CN109248711A - A kind of load TiO2PPS photocatalysis membrana preparation method - Google Patents
A kind of load TiO2PPS photocatalysis membrana preparation method Download PDFInfo
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- CN109248711A CN109248711A CN201811197401.5A CN201811197401A CN109248711A CN 109248711 A CN109248711 A CN 109248711A CN 201811197401 A CN201811197401 A CN 201811197401A CN 109248711 A CN109248711 A CN 109248711A
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- tio
- pps
- photocatalysis membrana
- sulfate
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- 238000007146 photocatalysis Methods 0.000 title claims abstract description 89
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 102
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000002243 precursor Substances 0.000 claims abstract description 52
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 46
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 37
- 230000004888 barrier function Effects 0.000 claims abstract description 35
- 235000019441 ethanol Nutrition 0.000 claims abstract description 33
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000010936 titanium Substances 0.000 claims abstract description 23
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 13
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 13
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 13
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical group [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 7
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 5
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 4
- HHDOORYZQSEMGM-UHFFFAOYSA-L potassium;oxalate;titanium(4+) Chemical compound [K+].[Ti+4].[O-]C(=O)C([O-])=O HHDOORYZQSEMGM-UHFFFAOYSA-L 0.000 claims description 3
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 3
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 3
- KKDBZWZRJNRBGA-UHFFFAOYSA-L Cl[Ti]Cl.[CH]1C=CC=C1 Chemical compound Cl[Ti]Cl.[CH]1C=CC=C1 KKDBZWZRJNRBGA-UHFFFAOYSA-L 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 239000010919 dye waste Substances 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 20
- 239000003054 catalyst Substances 0.000 abstract description 12
- 239000000853 adhesive Substances 0.000 abstract description 5
- 230000001070 adhesive effect Effects 0.000 abstract description 5
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 71
- 239000000463 material Substances 0.000 description 15
- 239000002957 persistent organic pollutant Substances 0.000 description 15
- 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 14
- 229960000907 methylthioninium chloride Drugs 0.000 description 14
- 230000004907 flux Effects 0.000 description 12
- 230000007423 decrease Effects 0.000 description 11
- 239000007788 liquid Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 239000004408 titanium dioxide Substances 0.000 description 11
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 10
- 239000012528 membrane Substances 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 150000003462 sulfoxides Chemical class 0.000 description 2
- 229920006269 PPS film Polymers 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- 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
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
- B01J35/59—Membranes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of load TiO2PPS photocatalysis membrana preparation method, comprising the following steps: titanium source, sulfate are mixed with the composite solution of ethyl alcohol, water and hydrochloric acid, and stirred at normal temperature to homogeneous, TiO is obtained2Precursor solution；PPS microporous barrier is placed in ethyl alcohol and is soaked, being then transferred to concentration is to handle in nitric acid solution；PPS microporous barrier is immersed into TiO2It in precursor solution, is together transferred in hydrothermal reaction kettle and carries out hydro-thermal reaction, PPS@TiO is obtained after washing and drying2Photocatalysis membrana.This method uses high temperature hydro-thermal method by TiO2Growth in situ promotes TiO in PPS micropore film surface2The crystallinity of nanoparticle obtains uniform aperture in the case where avoiding using adhesive, high porosity, bigger serface, high load amount, high catalyst crystallinity, is firmly combined, lateral load nano-TiO in the surface and duct of morphology controllable2PPS photocatalysis membrana, effectively improve the specific surface area and catalytic activity of catalyst.
Description
Technical field
The invention belongs to photocatalysis membrana preparation field, specially a kind of load TiO2PPS photocatalysis membrana preparation method.
Background technique
Organic pollutant is one of environmental contaminants difficult to deal with because of its stable structure, not easily biological-degradable.Semiconductor
Photocatalysis technology can directly be removed the thorough mineralising of Some Organic Pollutants using luminous energy, be ideal organic pollutant processing
One of technology.In a semiconductor material, nano-TiO2It is had received widespread attention with efficient, environmentally friendly, nontoxic, stable feature.
