CN108585111A - The method that semi-conducting material Zinc Tungstate is catalyzed ultrasonotomography Meloxicam - Google Patents

The method that semi-conducting material Zinc Tungstate is catalyzed ultrasonotomography Meloxicam Download PDF

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CN108585111A
CN108585111A CN201810451859.2A CN201810451859A CN108585111A CN 108585111 A CN108585111 A CN 108585111A CN 201810451859 A CN201810451859 A CN 201810451859A CN 108585111 A CN108585111 A CN 108585111A
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znwo
meloxicam
ultrasonotomography
catalyzed
semi
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CN108585111B (en
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王新
许明玲
郝俊旭
周玲玲
王晓芳
刘彬
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Liaoning University
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Liaoning University
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    • 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
    • C02F1/34—Treatment of water, waste water, or sewage with mechanical oscillations
    • C02F1/36—Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
    • 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
    • C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
    • 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
    • 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
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/40—Organic compounds containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Catalysts (AREA)
  • Physical Water Treatments (AREA)

Abstract

The present invention discloses a kind of semi-conducting material Zinc Tungstate (ZnWO4) catalysis ultrasonotomography Meloxicam method, including by semiconductor nano material ZnWO4It mixes and is put into container with Meloxicam, ultrasonotomography is carried out in Vltrasonic device；Sample centrifuging and taking upper layer clear solution does UV, visible light (UV vis) absorption spectromtry.The present invention judges ZnWO by ultrasonotomography Meloxicam4Sound catalytic activity, with the variation of ultraviolet spectroscopy Meloxicam absorbance to judge ZnWO4Sound catalytic activity.ZnWO4It is safe and non-toxic, physico-chemical property is stable, efficiently recyclable, non-secondary pollution.Show ZnWO by verification4There is considerable foreground in terms of being catalyzed ultrasonotomography pharmacy waste water.

Description

The method that semi-conducting material Zinc Tungstate is catalyzed ultrasonotomography Meloxicam
Technical field
The present invention relates to ultrasonotomography pharmacy waste water technical field, more particularly to a kind of semi-conducting material ZnWO4Catalysis is super The method of sound degradation Meloxicam.
Background technology
Medicine material complicated component, production process are various, product category is various, and Wastewater Pollutant content is high, can give birth to Change degradability is poor, water quality and quantity changes greatly, after these Recalcitrant chemicals are discharged into water body, remains in water body for a long time, and big There is stronger toxicity and " three cause " effect more, and by food chain accumulation, enrichment, eventually enter into human body and generate toxicity, be generation Generally acknowledged one of the waste water difficult to deal in boundary.
ZnWO4It is a kind of monoclinic crystal, usual physicochemical properties are stablized, the ability with radioresistance, anti-strong light, because of it With special structure and property, it is typically considered a kind of effective material of processing water pollution problem, is obtained in recent years wide General research.In recent years, advanced oxidation processes are increasingly drawn attention with its unique advantage, and ultrasonic irradiation is a kind of advanced height Grade oxidation process is a kind of emerging technology for handling waste water.Ultrasonic degradation includes mainly free-radical oxidation, high temperature pyrolysis and surpasses Critical aoxidizes three kinds of approach, and " cavitation effect " makes molecule valence link be broken and form hydroxy radical, to degradation of organic substances；It is empty Changing the high temperature and pressure generated when break up gas bubbles can make sound catalyst play catalytic action.Ultrasonic energy is concentrated, propagation distance is remote, Because of the peculiar property of its own, it can be degraded to organic matter with aided nano catalyst, there is good Research Prospects.
Invention content
The purpose of the present invention is to provide a kind of semi-conducting material ZnWO4The method for being catalyzed ultrasonotomography Meloxicam, should Method is with ZnWO4As semiconductor sound catalyst, catalysis ultrasonotomography is carried out to Meloxicam in Vltrasonic device, passes through change ZnWO4PH value, addition, the initial concentration of Meloxicam, ultrasonic time, power etc. investigated, and then to the technology Feasibility probed into, by studies have shown that the technology can be applied to Pharmaceutical Wastewater Treatment field.
The purpose of the present invention is what is be achieved through the following technical solutions：
Semi-conducting material ZnWO4The method for being catalyzed ultrasonotomography Meloxicam, including by semiconductor nano material ZnWO4With Meloxicam mixing is put into container, and ultrasonotomography is carried out in Vltrasonic device；Sample centrifuging and taking upper layer clear solution, is UV- Vis spectroscopic assays.
The method, the ZnWO4PH value be 5-9.
The method, the ZnWO4Addition be 0.50-1.50gL-1。
The method, the Meloxicam initial concentration are 6-18mgL-1。
The method, the ultrasonic time are 0-150min.
The method, the ultrasonic power 100-200W.
Advantages of the present invention is with effect：
1. the present invention is with ZnWO4As semiconductor catalyst, have safe and non-toxic, physico-chemical property is stable, it is efficiently recyclable, Non-secondary pollution.Show ZnWO by verification4There is considerable foreground in terms of being catalyzed ultrasonotomography waste water.
2. the main function of ultrasonic wave is cavitation, fuel factor and chemical effect in the present invention.ZnWO4It is catalyzed as sound Agent, to there is Meloxicam that there is good catalytic degradation effect.Present invention process gives up using supercritical ultrasonics technology as a kind of novel pharmacy Water technology, have the advantages that it is easy to operate, efficient, applied widely, do not generate secondary pollution.
Description of the drawings
Fig. 1 (a) is product ZnWO prepared by embodiment 14X-ray diffraction (XRD) spectrogram；
Fig. 1 (b) and the electron scanning micrograph that (c) is product prepared by embodiment 1；
Fig. 2 is Meloxicam structure chart；
Fig. 3 is that embodiment 3 utilizes ZnWO4Its addition is to being catalyzed ultrasonotomography meloxicam solutions when as sound catalyst The influence of effect；
Fig. 4 is that embodiment 4 utilizes ZnWO4When as sound catalyst ultrasonotomography Meloxicam, different ultrasonic times To being catalyzed the influence of ultrasonotomography effect.
Specific implementation mode
The following describes the present invention in detail with reference to examples.
Tungstates semi-conducting material ZnWO4Have the effect of good catalysis ultrasonotomography Meloxicam, preparation method Starting material is ZnWO cheap and easy to get4, it is not necessarily to any auxiliary addition agent, Meloxicam of degrading is achieved the purpose that by ultrasound.Water ZnWO prepared by hot method4It is nano semiconductor material.ZnWO4Possess nutty structure, belongs to monoclinic crystal, physics and chemistry Property is stablized, and has good sound catalytic performance.
Embodiment 1ZnWO4Preparation method
Include the following steps：
Step 1：According to a certain amount of ratio, by 0.17molL-1Na2WO4·2H2O solution is added in beaker, in stirring bar 0.17molL is added under part-1Zn(NO3)2·6H2O, it is 6 or so to adjust pH value with NaOH or HCl solution, and magnetic force stirs at room temperature Mix 30min, ultrasonic 30min.
Step 2：Solution made from step 1 is put into the autoclave of polytetrafluoroethyllining lining in 180 DEG C of conditions Under reacted, naturally cool to room temperature after reaction.
Step 3：ZnWO is made through suction filtration, washing, drying, grinding in product4Powder.
Fig. 1 (a) is product ZnWO prepared by embodiment 14X-x ray diffraction (XRD) spectrogram；Fig. 1 (b) and (c) are real Apply the electron scanning micrograph of the product of the preparation of example 1；As seen from the figure, the product synthesized by embodiment 1 is ZnWO4, shape State is rendered as graininess.
Fig. 2 is Meloxicam structure chart.
The method that 2 semi-conducting material Zinc Tungstate of embodiment is catalyzed ultrasonotomography Meloxicam
Include the following steps：
Step 1：It takes the meloxicam solutions 20mL of a concentration of 10mg/L in conical flask, the 10mg accurately weighed is added Nanometer Zn WO4Powder carries out ultrasonotomography.
Step 2：Suspension sampling takes supernatant after centrifuging.
Step 3：Its UV-vis spectrum is surveyed in 200~450nm.The degradation rate of Meloxicam can use solution in its λmax= Absorbance at 360nm calculates, and formula is：Degradation rate (%)=[(A0-At)/A0] × 100%, A0It is meloxicam solutions Initial absorbance, AtIt is absorbance of the meloxicam solutions under different experimental conditions.
The method that 3 semi-conducting material Zinc Tungstate of embodiment is catalyzed ultrasonotomography Meloxicam
ZnWO4Degradation experiment to Meloxicam is in ZnWO4Addition is 0.50-1.50g/L progress, ZnWO4PH Value is 6, a concentration of 10mg/L of Meloxicam, ultrasonic power 200W, and ultrasonic time is what 120min was carried out.
The meloxicam solutions of 20mL 10mg/L are taken, the primary nanometer Zn WO that 0.50g/L is added4Powder ultrasonic processing 120min.Suspension sampling takes supernatant after centrifuging, its UV-vis spectrum is surveyed in 200~450nm.
By ZnWO4Addition be changed to 0.75 successively, 1.00,1.25,1.50g/L, repeat above-mentioned experiment.
Fig. 3 is that embodiment 3 utilizes ZnWO4Its addition is to being catalyzed ultrasonotomography meloxicam solutions when as sound catalyst Influential effect figure；Known by Fig. 3, works as ZnWO4Addition be 1.00g/L when, degradation effect is best, and degradation rate can reach 75.67%.
The method that 4 semi-conducting material Zinc Tungstate of embodiment is catalyzed ultrasonotomography Meloxicam
ZnWO4Degradation experiment to Meloxicam is in ZnWO4Addition be 1.00g/L carry out, ZnWO4PH value Be 6, a concentration of 10mg/L of Meloxicam, ultrasonic power 200W, ultrasonic time is followed successively by 0,30,60,90,120, 150min。
The meloxicam solutions of 20mL 10mg/L are taken, the primary nanometer Zn WO that 1.00g/L is added4Powder is ultrasonically treated 30min.Suspension sampling takes supernatant after centrifuging, its UV-vis spectrum is surveyed in 200~450nm.
Fig. 4 is that embodiment 4 utilizes ZnWO4When as sound catalyst ultrasonotomography Meloxicam, different ultrasonic times To being catalyzed ultrasonotomography influential effect figure, as shown in Figure 4, with the extension of ultrasonic time, ZnWO4It is catalyzed the effect of ultrasonotomography It gradually increases, ultrasonic effect reaches best after 120min.

