CN109590009A - SiC/C3N4/BiVO4The preparation method of composite photo-catalyst - Google Patents
SiC/C3N4/BiVO4The preparation method of composite photo-catalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 55
- 239000000243 solution Substances 0.000 claims abstract description 53
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910001868 water Inorganic materials 0.000 claims abstract description 25
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 23
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 23
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 230000006837 decompression Effects 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 239000008247 solid mixture Substances 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000011363 dried mixture Substances 0.000 claims 2
- 238000000034 method Methods 0.000 abstract description 25
- 238000006731 degradation reaction Methods 0.000 abstract description 19
- 230000015556 catabolic process Effects 0.000 abstract description 18
- 239000002351 wastewater Substances 0.000 abstract description 8
- 238000012545 processing Methods 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 description 18
- 238000007146 photocatalysis Methods 0.000 description 15
- 238000011160 research Methods 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 13
- 239000000126 substance Substances 0.000 description 11
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 9
- 229940043267 rhodamine b Drugs 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical class O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000002306 biochemical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- DPSWNBLFKLUQTP-UHFFFAOYSA-N bismuth vanadium Chemical compound [V].[Bi] DPSWNBLFKLUQTP-UHFFFAOYSA-N 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 239000007857 degradation product Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000013102 re-test Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 241000544061 Cuculus canorus Species 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 bismuthino Chemical group 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 244000144992 flock Species 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052500 inorganic mineral Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical class C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011707 mineral Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
Abstract
The invention belongs to the technical field of waste water processing using solar energy, and in particular to a kind of SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, comprising the following steps: silicon carbide ultrasonic disperse in the aqueous solution of melamine, 10-60min is stirred at 60-100 DEG C, is then cooled down by A., and decompression filters, and obtains solid mixture A;B. it will be ground after solid mixture A drying, be heated to 400-600 DEG C from room temperature under 5-20 DEG C/min, 2-5h is then kept the temperature at 400-600 DEG C, cooling, grinding obtains SiC-C3N4;C. by SiC-C3N4It is added in ammonium metavanadate solution, then bismuth nitrate solution is added in ultrasonic disperse again, adjust the pH to 2-14 of solution, be stirred to react in a water bath, and decompression filters, and obtained mixture B is washed to neutrality, then by mixture B drying, grinding.SiC/C made from method of the invention3N4/BiVO4The light degradation ability of composite photo-catalyst is significantly improved.
Description
Technical field
The invention belongs to the technical field of waste water processing using solar energy, and in particular to a kind of SiC/C3N4/BiVO4It is compound
The preparation method of photochemical catalyst.
Background technique
The abundant and effective supply of the energy is to ensure the national economic development, and (" coal is more for the fundamental safeguarded national security
Co-production technology and Hydrogen Technology ", Xiao Yunhan etc., North China Electric Power University's journal are the 6th phase of volume 31 in 2004, the 5-9 pages, open
On November 30th, 2004 day).It is that the whole world disappears using coal, oil and natural gas as the fossil energy of representative over the past decades
The main energy of consumption.However, long-term exhaustive exploitation causes fossil energy increasingly withered with the development of economy and human society
It exhausts, in addition the production of the energy, conversion and use bring serious environmental pollution, ecosystem destruction and climate change etc. are asked
Topic constitutes serious threat (" new energy strategy and national economy sustainable development ", Lee to the survival and development of mankind itself
Fine jade, Chinese collective economy, the 5th phase in 2017, the 29-31 pages, publication date on 04 06th, 2017;" coal poly-generation technology and
