CN104128209B - A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst - Google Patents

A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst Download PDF

Info

Publication number
CN104128209B
CN104128209B CN201410395030.7A CN201410395030A CN104128209B CN 104128209 B CN104128209 B CN 104128209B CN 201410395030 A CN201410395030 A CN 201410395030A CN 104128209 B CN104128209 B CN 104128209B
Authority
CN
China
Prior art keywords
photochemical catalyst
loaded
tio
nano particle
shell structure
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201410395030.7A
Other languages
Chinese (zh)
Other versions
CN104128209A (en
Inventor
姚同杰
汪浩
崔铁钰
崔放
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Harbin Institute of Technology
Original Assignee
Harbin Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Harbin Institute of Technology filed Critical Harbin Institute of Technology
Priority to CN201410395030.7A priority Critical patent/CN104128209B/en
Publication of CN104128209A publication Critical patent/CN104128209A/en
Application granted granted Critical
Publication of CN104128209B publication Critical patent/CN104128209B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Catalysts (AREA)

Abstract

A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst, the present invention relates to TiO 2the preparation method of photochemical catalyst.The present invention's traditional catalysis material that will solve based on existing titanium dioxide has photoresponse narrow range and the not high problem of catalyst activity.Method: by Electrospun TiO 2join in the aqueous solution in silver-colored source, ultrasonic agitation, then centrifugal treating washing, again the product after washing is scattered in distilled water, add in system by polymer monomer and Iron trichloride hexahydrate, centrifugal treating is also washed, and namely obtains the polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2photochemical catalyst.The present invention is used for a kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation of photochemical catalyst.