However, nano-TiO2Catalysis material there is hardly possible recycling, it is easy to reunite the disadvantages of, be easy to cause secondary pollution and catalytic efficiency
It reduces.Therefore, the catalysis material of support type is more and more applied.
In the research of load type photocatalytic material, the selection of matrix is the key that research, currently, matrix mainly has microballoon material
Material, two-dimensional material, fabric, inorganic material and membrane material.Wherein, polymeric film material is with high porosity, high-ratio surface
Long-pending and strong adsorption capacity receives significant attention.Currently, the mode of loading of load type photocatalytic material mainly has blending method, deposition
Method, sol-gal process, adhesive bonding method and hydrothermal reaction at low temperature.Wherein blending method needs catalyst being embedded in polymeric matrix
In, limit the load capacity and catalytic efficiency of catalyst.Material obtained by sedimentation, sol-gal process there is catalyst with
The problem of basal body binding force difference.The use of adhesive not only increases production cost, can also bring environmental pollution.Hydrothermal reaction at low temperature
Catalyst exists in prepared Film Photocatalyst with amorphous forms, and crystallinity is lower, and the light for greatly reducing material is urged
Change performance.
The document of application number 201611156787.6 discloses a kind of activated carbon fiber-loaded nano-TiO2The preparation of film
Method.This method using induction reverse micelle method in situ prepare activated carbon fiber-loaded uniform flawless, adhesive force by force, film thickness
Controllable compact nanometer TiO2The composite photocatalyst material of film.This method effective solution nano-TiO2Catalysis material is difficult
The disadvantages of recycling, be easy to reunite, but the preparation condition and longer preparation path of complicated process flow, more harshness limit the party
Method is further applied and development.The document of application number 2017111579844 discloses a kind of area load TiO2Nano wire
The preparation method of polyetherimide photocatalysis ultrafiltration membrane grows TiO in film surface by low temperature crystallization technology2Nano wire improves
The film to improve the flux of film keep high stage cut while, and is applied to photocatalysis pollution by the hydrophily of film
The fields such as improvement.But the contribution that the relatively limited and matrix of the active site of catalyst exposure improves catalytic efficiency is smaller, function
It can be more single.
Summary of the invention
In view of the deficiencies of the prior art, the technical issues of present invention intends to solve is to provide a kind of load TiO2PPS light urge
Change the preparation method of film.
The technical solution that the present invention solves the technical problem is to provide a kind of load TiO2PPS photocatalysis membrana system
Preparation Method, it is characterised in that method includes the following steps:
1)TiO2The preparation of precursor solution: titanium source, sulfate are mixed with the composite solution of ethyl alcohol, water and hydrochloric acid, and
It is stirred at normal temperature to homogeneous, obtains TiO2Precursor solution；TiO2The concentration of titanium source is 1~500g/L, sulphur in precursor solution
The concentration of hydrochlorate is 1~50g/L；The volume ratio of the ethyl alcohol, water and hydrochloric acid is 2-6:1-3:1-3；
2) pretreatment of PPS microporous barrier: PPS microporous barrier being placed in ethyl alcohol and is soaked, be then transferred to concentration be 5~
It is stirred 0.5~8 hour at 10~50 DEG C in the nitric acid solution of 55wt.%；
3) high temperature hydro-thermal method in-situ preparation PPS TiO2Photocatalysis membrana: the PPS microporous barrier that step 2) is obtained immerses step
1) TiO obtained2In precursor solution, it is together transferred to progress 2~30h of hydro-thermal reaction, reaction temperature in hydrothermal reaction kettle
It is 80~240 DEG C, PPS@TiO is obtained after washing and drying2Photocatalysis membrana；
0.01~1 milliliter of TiO is added in PPS microporous barrier every square centimeter2Precursor solution.
Compared with prior art, the beneficial effects of the invention are that:
(1) nontoxic, green, stable, antibacterial TiO is used2As major catalyst, using high temperature hydro-thermal method by TiO2It is in situ
It is grown on PPS micropore film surface, promotes TiO2The crystallinity of nanoparticle obtains uniform in the case where avoiding using adhesive
Aperture, bigger serface, high load amount, high catalyst crystallinity, is firmly combined, the surface and hole of morphology controllable high porosity
Lateral load nano-TiO in road2PPS photocatalysis membrana, effectively improve the specific surface area and catalytic activity of catalyst.
