CN108704643A - Vanadium Boratex area load ag material is degraded the method for chlorine atmosphere pollutant under visible light - Google Patents

Vanadium Boratex area load ag material is degraded the method for chlorine atmosphere pollutant under visible light Download PDF

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Publication number
CN108704643A
CN108704643A CN201810518093.5A CN201810518093A CN108704643A CN 108704643 A CN108704643 A CN 108704643A CN 201810518093 A CN201810518093 A CN 201810518093A CN 108704643 A CN108704643 A CN 108704643A
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China
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xenon lamp
vanadium
boratex
chlorophenol
pollutant
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CN201810518093.5A
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Chinese (zh)
Inventor
王富
翟羽飞
范晓芸
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Priority to CN201810518093.5A priority Critical patent/CN108704643A/en
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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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/66—Silver or gold
    • B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/682—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium, tantalum or polonium
    • 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
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • 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
    • C02F2101/36—Organic compounds containing halogen

Abstract

It degrades under visible light the present invention relates to a kind of vanadium Boratex area load ag material the method for chlorine atmosphere pollutant, this method is in vanadium Boratex area load silver, using chlorophenol as pollutant, pollutant concentration 20 mg/L aqueous solution, photocatalytic oxidation degradation is carried out to it under visible light illumination, being found by high performance liquid chromatograph analysis 120 minutes can be degradable by 2-chlorophenol, i.e., degradation rate is 100%.Operating procedure of the present invention is simple, at low cost, the dechlorination that can efficiently, be quickly used in chlorinated aromatic hydrocarbons, it is often more important that having widened the photoresponse range of catalysis material makes it under visible light and also have the ability of good degrading chlorophenol pollutant.

