CN106311344B - A kind of polypyrrole-TiO2The preparation method of photocatalysis film - Google Patents
A kind of polypyrrole-TiO2The preparation method of photocatalysis film Download PDFInfo
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- CN106311344B CN106311344B CN201610588745.3A CN201610588745A CN106311344B CN 106311344 B CN106311344 B CN 106311344B CN 201610588745 A CN201610588745 A CN 201610588745A CN 106311344 B CN106311344 B CN 106311344B
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- 238000007146 photocatalysis Methods 0.000 title claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000008021 deposition Effects 0.000 claims abstract description 19
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 46
- 239000011521 glass Substances 0.000 claims description 46
- 239000012153 distilled water Substances 0.000 claims description 40
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 238000011010 flushing procedure Methods 0.000 claims description 24
- 239000000178 monomer Substances 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 16
- 229910019985 (NH4)2TiF6 Inorganic materials 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000009832 plasma treatment Methods 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 229920000128 polypyrrole Polymers 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 21
- 239000000975 dye Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000003851 corona treatment Methods 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- LQJVOKWHGUAUHK-UHFFFAOYSA-L disodium 5-amino-4-hydroxy-3-phenyldiazenylnaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].OC1=C2C(N)=CC(S([O-])(=O)=O)=CC2=CC(S([O-])(=O)=O)=C1N=NC1=CC=CC=C1 LQJVOKWHGUAUHK-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/063—Polymers comprising a characteristic microstructure
- B01J31/067—Molecularly imprinted polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/349—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of flames, plasmas or lasers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Crystallography & Structural Chemistry (AREA)
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Abstract
The present invention provides a kind of polypyrrole TiO2The preparation method of photocatalysis film, this method use liquid phase deposition to prepare TiO first2Photocatalysis film, then using plasma polymerization technique is in TiO2Photocatalysis film surface aggregate polypyrrole organic film；It is not only easy to operate, it is environmentally protective, and resulting materials photocatalytic activity is high.
Description
Technical field
The invention belongs to field of new materials, and in particular to a kind of polypyrrole-TiO2The preparation method of photocatalysis film.
Background technology
Photocatalytic Oxidation With Semiconductors technology is as a kind of novel, green organic pollutant degradation technology, by scientific research work
The extensive concern of author.TiO2Because of the characteristics such as its photocatalytic activity is high, reaction rate is fast, at low cost, nontoxic, it is acknowledged as most
The conductor photocatalysis material of potentiality.Powdered form nano-TiO2There is difficulties in dispersion in photochemical catalyst, easily reunite in use
Inactivation recycles the shortcomings of difficult, prepares TiO2Photocatalysis film is a kind of effective ways to solve the above problems.
Due to TiO2Energy gap is wider, can only absorb the shorter ultraviolet light of sunlight medium wavelength, and ultraviolet in sunlight
Line only accounts for 4%-6%, therefore TiO2Photocatalytic activity under visible light is relatively low.
Invention content
Technical problem to be solved by the invention is to provide the polypyrroles under visible light with excellent photocatalytic activity to repair
Adorn TiO2Photocatalysis film.
Realizing the technical solution of above-mentioned purpose is：Liquid phase deposition is used to prepare TiO first2Then photocatalysis film is adopted
With plasma polymerization techniques in TiO2Photocatalysis film surface aggregate polypyrrole organic film.
