CN106238084A - The preparation method and application of visible ray synergy ozone catalytic degradation organic acid catalyst - Google Patents

The preparation method and application of visible ray synergy ozone catalytic degradation organic acid catalyst Download PDF

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Publication number
CN106238084A
CN106238084A CN201610538635.6A CN201610538635A CN106238084A CN 106238084 A CN106238084 A CN 106238084A CN 201610538635 A CN201610538635 A CN 201610538635A CN 106238084 A CN106238084 A CN 106238084A
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organic acid
catalyst
catalytic degradation
visible ray
mixture
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CN106238084B (en
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李亮
杨玉飞
黄远星
姚吉
胡守波
貟亚峰
罗梦玉
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University of Shanghai for Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • B01J35/39
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/725Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/78Treatment of water, waste water, or sewage by oxidation with ozone
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention provides the preparation method of a kind of visible ray synergy ozone catalytic degradation organic acid catalyst, comprise the following steps: step one, weigh manganese acetate and be dissolved in ultra-pure water, after stirring, add tripolycyanamide, obtain mixed solution;Step 2, is heated to mixed solution moisture while stirring and is evaporated and obtains mixture, is dried by mixture, obtains dried mixture;Step 3, calcines after dried mixture step 2 obtained grinding, the mixture after being calcined;Step 4, after the mixture after calcining step 3 obtained grinds, screening obtains catalyst.Use this catalyst to join in organic acid, be passed through ozone and under visible ray illumination condition the organic acid in catalytic degradation industrial wastewater, catalytic degradation efficiency is high, can effectively process the organic acid in industrial wastewater, it is adaptable to industrial applications.