Description

Vanadium Boratex area load ag material is degraded chlorine atmosphere pollutant under visible light Method
Technical field
Efficient fast degradation in being polluted under visible light to chlorine atmosphere class the present invention relates to vanadium Boratex area load ag material Method.
Background technology
Chlorophenols aromatic compound toxicity is big, difficult for biological degradation is grown in the environment with " three cause " effect and genetoxic Phase residual, degradation cycle are long, and priority pollutants are classified as by Environmental Protection Agency USA.Chlorophenols compound has stench, different The features such as taste and high toxicity, is widely used in the industry such as the preservation of timber against decay agent, antirust agent, herbicide, fungicide and papermaking, It is additionally operable to the prevention of snail fever in Asia, Africa and South America, the production scale of many industrialized country's chlorophenols is very huge. Chlorinated phenols it is a large amount of use, the understanding of the harm of early stage parachlorphenol and toxicity is insufficient and it is incident ignore for a long time, lead Cause chlorophenol pollution very serious, causing the great control for endangering chlorophenol pollution to the mankind and environment, oneself becomes whole world environment The research hotspot of subject is one of key subjects of field of environmental improvement.
The main methods of chlorophenol have biochemical process, physico-chemical process and oxidizing process etc..Photocatalytic degradation chlorophenol pollutant is A kind of new method and new technology efficiently, inexpensive.The defect of catalysis material generally existing is to utilize utilization to light at present Rate is low, and the ultraviolet light in sunlight can only be absorbed similar to catalysis material as titanium dioxide, and ultraviolet light only accounts for the sun 4% or so of light energy, therefore, exploitation are efficient, it is seen that the photocatalysis new material of photoresponse has great importance.
The photoresponse of vanadium Boratex ranging from ultraviolet region, that is, wave-length coverage is less than 420nm, and silver load is carried out to it can be with Its photoresponse range is widened, it is made also to have preferable photo-catalysis capability in visible-range.
Invention content
It is an object of the present invention to provide a kind of vanadium Boratex area load ag material photocatalytic oxidation degradations under visible light The method of chlorophenol pollutant, this method are dense in vanadium Boratex area load ag material, pollutant using chlorophenol as pollutant Degree under visible light illumination carries out it photocatalytic oxidation degradation under the aqueous conditions of 20mg/L, 120 minutes can be by 2- chlorine Phenol is degradable, finds that chlorophenol degradation rate is 100% by high performance liquid chromatograph analysis.Operating procedure of the present invention is simple, at This is low, the dechlorination that can efficiently, be quickly used in chlorinated aromatic hydrocarbons, it is important that having widened the photoresponse range of catalysis material makes It also has the ability of good degrading chlorophenol pollutant under visible light.
A kind of vanadium Boratex area load ag material of the present invention is degraded the side of chlorine atmosphere pollutant under visible light Method follows these steps to carry out：
A, the silver nitrate solution of a concentration of 0.039-1.969g/L of configuration quality takes configured good silver nitrate solution 20ml, vanadium Boratex 0.5g are placed in the crystallising dish of a diameter of 60mm, are shaken up ultrasonic 10min, are then irradiated under xenon lamp 30min, xenon lamp launch wavelength are λ >200nm, system away from xenon lamp export 18cm, xenon lamp spot diameter be 80mm, electric current 20A, Solution is transferred in 50ml centrifuge tubes after reaction, centrifuge washing 3 times, powder sample is collected in freeze-drying, obtains vanadium boron The powder sample of sour sodium area load silver；
B, 2-chlorophenol 1g is dissolved in 100ml methanol, ultrasonic 30-60min, makes the solution that it is stable homogeneous, takes The 2-chlorophenol solution that 0.1mL stablizes is placed in the beaker that volume is 250mL, adds water that it is made to be diluted to 20-100mg/L, step is added The powder sample 50-100mg for the vanadium Boratex area load silver that rapid a is obtained, 30-60min is stirred under the conditions of being protected from light, is then moved 1mL is taken to be placed in be measured in liquid phase bottle；
C, remaining step b solution is irradiated into 120-210min under the xenon lamp of stabilized illumination, it is natural at 25 DEG C of room temperature Optical energy density is 0.5-2mw/cm2, xenon lamp irradiation wavelengths λ >420nm, energy averag density are 502mw/cm2, system is away from xenon lamp Export 18cm, xenon lamp spot diameter be 80mm, every the time be 10-30min sample 1mL, to all samples having been taken out into Row efficient liquid phase chromatographic analysis analyzes the degradation efficiency of pollutant.
A kind of vanadium Boratex area load ag material of the present invention photocatalytic oxidation degradation chlorophenols under visible light The method of pollutant, the material obtained by this method can generate various concentration freedom with the variation of time under visible light Base efficiently, quickly by chlorophenol pollutant dechlorination chain rupture forms small carboxylic acid molecules and containing the solution of chlorine.
Chlorophenol uses commercially available raw material in the present invention.
In the present invention embodiment use method for visible light under irradiation 120min, sampling interval time 30min, be protected from light stirring Time carries out under conditions of being 30min.It can be obtained required result under this condition.
Description of the drawings：
Vanadium Boratex abbreviation NVB；
Fig. 1 is the XRD diffracting spectrums after vanadium Boratex powder of the present invention and area load silver, and wherein Ag/NVB is quality Than；
It is 50mg, a concentration of 20mg/L of 2-chlorophenol that Fig. 2, which is vanadium Boratex area load ag material powder dosage of the present invention, Degradation efficiency figure under radiation of visible light 120min, wherein：-- it is vanadium Boratex powder ,-●-it is that Ag/NVB mass ratioes are 0.1%, -- be Ag/NVB mass ratioes it is 0.5%, -- be Ag/NVB mass ratioes it is 1.0%.
Specific implementation mode
Below in conjunction with drawings and examples, the present invention is described in detail：
Embodiment 1
A, the silver nitrate solution of a concentration of 0.039g/L of configuration quality takes configured good silver nitrate solution 20ml, vanadium boron Sour sodium 0.5g is placed in the crystallising dish of a diameter of 60mm, shakes up ultrasonic 10min, and the transmitting of 30min xenon lamps is then irradiated under xenon lamp Wavelength is λ >200nm, system away from xenon lamp export 18cm, xenon lamp spot diameter be 80mm, electric current 20A, after reaction will be molten Liquid is transferred in 50ml centrifuge tubes, centrifuge washing 3 times, and powder sample is collected in freeze-drying, obtains vanadium Boratex area load silver Content be 0.1% powder sample；
B, 2-chlorophenol 1g is dissolved in 100ml methanol, ultrasonic 40min, makes the solution that it is stable homogeneous, takes 0.1mL Stable 2-chlorophenol solution is placed in the beaker that volume is 250mL, adds water that it is made to be diluted to 40mg/L, is added what step a was obtained The powder sample 70mg of vanadium Boratex area load silver, stirs 30min under the conditions of being protected from light, and then pipettes 1mL and is placed in liquid phase bottle It is interior to be measured；