(2) using high temperature resistant, solvent resistant, acid-alkali-corrosive-resisting high performance material PPS as catalyst carrier, PPS main chain
Containing a large amount of phenyl ring, π type Absorptive complex wave can be formed, improves the chemical adsorptivity to organic pollutant from matrix angle, thus
Further improve the efficiency of the catalysis of catalyst.
(3) PPS microporous barrier has dendritic structure, and specific surface area and porosity with higher is further improved and urged
Change the adsorptivity of membrane material.The raising of chemical adsorptivity is conducive to improve the catalytic efficiency of heterogeneous catalysis, to obtain high catalysis
The photocatalysis membrana of efficiency.
(4) technique to PPS microporous barrier nitric acid pretreatment is introduced, it is main under the premise of not destroying former PPS film dynamic performance
Thioether bond on chain can be partially oxidized into sulfoxide key, provide chemical bonds site, and sulfoxide key has electronegativity, can be with band just
The titanium source hydrolysis intermediate product of electricity attracts each other to form electrostatic force combination, firm interaction is formed, to improve inorganic
The binding force of nanocatalyst particles and film matrix avoids the use of adhesive.
(5) preparation process is simple, preparation flow is shorter, reaction condition is mild controllably, operation is more convenient.
Detailed description of the invention
Fig. 1 is present invention load TiO2PPS photocatalysis membrana preparation method embodiment 2 in the photocatalysis membrana for preparing
SEM photograph；
Fig. 2 is present invention load TiO2PPS photocatalysis membrana preparation method embodiment 2 in the photocatalysis membrana for preparing
XRD diagram；
Fig. 3 is present invention load TiO2PPS photocatalysis membrana preparation method embodiment 2 in the photocatalysis membrana for preparing to Asia
The photocatalytic degradation curve graph of methyl blue organic solvent；
Fig. 4 is present invention load TiO2PPS photocatalysis membrana preparation method comparative example 1 in the photocatalysis membrana for preparing
SEM photograph；
Specific embodiment
Specific embodiments of the present invention are given below.Specific embodiment is only used for that present invention be described in more detail, unlimited
The protection scope of the claim of this application processed.
The present invention provides a kind of load TiO2PPS photocatalysis membrana preparation method (abbreviation method), it is characterised in that
Method includes the following steps:
1)TiO2The preparation of precursor solution: titanium source, sulfate are mixed with the composite solution of ethyl alcohol, water and hydrochloric acid, and
It is stirred at normal temperature to homogeneous, obtains TiO2Precursor solution；TiO2The concentration of titanium source is 1~500g/L, sulphur in precursor solution
The concentration of hydrochlorate is 1~50g/L；The volume ratio of the ethyl alcohol, water and hydrochloric acid is 2-6:1-3:1-3；
Preferably, titanium source concentration is 10~200g/L, and sulfate concentration is 2~10g/L, ethyl alcohol, water and hydrochloric acid volume ratio
For 3-5:1-3:1-3；
The titanium source be butyl titanate, titanium tetrachloride, titanium sulfate, titanium trichloride, isopropyl titanate, cyclopentadienyl titanium dichloride,
At least one of titanium tetrafluoride or titanium potassium oxalate；
The sulfate is ferric sulfate, ammonium sulfate, titanium sulfate, sodium sulphate, magnesium sulfate, copper sulphate, potassium sulfate or aluminum sulfate
At least one of；
2) pretreatment of PPS microporous barrier: PPS microporous barrier being placed in ethyl alcohol and is soaked, be then transferred to concentration be 5~
It is stirred 0.5~8 hour at 10~50 DEG C in the nitric acid solution of 55wt.%；
3) high temperature hydro-thermal method in-situ preparation PPS TiO2Photocatalysis membrana: the PPS microporous barrier that step 2) is obtained immerses step
1) TiO obtained2In precursor solution, it is together transferred to progress 2~30h of hydro-thermal reaction, reaction temperature in hydrothermal reaction kettle
It is 80~240 DEG C, resulting film will be reacted and be washed with deionized, dries 6~24 hours obtain PPS@TiO in an oven2Light
Catalytic membrane.