Description

The preparation method and application of visible ray synergy ozone catalytic degradation organic acid catalyst
Technical field
The present invention relates to the preparation method and application of a kind of catalytic degradation organic acid catalyst.
Background technology
Being usually present certain density hardly degraded organic substance in industrial wastewater, these materials are through chemistry or biological treatment After, generally produce the Organic substance of some little molecules, it is difficult to directly mineralising is CO2And H2O.The organic acid of little molecule is typically Organic product after pollutant chemistry oxidation, its mesoxalic acid is the primary product of phenol ozone degradation.Oxalic acid and ozone molecule The least (k < 0.04M of reaction rate constant-1s-1), but with OH radical reaction quickly (k ≈ 106M-1s-1).Therefore single Only ozone oxidation is difficult to completely oxalic acid is converted into CO2With H2O, catalysis ozone has bigger compared to independent ozone oxidation Degradation effect.
Additionally, ultraviolet catalytic oxidation has good effect in terms of the removal of pollutant, and and ozone oxidation between have Well synergism.But, ultraviolet light ratio shared by sunlight is the least, and penetration power is the most weak, easily by air Layer absorbs.Artificial ultraviolet source energy consumption in actual production process is the biggest, it is difficult to large-scale application.Therefore visible light catalytic neck Territory becomes the focus of research, g-C3N4Chemical property is more stable, forbidden band is narrower, becomes the hot topic of photocatalysis field, g-C3N4Negative Carry metal-oxide and can optimize g-C further3N4Catalytic effect, improve responsiveness to visible ray, before there is wide development Scape.With metal oxide-loaded g-C3N4For catalyst, not yet appear in the newspapers at visible ray synergy ozone catalytic degradation water mesoxalic acid Road.
Summary of the invention
The present invention is carried out for solving the problems referred to above, it is therefore intended that provide a kind of visible ray synergy ozone catalytic degradation The preparation method and application of organic acid catalyst, carrys out the organic acid in catalytic degradation industrial wastewater effectively.
Present invention employs following technical scheme:
The invention provides the preparation method of a kind of visible ray synergy ozone catalytic degradation organic acid catalyst, its feature exists In, comprise the following steps:
Step one, weighs manganese acetate and is dissolved in ultra-pure water, after stirring 5~10min, adds tripolycyanamide, is mixed Solution;
Step 2, is heated to mixed solution moisture while stirring and is evaporated and obtains mixture, and mixture is put into temperature is Dry under conditions of 80~120 DEG C, obtain dried mixture;
Step 3, dried mixture step 2 obtained is forged after grinding under conditions of temperature is 500~600 DEG C Burn 3~5 hours, the mixture after being calcined;
Step 4, after the mixture after calcining step 3 obtained grinds, screening obtains catalyst.
In the preparation method of the visible ray synergy ozone catalytic degradation organic acid catalyst of present invention offer, it is also possible to tool Having such feature: wherein, catalyst is the oxide M nO of manganesexWith graphite type carbon nitride g-C3N4Complex MnOx/g- C3N4
In the preparation method of the visible ray synergy ozone catalytic degradation organic acid catalyst of present invention offer, it is also possible to tool Have such feature: wherein, in step one, the mass ratio of manganese acetate, ultra-pure water and tripolycyanamide be 1:80~100:5~ 10。
In the preparation method of the visible ray synergy ozone catalytic degradation organic acid catalyst of present invention offer, it is also possible to tool There is such feature: wherein, the oxide M nO of manganesexThe value of middle X is 1~2.
In the preparation method of the visible ray synergy ozone catalytic degradation organic acid catalyst of present invention offer, it is also possible to tool Having such feature: wherein, in step one, manganese acetate is manganese acetate (III) dihydrate.
In the preparation method of the visible ray synergy ozone catalytic degradation organic acid catalyst of present invention offer, it is also possible to tool Having such feature: wherein, in step 4, the particle diameter of screening is 100 under Tyler standard screen scale~200 mesh.
It addition, present invention also offers the preparation method system of above-mentioned visible ray synergy ozone catalytic degradation organic acid catalyst The application in catalytic degradation organic acid of the standby catalyst obtained.
In the above-mentioned catalyst application in catalytic degradation organic acid that the present invention provides, it is also possible to there is such spy Levy: catalyst and visible ray, ozone cooperative effect carry out catalytic degradation to organic acid.
In the above-mentioned catalyst application in catalytic degradation organic acid that the present invention provides, it is also possible to there is such spy Levy: catalyst is added to the organic acid soln that concentration is 40~120mg/L, is passed through ozone and under visible ray illumination condition Organic acid in catalytic degradation water.