A kind of polypyrrole-TiO provided by the invention2The preparation method of photocatalysis film carries out as steps described below：
(1) commercially available glass slide is soaked in 2-5molL-1NaOH solution in, after 1-2h take out use distilled water flushing 3-5
It is secondary, use 1-3molL-1HNO3Solution supersound washing 15-30min, with distilled water flushing 3-5 times after taking-up, then with anhydrous second
Alcohol supersound washing 15-30min finally uses distilled water supersound washing 15-30min, is dried at 60-80 DEG C for use；
(2) a certain amount of (NH is added in polytetrafluoroethylene beaker4)2TiF6、H3BO3And distilled water, it is stirred at room temperature,
After above-mentioned substance is completely dissolved, the pH for adjusting solution is 2-4；Then TiO is added into solution in the ratio of 0.04g/L2, together
When in the ratio of 0.005-0.01g/L pyrrole monomer is added, ultrasonic disperse 10-20min makes uniform suspension disperse, and use is qualitative
Filter paper filters above-mentioned solution up to deposition solution；
Above-mentioned (NH4)2TiF6Solution concentration is 0.05mol/L, H3BO3With (NH4)2TiF6Molar ratio is 2-5:1；
(3) will through step (1), treated that glass slide is vertically put into above-mentioned deposition solution, deposited in water bath with thermostatic control certain
Time takes out glass slide after reaction, and with distilled water flushing 3-5 times, then glass slide is placed in 300 DEG C by naturally dry
2-3h is calcined in Muffle furnace, removes pyrrole monomer；
Above-mentioned water bath with thermostatic control temperature is 40-50 DEG C, sedimentation time 3-5h；
(4) it will be placed in plasma processor cavity through step (3) processed glass slide, and vacuum pump be opened, when anti-
When to answer in cavity vacuum degree be 5Pa, it be passed through argon gas, while pyrrole monomer steam being introduced in plasma processor cavity, adjusted
When vacuum degree is 5Pa or less in section argon flow amount to reaction cavity, radio frequency discharge causes polymerization, after reaction, by glass slide
It takes out, after using absolute ethyl alcohol and deionized water to impregnate 12-24h respectively, is dried at 60-80 DEG C；
Above-mentioned radio frequency discharge power is 15-30W, plasma treatment time 15-45min.
As shown from the above technical solution：Molecular engram TiO is prepared using liquid phase deposition first2Film, then use etc.
Gas ions polymerization technique is in TiO2Film surface coats polypyrrole film, and molecular imprinting technology keeps the two contact closer, this is advantageous
The transmission of light induced electron in photocatalytic process is conducive to the active raising of material light catalysis.
The beneficial effects of the invention are as follows：
(1) molecular imprinting technology is utilized to promote polypyrrole film and TiO2Combination between film.
(2) using plasma polymerization technique realizes pyrrole monomer in TiO2The polymerization of film surface, it is easy to operate, green
Environmental protection.
Specific implementation mode
With reference to specific embodiment, description is of the invention in further detail.It should be understood that these embodiments are intended merely to
It illustrates the present invention, rather than limits the scope of the invention in any way.
Embodiment 1
(1) commercially available glass slide is soaked in 2molL-1NaOH solution in, taken out after 2h with distilled water flushing 3 times, used
1mol·L-1HNO3Solution supersound washing 30min, with distilled water flushing 3 times after taking-up, then with absolute ethyl alcohol supersound washing
30min finally uses distilled water supersound washing 30min, is dried at 60 DEG C for use；
(2) a certain amount of (NH is added in polytetrafluoroethylene beaker4)2TiF6And distilled water, prepare 0.05mol/L (NH4)2TiF6Solution, while a certain amount of H is added3BO3, wherein H3BO3With (NH4)2TiF6Molar ratio is 2:1, it is stirred at room temperature, waits for
After above-mentioned substance is completely dissolved, the pH for adjusting solution is 2；Then TiO is added into solution in the ratio of 0.04g/L2, press simultaneously
Pyrrole monomer is added in the ratio of 0.005g/L, and ultrasonic disperse 10min makes uniform suspension disperse, and is filtered using qualitative filter paper above-mentioned
Solution is up to deposition solution；
(3) will through step (1), treated that glass slide is vertically put into above-mentioned deposition solution, sink in 40 DEG C of waters bath with thermostatic control
Product 3h takes out glass slide after reaction, and with distilled water flushing 3 times, then glass slide is placed in 300 DEG C by naturally dry
2h is calcined in Muffle furnace, removes pyrrole monomer；
(4) it will be placed in plasma processor cavity through step (3) processed glass slide, and vacuum pump be opened, when anti-
When to answer in cavity vacuum degree be 5Pa, it be passed through argon gas, while pyrrole monomer steam being introduced in plasma processor cavity, adjusted
When vacuum degree is 5Pa in section argon flow amount to reaction cavity, radio frequency discharge, discharge power 15W, corona treatment 45min
Afterwards, glass slide is taken out, after using absolute ethyl alcohol and deionized water to impregnate 12h respectively, is dried at 60 DEG C.
