CN102294271B - Preparation method of synthetic resin loaded nanometer bismuth niobate photocatalyst - Google Patents

Preparation method of synthetic resin loaded nanometer bismuth niobate photocatalyst Download PDF

Info

Publication number
CN102294271B
CN102294271B CN2011101735675A CN201110173567A CN102294271B CN 102294271 B CN102294271 B CN 102294271B CN 2011101735675 A CN2011101735675 A CN 2011101735675A CN 201110173567 A CN201110173567 A CN 201110173567A CN 102294271 B CN102294271 B CN 102294271B
Authority
CN
China
Prior art keywords
synthetic resin
photochemical catalyst
solution
preparation
niobic acid
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.)
Expired - Fee Related
Application number
CN2011101735675A
Other languages
Chinese (zh)
Other versions
CN102294271A (en
Inventor
赵洁
姚秉华
何强
余晓皎
张健
钮金芬
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.)
Xian University of Technology
Original Assignee
Xian University 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 Xian University of Technology filed Critical Xian University of Technology
Priority to CN2011101735675A priority Critical patent/CN102294271B/en
Publication of CN102294271A publication Critical patent/CN102294271A/en
Application granted granted Critical
Publication of CN102294271B publication Critical patent/CN102294271B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Catalysts (AREA)

Abstract

The invention discloses a preparation method of a synthetic resin loaded nanometer bismuth niobate photocatalyst. The preparation method comprises the following steps of 1, preparing a nanometer bismuth niobate photocatalyst, 2, weighing an appropriate amount of the prepared nanometer bismuth niobate photocatalyst and a synthetic resin LSA900C, wherein a mass ratio of the nanometer bismuth niobate photocatalyst to the synthetic resin LSA900C is controlled so that a resin load capacity is in a range of 5 to 25%, adding the nanometer bismuth niobate photocatalyst and the synthetic resin LSA900C into absolute ethanol, and putting the mixed solution into an ultrasonic cleaner for a full ultrasonic reaction, and 3, carrying out extraction filtration of the mixture obtained by the step 2, drying in air, putting the dried mixture into a vacuum drying oven to heat it to a temperature of 180 to 200 DEG C at a rate of 8 to 10 DEG C per minute, keeping warm for 0.5 to 1 hour, cooling in vacuum drying oven to obtain a desired product, and taking the desired product out. In the invention, the synthetic resin LSA900C is utilized for loading of a photocatalyst bismuth niobate for the first time. Compared with the prior art, the synthetic resin loaded nanometer bismuth niobate photocatalyst prepared by the preparation method has the advantages of high catalytic efficiency, high catalytic activity, strong loading soundness and long service life.