0.01~1 milliliter of TiO is added in PPS microporous barrier every square centimeter2Precursor solution；Preferably, every square centimeter
0.02~0.04 milliliter of TiO is added in PPS microporous barrier2Precursor solution.
PPS@TiO2Photocatalysis membrana can be applied in organic dye waste water.
Embodiment 1
1) titanium tetrachloride, ammonium sulfate are mixed and is stirred at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 2:1:1
It mixes to homogeneous, obtains TiO2Precursor solution；TiO2The concentration of titanium source is 50g/L in precursor solution, the concentration of sulfate is
1g/L；
2) PPS microporous barrier is placed in ethyl alcohol and is soaked, is then transferred in the nitric acid solution that concentration is 20% at 20 DEG C
Stirring 4 hours.
3) by 20cm2Resulting pretreated PPS microporous barrier immerses 20ml precursor solution and is transferred to hydrothermal reaction kettle
For 24 hours, reaction temperature is 220 DEG C to middle progress hydro-thermal reaction, will react resulting film and is washed with deionized completely, does in an oven
Obtain PPS@TiO within dry 24 hours2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 78.1%, and the load factor of titanium dioxide is 19.2%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, the specific steps are as follows: the PPS TiO for being 2.5cm by diameter2
Photocatalysis membrana is placed in the aqueous solution of methylene blue of 25mL (20mg/L), is carried out under the magnetic agitation in 200rmp dark first
1h is adsorbed, ultraviolet lamp is then opened and carries out photocatalytic degradation, after tested, prepared PPS@TiO2Photocatalysis membrana is to methylene blue
Catalytic efficiency 93% or more.Through current scour experimental test (the current scour 150min under 2bar pressure), the photocatalysis
The decline of membrane flux 11%, the TiO of load2It is relatively firm, it is not easily to fall off.
Embodiment 2
1) butyl titanate, ammonium sulfate are mixed simultaneously at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 4:1:2
Stirring obtains TiO to homogeneous2Precursor solution；TiO2The concentration of titanium source is the concentration of 150g/L, sulfate in precursor solution
For 5g/L；
2) PPS microporous barrier is placed in ethyl alcohol and is soaked, is then transferred in the nitric acid solution that concentration is 10% at 50 DEG C
Stirring 1 hour.
3) by 20cm2Resulting pretreated PPS microporous barrier immerses 10ml precursor solution and is transferred to hydrothermal reaction kettle
Middle progress hydro-thermal reaction 12h, reaction temperature are 180 DEG C, will react resulting film and are washed with deionized completely, do in an oven
Obtain PPS@TiO within dry 24 hours2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 73.4%, and the load factor of titanium dioxide is 50.6%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, after tested, prepared PPS TiO2Photocatalysis membrana is to Asia
The catalytic efficiency of methyl blue is 99% or more.Through current scour experimental test, the photocatalysis membrana flux decline 17%, load
TiO2It is relatively firm, it is not easily to fall off.
Embodiment 3
1) solution that titanium sulfate, ammonium sulfate and ethyl alcohol, water and hydrochloric acid volume ratio are 6:2:3 is mixed and stirred at normal temperature
To homogeneous, TiO is obtained2Precursor solution；TiO2The concentration of titanium source is 400g/L in precursor solution, the concentration of sulfate is
50g/L；
2) PPS microporous barrier is placed in ethyl alcohol and is soaked, is then transferred in the nitric acid solution that concentration is 30% at 20 DEG C
Stirring 1 hour.
3) by 20cm2Resulting pretreated PPS microporous barrier immerses 10ml precursor solution and is transferred to hydrothermal reaction kettle
Middle progress hydro-thermal reaction 30h, reaction temperature are 120 DEG C, will react resulting film and are washed with deionized completely, do in an oven
Obtain PPS@TiO within dry 24 hours2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 76.8%, and the load factor of titanium dioxide is 38.7%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, after tested, prepared PPS TiO2Photocatalysis membrana is to Asia
The catalytic efficiency of methyl blue is 98% or more.Through current scour experimental test, the photocatalysis membrana flux decline 13%, load
TiO2It is relatively firm, it is not easily to fall off.