Description

A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst
Technical field
The present invention relates to TiO 2the preparation method of photochemical catalyst.
Background technology
Metal nanoparticle has attracted the attention of increasing scientific researcher because it has unique physics, chemistry and biological nature.These characteristics make metal nanoparticle be widely used in energy conversion, sensor, biological medicine, especially catalyst aspect.Research display, nano particle has very high specific area, makes it have very high catalytic activity.But nano material also also exists weak point in the process of practical application.Can be there is serious gathering in nano particle, thus result in the obvious reduction of its catalytic activity in the solution, and what this point was serious hinders nano particle in real-life extensive use.
Conducting polymer macromolecular material, polymer is cross-linked polymer, nano particle can be anchored in polymeric system in the course of the polymerization process.Can effectively prevent nano particle from assembling.Polymeric color is dark simultaneously, easily absorbs more visible ray.
Along with economic development and population expansion, environmental pollution threatens human survival, and environmental problem has become global important topic.Compared with conventional method, photocatalysis degradation organic contaminant has nontoxic, and efficiently, the advantage such as inexpensive, is expected to become new energy-efficient environmental pollution improvement's method.At present, the traditional catalysis material based on titanium dioxide has photoresponse narrow range and the not high shortcoming of catalyst activity.
Summary of the invention
The present invention's traditional catalysis material that will solve based on existing titanium dioxide has photoresponse narrow range and the not high problem of catalyst activity, and provides a kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst.
A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst, specifically carries out according to following steps:
One, by Electrospun TiO 2join in the aqueous solution in silver-colored source, ultrasonic 1min ~ 60min, then stirs 1h ~ 10h, obtains dispersion soln A;
Described Electrospun TiO 2quality and the volume ratio of the aqueous solution in silver-colored source be 1mg:(0.01 ~ 0.5) mL;
Two, under rotating speed is 1000r/min ~ 8000r/min, dispersion soln A centrifugal treating 3min ~ 15min that step one is obtained, then spend deionized water 1 time ~ 10 times, then the product after washing is scattered in distilled water, and ultrasonic 1min ~ 10min, obtain dispersion soln B;
Described Electrospun TiO 2quality and the volume ratio of distilled water be 1mg:(1 ~ 100) mL;
Three, under agitation, polymer monomer is joined in dispersion soln B, stir 1h ~ 8h, Iron trichloride hexahydrate is added again in system, stirring reaction 3h ~ 20h, then under rotating speed is 1000r/min ~ 8000r/min, centrifugal treating 3min ~ 15min, finally spend deionized water again 1 time ~ 10 times, namely obtain the polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2photochemical catalyst;
The quality of described polymer monomer and the volume ratio of dispersion soln B are 1g:(10 ~ 1000) mL; Described polymer monomer and the mass ratio of Iron trichloride hexahydrate are 1:(1 ~ 10000).
The invention has the beneficial effects as follows: the catalyst that 1, prepared by the present invention has the stability higher than general catalyst, avoiding material because assembling the low problem of the catalytic activity that causes, can service life of extending catalyst, reduce financial cost.
2, the catalyst prepared by the present invention has the quantum efficiency of the catalysis material of wider response range and Geng Gao than traditional titanium dioxide optical catalyst.
3, the catalyst prepared by the present invention has very strong degradation to dyestuff in sewage.
The present invention is used for a kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation of photochemical catalyst.
Accompanying drawing explanation
Fig. 1 is Electrospun TiO 2the SEM photo of nano wire;
Fig. 2 is Ag-AgCl/PTTiO prepared by embodiment 2the SEM photo of composite;
Fig. 3 is Ag-AgCl/PTTiO prepared by embodiment 2the TEM photo of composite;
Fig. 4 is the catalytic performance figure of photochemical catalyst prepared by embodiment; A is the curve of titanium dioxide as the ultraviolet-visible absorption spectroscopy test gained of photochemical catalyst; B is the curve of the ultraviolet-visible absorption spectroscopy test gained after the photochemical catalyst catalysis prepared of embodiment;
Fig. 5 is that photochemical catalyst prepared by embodiment carries out catalysis to reaction system, uses different number of times, the curve of the time of dye degrades sodium borohydride reduction methylene blue required for 10% of original vol through reclaiming.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises any combination between each detailed description of the invention.
Detailed description of the invention one: the polymer core-shell structure TiO of a kind of loaded Ag-AgCl nano particle described in present embodiment 2the preparation method of photochemical catalyst, specifically carries out according to following steps:
One, by Electrospun TiO 2join in the aqueous solution in silver-colored source, ultrasonic 1min ~ 60min, then stirs 1h ~ 10h, obtains dispersion soln A;
Described Electrospun TiO 2quality and the volume ratio of the aqueous solution in silver-colored source be 1mg:(0.01 ~ 0.5) mL;
Two, under rotating speed is 1000r/min ~ 8000r/min, dispersion soln A centrifugal treating 3min ~ 15min that step one is obtained, then spend deionized water 1 time ~ 10 times, then the product after washing is scattered in distilled water, and ultrasonic 1min ~ 10min, obtain dispersion soln B;
Described Electrospun TiO 2quality and the volume ratio of distilled water be 1mg:(1 ~ 100) mL;
Three, under agitation, polymer monomer is joined in dispersion soln B, stir 1h ~ 8h, Iron trichloride hexahydrate is added again in system, stirring reaction 3h ~ 20h, then under rotating speed is 1000r/min ~ 8000r/min, centrifugal treating 3min ~ 15min, finally spend deionized water again 1 time ~ 10 times, namely obtain the polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2photochemical catalyst;