Description

A kind of preparation method of synthetic resin loaded with nano niobic acid bismuth photochemical catalyst
Technical field
The invention belongs to the photochemical catalyst preparing technical field, be specifically related to a kind of preparation method of synthetic resin loaded with nano niobic acid bismuth photochemical catalyst.
Background technology
From TiO in 1972 2Be used to since the photodissociation water, the research and development conductor photocatalysis material is also used it for the degraded of organic pollution, is the heat subject of field of materials.This photocatalysis oxidation technique can change poisonous and hazardous organic pollution into carbon dioxide, water, inorganic ions or than the little material of former organic matter toxicity, have of low pollution or pollution-free, equipment is simple, advantage such as easy to operate, efficient.In the last thirty years, with TiO 2For representing traditional photochemical catalyst and with niobic acid silver (AgNbO 3), lead niobate (Pb 2Nb 2O 7), niobic acid indium (InNbO 4) and niobic acid bismuth (BiNbO 4) be the new catalyst of representative, wait to have obtained extensive and deep research.But what Most scholars adopted is the direct catalysis of powder, and this method difficult separation and recycling makes this technology be difficult to applied.Therefore, seek suitable carriers, realize the load of catalysis material, have great importance for extensive practicability of this technology and commercialization.
At present, bead, lamellar graphite, Ceramic Balls, extra large sand, natural minerals etc. are adopted in the load of photochemical catalyst more.These carriers can improve the catalytic effect of photochemical catalyst in various degree, but all have the problems such as characteristics that the carrier source is unstable, carrier lacks and be difficult to bring into play carrier self service life, are unfavorable for promoting the use of.
Synthetic resin is the synthetic high molecular polymer of one type of manual work; The resin of different model has different performances, and existing application more widely in fields such as food, biological medicine, chemical industry catalysis and water treatment is along with the development of synthetic resin industry; Many new type resins are by successfully exploitation; Like homemade LSA900C type synthetic resin, but less to the application technical research of these resins, restricted promoting the use of of these resins.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of synthetic resin loaded with nano niobic acid bismuth photochemical catalyst; First LSA900C type synthetic resin is used for the load of photochemical catalyst niobic acid bismuth; Compared with prior art, the synthetic resin loaded with nano niobic acid bismuth photochemical catalyst catalytic efficiency that makes is high, catalytic activity is big, the load fastness is strong and long service life.
The technical scheme that the present invention adopted is that a kind of preparation method of synthetic resin loaded with nano niobic acid bismuth photochemical catalyst may further comprise the steps:
Step 1, preparation nanometer niobic acid bismuth photochemical catalyst:
Step 1a, to take by weighing mol ratio be 1: 2 niobium pentaoxide and bismuth and ammonium citrate;
Step 1b, niobium pentaoxide that step 1a is taken by weighing are fully dissolving in 48%~51% the hydrofluoric acid in concentration; With the mixed solution that obtains hydro-thermal reaction 3h~6h under 70 ℃~100 ℃ temperature; Naturally after the cooling, add concentration and be 28% ammoniacal liquor until separating out deposition, using concentration is this sediment of ammonia scrubbing of 5%~8%; Is fully dissolving in the citric acid solution of 0.2mol/L with this sediment after the washing in concentration, and gained solution is designated as A solution; The hydro-thermal reaction device therefor is for there being the teflon-lined autoclave;
Step 1c, bismuth and ammonium citrate that step 1a is taken by weighing are fully dissolving in the ammonium citrate solution of 0.2mol/L in concentration, and with the mixed solution magnetic agitation 1h~2h that obtains, gained solution is designated as B solution; The magnetic agitation device therefor is a magnetic stirring apparatus;
The B solution that step 1d, the A solution that step 1b is obtained and step 1c obtain mixes and stirs, and obtains spawn, oven dry, and under 200 ℃~600 ℃ temperature, calcining 8h~10h promptly gets nanometer niobic acid bismuth photochemical catalyst.
Step 2, take by weighing proper amount of nano niobic acid bismuth photochemical catalyst and LSA900C type synthetic resin; Controlling its both mass ratioes, to make resin-carried amount be 5%~25%; Both are positioned in the absolute ethyl alcohol with it; Ultrasonic reaction 30min~40min in supersonic wave cleaning machine fully reacts nanometer niobic acid bismuth photochemical catalyst and LSA900C type synthetic resin, obtains solidliquid mixture.
Step 3, with the solidliquid mixture suction filtration that step 2 obtains, behind air dry 12h~14h, place vacuum drying chamber to be warming up to 180 ℃~200 ℃ with the speed of 8 ℃~10 ℃/min; Insulation 0.5h~1h; With the stove cooling, take out, promptly get synthetic resin loaded with nano niobic acid bismuth photochemical catalyst.
The beneficial effect of the inventive method is: 1, method is easy and simple to handle, does not need special installation, and is with low cost, and repeatability is good, is fit to a large amount of preparations of industry.2, the synthetic resin loaded with nano niobic acid bismuth photochemical catalyst that makes through the inventive method can efficient catalytic degraded water body in organic pollution, its catalytic efficiency is high, catalytic activity is big, the load fastness is strong, long service life.The synthetic resin loaded with nano niobic acid bismuth photochemical catalyst that makes can swim in the water surface, has easily separatedly, easy and simple to handle, and advantage such as can be recycled.3, expanded the application of homemade novel synthetic resin LSA900C type synthetic resin.