C, remaining step b solution is irradiated into 150min under the xenon lamp of stabilized illumination, at 25 DEG C of room temperature, natural luminous energy Metric density is 0.5-2mw/cm2, xenon lamp irradiation wavelengths λ >420nm, energy averag density are 502mw/cm2, system is away from xenon lamp outlet 18cm, xenon lamp spot diameter are 80mm, are that 30min samples 1mL every the time, efficient liquid is carried out to all samples having been taken out Analysis of hplc analyzes the degradation efficiency of pollutant.Analysis result shows that 120 minutes 2-chlorophenol dechlorination efficiencies are 85%.
Embodiment 2
A, the silver nitrate solution of a concentration of 0.197g/L of configuration quality takes configured good silver nitrate solution 20ml, vanadium boron Sour sodium 0.5g is placed in the crystallising dish of a diameter of 60mm, shakes up ultrasonic 10min, and the transmitting of 30min xenon lamps is then irradiated under xenon lamp Wavelength is λ >200nm, system away from xenon lamp export 18cm, xenon lamp spot diameter be 80mm, electric current 20A, after reaction will be molten Liquid is transferred in 50ml centrifuge tubes, centrifuge washing 3 times, and powder sample is collected in freeze-drying, obtains vanadium Boratex area load silver Content be 0.5% powder sample；
B, 2-chlorophenol 1g is dissolved in 100ml methanol, ultrasonic 60min, makes the solution that it is stable homogeneous, takes 0.1mL Stable 2-chlorophenol solution is placed in the beaker that volume is 250mL, adds water that it is made to be diluted to 80mg/L, is added what step a was obtained The powder sample 80mg of vanadium Boratex area load silver, stirs 30min under the conditions of being protected from light, and then pipettes 1mL and is placed in liquid phase bottle It is interior to be measured；
C, remaining step b solution is irradiated into 120-210min under the xenon lamp of stabilized illumination, it is natural at 25 DEG C of room temperature Optical energy density is 0.5-2mw/cm2, xenon lamp irradiation wavelengths λ >420nm, energy averag density are 502mw/cm2, system is away from xenon lamp 18cm is exported, xenon lamp spot diameter is 80mm, is that 30min samples 1mL every the time, is carried out to all samples having been taken out high Effect liquid phase chromatogram is analyzed, and the degradation efficiency of pollutant is analyzed, and analysis result shows that 120 minutes 2-chlorophenol dechlorination efficiencies are 90%.
Embodiment 3
A, the silver nitrate solution of a concentration of 0.393g/L of configuration quality takes configured good silver nitrate solution 20ml, vanadium boron Sour sodium 0.5g is placed in the crystallising dish of a diameter of 60mm, shakes up ultrasonic 10min, and the transmitting of 30min xenon lamps is then irradiated under xenon lamp Wavelength is λ >200nm, system away from xenon lamp export 18cm, xenon lamp spot diameter be 80mm, electric current 20A, after reaction will be molten Liquid is transferred in 50ml centrifuge tubes, centrifuge washing 3 times, and powder sample is collected in freeze-drying, obtains vanadium Boratex area load silver Content be 1.0% powder sample；
B, 2-chlorophenol 1g is dissolved in 100ml methanol, ultrasonic 50min, makes the solution that it is stable homogeneous, takes 0.1mL Stable 2-chlorophenol solution is placed in the beaker that volume is 250mL, adds water that it is made to be diluted to 100mg/L, and step a is added and obtains Vanadium Boratex area load silver powder sample 100mg, 30min is stirred under the conditions of being protected from light, 1mL is then pipetted and is placed in liquid phase It is to be measured in bottle；
C, remaining step b solution is irradiated into 120-210min under the xenon lamp of stabilized illumination, it is natural at 25 DEG C of room temperature Optical energy density is 0.5-2mw/cm2, xenon lamp irradiation wavelengths λ >420nm, energy averag density are 502mw/cm2, system is away from xenon lamp 18cm is exported, xenon lamp spot diameter is 80mm, is that 30min samples 1mL every the time, is carried out to all samples having been taken out high Effect liquid phase chromatogram is analyzed, and the degradation efficiency of pollutant is analyzed.Analysis result shows that 120 minutes 2-chlorophenol dechlorination efficiencies are 100%.
Embodiment 4
A, the silver nitrate solution of a concentration of 1.969g/L of configuration quality takes configured good silver nitrate solution 20ml, vanadium boron Sour sodium 0.5g is placed in the crystallising dish of a diameter of 60mm, shakes up ultrasonic 10min, and the transmitting of 30min xenon lamps is then irradiated under xenon lamp Wavelength is λ >200nm, system away from xenon lamp export 18cm, xenon lamp spot diameter be 80mm, electric current 20A, after reaction will be molten Liquid is transferred in 50ml centrifuge tubes, centrifuge washing 3 times, and powder sample is collected in freeze-drying, obtains vanadium Boratex area load silver Powder sample；
B, 2-chlorophenol 1g is dissolved in 100ml methanol, ultrasonic 30-60min, makes the solution that it is stable homogeneous, takes The 2-chlorophenol solution that 0.1mL stablizes is placed in the beaker that volume is 250mL, adds water that it is made to be diluted to 20mg/L, step a is added The powder sample 50mg of obtained vanadium Boratex area load silver, 30min is stirred under the conditions of being protected from light, 1mL is then pipetted and is placed in It is to be measured in liquid phase bottle；
C, remaining step b solution is irradiated into 120min under the xenon lamp of stabilized illumination, at 25 DEG C of room temperature, natural luminous energy Metric density is 0.5-2mw/cm2, xenon lamp irradiation wavelengths λ >420nm, energy averag density are 502mw/cm2, system is away from xenon lamp outlet 18cm, xenon lamp spot diameter are 80mm, are that 10min samples 1mL every the time, efficient liquid is carried out to all samples having been taken out Analysis of hplc analyzes the degradation efficiency of pollutant.Analysis result shows that 120 minutes 2-chlorophenol dechlorination efficiencies are 100%.
Embodiment 5
The present embodiment is contrast experiment：
A, 2-chlorophenol 1g is dissolved in 100ml methanol, ultrasonic 30-60min, makes the solution that it is stable homogeneous, takes The 2-chlorophenol solution that 0.1mL stablizes is placed in the beaker that volume is 250mL, adds water that it is made to be diluted to 20mg/L, vanadium boric acid is added Sodium powder sample 50mg, stirs 30min under the conditions of being protected from light, then pipette 1mL be placed in it is to be measured in liquid phase bottle；
B, remaining step a solution is irradiated into 120min under the xenon lamp of stabilized illumination, at 25 DEG C of room temperature, natural luminous energy Metric density is 0.5-2mw/cm2, xenon lamp irradiation wavelengths λ >420nm, energy averag density are 502mw/cm2, system is away from xenon lamp outlet 18cm, xenon lamp spot diameter are 80mm, are that 10min samples 1mL every the time, efficient liquid is carried out to all samples having been taken out Analysis of hplc analyzes the degradation efficiency of pollutant.Analysis result shows that 120 minutes 2-chlorophenol dechlorination efficiencies are 83%.
1,2,3,4 comparative example 5 of embodiment, after showing the lower 120 minutes vanadium Boratex area load silver of radiation of visible light Performance with better degradation 2-chlorophenol greatly improves the degradation efficiency to 2-chlorophenol in same time.
Operating procedure of the present invention is simple, at low cost, the dechlorination that can efficiently, be quickly used in chlorinated aromatic hydrocarbons, prior It is to have widened the photoresponse range of catalysis material to make it under visible light and also have the ability of excellent degrading chlorophenol pollutant.

