitrate, copper nitrate and erbium nitrate be dissolved in this
In nitric acid solution；Be slowly added dropwise under the lasting stirring of 700r/min into above-mentioned nitric acid solution sodium hydroxide solution until
Precipitating completely, forms colloid；Spare foam copper is immersed in the colloid again, dipping takes out after 1 hour and is placed in baking oven 80 DEG C
It is 0.5 hour dry, it is 0.5 hour dry after then impregnating 1 hour again, it is so repeated 2 times, then foam copper is put into Muffle furnace
300 DEG C are calcined 3 hours, obtain the erbium-codoped bismuth ferrite photocatalyst of the immobilized copper of foam copper, photocatalyst amount is
13.4%, 90 minutes degradation rates to aniline sewage are 86.8%.
Embodiment 5:
Foam iron sample is put into 15% acetum and is impregnated 1 hour, is rinsed after taking-up with deionized water, is then set
80 DEG C drying 2 hours in baking oven are put into 200 DEG C of Muffle furnace and calcine 4 hours, spare.The nitric acid solution 20mL of 5mol/L is prepared,
According to Bi0.92Er0.08Fe0.97Cu0.03O3Chemical formula metering than ferric nitrate, bismuth nitrate, copper nitrate and erbium nitrate be dissolved in the nitre
In acid solution；Potassium hydroxide solution is slowly added dropwise into above-mentioned nitric acid solution under the lasting stirring of 700r/min until heavy
It forms sediment completely, forms colloid；Spare foamed iron is immersed in the colloid again, dipping takes out to be placed in baking oven after 1 hour and do for 80 DEG C
It is dry 0.5 hour, 0.5 hour dry after then impregnating 1 hour again, it is so repeated 10 times, then foamed iron is put into Muffle furnace 200
DEG C calcining 4 hours, obtaining the erbium-codoped bismuth ferrite photocatalyst of the immobilized copper of foamed iron, photocatalyst amount is 14.5%,
90 minutes degradation rates to aniline sewage are 87.3%.
Comparative example 1
Ceramic honey comb sample is put into 10% dilute nitric acid solution and is impregnated 1 hour, is rinsed after taking-up with deionized water, so
80 DEG C drying 2 hours in baking oven are placed on, 300 DEG C of Muffle furnace is put into and calcines 3 hours, it is spare.Then by spare ceramic honey comb
It immerses in deionized water, dipping takes out after 0.5 hour and is placed in 80 DEG C drying 0.5 hour in baking oven, then impregnates 0.5 hour again
It dries 0.5 hour, is so repeated 8 times afterwards, then ceramic honey comb is put into 600 DEG C of Muffle furnace calcinings 1 hour to get ceramic honey comb,
90 minutes degradation rates to aniline sewage are 10.2%.
Comparative example 2
Ceramic honey comb sample is put into 10% dilute nitric acid solution and is impregnated 1 hour, is rinsed after taking-up with deionized water, so
80 DEG C drying 2 hours in baking oven are placed on, 300 DEG C of Muffle furnace is put into and calcines 3 hours, it is spare.Prepare the nitric acid solution of 2mol/L
Ferric nitrate and bismuth nitrate are dissolved in the nitric acid solution by 20mL according to the dosage that the molar ratio of Fe element and Bi element is 1:1；?
Sodium hydroxide solution is slowly added dropwise under the lasting stirring of 700r/min into above-mentioned nitric acid solution until precipitating completely, is formed
Colloid；Spare ceramic honey comb is immersed in the colloid again, it is small to be placed in 80 DEG C of dryings 0.5 in baking oven for taking-up after impregnating 0.5 hour
When, it is 0.5 hour dry after then impregnating 0.5 hour again, it is so repeated 8 times, then ceramic honey comb is put into 600 DEG C of Muffle furnace and is forged
It burns 1 hour, obtains the immobilized bismuth ferrite photocatalyst of ceramic honey comb, photocatalyst amount is 24.5%, and 90 minutes to aniline
The degradation rate of sewage is 83.6%.
Photocatalytic Degradation Property verifying to aniline:
The aniline solution that 50mL concentration is 10mg/L is added into photo catalysis reactor, takes bee made from above-described embodiment 1
The immobilized erbium-codoped bismuth ferrite photocatalyst of copper of nest ceramics is placed in one, and adsorption equilibrium is reached after dark reaction 30min, is then existed
Under the irradiation of 300W xenon lamp, every 30min takes a sample, again with the extinction of ultraviolet-visible spectrophotometer measurement solution after dyeing
It spends and calculates remaining aniline content；Likewise, similarly being operated to photochemical catalyst obtained in comparative example 1 and 2, drop
Solution result is as shown in Figure 1, from figure 1 it appears that the immobilized erbium-codoped ferrous acid of copper of the ceramic honey comb that is prepared of the present invention
The degradation effect of bismuth photochemical catalyst is best, and just substantially degradation is complete by 90min.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper, it is characterised in that mainly include following step
It is rapid:
(1) carrier of photocatalyst is put into dilute acidic solution under room temperature and is impregnated 1 hour, then taken out and clean and dry, finally
High-temperature calcination, it is spare；
(2) it is dissolved in iron containing compounds, bismuth-containing compound, copper-containing compound and in batches containing erbium compound same nitric acid solution
In, obtain solution A；
(3) continue that alkaline solution is added dropwise into solution A under stirring condition, until precipitating completely, forms colloid；
(4) the calcined carrier of photocatalyst of step (1) high temperature is immersed in the colloid in step (3), time of infusion
Drying is taken out afterwards to immerse again, is taken out to calcine under the high temperature conditions after being repeated several times and be urged up to the erbium-codoped bismuth ferrite light of solid-carrying type copper
Agent.
2. the preparation method of the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper according to claim 1, it is characterised in that:
Carrier of photocatalyst described in step (1) is ceramic honey comb, foamed iron, foam copper, glass, magnesium alloy, aluminium alloy, pottery
At least one of porcelain film；The acid solution is one or more of acetic acid, sulfuric acid, nitric acid, hydrochloric acid, the acid
Property solution concentration be 5wt%~15wt%；
High-temperature calcination described in step (1) refers in 200~800 DEG C of 0.5~4h of calcining.
3. the preparation method of the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper according to claim 1, it is characterised in that:
Iron containing compounds described in step (2) are ferric nitrate；The bismuth-containing compound is bismuth nitrate；The cupric chemical combination
Object is copper nitrate；Described is erbium nitrate containing erbium compound.
4. the preparation method of the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper according to claim 1, it is characterised in that:
The concentration of nitric acid solution described in step (2) is 0.01~6mol/L；Iron containing compounds described in step (2) contain
Bismuth compound, copper-containing compound and the dosage containing erbium compound are the change of the erbium-codoped bismuth ferrite of copper formed in step (2)
Formula metered proportions are Bi1-xErxFe1-yCuyO3, wherein 0 < x≤0.1,0 < y≤0.1.
5. the preparation method of the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper according to claim 1, it is characterised in that:
Alkaline solution described in step (3) is at least one of sodium hydroxide solution, potassium hydroxide solution, ammonium hydroxide；Step
(3) stirring described in refers to that mixing speed is 300~1000r/min, and dropwise addition described in step (3) refers to that rate of addition is
1~2 drop/s.
6. the preparation method of the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper according to claim 1, it is characterised in that:
Time of infusion described in step (4) refers to 0.5~1h of dipping；The drying refers in 60~100 DEG C of dryings
0.5~2h；The dipping refers to dipping 1~10 time for several times；
High-temperature calcination described in step (4) refers to 0.5~4h of calcining at 200~800 DEG C.
7. a kind of erbium-codoped bismuth ferrite light of solid-carrying type copper that methods described in any item according to claim 1~6 are prepared
Catalyst.
8. the application of the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper according to claim 7 in the treatment of waste water.
9. the erbium-codoped bismuth ferrite photocatalyst of solid-carrying type copper according to claim 7 contains aniline waste water in photocatalytic degradation
In application.
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