Hydrogen Technology ", Xiao Yunhan etc., North China Electric Power University's journal, the 6th phase of volume 31 in 2004, the 5-9 pages, publication date 2004 years 11
The moon 30).Simultaneously as the sharp increase of the size of population, the random row of modern industry waste water left about, municipal refuse, rural area pesticide
Sprinkling etc., causing is already few freshwater resources aggravation shortage, and wherein dyeing is all to cause water all the time
(" solving dyeing water pollution problems by technological progress ", Sun Ruizhe etc., environment is protected in pollution problem more serious source
Shield, the 19th phase in 2007, the 33-35 pages, publication date on December 31st, 2007;" dyeing water pollution control technical problem with
It is recommended that ", Zhang Qiongfang, the economic guide of science and technology, the 27th phase in 2016, page 80, publication date on December 31st, 2016).Moreover, dyestuff
Waste water has that complicated component, coloration are high, concentration is big, strong toxicity, hard-degraded substance are more, water quality and quantity fluctuates big and unstable etc. spies
Point, current dye species increase in addition, and have the characteristics that anti-light solution, anti-oxidant, antibiooxidation mostly, to increase dye
Expect processing difficulty (" the composite photocatalyst Co of waste water2+/TiO2Degradation dye wastewater methylene blue ", Wan Xiang, Jiangsu are big
Learn master thesis, 2010, page 1, publication date on October 31st, 2010;" it is useless that Fenton oxidation handles methyl orange dye
The research of water ", sudden and violent refined refined, Jiangsu University's master thesis, 2006, page 2, publication date on December 31st, 2006).
Treatment method of printing and dying wastewater can be divided into physical method, chemical method and biochemical method three categories.Wherein, physical method passes through suction
Pollutant is separated from the water by the processes such as attached, sedimentation, mechanically decoupled, so that big sand grains and solids Soft flocks are removed, including from
The right precipitation method, filtration method, absorption method and centrifugal separation etc..Chemical method utilizes the chemical characteristic of organic pollutant, makes itself and its
His compound reaction generates precipitating, gas or is transformed into the method for other innocuous substances to handle waste water, including neutralisation, cohesion
Method (flocking settling method and cohesion buoyance lift method) etc..Contaminant degradation is harmless substance by the effect of microorganism by biochemical method,
It is removed to decompose useless Organic substance in water, including activated sludge process, biological filter process, anaerobic digestion and oxidation pond process etc..
But above method has the disadvantage that (1) part that hardly degraded organic substance cannot effectively be degraded;(2) physical treatment method
It is merely able to shift harmful substance, cannot thoroughly eliminate;It is (3) lower for low-concentration organic waste water treatment efficiency that (" printing and dyeing are useless
The progress of method for treating water ", Wang Ping, chemical industry environmental protection, its 5 phase of volume 17 in 1997, the 273-277 pages, publication date 1997
On December 31, in;" research of Degradation of Organo-pollutants in Water with Photo-catalysis ", Chen Jianqiu, Chinese Marine University's master thesis,
2006, the 15-16 pages, publication date on December 31st, 2006).
Photocatalysis technology is the binding site of photochemistry and catalytic chemistry, is a kind of emerging, efficient, energy-efficient modernization sewage
Processing technique, have it is easily controllable, secondary pollution will not be generated, low energy consumption, and oxidability is strong, and most organic pollutants can
It is carbon dioxide, water and mineral salt by exhaustive oxidation, degree of purification is high, and the advantages such as applied widely receive the extensive of people
Concern (" Degradation of Organo-pollutants in Water with Photo-catalysis status and prospectives ", Cui Yumin etc., chemistry of fuel journal, 2004 years the
The phase of volume 32 the 1st, the 123-128 pages, publication date on February 29th, 2004;" nanometer H3P12O40/TiO2Composite material is to two kinds of dyestuffs
Photocatalytic degradation research ", Zhang Hao, Northeast Normal University's master thesis, 2010, page 1, publication date in December, 2010
31 days;" photocatalytic degradation of large biological molecule is studied ", Yang Guiqin, University of Fuzhou's master thesis, 2005, abstract was public
Open on December 2005 day 31).