Description of drawings
The X ray diffracting spectrum of the nanometer niobic acid bismuth photochemical catalyst that Fig. 1 makes for the inventive method;
Fig. 2 is the sem photograph of the employed LSA900C type of the inventive method synthetic resin;
Fig. 3 is the sem photograph of the synthetic resin loaded with nano niobic acid bismuth photochemical catalyst of the inventive method preparation;
Fig. 4 is the degradation curve figure of the synthetic resin loaded with nano niobic acid bismuth photochemical catalyst of the inventive method preparation.
The specific embodiment
Step 1, preparation nanometer niobic acid bismuth photochemical catalyst, its concrete steps are:
Step 1a, take by weighing the niobium pentaoxide (Nb that quality is 1.0004g 2O 5), and quality is the bismuth and ammonium citrate (Bi (NH of 3.4017g 3) 2C 6H 7O 7H 2O), its both mol ratio is 1: 2.
Step 1b, niobium pentaoxide that step 1a is taken by weighing are fully dissolving in 48%~51% the hydrofluoric acid in 30mL~50mL and concentration; With the mixed solution that obtains in the teflon-lined autoclave is arranged; Hydro-thermal reaction 3h~6h under 70 ℃~100 ℃ temperature; Naturally after the cooling, add concentration and be 28% ammoniacal liquor until separating out deposition, using concentration is this sediment of ammonia scrubbing of 5%~8%; Is fully dissolving in the citric acid solution of 0.2mol/L with this sediment after the washing in concentration, and gained solution is designated as A solution;
Step 1c, bismuth and ammonium citrate that step 1a is taken by weighing are fully dissolving in the ammonium citrate solution of 0.2mol/L in concentration, and with the mixed solution that obtains magnetic agitation 1h~2h in magnetic stirring apparatus, gained solution is designated as B solution;
The B solution that step 1d, the A solution that step 1b is obtained and step 1c obtain mixes and stirs, and obtains spawn, and oven dry places Muffle furnace, and under 200 ℃~600 ℃ temperature, calcining 8h~10h promptly gets nanometer niobic acid bismuth photochemical catalyst.
As shown in Figure 1, lines 2 are the X ray diffracting spectrum of the nanometer niobic acid bismuth photochemical catalyst that makes in the present embodiment among the figure.
Step 2, taking by weighing the nanometer niobic acid bismuth photochemical catalyst that quality is 0.1g, is the LSA900C type synthetic resin of 0.4~2g with quality, and at this moment, resin-carried amount is 5%~25%; With claim nanometer niobic acid bismuth photochemical catalyst and LSA900C type synthetic resin be positioned in 20mL~80mL absolute ethyl alcohol; Nanometer niobic acid bismuth photochemical catalyst and LSA900C type synthetic resin are in anhydrous ethanol medium; Use supersonic wave cleaning machine ultrasonic reaction 30min~40min; Nanometer niobic acid bismuth photochemical catalyst and LSA900C type synthetic resin are fully reacted, obtain solidliquid mixture.
Step 3, with the solidliquid mixture suction filtration that step 2 obtains, behind air dry 12h~14h, place vacuum drying chamber to be warming up to 180 ℃~200 ℃ with the speed of 8 ℃~10 ℃/min; Insulation 0.5h~1h; With the stove cooling, take out, promptly get synthetic resin loaded with nano niobic acid bismuth photochemical catalyst.
Be illustrated in figure 2 as the sem photograph of the employed macroporous absorbent resin LSA900C of the inventive method type synthetic resin.Be illustrated in figure 3 as, the inventive method is utilized the sem photograph of the synthetic resin loaded with nano niobic acid bismuth photochemical catalyst of LSA900C type synthetic resin preparation.
Use the synthetic resin loaded with nano niobic acid bismuth photochemical catalyst of the inventive method preparation to carry out the photocatalytic degradation experiment.With the degradation model of Ornidazole as photocatalytic activity.Getting concentration is 10mgL -1Ornidazole solution and 0.1g synthetic resin loaded with nano niobic acid bismuth photochemical catalyst together add reactor, light source is a 300W ultraviolet high-pressure sodium lamp.Before each illumination began, ultrasonic 30min reached the absorption-desorption balance earlier, and the sample that extracts a 0min then is as the reference of data afterwards.Open ultraviolet light source and begin illumination, lead to the cooling water and air in the experimentation, every separated 10min sampling once after loaded optic catalyst is removed in separation, is got its uv-visible absorption spectra of supernatant liquor test.The ratio of mother liquor peak value is exactly degradation rate when the absworption peak peak value of different time sampling and 0min.Result of the test is as shown in Figure 4.
Among Fig. 4, abscissa is a degradation time, and ordinate is a degradation rate, and line 1 is the Ornidazole blank solution, and line 2 is the degradation curve of niobic acid bismuth, and line 4 is the degradation curve of the synthetic resin loaded with nano niobic acid bismuth photochemical catalyst of present embodiment preparation.As can beappreciated from fig. 4, the degradation rate of the synthetic resin loaded with nano niobic acid bismuth photochemical catalyst of the inventive method preparation explains that greater than the degradation rate of niobic acid bismuth and Ornidazole blank solution its degradation effect is superior to directly using the degradation effect of nanometer niobic acid bismuth photochemical catalyst.