In the above-mentioned catalyst application in catalytic degradation organic acid that the present invention provides, it is also possible to there is such spy Levy: organic acid is oxalic acid, it is seen that the wavelength of light is more than 400nm.
Invention effect and effect
The invention provides the preparation method and application of a kind of visible ray synergy ozone catalytic degradation organic acid catalyst, this The preparation method of the visible ray synergy ozone catalytic degradation organic acid catalyst of invention is by manganese acetate, ultra-pure water and tripolycyanamide Mixing, be evaporated by heating, dry, grind, calcine and the operation such as screening prepares catalyst MnOx/g-C3N4, preparation method Simply, it is easy to operation, industrialized production is suitable to.
The application of the visible ray synergy ozone catalytic degradation organic acid catalyst of the present invention is by catalyst MnOx/g-C3N4Add Enter in organic acid, be passed through ozone and under visible ray illumination condition the organic acid in catalytic degradation industrial wastewater, organic acid enters Oxidation step is CO2And H2O, catalytic degradation efficiency is high, can effectively process the organic acid in industrial wastewater, it is adaptable to industrialization Application.
Accompanying drawing explanation
Fig. 1 is the preparation of the visible ray synergy ozone catalytic degradation organic acid catalyst provided according to the embodiment of the present invention one The catalyst MnO that method preparesx/g-C3N4X-ray diffractogram;And
Fig. 2 is the oxalic acid degradation effect figure during the present invention implements under different condition.
Detailed description of the invention
The system to the visible ray synergy ozone catalytic degradation organic acid catalyst of the present invention below in conjunction with embodiment and accompanying drawing Preparation Method and application are further described.
Embodiment one prepares MnOx/g-C3N4Catalyst
The preparation method of the catalyst of the visible ray synergy ozone catalytic degradation organic acid that the present embodiment provides, including following Step:
Step one, weighs manganese acetate (III) dihydrate (C of 0.4g6H13MnO8) and be dissolved in the ultra-pure water of 40ml, stir After mixing 5min, add 4g tripolycyanamide, obtain mixed solution.
Step 2, is heated to mixed solution moisture while stirring and is evaporated and obtains mixture, and mixture is put into temperature is The baking oven of 90 DEG C is dried, obtains dried mixture;
Step 3, dried mixture step 2 obtained is put in crucible the horse that temperature is 550 DEG C after grinding Not calcining 4 hours, the mixture after being calcined in stove (ascending temperature is 10 DEG C/min);
Step 4, at the screen cloth of 100 mesh (Tyler standard screen scale) after the mixture grinding after calcining step 3 obtained Lower screening obtains MnOx/g-C3N4Catalyst.
Fig. 1 is the preparation method system of the visible ray synergy ozone catalytic degradation organic acid catalyst provided according to the present embodiment The MnO obtainedx/g-C3N4X-ray diffractogram.
As it is shown in figure 1, at catalyst MnOx/g-C3N4In, the diffraction maximum in the double angle of diffraction 2 θ=27.6 ° correspond to g- C3N4002 crystal face, other indicate diffraction maximum belong to JCPDS establishment numbered JCPDS80- The Mn of 03823O4And Mn2O3, MnO is describedxMain with Mn3O4Form exists.
Embodiment two prepares MnOx/g-C3N4Catalyst
The preparation method of the visible ray synergy ozone catalytic degradation organic acid catalyst that the present embodiment provides, including following step Rapid:
Step one, weighs manganese acetate (III) dihydrate (C of 0.4g6H13MnO8) and the ultra-pure water of molten 32ml in, stirring After 10min, add 2g tripolycyanamide, obtain mixed solution.
Step 2, is heated to mixed solution moisture while stirring and is evaporated and obtains mixture, mixture is placed in temperature It is that the baking oven of 80 DEG C is dried, obtains dried mixture.
Step 3, dried mixture step 2 obtained is put in crucible the horse that temperature is 500 DEG C after grinding Not calcining 3 hours, the mixture after being calcined in stove (ascending temperature is 10 DEG C/min).
Step 4, at the screen cloth of 150 mesh (Tyler standard screen scale) after the mixture grinding after calcining step 3 obtained Lower screening obtains MnOx/g-C3N4Catalyst.
Embodiment three prepares MnOx/g-C3N4Catalyst
The preparation method of the visible ray synergy ozone catalytic degradation organic acid catalyst that the present embodiment provides, including following step Rapid:
Step one, weighs manganese acetate (III) dihydrate (C of 0.4g6H13MnO8) and be dissolved in the ultra-pure water of 36ml, stir After mixing 8min, add 3.2g tripolycyanamide, obtain mixed solution.
Step 2, is heated to mixed solution moisture while stirring and is evaporated and obtains mixture, mixture is placed in temperature It is that the baking oven of 120 DEG C is dried, obtains dried mixture.
Step 3, dried mixture step 2 obtained is put in crucible at the bar that temperature is 600 DEG C after grinding Calcining 5 hours, the mixture after being calcined in the Muffle furnace (ascending temperature is 10 DEG C/min) of part.