Comparative example 1
(1) commercially available glass slide is soaked in 2molL-1NaOH solution in, taken out after 2h with distilled water flushing 3 times, used
1mol·L-1HNO3Solution supersound washing 30min, with distilled water flushing 3 times after taking-up, then with absolute ethyl alcohol supersound washing
30min finally uses distilled water supersound washing 30min, is dried at 60 DEG C for use；
(2) a certain amount of (NH is added in polytetrafluoroethylene beaker4)2TiF6And distilled water, prepare 0.05mol/L (NH4)2TiF6Solution, while a certain amount of H is added3BO3, wherein H3BO3With (NH4)2TiF6Molar ratio is 2:1, it is stirred at room temperature, waits for
After above-mentioned substance is completely dissolved, the pH for adjusting solution is 2；Then TiO is added into solution in the ratio of 0.04g/L2, ultrasound point
Scattered 10min makes uniform suspension disperse, and above-mentioned solution is filtered up to deposition solution using qualitative filter paper；
(3) will through step (1), treated that glass slide is vertically put into above-mentioned deposition solution, sink in 40 DEG C of waters bath with thermostatic control
Product 3h takes out glass slide after reaction, and with distilled water flushing 3 times, then glass slide is placed in 300 DEG C by naturally dry
2h is calcined in Muffle furnace, removes pyrrole monomer；
(4) it will be placed in plasma processor cavity through step (3) processed glass slide, and vacuum pump be opened, when anti-
When to answer in cavity vacuum degree be 5Pa, it be passed through argon gas, while pyrrole monomer steam being introduced in plasma processor cavity, adjusted
When vacuum degree is 5Pa in section argon flow amount to reaction cavity, radio frequency discharge, discharge power 15W, corona treatment 45min
Afterwards, glass slide is taken out, after using absolute ethyl alcohol and deionized water to impregnate 12h respectively, is dried at 60 DEG C.
Embodiment 2
(1) commercially available glass slide is soaked in 5molL-1NaOH solution in, taken out after 1h with distilled water flushing 5 times, used
3mol·L-1HNO3Solution supersound washing 15min, with distilled water flushing 5 times after taking-up, then with absolute ethyl alcohol supersound washing
15min finally uses distilled water supersound washing 15min, is dried at 80 DEG C for use；
(2) a certain amount of (NH is added in polytetrafluoroethylene beaker4)2TiF6、H3BO3And distilled water, prepare 0.05mol/L
(NH4)2TiF6Solution, while a certain amount of H is added3BO3, wherein H3BO3With (NH4)2TiF6Molar ratio is 5:1, it stirs at room temperature
It mixes, after above-mentioned substance is completely dissolved, the pH for adjusting solution is 4；Then TiO is added into solution in the ratio of 0.04g/L2,
Pyrrole monomer is added in the ratio of 0.01g/L simultaneously, ultrasonic disperse 20min makes uniform suspension disperse, using qualitative filter paper mistake
Above-mentioned solution is filtered up to deposition solution；
(3) will through step (1), treated that glass slide is vertically put into above-mentioned deposition solution, sink in 50 DEG C of waters bath with thermostatic control
Product 5h takes out glass slide after reaction, and with distilled water flushing 5 times, then glass slide is placed in 300 DEG C by naturally dry
3h is calcined in Muffle furnace, removes pyrrole monomer；
(4) it will be placed in plasma processor cavity through step (3) processed glass slide, and vacuum pump be opened, when anti-
When to answer in cavity vacuum degree be 5Pa, it be passed through argon gas, while pyrrole monomer steam being introduced in plasma processor cavity, adjusted
When vacuum degree is 3Pa in section argon flow amount to reaction cavity, radio frequency discharge, discharge power 30W, corona treatment 15min
Afterwards, glass slide is taken out, after using absolute ethyl alcohol and deionized water to impregnate for 24 hours respectively, is dried at 80 DEG C.
Comparative example 2
(1) commercially available glass slide is soaked in 5molL-1NaOH solution in, taken out after 1h with distilled water flushing 5 times, used
3mol·L-1HNO3Solution supersound washing 15min, with distilled water flushing 5 times after taking-up, then with absolute ethyl alcohol supersound washing
15min finally uses distilled water supersound washing 15min, is dried at 80 DEG C for use；
(2) a certain amount of (NH is added in polytetrafluoroethylene beaker4)2TiF6、H3BO3And distilled water, prepare 0.05mol/L
(NH4)2TiF6Solution, while a certain amount of H is added3BO3, wherein H3BO3With (NH4)2TiF6Molar ratio is 5:1, it stirs at room temperature
It mixes, after above-mentioned substance is completely dissolved, the pH for adjusting solution is 4；Then TiO is added into solution in the ratio of 0.04g/L2,
Pyrrole monomer is added in the ratio of 0.01g/L simultaneously, ultrasonic disperse 20min makes uniform suspension disperse, using qualitative filter paper mistake
Above-mentioned solution is filtered up to deposition solution；
(3) will through step (1), treated that glass slide is vertically put into above-mentioned deposition solution, sink in 50 DEG C of waters bath with thermostatic control
Product 5h takes out glass slide after reaction, and with distilled water flushing 5 times, then glass slide is placed in 300 DEG C by naturally dry
3h is calcined in Muffle furnace, removes pyrrole monomer；Up to molecular engram TiO2Photocatalysis film.