The quality of described polymer monomer and the volume ratio of dispersion soln B are 1g:(10 ~ 1000) mL; Described polymer monomer and the mass ratio of Iron trichloride hexahydrate are 1:(1 ~ 10000).
The catalysis light district scope of titanium dioxide is narrow, by carrying out it can reducing its electronic transition energy when illumination is penetrated with the doping of Nano silver grain, photocatalysis scope is moved to visible region.Silver chloride nanoparticles with titania additive recombination process in can introduce Lattice Oxygen room or part Lacking oxygen is substituted, this makes titanium dioxide forbidden band narrow, thus expand the coverage of radiant light, therefore, prepared catalyst has wider response range than traditional titanium dioxide optical catalyst.The black shell of polypyrrole can absorb more visible ray simultaneously, and this also has certain facilitation to raising photocatalysis efficiency.
The beneficial effect of present embodiment is: the catalyst that 1, prepared by present embodiment has the stability higher than general catalyst, avoids material because assembling the low problem of the catalytic activity that causes, can service life of extending catalyst, reduces financial cost.
2, the catalyst prepared by present embodiment has the quantum efficiency of the catalysis material of wider response range and Geng Gao than traditional titanium dioxide optical catalyst.
3, the catalyst prepared by present embodiment has very strong degradation to dyestuff in sewage.
Detailed description of the invention two: present embodiment and detailed description of the invention one are unlike the Electrospun TiO described in step one 2diameter be 100nm ~ 1000nm.Other is identical with detailed description of the invention one.
Detailed description of the invention three: one of present embodiment and detailed description of the invention one or two unlike: the concentration of the aqueous solution in the silver-colored source described in step one is 0.01mol/L ~ 10mol/L.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three unlike: the aqueous solution in the silver-colored source described in step one is a kind of or wherein several mixture in the aqueous solution of the aqueous solution of silver sulfate, the aqueous solution of silver cyanide, the aqueous solution of silver oxide and silver nitrate.Other is identical with detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four unlike: the polymer monomer described in step 3 is thiophene monomer, pyrrole monomer or aniline monomer.Other is identical with detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five unlike: in step 2 under rotating speed is 1000r/min ~ 8000r/min, the dispersion soln A centrifugal treating 15min that step one is obtained.Other is identical with detailed description of the invention one to five.
Present embodiment act as removing and is not attached to TiO 2on silver ion.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six unlike: in step 3 under rotating speed is 1000r/min ~ 8000r/min, centrifugal treating 15min.Other is identical with detailed description of the invention one to six.
Present embodiment act as the responseless polymer monomer of removing and iron ion.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment:
The polymer core-shell structure TiO of a kind of loaded Ag-AgCl nano particle described in the present embodiment 2the preparation method of photochemical catalyst, specifically carries out according to following steps:
One, by 100mg diameter be the Electrospun TiO of 300nm 2joining 10mL concentration is in the silver nitrate aqueous solution of 0.5mol/mL, and ultrasonic 30min, then stirs 1h, dispersion soln A;
Two, under rotating speed is 6000r/min, the dispersion soln A centrifugal treating 5min that step one is obtained, then wash 3 times by deionized water, then the product after washing is scattered in 120mL distilled water, and ultrasonic 20min, obtain dispersion soln B;
Three, under agitation, 0.05mg thiophene monomer is joined in dispersion soln B, stir 5h, 100mg Iron trichloride hexahydrate is added again in system, stirring reaction 20h, then under rotating speed is 7000r/min, centrifugal treating 10min, finally spend deionized water again 3 times, obtain the polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2photochemical catalyst, i.e. Ag-AgCl/PTTiO 2composite.
Fig. 1 is Electrospun TiO 2the SEM photo of nano wire, Fig. 2 is Ag-AgCl/PTTiO prepared by embodiment 2the SEM photo of composite, as seen from the figure, its diameter increases to some extent, and outward appearance is mellow and full, and the composite of synthesis is very well apparent.
Fig. 3 is Ag-AgCl/PTTiO prepared by embodiment 2the TEM photo of composite, as seen from the figure, nano wire is nucleocapsid structure, outside coated PT has been described, can have found out that on housing, some inorganic matter nano particles in grappling simultaneously in picture.
Fig. 4 is the catalytic performance figure of photochemical catalyst prepared by embodiment; A is the curve of titanium dioxide as the ultraviolet-visible absorption spectroscopy test gained of photochemical catalyst; B is the curve of the ultraviolet-visible absorption spectroscopy test gained after the photochemical catalyst catalysis prepared of embodiment; As seen from the figure, photochemical catalyst prepared by the present embodiment can be found out to the photocatalytic activity of dye degrades sodium borohydride reduction methylene blue from curve far away higher than the photochemical catalyst not carrying out modification, confirm that the photochemical catalyst that the present embodiment synthesizes has higher photocatalytic activity.
Fig. 5 is that photochemical catalyst prepared by embodiment carries out catalysis to reaction system, uses different number of times, the curve of the time of dye degrades sodium borohydride reduction methylene blue required for 10% of original vol through reclaiming.As seen from the figure, the catalysis time of catalyst increases to some extent through increasing of access times, but the time that six tests increase does not have too great fluctuation process, and this illustrates that catalyst has good stability.