Step 4, at the screen cloth of 200 mesh (Tyler standard screen scale) after the mixture grinding after calcining step 3 obtained Lower screening obtains MnOx/g-C3N4Catalyst.
Embodiment four ozone oxidation degraded oxalic acid
Configuration concentration is that the oxalic acid solution of 80mg/L is (additionally, the concentration of oxalic acid solution can also be for 40mg/L and 120mg/ L, choosing optimal concentration is 80mg/L), and make its initial pH=3;Then, under the conditions of lucifuge, being passed through concentration is the smelly of 6mg/L Oxygen, is that 5min, 10min, 20min, 40min and 60min sample and detect concentration of oxalic acid in the time of being passed through respectively.
Fig. 2 is the oxalic acid degradation effect figure during the present invention implements under different condition.
As in figure 2 it is shown, oxalic acid reaches 1.2% at 60min clearance under conditions of this experiment.
Embodiment five MnOx/g-C3N4Catalytic degradation oxalic acid
Configuration concentration is that the oxalic acid solution of 80mg/L is (additionally, the concentration of oxalic acid solution can also be for 40mg/L and 120mg/ And make its initial pH=3 L),;It is subsequently adding the MnO of 0.15g/Lx/g-C3N4Catalyst, under the conditions of lucifuge, is adding respectively Time is that 5min, 10min, 20min, 40min and 60min sample and detect concentration of oxalic acid.
Result as in figure 2 it is shown, under conditions of this experiment oxalic acid reach 6.6% at 60min clearance.
Embodiment six visible ray (λ > 400nm) illumination degrading oxalic acid
Configuration concentration is that the oxalic acid solution of 80mg/L is (additionally, the concentration of oxalic acid solution can also be for 40mg/L and 120mg/ And make its initial pH=3 L),;Then under visible ray (λ > 400nm) illumination condition, respectively light application time be 5min, 10min, 20min, 40min and 60min sample and detect concentration of oxalic acid.
Result as in figure 2 it is shown, under conditions of this experiment oxalic acid reach 0.9% at 60min clearance.
Embodiment seven MnOx/g-C3N4Catalytic Ozonation oxalic acid
Configuration concentration is that the oxalic acid solution of 80mg/L is (additionally, the concentration of oxalic acid solution can also be for 40mg/L and 120mg/ And make its initial pH=3 L),;It is subsequently adding the MnO of 0.15g/Lx/g-C3N4Catalyst, being passed through concentration under the conditions of lucifuge is The ozone of 6mg/L, is that 5min, 10min, 20min, 40min and 60min sample and to detect oxalic acid dense in light application time respectively Degree.
Result as in figure 2 it is shown, under conditions of this experiment oxalic acid reach 86.3% at 60min clearance.
The collaborative lower MnO of embodiment eight visible rayx/g-C3N4Catalytic Ozonation oxalic acid
Configuration concentration is that the oxalic acid solution of 80mg/L is (additionally, the concentration of oxalic acid solution can also be for 40mg/L and 120mg/ And make its initial pH=3 L),;It is subsequently adding the MnO of 0.15g/Lx/g-C3N4Catalyst, irradiates under the xenon lamp of 300W, uses Optical filter cuts off the light of below wavelength 400nm;Under visible ray (λ > 400nm) illumination condition, being passed through concentration is the smelly of 6mg/L Oxygen, is that 5min, 10min, 20min, 40min and 60min sample and detect concentration of oxalic acid in the time respectively.
Result as in figure 2 it is shown, under conditions of this experiment oxalic acid reach 91.1% at 60min clearance, ratio implement seven degraded grass Mollic acid is fast.
The effect of embodiment and effect
Embodiment one to embodiment eight provides the preparation side of a kind of visible ray synergy ozone catalytic degradation Catalyzed by Oxalic Acid agent Method and application, what embodiment one to embodiment three provided the preparation method of visible ray synergy ozone catalytic degradation Catalyzed by Oxalic Acid agent By the mixing of manganese acetate, ultra-pure water and tripolycyanamide, it is evaporated by heating, dries, grinds, calcines and the operation system such as screening Obtain catalyst MnOx/g-C3N4, preparation method is simple, it is easy to operation, is suitable to industrialized production.
The application of the visible ray synergy ozone catalytic degradation Catalyzed by Oxalic Acid agent that embodiment four to embodiment eight provides, will catalysis Agent MnOx/g-C3N4Join in oxalic acid, be passed through ozone and under visible ray illumination condition the grass in catalytic degradation industrial wastewater Acid, compared to being individually passed through ozone degradation oxalic acid, being individually added into catalyst MnOx/g-C3N4, individually with visible ray illumination and urge Agent MnOx/g-C3N4Catalytic Ozonation oxalic acid clearance is high, can the oxalic acid in catalytic degradation industrial wastewater effectively, suitable For industrial applications.
The most in an embodiment of the present invention, use the xenon lamp of 300W to irradiate, compare and traditional ultraviolet source irradiation, Breaking through higher, energy consumption is little, can large-scale application.
Above example is only the basic explanation under present inventive concept, does not limits the invention.And according to the present invention Any equivalent transformation of being made of technical scheme, belong to protection scope of the present invention.