Embodiment 3
(1) commercially available glass slide is soaked in 3molL-1NaOH solution in, taken out after 1.5h with distilled water flushing 4 times,
Use 2molL-1HNO3Solution supersound washing 20min, with distilled water flushing 4 times after taking-up, then with absolute ethyl alcohol supersound washing
20min finally uses distilled water supersound washing 20min, is dried at 70 DEG C for use；
(2) a certain amount of (NH is added in polytetrafluoroethylene beaker4)2TiF6、H3BO3And distilled water, prepare 0.05mol/L
(NH4)2TiF6Solution, while a certain amount of H is added3BO3, wherein H3BO3With (NH4)2TiF6Molar ratio is 3:1, it stirs at room temperature
It mixes, after above-mentioned substance is completely dissolved, the pH for adjusting solution is 3；Then TiO is added into solution in the ratio of 0.04g/L2,
Pyrrole monomer is added in the ratio of 0.008g/L simultaneously, ultrasonic disperse 15min makes uniform suspension disperse, using qualitative filter paper mistake
Above-mentioned solution is filtered up to deposition solution；
(3) will through step (1), treated that glass slide is vertically put into above-mentioned deposition solution, deposited in 45 DEG C of waters bath with thermostatic control
4h takes out glass slide after reaction, and with distilled water flushing 4 times, then glass slide is placed in 300 DEG C of Muffle by naturally dry
2.5h is calcined in stove, removes pyrrole monomer；
(4) it will be placed in plasma processor cavity through step (3) processed glass slide, and vacuum pump be opened, when anti-
When to answer in cavity vacuum degree be 5Pa, it be passed through argon gas, while pyrrole monomer steam being introduced in plasma processor cavity, adjusted
When vacuum degree is 4Pa in section argon flow amount to reaction cavity, radio frequency discharge, discharge power 25W, corona treatment 30min
Afterwards, glass slide is taken out, after using absolute ethyl alcohol and deionized water to impregnate 18h respectively, is dried at 70 DEG C.
Embodiment 4
(1) commercially available glass slide is soaked in 4molL-1NaOH solution in, taken out after 1h with distilled water flushing 5 times, used
2.5mol·L-1HNO3Solution supersound washing 25min, with distilled water flushing 5 times after taking-up, then with absolute ethyl alcohol supersound washing
25min finally uses distilled water supersound washing 25min, is dried at 75 DEG C for use；
(2) a certain amount of (NH is added in polytetrafluoroethylene beaker4)2TiF6、H3BO3And distilled water, prepare 0.05mol/L
(NH4)2TiF6Solution, while a certain amount of H is added3BO3, wherein H3BO3With (NH4)2TiF6Molar ratio is 4:1, it stirs at room temperature
It mixes, after above-mentioned substance is completely dissolved, the pH for adjusting solution is 2.5；Then it is added into solution in the ratio of 0.04g/L
TiO2, while pyrrole monomer is added in the ratio of 0.006g/L, ultrasonic disperse 18min makes uniform suspension disperse, and use is qualitative
Filter paper filters above-mentioned solution up to deposition solution；
(3) will through step (1), treated that glass slide is vertically put into above-mentioned deposition solution, deposited in 48 DEG C of waters bath with thermostatic control
3.5h takes out glass slide after reaction, and with distilled water flushing 5 times, then glass slide is placed in 300 DEG C of horse by naturally dry
2h is not calcined in stove, removes pyrrole monomer；
(4) it will be placed in plasma processor cavity through step (3) processed glass slide, and vacuum pump be opened, when anti-
When to answer in cavity vacuum degree be 5Pa, it be passed through argon gas, while pyrrole monomer steam being introduced in plasma processor cavity, adjusted
When vacuum degree is 2Pa or less in section argon flow amount to reaction cavity, radio frequency discharge, discharge power 20W, corona treatment
After 25min, glass slide is taken out, after using absolute ethyl alcohol and deionized water to impregnate 20h respectively, is dried at 75 DEG C.