Claims (3)

1. the preparation method of a synthetic resin loaded with nano niobic acid bismuth photochemical catalyst is characterized in that, may further comprise the steps:
Step 1, preparation nanometer niobic acid bismuth photochemical catalyst:
Step 1a, to take by weighing mol ratio be 1: 2 niobium pentaoxide and bismuth and ammonium citrate;
Step 1b, niobium pentaoxide that step 1a is taken by weighing are fully dissolving in 48%~51% the hydrofluoric acid in concentration; With the mixed solution that obtains hydro-thermal reaction 3h~6h under 70 ℃~100 ℃ temperature; Naturally after the cooling, add concentration and be 28% ammoniacal liquor until separating out deposition, using concentration is this sediment of ammonia scrubbing of 5%~8%; Is fully dissolving in the citric acid solution of 0.2mol/L with this sediment after the washing in concentration, and gained solution is designated as A solution;
Step 1c, bismuth and ammonium citrate that step 1a is taken by weighing are fully dissolving in the ammonium citrate solution of 0.2mol/L in concentration, and with the mixed solution magnetic agitation 1h~2h that obtains, gained solution is designated as B solution;
The B solution that step 1d, the A solution that step 1b is obtained and step 1c obtain mixes and stirs, and obtains spawn, oven dry, and under 200 ℃~600 ℃ temperature, calcining 8h~10h promptly gets nanometer niobic acid bismuth photochemical catalyst;
Step 2, take by weighing proper amount of nano niobic acid bismuth photochemical catalyst and LSA900C type synthetic resin; Controlling its both mass ratioes, to make resin-carried amount be 5%~25%; Both are positioned in the absolute ethyl alcohol with it; Ultrasonic reaction 30min~40min in supersonic wave cleaning machine fully reacts nanometer niobic acid bismuth photochemical catalyst and LSA900C type synthetic resin, obtains solidliquid mixture;
Step 3, with the solidliquid mixture suction filtration that step 2 obtains, behind air dry 12h~14h, place vacuum drying chamber to be warming up to 180 ℃~200 ℃ with the speed of 8 ℃~10 ℃/min; Insulation 0.5h~1h; With the stove cooling, take out, promptly get synthetic resin loaded with nano niobic acid bismuth photochemical catalyst.
2. according to the preparation method of the said synthetic resin loaded with nano of claim 1 niobic acid bismuth photochemical catalyst, it is characterized in that among the said step 1b, said hydro-thermal reaction device therefor is for there being the teflon-lined autoclave.
3. according to the preparation method of the said synthetic resin loaded with nano of claim 1 niobic acid bismuth photochemical catalyst, it is characterized in that among the said step 1c, said magnetic agitation device therefor is a magnetic stirring apparatus.
CN2011101735675A 2011-06-24 2011-06-24 Preparation method of synthetic resin loaded nanometer bismuth niobate photocatalyst Expired - Fee Related CN102294271B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2011101735675A CN102294271B (en) 2011-06-24 2011-06-24 Preparation method of synthetic resin loaded nanometer bismuth niobate photocatalyst

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2011101735675A CN102294271B (en) 2011-06-24 2011-06-24 Preparation method of synthetic resin loaded nanometer bismuth niobate photocatalyst

Publications (2)

Publication Number Publication Date
CN102294271A CN102294271A (en) 2011-12-28
CN102294271B true CN102294271B (en) 2012-11-28

Family

ID=45355087

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2011101735675A Expired - Fee Related CN102294271B (en) 2011-06-24 2011-06-24 Preparation method of synthetic resin loaded nanometer bismuth niobate photocatalyst

Country Status (1)

Country Link
CN (1) CN102294271B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105236488B (en) * 2015-08-27 2017-06-20 中南民族大学 A kind of Bi3NbO7The preparation and application of porous nano-sheet