Currently, the research of catalyzing and degrading pollutant has been achieved for biggish progress under ultraviolet light conditions.But it is ultraviolet
Light is less than 4% in solar spectrum, and visible light accounts for 43%.Therefore, development efficiently has the corresponding photochemical catalyst of visible light
It is an important research topic of current photocatalysis field, there is important research significance (" Ag- base plasma resonance light
The progress of catalyst ", Xing Yangyang etc., functional material, the 16th phase of volume 43 in 2012, the 2126-2130 pages, publication date
On December 31st, 2012).
Bi series photocatalyst (such as Bi2O3、Bi2WO4、BiVO4, BiOBr, BiOCl etc.), because it is with visible light-responded, nothing
Evil is nontoxic, and stable, at low cost, advantages of environment protection has been widely studied the (" modification of bismuthino visible light catalytic material
And its research of photocatalysis performance ", Liu Houguang, Central China University of Science and Technology's master thesis, 2012, the 6-7 pages, publication date
On December 31st, 2012;" pucherite preparation and the research of photocatalysis performance ", Xu Yupeng, Heilongjiang University's master thesis,
2014, abstract, publication date on December 31st, 2014;" the design synthesis of silver-based nanocomposite and its visible light catalytic
Can research ", Chen Changfeng, Jiangxi Normal University's master thesis, 2018, page 6, publication date on December 31st, 2018).Its
In, pucherite (BiVO4) there is nontoxic, pollution-free, good weatherability, good corrosion resistance, advantages of environment protection, especially have
The advantages that forbidden bandwidth is narrow, high chemical stability, Gao Taiyang light utilization efficiency, and become the research hotspot (" vanadic acid of photocatalysis field
The preparation of bismuth yellow ceramic decoration material and its research of color generation property ", Zhang Lian, Shaanxi Tech Univ's master thesis,
2013, abstract, publication date on October 08th, 2013;" controlledly synthesis of pucherite and the research of photocatalysis performance ", cuckoo, Shan
Western University of Science and Technology, 2012 page 1, publication date on 09 03rd, 2012;" the modifying agent photocatalysis of composite bismuth vanadium photocatalyst
The research of performance ", Zhang Lili, Shaanxi Tech Univ's master thesis, abstract, publication date on December 31st, 2014).
However, the photocatalytic activity of pucherite is lower.Although using different synthetic methods, such as change reaction temperature, instead
Between seasonable, precursor liquid pH value, the means such as template are added can improve its photocatalytic activity to a certain extent, however, with big
Most photochemical catalysts are the same, and the high recombination rate of photo-generate electron-hole is the main reason for causing the photocatalysis rate of pucherite low,
Therefore, the recombination probability for reducing photo-generate electron-hole is to improve active crucial (" the pucherite complex light of bismuth vanadate photocatalyst
The research of the modifying agent photocatalysis performance of catalyst ", Zhang Lili, Shaanxi Tech Univ's master thesis, page 4, publication date
On December 31st, 2014).
Currently, being modified to photochemical catalyst so that the common method for the recombination probability for reducing photo-generate electron-hole is main
Have: (" the modifying agent photocatalysis performance of composite bismuth vanadium photocatalyst is ground for noble metal loading, ion doping, semiconductors coupling etc.
Study carefully ", Zhang Lili, Shaanxi Tech Univ's master thesis, page 4, publication date on December 31st, 2014).These methods although
Short time its photocatalysis efficiency can be improved, however, being easy to appear and partly leading if depth extends the light-catalyzed reaction time or recycles
The problem of body structural instability.Therefore, how to improve that efficiency of light absorption existing for pucherite is low, photo-generated carrier separation energy comprehensively
The problems such as power is weaker, photocatalytic activity is poor, catalyst structure stability is still the technical problem of this field urgent need to resolve.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of SiC/C3N4/BiVO4The preparation method of composite photo-catalyst.