Claims (6)

1. the polymer core-shell structure TiO of a loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst, is characterized in that a kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst carries out according to following steps:
One, by Electrospun TiO 2join in the aqueous solution in silver-colored source, ultrasonic 1min ~ 60min, then stirs 1h ~ 10h, obtains dispersion soln A;
Described Electrospun TiO 2quality and the volume ratio of the aqueous solution in silver-colored source be 1mg:(0.01 ~ 0.5) mL;
Two, under rotating speed is 1000r/min ~ 8000r/min, dispersion soln A centrifugal treating 3min ~ 15min that step one is obtained, then spend deionized water 1 time ~ 10 times, then the product after washing is scattered in distilled water, and ultrasonic 1min ~ 10min, obtain dispersion soln B;
Described Electrospun TiO 2quality and the volume ratio of distilled water be 1mg:(1 ~ 100) mL;
Three, under agitation, polymer monomer is joined in dispersion soln B, stir 1h ~ 8h, Iron trichloride hexahydrate is added again in system, stirring reaction 3h ~ 20h, then under rotating speed is 1000r/min ~ 8000r/min, centrifugal treating 3min ~ 15min, finally spend deionized water again 1 time ~ 10 times, namely obtain the polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2photochemical catalyst;
The quality of described polymer monomer and the volume ratio of dispersion soln B are 1g:(10 ~ 1000) mL; Described polymer monomer and the mass ratio of Iron trichloride hexahydrate are 1:(1 ~ 10000);
Polymer monomer described in step 3 is thiophene monomer, pyrrole monomer or aniline monomer.
2. the polymer core-shell structure TiO of a kind of loaded Ag-AgCl nano particle according to claim 1 2the preparation method of photochemical catalyst, is characterized in that the Electrospun TiO described in step one 2diameter be 100nm ~ 1000nm.
3. the polymer core-shell structure TiO of a kind of loaded Ag-AgCl nano particle according to claim 1 2the preparation method of photochemical catalyst, is characterized in that the concentration of the aqueous solution in the silver-colored source described in step one is 0.01mol/L ~ 10mol/L.
4. the polymer core-shell structure TiO of a kind of loaded Ag-AgCl nano particle according to claim 1 2the preparation method of photochemical catalyst, is characterized in that the aqueous solution in the silver-colored source described in step one is a kind of or wherein several mixture in the aqueous solution of the aqueous solution of silver sulfate, the aqueous solution of silver cyanide and silver nitrate.
5. the polymer core-shell structure TiO of a kind of loaded Ag-AgCl nano particle according to claim 1 2the preparation method of photochemical catalyst, is characterized in that in step 2 under rotating speed is 1000r/min ~ 8000r/min, dispersion soln A centrifugal treating 15min step one obtained.
6. the polymer core-shell structure TiO of a kind of loaded Ag-AgCl nano particle according to claim 1 2the preparation method of photochemical catalyst, is characterized in that in step 3 under rotating speed is 1000r/min ~ 8000r/min, centrifugal treating 15min.
CN201410395030.7A 2014-08-12 2014-08-12 A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst Active CN104128209B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410395030.7A CN104128209B (en) 2014-08-12 2014-08-12 A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410395030.7A CN104128209B (en) 2014-08-12 2014-08-12 A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst

Publications (2)

Publication Number Publication Date
CN104128209A CN104128209A (en) 2014-11-05
CN104128209B true CN104128209B (en) 2016-03-30

Family

ID=51801208

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410395030.7A Active CN104128209B (en) 2014-08-12 2014-08-12 A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst

Country Status (1)

Country Link
CN (1) CN104128209B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107008238B (en) * 2017-03-30 2019-11-12 焦正 The synthetic method of titanium dioxide hollow structure material for organic pollutant degradation
CN108525662B (en) * 2018-04-09 2021-01-08 福建师范大学 Truncated cube Ag2O modified TiO2Preparation and application of hollow nanofiber photocatalyst