Embodiment 4
1) titanium potassium oxalate, ammonium sulfate are mixed and is stirred at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 4:2:1
It mixes to homogeneous, obtains TiO2Precursor solution；TiO2The concentration of titanium source is 300g/L in precursor solution, the concentration of sulfate is
20g/L；
2) PPS microporous barrier is placed in ethyl alcohol and is soaked, is then transferred in the nitric acid solution that concentration is 30% at 20 DEG C
Stirring 1 hour.
3) by 20cm2Resulting pretreated PPS microporous barrier immerses 20ml precursor solution and is transferred to hydrothermal reaction kettle
Middle progress hydro-thermal reaction 12h, reaction temperature are 150 DEG C, will react resulting film and are washed with deionized completely, do in an oven
Obtain PPS@TiO within dry 12 hours2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 74.6%, and the load factor of titanium dioxide is 41.4%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, after tested, prepared PPS TiO2Photocatalysis membrana is to Asia
The catalytic efficiency of methyl blue is 98% or more.Through current scour experimental test, the photocatalysis membrana flux decline 14%, load
TiO2It is relatively firm, it is not easily to fall off.
Embodiment 5
1) isopropyl titanate, ammonium sulfate are mixed simultaneously at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 4:1:2
Stirring obtains TiO to homogeneous2Precursor solution；TiO2The concentration of titanium source is the concentration of 250g/L, sulfate in precursor solution
For 10g/L；
2) PPS microporous barrier is placed in ethyl alcohol and is soaked, be then transferred in the nitric acid solution that concentration is 5% and stirred at 20 DEG C
It mixes 5 hours.
3) by 20cm2Resulting pretreated PPS microporous barrier immerses 10ml precursor solution and is transferred to hydrothermal reaction kettle
Middle progress hydro-thermal reaction 10h, reaction temperature are 200 DEG C, will react resulting film and are washed with deionized completely, do in an oven
Obtain PPS@TiO within dry 12 hours2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 73.0%, and the load factor of titanium dioxide is 49.3%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, after tested, prepared PPS TiO2Photocatalysis membrana is to Asia
The catalytic efficiency of methyl blue is 99% or more.Through current scour experimental test, the photocatalysis membrana flux decline 16%, load
TiO2It is relatively firm, it is not easily to fall off.
Embodiment 6
1) titanium trichloride, ammonium sulfate are mixed and is stirred at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 6:1:2
It mixes to homogeneous, obtains TiO2Precursor solution；TiO2The concentration of titanium source is 100g/L in precursor solution, the concentration of sulfate is
20g/L；
2) PPS microporous barrier is placed in ethyl alcohol and is soaked, is then transferred in the nitric acid solution that concentration is 20% at 30 DEG C
Stirring 2 hours.
3) by 20cm2Resulting pretreated PPS microporous barrier immerses 10ml precursor solution and is transferred to hydrothermal reaction kettle
For 24 hours, reaction temperature is 200 DEG C to middle progress hydro-thermal reaction, will react resulting film and is washed with deionized completely, does in an oven
Obtain PPS@TiO within dry 12 hours2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 74.2%, and the load factor of titanium dioxide is 45.6%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, after tested, prepared PPS TiO2Photocatalysis membrana is to Asia
The catalytic efficiency of methyl blue is 99% or more.Through current scour experimental test, the photocatalysis membrana flux decline 15%, load
TiO2It is relatively firm, it is not easily to fall off.
Embodiment 7
1) titanium tetrachloride, ammonium sulfate are mixed and is stirred at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 5:2:2
It mixes to homogeneous, obtains TiO2Precursor solution；TiO2The concentration of titanium source is 100g/L in precursor solution, the concentration of sulfate is
10g/L；
2) PPS microporous barrier is placed in ethyl alcohol and is soaked, is then transferred in the nitric acid solution that concentration is 20% at 40 DEG C
Stirring 1 hour.