To achieve the above object, the technical solution of the present invention is as follows:
SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, comprising the following steps:
A. by silicon carbide ultrasonic disperse in the aqueous solution of melamine, 10min is stirred at 60-100 DEG C, it is then cold
But, decompression filters, and obtains solid mixture A;
B. will solid mixture A drying after grind, be heated to 400-600 DEG C from room temperature under 5-20 DEG C/min, then in
1-5h is kept the temperature at 400-600 DEG C, cooling, grinding obtains SiC-C3N4;
C. by SiC-C3N4It is added in ammonium metavanadate solution, ultrasonic disperse, bismuth nitrate solution is then added again, adjust molten
The pH to 2-14 of liquid, is stirred to react in a water bath, and decompression filters, and obtained mixture B is washed to neutrality, then by mixture
B drying, grinding.
Further, in step A, the mass ratio of the melamine contained in the aqueous solution of silicon carbide and melamine are as follows: 1:
25-1:200。
Further, the parameter setting during the ultrasonic disperse are as follows: power 100-500W, working frequency 20-
60KHz, time 1-30min.
Further, it is specially to filter under -0.1MPa pressure that the decompression, which filters,.
Further, the temperature of the drying is 60-120 DEG C, time 1-6h.
Further, in step C, the mass ratio of the ammonium metavanadate and silicon carbide that contain in ammonium metavanadate solution is 1:500-1:
10。
Further, the temperature of the stirred in water bath reaction is 60-100 DEG C, time 1-6h.
Further, the SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, comprising the following steps:
A. by silicon carbide ultrasonic disperse in the aqueous solution of melamine, 1-300min is stirred at 60-100 DEG C, then
Cooling, decompression filters, and obtains solid mixture A, the quality of the melamine contained in the aqueous solution of silicon carbide and melamine
Than are as follows: 1:25-1:200;
B. will solid mixture A drying after grind, be heated to 400-600 DEG C from room temperature under 5-20 DEG C/min, then in
1-5h is kept the temperature at 400-600 DEG C, cooling, grinding obtains SiC-C3N4;
C. by SiC-C3N4It is added in ammonium metavanadate solution, ultrasonic disperse, bismuth nitrate solution is then added again, adjust molten
The pH to 2-14 of liquid, is stirred to react in a water bath, and decompression filters, and obtained mixture B is washed to neutrality, then by mixture
B drying is ground, and the mass ratio of the ammonium metavanadate and silicon carbide that contain in ammonium metavanadate solution is 500:1-10:1, the water-bath
In the temperature that is stirred to react be 60-100 DEG C, time 1-5h;
Parameter setting during the ultrasonic disperse are as follows: 100-500W, working frequency 20-60KHz, time 1-
30min.;It is specially to filter under -0.1MPa pressure that the decompression, which filters,;The temperature of the drying is 60-120 DEG C, and the time is
1-5h。
Further, the SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, further comprising the steps of: D. will be walked
Grinding obtained solid is heated to 200-500 DEG C from room temperature under 5-20 DEG C/min in rapid C, then calcines 1- at 200-500 DEG C
5h。
Further, the SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, comprising the following steps:
A. by silicon carbide ultrasonic disperse in the aqueous solution of melamine, 1-300min is stirred at 60-100 DEG C, then
Cooling, decompression filters, and obtains solid mixture A, the quality of the melamine contained in the aqueous solution of silicon carbide and melamine
Than are as follows: 1:25-1:200;
B. will solid mixture A drying after grind, be heated to 400-600 DEG C from room temperature under 5-20 DEG C/min, then in
1-5h is kept the temperature at 400-600 DEG C, cooling, grinding obtains SiC-C3N4;
C. by SiC-C3N4It is added in ammonium metavanadate solution, ultrasonic disperse, bismuth nitrate solution is then added again, adjust molten
The pH to 2-14 of liquid, is stirred to react in a water bath, and decompression filters, and obtained mixture B is washed to neutrality, then by mixture
B drying is ground, and the mass ratio of the ammonium metavanadate and silicon carbide that contain in ammonium metavanadate solution is 500:1-10:1, the water-bath
In the temperature that is stirred to react be 60-100 DEG C, time 1-6h;
D. obtained solid will be ground in step C and be heated to 200-500 DEG C from room temperature under 5-20 DEG C/min, then in 200-
1-5h is calcined at 500 DEG C.
The beneficial effects of the present invention are:
SiC/C made from method of the invention3N4/BiVO4The light degradation ability of composite photo-catalyst has obtained significantly mentioning
Height, when the rhodamine B solution for being 10mg/L with 0.01g catalyst degradation 100mL concentration, the degradation rate of rhodamine B is in 30min
When can reach 83-95%.
The present invention solves the problems, such as that semiconductor structure is unstable in the prior art.
Specific embodiment
Illustrated embodiment is to preferably be illustrated to the contents of the present invention, but is not that the contents of the present invention only limit
In illustrated embodiment.So those skilled in the art carry out nonessential change to embodiment according to foregoing invention content
Into and adjustment, still fall within protection scope of the present invention.
Embodiment 1
SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, the specific steps are as follows:
A. it weighs 1.2g melamine and is dissolved in 60mL100 DEG C of hot water (100 DEG C of water-bath heat preservations), be denoted as solution A, then will
0.02g silicon carbide is 300W in power, and into solution A, the time of ultrasonic disperse is ultrasound under the conditions of working frequency is 40KHz
2min stirs 10min under 90 DEG C of heated conditions;It then cools to room temperature, depressurizes and filter under -0.1MPa pressure, consolidate
Body mixture A;
B. solid mixture A is put into baking oven, 1h is dried at 80 DEG C, is then ground, then from room under 5 DEG C/min
Temperature is heated to 550 DEG C, then keeps the temperature 2h at 550 DEG C, is cooled to room temperature, and grinding obtains SiC-C3N4;
C. 0.1g SiC-C is weighed3N4It is added in the ammonium metavanadate solution that 10mL concentration is 0,05mol/L, is in power
300W, working frequency are ultrasonic disperse 2min under the conditions of 40KHz, and being then slowly added to 10mL concentration again is 0,05mol/L's
Bismuth nitrate solution adjusts the pH to 4 of solution, is stirred to react 3h at 90 DEG C in water-bath, and decompression filters, the mixing that will be obtained
Object B is washed to pH=7, and then mixture B is put into baking oven, and 1h is dried at 80 DEG C, then grind to get.
Embodiment 2
SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, the specific steps are as follows:
A. it weighs 1.2g melamine and is dissolved in 60mL100 DEG C of hot water (100 DEG C of water-bath heat preservations), be denoted as solution A, then will
0.02g silicon carbide is 300W in power, and into solution A, the time of ultrasonic disperse is ultrasound under the conditions of working frequency is 40KHz
2min stirs 10min under 90 DEG C of heated conditions;It then cools to room temperature, depressurizes and filter under -0.1MPa pressure, consolidate
Body mixture A;
B. solid mixture A is put into baking oven, 1h is dried at 80 DEG C, is then ground, then from room under 5 DEG C/min
Temperature is heated to 550 DEG C, then keeps the temperature 2h at 550 DEG C, is cooled to room temperature, and grinding obtains SiC-C3N4;
C. 0.1g SiC-C is weighed3N4It is added in the ammonium metavanadate solution that 10mL concentration is 0,05mol/L, is in power
300W, working frequency are ultrasonic disperse 2min under the conditions of 40KHz, and being then slowly added to 10mL concentration again is 0,05mol/L's
Bismuth nitrate solution adjusts the pH to 4 of solution, is stirred to react 3h at 90 DEG C in water-bath, and decompression filters, the mixing that will be obtained
Object B is washed to pH=7, and then mixture B is put into baking oven, and 1h is dried at 80 DEG C, is then ground;
D. obtained solid will be ground in step C to be placed in crucible with cover, be heated to 400 DEG C from room temperature under 5 DEG C/min,
Then at 400 DEG C calcine 2h to get.