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101537350A (en) * 2009-04-27 2009-09-23 武汉理工大学 Ag/AgCl/TiO* nanotube array plasma visible-light photocatalyst and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10022750A1 (en) * 2000-05-10 2001-11-22 Wolfgang Schuhmann Preparing surface with immobilized recognition elements, useful e.g. in biosensors, by electrodeposition of resin from emulsion containing active substances

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101537350A (en) * 2009-04-27 2009-09-23 武汉理工大学 Ag/AgCl/TiO* nanotube array plasma visible-light photocatalyst and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Polypyrrole-Decorated Ag-TiO2 Nanofibers Exhibiting Enhanced Photocatalytic Activity under Visible-Light Illumination;Yucheng Yang et al.;《ACS Appl.Mater.Interfaces.》;20130617;第5卷;第6201-6207页 *

Also Published As

Publication number Publication date
CN104128209A (en) 2014-11-05

Similar Documents

Publication Publication Date Title
CN103433060B (en) Core-shell TiO2/ZnIn2S4 composite photocatalyst and preparation method and application thereof
Zhang et al. Influence of semiconductor/insulator/semiconductor structure on the photo-catalytic activity of Fe3O4/SiO2/polythiophene core/shell submicron composite
CN104689835B (en) CeO2Nano-particle/CdS nanometer rods composite photo-catalyst and its preparation method and application
CN107008259B (en) Nuclear shell structure nano Aurum clusters-titanium dioxide composite catalyst
CN106881111A (en) Composite bismuth vanadium photocatalyst of cuprous oxide and silver-colored mutual load and its preparation method and application
CN105312088B (en) Fe2O3 doping covalent triazine organic polymer visible light catalyst and its preparation and application
CN106732232B (en) A kind of preparation method of the yolk type Fenton microreactor of inner surface supported precious metal nano-particle
Liu et al. Construction of hierarchical Prussian blue microcrystal with high sunlight absorption for efficient photo-thermal degradation of organic pollutants
CN105664980A (en) Preparation method and application of pine needle biochar flower-shaped BiOCl-loaded composite photocatalyst
CN108654642B (en) Efficient composite photocatalyst Ag with visible light response2Preparation method of O/alpha-FeOOH
Liao et al. Photocatalyst immobilized by hydrogel, efficient degradation and self regeneration: A review
CN106582626A (en) Preparation method and application of novel silver ion doped TiO2 composite material
CN104128209B (en) A kind of polymer core-shell structure TiO of loaded Ag-AgCl nano particle 2the preparation method of photochemical catalyst
Su et al. Heterostructured Bi2O2CO3/rGO/PDA photocatalysts with superior activity for organic pollutant degradation: Structural characterization, reaction mechanism and economic assessment
CN108295873B (en) The preparation of porous magnetic compound protein load Er ions BiOCl photochemical catalyst
Qin et al. Efficient photocatalytic H2O2 production by using unstable SO functional groups as oxygen adsorption and active sites in shuttlecock waste-derived N, S-doped carbon dots
CN113181912B (en) Cu (copper) alloy 2 O-TiO 2 Composite photocatalyst, preparation method and application thereof
Wu et al. Construction of Z-Scheme BiFeO3/Bi2O4 heterojunction for significantly boosted photocatalytic degradation of tetracycline under visible irradiation
CN103723760B (en) A kind of cadmium sulfide photochemical catalyst and preparation method thereof
CN104826639B (en) Silver phosphate/reduced graphene/titanic oxide nano compound material and preparation method
CN103831119B (en) A kind of sheet silver@silver iodate visible-light photocatalyst and preparation method thereof
CN110237870A (en) A kind of polyphenyl phenol/composite titania material and preparation method and application
Yan et al. Photocatalytic activity of nanocomposites of ZnO and multi-walled carbon nanotubes for dye degradation
CN103831117A (en) Preparation method for synthesizing platinum nanoparticles supported magnetic hollow capsule type catalyst by taking polystyrene as soft template
CN108554427A (en) A kind of In2O3/ BiOI semiconductor compound photocatalysts and its preparation method and application

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant