CN103127946B - Near-infrared response photocatalysis material Cu2(OH)PO4 and preparation method - Google Patents

Near-infrared response photocatalysis material Cu2(OH)PO4 and preparation method Download PDF

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CN103127946B
CN103127946B CN201310066882.7A CN201310066882A CN103127946B CN 103127946 B CN103127946 B CN 103127946B CN 201310066882 A CN201310066882 A CN 201310066882A CN 103127946 B CN103127946 B CN 103127946B
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preparation
hpo
suspension
deionized water
hours
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CN103127946A (en
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黄柏标
王刚
张晓阳
秦晓燕
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Shandong University
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Shandong University
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    • 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

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Abstract

The invention relates to a near-infrared response photocatalysis material Cu2(OH)PO4 and a preparation method, the preparation method comprises the following steps: mixing Cu(NO3)2 and Na2HPO4 and adding in deionized water, adjusting the pH value of suspending liquid to 4-7, performing hydrothermal reaction for 6-12 hours at 120 DEG C, separating and purifying, and drying to obtain the product of micro-nano crystal having a quadrature structure, wherein the crystal length is 4-5 micrometers, the width is 1.4-1.6 micrometers, and the surface has ravine. The near-infrared response photocatalysis material Cu2(OH)PO4 has good photocatalysis performance under the near infrared irradiation (Lambda is greater than 800 nanometers), 90% of 2,4dichlorophenol can be degraded in six house, and the performance is excellent.

Description

A kind of catalysis material Cu of near infrared light response 2(OH) PO 4and preparation method thereof
Technical field
The present invention relates to a kind of catalysis material Cu of micro-nano near-infrared response 2(OH) PO 4and preparation method thereof, belong to the synthesis field of micro-nano near-infrared photocatalysis powder material.
Background technology
In recent years, becoming increasingly conspicuous of the energy and environmental problem, seriously have impact on expanding economy.Environmental pollution brings huge harm to the production of the mankind and life, and especially the pollution of water resource has jeopardized the healthy of the mankind, and the method being badly in need of feasibility is disposed of sewage.Traditional method is administered water pollutions and is also existed that power consumption is large, equipment is complicated, costly, easily bring the shortcomings such as secondary pollution.Therefore, the focus that a kind of novel, efficient, practical environmental protection treatment technology becomes people's research is developed.
Along with going deep into of research, it is found that Heterogeneous Photocatalysis of Semiconductors carrys out degradable organic pollutant by environmentally friendly redox reaction, photocatalysis technology well combines this two big worlds Sexual Themes of energy and environment, have that energy consumption is low, easy and simple to handle, reaction condition is gentle, usage range is wide, can reduce the advantages such as secondary pollution, utilize solar energy green energy resource to the problem of curbing environmental pollution, in waste water control, thus more and more receive the concern of people.
Most catalysis material is visible ray or ultraviolet light response, catalysis material is seldom had to have photo-catalysis capability under the irradiation of near infrared light, and the part of sunshine spectrum mid-infrared light occupies the ratio of similar 45%, if can obtain near infrared light response catalysis material by more meaningful for the waste water control under the environment of reality.
Summary of the invention
For existing deficiency, the invention provides the catalysis material Cu of a kind of near infrared light response 2(OH) PO 4and preparation method thereof, can under the irradiation of near infrared light degradation of organic substances.
The technical scheme that the present invention takes is:
A kind of catalysis material Cu of near infrared light response 2(OH) PO 4, it is the micro-nano crystal with orthohormbic structure, and crystal length is 4-5 micron, and width is 1.5 ± 0.1 microns, and there is gully on its surface.
Above-mentioned catalysis material Cu 2(OH) PO 4preparation method, comprise the steps:
(1) by Cu (NO 3) 2and Na 2hPO 4be mixed to join in deionized water, strong stirring obtains suspension;
(2) regulate the pH value of suspension to be 4-7 by the NaOH solution that concentration is 5mol/L, continue to stir;
(3) obtained suspension is transferred in the reactor of polytetrafluoroethylene (PTFE), 120 DEG C of hydro-thermal reaction 6-12 hour;
(4) naturally cool to room temperature, by obtained sample suction filtration, spend deionized water 2 times, and then wash 2-5 time with ethanol, 60-80 DEG C of dry 6-12 hour.
Cu (NO in said method described in step (1) 3) 2, Na 2hPO 4mass ratio be 3.751:1.560, the consumption of water is 50-52ml every gram Na 2hPO 4.
Hydro-thermal reaction described in step (3) preferably 6 hours.
Catalysis material Cu of the present invention 2(OH) PO 4under the irradiation of near infrared light, there is certain photocatalysis performance, can be used for degradation of organic substances.
Near infrared light responsible photocatalytic material Cu of the present invention 2(OH) PO 4application, be applied to the removal of outdoor air, waste water, surface water or Organic Pollutants of Drinking Water.
Excellent results of the present invention is as follows:
1. the catalysis material Cu of near-infrared response of the present invention 2(OH) PO 4under the irradiation of near infrared light, (λ ﹥ 800 nanometer) has good photocatalysis performance, in the time of 6 hours, can be degraded by 2, the 4-chlorophenesic acids of 90%, function admirable.
2. catalysis material Cu of the present invention 2(OH) PO 4preparation method is simple, with low cost, synthetic method mild condition, has higher commercial applications prospect.
Accompanying drawing explanation
Fig. 1 is the SEM figure of embodiment 1 product;
Fig. 2 is the SEM figure of embodiment 2 product;
Fig. 3 is the X-ray diffractogram of embodiment 1 product;
Fig. 4 is the degraded figure under the near infrared light of embodiment 1 product, a figure is photocatalysis comparison diagram, and abscissa is time (unit: hour), and ordinate is 2 of degraded certain hour, the concentration (C) of 4-chlorophenesic acid solution and the initial concentration (C of 2,4 chlorophenesic acid solution 0) ratio; Wherein ● curve be near-infrared irradiate under, the volatilization figure of 2,4-chlorophenesic acids when 20-25 degree constant temperature; ■ is when 20-25 degree constant temperature, material degradation 2, the degraded figure of 4 chlorophenesic acids.
Detailed description of the invention
Be described further in the present invention below in conjunction with accompanying drawing, but be not limited thereto.
Embodiment 1
Get the Cu (NO of stoichiometric proportion 3) 2and Na 2hPO 4(wherein Cu (NO 3) 2for 3.751g, Na 2hPO 4for 1.560g), add the deionized water of 80 milliliters, strong stirring, the suspension concentration obtained is the pH value of the NaOH solution regulation system of 5mol/L is neutral, continue to stir, finally obtained suspension is transferred in the reactor of polytetrafluoroethylene (PTFE) of 120 milliliters, and react 6 hours under the condition of 120 DEG C.After question response terminates, take out reactor, cool under room temperature, the sample obtained carries out suction filtration, with deionized water and ethanol cyclic washing 3 times, then in the baking oven of 60 DEG C dry 12 hours.Fig. 1 is the Electronic Speculum figure of obtained sample.
Embodiment 2
Get the Cu (NO of stoichiometric proportion 3) 2and Na 2hPO 4(wherein Cu (NO 3) 2for 3.751g, Na 2hPO 4for 1.560g), add the deionized water of 80 milliliters, strong stirring, the suspension concentration obtained is the pH value of the NaOH solution regulation system of 5mol/L is 4.0, continue to stir, finally obtained suspension is transferred in the reactor of polytetrafluoroethylene (PTFE) of 120 milliliters, and react 6 hours under the condition of 120 DEG C.After question response terminates, take out reactor, cool under room temperature, the sample obtained carries out suction filtration, with deionized water and ethanol cyclic washing 3 times, then in the baking oven of 60 DEG C dry 12 hours.Fig. 2 is the Electronic Speculum figure of obtained sample.
Embodiment 3
Get the Cu (NO of stoichiometric proportion 3) 2and Na 2hPO 4(wherein Cu (NO 3) 2for 3.751g, Na 2hPO 4for 1.560g), add the deionized water of 80 milliliters, strong stirring, the suspension concentration obtained is the NaOH solution regulation system pH value of 5mol/L is after neutrality, put into reactor 120 DEG C reaction 12 hours, the sample obtained carries out suction filtration, with deionized water and ethanol cyclic washing 3 times, then in the baking oven of 60 DEG C dry 12 hours.Fig. 3 is the X-ray diffractogram of obtained sample.
Photocatalytic activity is tested:
The method of carrying out photocatalytic activity test to material prepared in embodiment 1 is as follows:
Photocatalysis test (cross section 30cm in glass beaker 2, high 5cm), and use cooling circulating water device to maintain the temperature of suspension at 20-25 DEG C.Light source selects the 300W xenon lamp that optical filter is housed, and makes optical source wavelength be greater than 800nm.With 2,4 chlorophenesic acids carry out the photocatalytic activity of assess sample.Take 0.1g sample dispersion in 2, the 4-chlorophenesic acid solution of 100mL (20mg/L).Before light-catalyzed reaction test, lucifuge magnetic agitation 30min makes 2,4-chlorophenesic acid reach adsorption equilibrium at catalyst surface, and every 1 hour sampling 5ml after logical light, centrifugation, gets supernatant measurement of ultraviolet-visible spectrophotometer absorbance.Other contrast test has carried out photocatalytic activity test under equal experiment condition.