Embodiment 5
Photocatalysis performance is evaluated：
Dyestuff (methylene blue, Weak Acid Red B) the solution 25mL for measuring mass concentration 50mg/L is placed in a diameter of 9cm
Culture dish photo catalysis reactor in, by the TiO of gained2Photocatalysis film (work area：40 × 40mm) two panels keeps flat into anti-
It answers in device；Using 500W xenon lamps as light source, 420nm light below is filtered using JZ-420 optical filters and carries out photocatalytic degradation reality
It tests, fluorescent tube is 10cm away from dye solution liquid level.After illumination 2h, measured at λ max with 722s visible spectrophotometers molten
The absorbance of liquid, to extrapolate after illumination remaining dye strength in solution.Degradation rate is calculated as follows：
In formula：η is degradation rate；C0Before light degradation, the concentration of dye solution；Ct be illumination t moment after, dye solution
Concentration.
Light degradation property of 1 sample of table to dyestuff
It can be seen that from upper table experimental data, present invention gained polypyrrole-TiO2Photocatalysis film has excellent photocatalysis
Activity.Comparative example 1 prepares TiO2Molecular imprinting technology is not used during photocatalysis film so that polypyrrole film and TiO2Light is urged
Change the combination defective tightness between film, gained sample photocatalytic activity is relatively low.Comparative example 2 does not use polypyrrole film to TiO2It is thin
Film is modified, and gained sample visible light activity is very poor.
Claims (4)
1. a kind of polypyrrole-TiO2The preparation method of photocatalysis film, it is characterised in that：It is as follows：
(1) commercially available glass slide is soaked in 2-5molL-1NaOH solution in, taken out after 1-2h with distilled water flushing 3-5 times,
Use 1-3molL-1HNO3Solution supersound washing 15-30min, uses distilled water flushing 3-5 times after taking-up, then super with absolute ethyl alcohol
Sound washs 15-30min, finally uses distilled water supersound washing 15-30min, is dried at 60-80 DEG C for use；
(2) a certain amount of (NH is added in polytetrafluoroethylene beaker4)2TiF6、H3BO3And distilled water, it is stirred at room temperature, waits for
It states after substance is completely dissolved, the pH for adjusting solution is 2-4；Then TiO is added into solution in the ratio of 0.04g/L2, press simultaneously
Pyrrole monomer is added in the ratio of 0.005-0.01g/L, and ultrasonic disperse 10-20min makes uniform suspension disperse, using qualitative filter paper
Above-mentioned solution is filtered up to deposition solution；
(3) will through step (1), treated that glass slide is vertically put into above-mentioned deposition solution, a timing is deposited in water bath with thermostatic control
Between, after reaction, glass slide is taken out, with distilled water flushing 3-5 times, then glass slide is placed in 300 DEG C of horse by naturally dry
2-3h is not calcined in stove, removes pyrrole monomer；
(4) it will be placed in plasma processor cavity through step (3) processed glass slide, and open vacuum pump, work as reaction chamber
When internal vacuum degree is 5Pa, it is passed through argon gas, while pyrrole monomer steam being introduced in plasma processor cavity, adjusts argon
When vacuum degree is 5Pa or less in throughput to reaction cavity, radio frequency discharge causes polymerization, after reaction, glass slide is taken
Go out, after using absolute ethyl alcohol and deionized water to impregnate 12-24h respectively, is dried at 60-80 DEG C.
2. a kind of polypyrrole-TiO according to claim 12The preparation method of photocatalysis film, it is characterised in that：Step
(2) (the NH described in4)2TiF6A concentration of 0.05mol/L, H3BO3With (NH4)2TiF6Molar ratio is 2-5:1.
3. a kind of polypyrrole-TiO according to claim 12The preparation method of photocatalysis film, it is characterised in that：Step
(3) the water bath with thermostatic control temperature described in is 40-50 DEG C, sedimentation time 3-5h.
4. a kind of polypyrrole-TiO according to claim 12The preparation method of photocatalysis film, it is characterised in that：Step
(4) the radio frequency discharge power described in is 15-30W, plasma treatment time 15-45min.
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