Claims (6)

1. semi-conducting material ZnWO4The method for being catalyzed ultrasonotomography Meloxicam, which is characterized in that including by semiconductor nano material Expect ZnWO4It mixes and is put into container with Meloxicam, ultrasonotomography is carried out in Vltrasonic device；The clarification of sample centrifuging and taking upper layer is molten Liquid does UV-vis spectroscopic assays.
2. the method as described in claim 1, which is characterized in that the ZnWO4PH value be 5-9.
3. the method as described in claim 1, which is characterized in that the ZnWO4Addition be 0.50-1.50gL-1。
4. the method as described in claim 1, which is characterized in that the Meloxicam initial concentration is 6-18mgL-1。
5. the method as described in claim 1, which is characterized in that the ultrasonic time is 0-150min.
6. the method as described in claim 1, which is characterized in that the ultrasonic power 100-200W.
CN201810451859.2A 2018-05-12 2018-05-12 Method for degrading meloxicam by catalyzing and ultrasonically degrading zinc tungstate serving as semiconductor material Active CN108585111B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113173665A (en) * 2021-03-31 2021-07-27 沈阳化工大学 ZnWO4/MgWO4Method for degrading organic wastewater by using composite semiconductor material
CN115957744A (en) * 2023-01-29 2023-04-14 辽宁大学 ZnWO 4 Preparation method and application of photocatalyst

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CN102923780A (en) * 2012-11-14 2013-02-13 陕西科技大学 Method for preparing cubic ZnWO4 nanocrystal photocatalysis material
WO2013049253A1 (en) * 2011-09-26 2013-04-04 Mccormack Richard A Clathrate desalination process using an ultrasonic actuator
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CN106944074A (en) * 2017-03-17 2017-07-14 佛山科学技术学院 A kind of visible-light response type composite photo-catalyst and its preparation method and application

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113173665A (en) * 2021-03-31 2021-07-27 沈阳化工大学 ZnWO4/MgWO4Method for degrading organic wastewater by using composite semiconductor material
CN113173665B (en) * 2021-03-31 2022-10-04 沈阳化工大学 ZnWO 4 /MgWO 4 Method for degrading organic wastewater by using composite semiconductor material
CN115957744A (en) * 2023-01-29 2023-04-14 辽宁大学 ZnWO 4 Preparation method and application of photocatalyst
CN115957744B (en) * 2023-01-29 2023-11-10 辽宁大学 ZnWO (zinc-oxygen) device 4 Preparation method and application of photocatalyst

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