Claims (1)

1. the catalysis material Cu of a near infrared light response 2(OH) PO 4preparation method, it is characterized in that, comprise the steps:
(1) by Cu (NO 3) 2and Na 2hPO 4be mixed to join in deionized water, strong stirring obtains suspension; Described Cu (NO 3) 2, Na 2hPO 4mass ratio be 3.751:1.560, the consumption of water is 50-52ml every gram Na 2hPO 4;
(2) regulate the pH value of suspension to be 4-7 by the NaOH solution that concentration is 5mol/L, continue to stir;
(3) obtained suspension is transferred in the reactor of polytetrafluoroethylene (PTFE), 120 DEG C of hydro-thermal reactions 6 hours;
(4) naturally cool to room temperature, by obtained sample suction filtration, spend deionized water 2 times, then wash 2-5 time with ethanol, 60-80 DEG C of dry 6-12 hour.
CN201310066882.7A 2013-03-04 2013-03-04 Near-infrared response photocatalysis material Cu2(OH)PO4 and preparation method Expired - Fee Related CN103127946B (en)

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CN107512709B (en) * 2017-09-29 2020-06-09 陕西科技大学 Preparation method of triangular prism self-assembled bow-tie-shaped hydroxyl copper phosphate electrode material
CN107706419B (en) * 2017-09-29 2020-01-21 陕西科技大学 Method for preparing flaky hydroxyl copper phosphate electrode material by controlling pH value
CN111272693A (en) * 2018-12-05 2020-06-12 山东大学 Cement raw material component on-line measuring device based on near infrared spectrum

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Title
新型催化剂Cu2(OH)PO4的制备及表征;吕长和等;《安徽化工》;20090831;第35卷(第4期);第19-21页 *

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