Embodiment 3
SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, the specific steps are as follows:
A. it weighs 1.2g melamine and is dissolved in 60mL100 DEG C of hot water (100 DEG C of water-bath heat preservations), be denoted as solution A, then will
0.02g silicon carbide is 300W in power, and into solution A, the time of ultrasonic disperse is ultrasound under the conditions of working frequency is 40KHz
2min stirs 10min under 90 DEG C of heated conditions;It then cools to room temperature, depressurizes and filter under -0.1MPa pressure, consolidate
Body mixture A;
B. solid mixture A is put into baking oven, 1h is dried at 80 DEG C, is then ground, then from room under 5 DEG C/min
Temperature is heated to 550 DEG C, then keeps the temperature 2h at 550 DEG C, is cooled to room temperature, and grinding obtains SiC-C3N4;
C. 0.1g SiC-C is weighed3N4It is added in the ammonium metavanadate solution that 10mL concentration is 0,05mol/L, is in power
300W, working frequency are ultrasonic disperse 2min under the conditions of 40KHz, and being then slowly added to 10mL concentration again is 0,05mol/L's
Bismuth nitrate solution adjusts the pH to 10 of solution, is stirred to react 3h at 90 DEG C in water-bath, and decompression filters, mixed by what is obtained
It closes object B to wash to pH=7, then mixture B is put into baking oven, 1h is dried at 80 DEG C, is then ground;
D. obtained solid will be ground in step C to be placed in crucible with cover, be heated to 400 DEG C from room temperature under 5 DEG C/min,
Then at 400 DEG C calcine 2h to get.
Embodiment 4
SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, the specific steps are as follows:
A. it weighs 1.2g melamine and is dissolved in 60mL100 DEG C of hot water (100 DEG C of water-bath heat preservations), be denoted as solution A, then will
0.02g silicon carbide is 300W in power, and into solution A, the time of ultrasonic disperse is ultrasound under the conditions of working frequency is 40KHz
2min stirs 10min under 90 DEG C of heated conditions;It then cools to room temperature, depressurizes and filter under -0.1MPa pressure, consolidate
Body mixture A;
B. solid mixture A is put into baking oven, 1h is dried at 80 DEG C, is then ground, then from room under 5 DEG C/min
Temperature is heated to 550 DEG C, then keeps the temperature 2h at 550 DEG C, is cooled to room temperature, and grinding obtains SiC-C3N4;
C. 0.1g SiC-C is weighed3N4It is added in the ammonium metavanadate solution that 10mL concentration is 0,05mol/L, is in power
300W, working frequency are ultrasonic disperse 2min under the conditions of 40KHz, and being then slowly added to 10mL concentration again is 0,05mol/L's
Bismuth nitrate solution adjusts the pH to 7 of solution, is stirred to react 3h at 90 DEG C in water-bath, and decompression filters, the mixing that will be obtained
Object B is washed to pH=7, and then mixture B is put into baking oven, and 1h is dried at 80 DEG C, is then ground;
D. obtained solid will be ground in step C to be placed in crucible with cover, be heated to 400 DEG C from room temperature under 5 DEG C/min,
Then at 400 DEG C calcine 2h to get.
Performance detection
To SiC/C made from embodiment 1-43N4/BiVO4Composite photo-catalyst and SiC/C3N4And BiVO4Carry out photocatalysis
Degradation effect experiment, the specific steps are as follows:
1, using colored dyes rhodamine B as target degradation product
(1) catalyst 10mg is weighed;
(2) in power be 300W, sieve that ultrasonic disperse is 10mg/L in 100mL concentration under the conditions of working frequency is 40KHz
In red bright B simulated water sample, jitter time 2min;Using the 300W xenon lamp equipped with 420nm edge filter as simulated solar irradiation
Source is measured the concentration of rhodamine B in water sample using the method for measuring solution absorbance, dropped according to formula under stirring conditions
Solution rate=[1- (initial concentration-endpoint concentration)/initial concentration] × 100% calculates the degradation rate of photochemical catalyst, 30min degradation
The results are shown in Table 1.