Claims (10)

1. the preparation method of a visible ray synergy ozone catalytic degradation organic acid catalyst, it is characterised in that include following step Rapid:
Step one, weighs manganese acetate and is dissolved in ultra-pure water, after stirring 5~10min, adds tripolycyanamide, obtains mixed solution;
Step 2, is heated to described mixed solution moisture while stirring and is evaporated and obtains mixture, described mixture is put into temperature Degree is dried under conditions of being 80~120 DEG C, obtains dried mixture;
Step 3, dried mixture step 2 obtained calcines 3 after grinding under conditions of temperature is 500~600 DEG C ~5 hours, the mixture after being calcined;
Step 4, after the mixture after calcining step 3 obtained grinds, screening obtains described catalyst.
The preparation method of visible ray synergy ozone catalytic degradation organic acid catalyst the most according to claim 1, its feature It is:
Wherein, described catalyst is the oxide M nO of manganesexWith graphite type carbon nitride g-C3N4Complex MnOx/g-C3N4
The preparation method of visible ray synergy ozone catalytic degradation organic acid catalyst the most according to claim 1, its feature It is:
Wherein, in described step one, the mass ratio of described manganese acetate, described ultra-pure water and described tripolycyanamide be 1:80~ 100:5~10.
The preparation method of visible ray synergy ozone catalytic degradation organic acid catalyst the most according to claim 2, its feature It is:
Wherein, the oxide M nO of described manganesexThe value of middle X is 1~2.
The preparation method of visible ray synergy ozone catalytic degradation organic acid catalyst the most according to claim 1, its feature It is:
Wherein, in described step one, described manganese acetate is manganese acetate (III) dihydrate.
The most according to claim 1, the preparation method of visible ray synergy ozone catalytic degradation organic acid catalyst, its feature exists In:
Wherein, in described step 4, the particle diameter of described screening is 100 under Tyler standard screen scale~200 mesh.
7. the preparation of the visible ray synergy ozone catalytic degradation organic acid catalyst as described in any one in claim 1~6 The catalyst that method prepares application in catalytic degradation organic acid.
8. according to the application in catalytic degradation organic acid of the catalyst described in claim 7, it is characterised in that:
Described catalyst and visible ray, ozone cooperative effect carry out catalytic degradation to organic acid.
9. according to the application in catalytic degradation organic acid of the catalyst described in claim 7, it is characterised in that:
Described catalyst is added to the organic acid soln that concentration is 40~120mg/L, is passed through ozone and in visible ray illumination Under the conditions of organic acid in catalytic degradation water.
10. according to the application in catalytic degradation organic acid of the catalyst described in claim 7, it is characterised in that:
Wherein, described organic acid is oxalic acid, and the wavelength of described visible ray is more than 400nm.
CN201610538635.6A 2016-07-11 2016-07-11 The preparation method and application of visible light synergy ozone catalytic degradation organic acid catalyst Expired - Fee Related CN106238084B (en)

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CN109078647A (en) * 2018-07-18 2018-12-25 上海师范大学 A kind of Mn3O4/g-C3N4Photo-thermal concerted catalysis composite material and preparation method and application
CN109772412A (en) * 2019-02-23 2019-05-21 辽宁大学 MnOx/g-C3N4Composite catalyst and its application in photo-thermal Synergistic degradation gaseous-phase organic pollutant
CN111889129A (en) * 2020-07-30 2020-11-06 大连工业大学 Preparation of ultrathin porous nano carbon nitride photocatalyst and application of ultrathin porous nano carbon nitride photocatalyst in synthesis of lactic acid by photocatalytic oxidation of fructose
CN115283003A (en) * 2022-10-10 2022-11-04 河北海鹰环境安全科技股份有限公司 Method for preparing ozone catalyst by microwave method

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CN106861746A (en) * 2017-03-22 2017-06-20 北京师范大学 A kind of carbonitride loads the preparation method of single dispersing oxidation state metal atom catalysis material
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CN109078647A (en) * 2018-07-18 2018-12-25 上海师范大学 A kind of Mn3O4/g-C3N4Photo-thermal concerted catalysis composite material and preparation method and application
CN109772412A (en) * 2019-02-23 2019-05-21 辽宁大学 MnOx/g-C3N4Composite catalyst and its application in photo-thermal Synergistic degradation gaseous-phase organic pollutant
CN111889129A (en) * 2020-07-30 2020-11-06 大连工业大学 Preparation of ultrathin porous nano carbon nitride photocatalyst and application of ultrathin porous nano carbon nitride photocatalyst in synthesis of lactic acid by photocatalytic oxidation of fructose
WO2022021506A1 (en) * 2020-07-30 2022-02-03 大连工业大学 Preparation of ultrathin porous carbon nitride nano-photocatalyst and applications thereof in photocatalytically oxidizing fructose to synthesize lactic acid
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CN115283003A (en) * 2022-10-10 2022-11-04 河北海鹰环境安全科技股份有限公司 Method for preparing ozone catalyst by microwave method

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