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101362084A (en) * 2008-09-18 2009-02-11 武汉理工大学 Visible-light response nano Bi3NbO7 photocatalyst preparation method and use thereof
CN101716503A (en) * 2009-11-23 2010-06-02 南京大学 Visible light catalyst BiNbO4, preparation method thereof and application thereof
CN101884917A (en) * 2010-06-29 2010-11-17 于建强 Method for preparing composite fiber material for visible light photocatalytic degradation of organic pollutants

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101362084A (en) * 2008-09-18 2009-02-11 武汉理工大学 Visible-light response nano Bi3NbO7 photocatalyst preparation method and use thereof
CN101716503A (en) * 2009-11-23 2010-06-02 南京大学 Visible light catalyst BiNbO4, preparation method thereof and application thereof
CN101884917A (en) * 2010-06-29 2010-11-17 于建强 Method for preparing composite fiber material for visible light photocatalytic degradation of organic pollutants

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
Gaoke Zhang et al..Preparation of nanosized Bi3NbO7 and its visible-light photocatalytic property.《Journal of Hazardous Materials》.2009,第172卷第987页第2节.
Lu Wang et al..Visible light responsive bismuth niobate photocatalyst: enhanced contaminant degradation and hydrogen generation.《Journal of Materials Chemistry》.2010,第20卷第8406页实验部分.
Preparation of nanosized Bi3NbO7 and its visible-light photocatalytic property;Gaoke Zhang et al.;《Journal of Hazardous Materials》;20090729;第172卷;第987页第2节 *
Visible light responsive bismuth niobate photocatalyst: enhanced contaminant degradation and hydrogen generation;Lu Wang et al.;《Journal of Materials Chemistry》;20101231;第20卷;第8406页实验部分 *

Also Published As

Publication number Publication date
CN102294271A (en) 2011-12-28

Similar Documents

Publication Publication Date Title
CN103736513B (en) A kind of TiO 2(B) g-C 3n 4the preparation method of composite nano plate photochemical catalyst
CN110075854B (en) Preparation and application method of monolithic catalyst
CN107159313A (en) A kind of core shell structure TiO2The preparation method of nanotube@Ti MOF catalyst
CN104128184A (en) A floating type CoFe2O4/TiO2/floating bead composite photocatalyst and its preparation method
CN109675581A (en) Ferrimanganic bimetallic oxide modification biological charcoal light Fenton composite material and preparation method
CN103721738B (en) A kind of non-metal optical catalysis material of efficient reducing carbon dioxide
CN102350354A (en) Magnetically supported titanium dioxide photocatalyst and preparation method thereof
CN107649130A (en) A kind of optic catalytic composite material and preparation method thereof
CN103980759A (en) Preparation method of adsorption-photocatalysis compound type formaldehyde removing coating
CN104826627A (en) High-performance photocatalyst for water treatment and preparation method thereof
CN112537783A (en) W18O49Modified g-C3N4Application of material in photocatalysis nitrogen fixation
CN106348280A (en) Preparation method for spherical porous carbon
CN102294271B (en) Preparation method of synthetic resin loaded nanometer bismuth niobate photocatalyst
CN105921153B (en) A kind of composite photo-catalyst and preparation method thereof
CN102416317B (en) Loading type photocatalyst, preparation method and application thereof
CN102430417B (en) Preparation and Application of Photocatalyst Lanthanum Oxyfluoride
CN102284305B (en) Method for preparing nano bismuth niobate resin-loaded photocatalyst
CN108355674A (en) A kind of zinc sulphide composite photo-catalyst and preparation method for sewage disposal
CN109126716A (en) The absorption and catalytic degradation method of Atrazine in a kind of pair of water
CN111054400B (en) CuInS2Quantum dot/BiOI composite photocatalyst and preparation method and application thereof
CN106512982A (en) Preparation method of quadrangle-star-shaped bismuth vanadate catalyst
CN107744833A (en) A kind of preparation method of MOF catalyst for catalytic eliminating organic sulfur
CN104971752B (en) Magnetic catalyst suitable for catalytic oxidation technique and its preparation method and application
CN105642320A (en) A samarium-doped KMgF3 perovskite-type visible light-responsive catalyst and its preparation method
CN214004349U (en) Sewage treatment device containing metal fragments

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
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20121128

Termination date: 20150624

EXPY Termination of patent right or utility model