3) by 20cm2Resulting pretreated PPS microporous barrier immerses 10ml precursor solution and is transferred to hydrothermal reaction kettle
Middle progress hydro-thermal reaction 12h, reaction temperature are 180 DEG C, will react resulting film and are washed with deionized completely, do in an oven
Obtain PPS@TiO within dry 12 hours2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 76.2%, and the load factor of titanium dioxide is 33.3%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, after tested, prepared PPS TiO2Photocatalysis membrana is to Asia
The catalytic efficiency of methyl blue is 98% or more.Through current scour experimental test, the photocatalysis membrana flux decline 15%, load
TiO2It is relatively firm, it is not easily to fall off.
Embodiment 8
1) butyl titanate, ammonium sulfate are mixed simultaneously at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 6:1:2
Stirring obtains TiO to homogeneous2Precursor solution；TiO2The concentration of titanium source is the concentration of 200g/L, sulfate in precursor solution
For 10g/L；
2) PPS microporous barrier is placed in ethyl alcohol and is soaked, is then transferred in the nitric acid solution that concentration is 25% at 25 DEG C
Stirring 1 hour.
3) by 20cm2Resulting pretreated PPS microporous barrier immerses 20ml precursor solution and is transferred to hydrothermal reaction kettle
Middle progress hydro-thermal reaction 12h, reaction temperature are 200 DEG C, will react resulting film and are washed with deionized completely, do in an oven
Obtain PPS@TiO within dry 12 hours2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 72.7%, and the load factor of titanium dioxide is 50.1%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, after tested, prepared PPS TiO2Photocatalysis membrana is to Asia
The catalytic efficiency of methyl blue is 99% or more.Through current scour experimental test, the photocatalysis membrana flux decline 17%, load
TiO2It is relatively firm, it is not easily to fall off.
Embodiment 9
1) butyl titanate, ammonium sulfate are mixed simultaneously at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 4:1:2
Stirring obtains TiO to homogeneous2Precursor solution；TiO2The concentration of titanium source is the concentration of 300g/L, sulfate in precursor solution
For 15g/L；
2) PPS microporous barrier is placed in ethyl alcohol and is soaked, is then transferred in the nitric acid solution that concentration is 40% at 20 DEG C
Stirring 1 hour.
3) by 20cm2Resulting pretreated PPS microporous barrier immerses 15ml precursor solution and is transferred to hydrothermal reaction kettle
For 24 hours, reaction temperature is 200 DEG C to middle progress hydro-thermal reaction, will react resulting film and is washed with deionized completely, does in an oven
Obtain PPS@TiO within dry 12 hours2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 72.1%, and the load factor of titanium dioxide is 53.5%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, after tested, prepared PPS TiO2Photocatalysis membrana is to Asia
The catalytic efficiency of methyl blue is 99% or more.Through current scour experimental test, the photocatalysis membrana flux decline 18%, load
TiO2It is relatively firm, it is not easily to fall off.
Comparative example 1
1) butyl titanate, ammonium sulfate are mixed simultaneously at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 4:1:2
Stirring obtains TiO to homogeneous2Precursor solution；TiO2The concentration of titanium source is the concentration of 150g/L, sulfate in precursor solution
For 5g/L；
2) by 20cm2Not pretreated PPS microporous barrier immerses 10ml precursor solution and is transferred in hydrothermal reaction kettle
Hydro-thermal reaction 12h is carried out, reaction temperature is 180 DEG C, will react resulting film and is washed with deionized completely, dries in an oven
Obtain within 24 hours PPS@TiO2Photocatalysis membrana.
After tested, PPS@TiO2The porosity of photocatalysis membrana is 74.6%, and the load factor of titanium dioxide is 47.8%.Using
Methylene blue simulates liquid organic pollutant and measures photocatalysis performance, after tested, prepared PPS TiO2Photocatalysis membrana is to Asia
The catalytic efficiency of methyl blue is 88% or more.Through current scour experimental test, the photocatalysis membrana flux decline 72%, load
TiO2Largely falling off leads to plug-hole, does not have application value.
Comparative example 2
1) butyl titanate, ammonium sulfate are mixed simultaneously at normal temperature with the solution that ethyl alcohol, water and hydrochloric acid volume ratio are 4:1:2
Stirring obtains TiO to homogeneous2Precursor solution；TiO2The concentration of titanium source is the concentration of 150g/L, sulfate in precursor solution
For 5g/L；
2) 10ml precursor solution being transferred to progress hydro-thermal reaction 12h in hydrothermal reaction kettle, reaction temperature is 180 DEG C,
Resulting TiO will be reacted2Powder is washed with deionized completely, dries 24 hours obtain TiO in an oven2Nano particle.By institute
Prepare TiO2Nano particle is added in casting solution in the ratio that mass fraction is 5% and PPS@TiO is made2Composite photocatalysis
Film.
After tested, PPS@TiO2The porosity of composite photocatalysis membrana is 79.1%, and the load factor of titanium dioxide is
5%.Photocatalysis performance, after tested, prepared PPS TiO are measured using methylene blue simulation liquid organic pollutant2It is blended
Composite photocatalysis membrane is to the catalytic efficiency of methylene blue 71% or more.Through current scour experimental test, which is urged
Change the decline of membrane flux 8%, the TiO of load2Securely, but it is embedded in film, catalytic site is few, and catalytic efficiency is poor more.
The present invention does not address place and is suitable for the prior art.
Claims (6)
1. a kind of load TiO2PPS photocatalysis membrana preparation method, it is characterised in that method includes the following steps:
1) TiO2The preparation of precursor solution: titanium source, sulfate are mixed with the composite solution of ethyl alcohol, water and hydrochloric acid, and in room temperature
Lower stirring obtains TiO to homogeneous2Precursor solution；TiO2The concentration of titanium source is 1 ~ 500g/L, sulfate in precursor solution
Concentration is 1 ~ 50g/L；The volume ratio of the ethyl alcohol, water and hydrochloric acid is 2-6:1-3:1-3；
2) pretreatment of PPS microporous barrier: PPS microporous barrier being placed in ethyl alcohol and is soaked, and being then transferred to concentration is 5 ~ 55wt.%'s
It is stirred 0.5 ~ 8 hour at 10 ~ 50 DEG C in nitric acid solution；
3) high temperature hydro-thermal method in-situ preparation PPS TiO2Photocatalysis membrana: the PPS microporous barrier that step 2 obtains is immersed into step 1) and is obtained
TiO2In precursor solution, it is together transferred to progress 2 ~ 30h of hydro-thermal reaction in hydrothermal reaction kettle, reaction temperature is 80 ~ 240
DEG C, PPS@TiO is obtained after washing and drying2Photocatalysis membrana；
0.01 ~ 1 milliliter of TiO is added in PPS microporous barrier every square centimeter2Precursor solution.
2. load TiO according to claim 12PPS photocatalysis membrana preparation method, it is characterised in that titanium source concentration is
10 ~ 200g/L, sulfate concentration are 2 ~ 10g/L, and ethyl alcohol, water and hydrochloric acid volume ratio are 3-5:1-3:1-3.
3. load TiO according to claim 12PPS photocatalysis membrana preparation method, it is characterised in that the titanium source is
Butyl titanate, titanium tetrachloride, titanium sulfate, titanium trichloride, isopropyl titanate, cyclopentadienyl titanium dichloride, titanium tetrafluoride or titanium potassium oxalate
At least one of.
4. load TiO according to claim 12PPS photocatalysis membrana preparation method, it is characterised in that the sulfate
It is at least one of ferric sulfate, ammonium sulfate, titanium sulfate, sodium sulphate, magnesium sulfate, copper sulphate, potassium sulfate or aluminum sulfate.
5. load TiO according to claim 12PPS photocatalysis membrana preparation method, it is characterised in that it is every square centimeter
0.02 ~ 0.04 milliliter of TiO is added in PPS microporous barrier2Precursor solution.
6. a kind of PPS@TiO that the preparation method as described in claim 1-5 is any obtains2Photocatalysis membrana is in organic dye waste water
Application.
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