2, using colourless organic pollutant phenol as target degradation product
(1) catalyst 25mg is weighed;
(2) in power be 300W, the phenol that ultrasonic disperse is 10mg/L in 50mL concentration under the conditions of working frequency is 40KHz
In simulated water sample, jitter time 2min;Using the 300W xenon lamp equipped with 420nm edge filter as simulated solar light source,
Under conditions of stirring, the concentration of Phenol in Aqueous Solution is measured using liquid chromatography, according to formula degradation rate=[1- (initial concentration-
Endpoint concentration)/initial concentration] × 100% degradation rate for calculating photochemical catalyst, 120min degradation results are as shown in table 1.
1 the performance test results of table
Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | SiC/C3N4 | BiVO4 |
To the degradation rate of rhodamine B | 85% | 95% | 83% | 94% | 75% | 8% |
The degradation rate of Pyrogentisinic Acid | 50% | 61% | 52% | 63% | 20% | 0% |
As shown in Table 1, with SiC/C3N4And BiVO4It compares, SiC/C made from embodiment 1-43N4/BiVO4Composite photocatalyst
Agent is significantly improved to the degradation rate of phenol in rhodamine B in rhodamine B solution and phenol solution.Thus it proves, this hair
SiC/C made from bright method3N4/BiVO4The light degradation ability of composite photo-catalyst is significantly improved.Due to this this three
First compound can effectively facilitate the transfer in light induced electron and hole, improve the utilization efficiency of photo-generated carrier, so three
Synergistic effect is so that SiC/C3N4/BiVO4The catalytic capability of composite photo-catalyst is significantly improved.
Repetitive test
Repeated experiment is carried out to rhodamine B photocatalytic degradation effect to composite photocatalyst material made from embodiment 1-4,
Test method is same as above, and three times, test result is as shown in table 2 for photochemical catalyst retest made from each embodiment.
The repeated the performance test results of table 2 (to the degradation rate of rhodamine B)
As shown in Table 2, the photocatalysis effect of composite photo-catalyst retest three times made from embodiment 1-4 is without under obvious
Drop.Thus it proves, SiC/C made from method of the invention3N4/BiVO4The performance of composite photo-catalyst is stablized, and the present invention solves
Semiconductor structure unstable problem in the prior art.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (10)
1.SiC/C3N4/BiVO4The preparation method of composite photo-catalyst, which comprises the following steps:
A. by silicon carbide ultrasonic disperse in the aqueous solution of melamine, 1-300min is stirred at 60-100 DEG C, is then cooled down,
Decompression filters, and obtains solid mixture A;
B. it will be ground after solid mixture A drying, 400-600 DEG C be heated to from room temperature under 5-20 DEG C/min, then in 400-
1-5h is kept the temperature at 600 DEG C, cooling, grinding obtains SiC-C3N4;
C. by SiC-C3N4It is added in ammonium metavanadate solution, then ultrasonic disperse adds bismuth nitrate solution, adjust the pH of solution
To 2-14, it is stirred to react in a water bath, decompression filters, and obtained mixture B is washed to neutrality, then dry mixture B,
Grinding.
2. SiC/C according to claim 13N4/BiVO4The preparation method of composite photo-catalyst, which is characterized in that step A
In, the mass ratio of the melamine contained in the aqueous solution of silicon carbide and melamine are as follows: 1:25-1:200.
3. SiC/C according to claim 1 or 23N4/BiVO4The preparation method of composite photo-catalyst, which is characterized in that
Parameter setting during the ultrasonic disperse are as follows: power 100-500W, working frequency 20-60KHz, time 1-
30min。
4. SiC/C according to claim 1,2 or 33N4/BiVO4The preparation method of composite photo-catalyst, which is characterized in that
It is specially to filter under -0.1MPa pressure that the decompression, which filters,.