Claims (1)

  1. A kind of method of chlorine atmosphere pollutant 1. vanadium Boratex area load ag material is degraded under visible light, it is characterised in that press The following steps carry out：
    A, the silver nitrate solution of a concentration of 0.039-1.969 g/L of configuration quality takes configured good silver nitrate solution 20ml, vanadium Boratex 0.5g is placed in the crystallising dish of a diameter of 60mm, shakes up ultrasonic 10min, and 30min, xenon lamp hair are then irradiated under xenon lamp The a length of λ &gt of ejected wave;200 nm, system away from xenon lamp export 18cm, xenon lamp spot diameter be 80 mm, electric current 20A, after reaction Solution is transferred in 50ml centrifuge tubes, centrifuge washing 3 times, powder sample is collected in freeze-drying, and it is negative to obtain vanadium Boratex surface Carry the powder sample of silver；
    B, 2-chlorophenol 1g is dissolved in 100ml methanol, ultrasonic 30-60min, makes the solution that it is stable homogeneous, takes 0.1 mL Stable 2-chlorophenol solution is placed in the beaker that volume is 250 mL, adds water that it is made to be diluted to 20-100 mg/L, step a is added The powder sample 50-100mg of obtained vanadium Boratex area load silver, 30-60min is stirred under the conditions of being protected from light, then pipettes 1 ML is placed in be measured in liquid phase bottle；
    C, remaining step b solution is irradiated into 120-210min under the xenon lamp of stabilized illumination, at 25 DEG C of room temperature, natural light Energy density is 0.5-2 mw/cm2, xenon lamp irradiation wavelengths λ >420 nm, energy averag density are 502 mw/cm2, system is away from xenon Lamp exports 18 cm, and xenon lamp spot diameter is 80 mm, be that 10-30 min sample 1 mL every the time, is had been taken out to all Sample carries out efficient liquid phase chromatographic analysis, analyzes the degradation efficiency of pollutant.
CN201810518093.5A 2018-05-27 2018-05-27 Vanadium Boratex area load ag material is degraded the method for chlorine atmosphere pollutant under visible light Pending CN108704643A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110075840A (en) * 2019-04-26 2019-08-02 暨南大学 The application of the sodium vanadium borate and its degrading chlorophenol pollutant of area load gold

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KR20120129858A (en) * 2012-11-12 2012-11-28 전남대학교산학협력단 Ag-photocatalyst-carbon nano fiber complex, and filter comprising the same
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Application publication date: 20181026