5. SiC/C according to claim 1,2,3 or 43N4/BiVO4The preparation method of composite photo-catalyst, feature exist
In the temperature of the drying is 60-120 DEG C, time 1-5h.
6. according to claim 1, SiC/C described in 2,3,4 or 53N4/BiVO4The preparation method of composite photo-catalyst, feature
It is, in step C, the mass ratio of the ammonium metavanadate and silicon carbide that contain in ammonium metavanadate solution is 500:1-10:1.
7. according to claim 1, SiC/C described in 2,3,4,5 or 63N4/BiVO4The preparation method of composite photo-catalyst, it is special
Sign is that the temperature of the stirred in water bath reaction is 60-100 DEG C, time 1-6h.
8. according to claim 1, SiC/C described in 2,3,4,5 or 63N4/BiVO4The preparation method of composite photo-catalyst, it is special
Sign is, comprising the following steps:
A. by silicon carbide ultrasonic disperse in the aqueous solution of melamine, 1-300min is stirred at 60-100 DEG C, is then cooled down,
Decompression filters, and obtains solid mixture A, the mass ratio of the melamine contained in the aqueous solution of silicon carbide and melamine are as follows:
1:25-1:200;
B. it will be ground after solid mixture A drying, 400-600 DEG C be heated to from room temperature under 5-20 DEG C/min, then in 400-
1-5h is kept the temperature at 600 DEG C, cooling, grinding obtains SiC-C3N4;
C. by SiC-C3N4It is added in ammonium metavanadate solution, then bismuth nitrate solution is added in ultrasonic disperse again, adjust solution
PH to 2-14, is stirred to react in a water bath, and decompression filters, and obtained mixture B is washed to neutrality, is then dried mixture B
It does, grinding, the mass ratio of the ammonium metavanadate and silicon carbide that contain in ammonium metavanadate solution is 500:1-10:1, is stirred in the water-bath
The temperature for mixing reaction is 60-100 DEG C, time 1-6h;
Parameter setting during the ultrasonic disperse are as follows: 100-500W, working frequency 20-60KHz, time 1-30min.
It is specially to filter under -0.1MPa pressure that the decompression, which filters,;The temperature of the drying is 60-120 DEG C, time 1-5h.
9. according to claim 1, SiC/C described in 2,3,4,5,6,7 or 83N4/BiVO4The preparation method of composite photo-catalyst,
It is characterized in that, further comprising the steps of: D. will grind obtained solid and be heated under 5-20 DEG C/min from room temperature in step C
200-500 DEG C, 1-5h then is calcined at 200-500 DEG C.
10. SiC/C according to claim 93N4/BiVO4The preparation method of composite photo-catalyst, which is characterized in that including
Following steps:
A. by silicon carbide ultrasonic disperse in the aqueous solution of melamine, 1-300min is stirred at 60-100 DEG C, is then cooled down,
Decompression filters, and obtains solid mixture A, the mass ratio of the melamine contained in the aqueous solution of silicon carbide and melamine are as follows:
1:25-1:200;
B. it will be ground after solid mixture A drying, 400-600 DEG C be heated to from room temperature under 5-20 DEG C/min, then in 400-
1-5h is kept the temperature at 600 DEG C, cooling, grinding obtains SiC-C3N4;
C. by SiC-C3N4It is added in ammonium metavanadate solution, then bismuth nitrate solution is added in ultrasonic disperse again, adjust solution
PH to 2-14, is stirred to react in a water bath, and decompression filters, and obtained mixture B is washed to neutrality, is then dried mixture B
It does, grinding, the mass ratio of the ammonium metavanadate and silicon carbide that contain in ammonium metavanadate solution is 500:1-10:1, is stirred in the water-bath
The temperature for mixing reaction is 60-100 DEG C, time 1-6h;
D. obtained solid will be ground in step C and be heated to 200-500 DEG C from room temperature under 5-20 DEG C/min, then in 200-500
1-5h is calcined at DEG C.
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