CN106902816A - A kind of Pd/ZnO composite nano materials with photocatalysis performance and its preparation method and application - Google Patents
A kind of Pd/ZnO composite nano materials with photocatalysis performance and its preparation method and application Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 47
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 34
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- 238000000034 method Methods 0.000 claims description 17
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- 241000894006 Bacteria Species 0.000 claims description 8
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 7
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- 229910052573 porcelain Inorganic materials 0.000 claims description 6
- 229910003244 Na2PdCl4 Inorganic materials 0.000 claims description 5
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
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- 239000000463 material Substances 0.000 abstract description 4
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- 229910052725 zinc Inorganic materials 0.000 description 1
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- 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
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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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
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Abstract
The invention discloses a kind of Pd/ZnO composite nano materials with photocatalysis performance and its preparation method and application.Belong to the synthesis technical field of nano material, with Pd nano-particles and four-footed shape zinc oxide as presoma, ethanol is solvent to the material, carrying out precious metals pd to ZnO using coupling method supports, and prepares Pd/ZnO composite nano materials.And prepared Pd/ZnO composite nano materials show excellent photo-catalytic degradation of methyl-orange performance and photocatalysis antibacterial performance.
Description
Technical field
It is more particularly to a kind of by four-footed shape ZnO and Pd nanocubes the present invention relates to a kind of composite nano materials
Synergy, is obviously improved the photocatalysis performance of catalyst, has boundless in the field such as catalytic degradation and biological medicine
The composite nano materials of application.
Background technology
The pollution of organic matter has potential grave danger to the ecological resources of China and the healthy of people in water body,
Water pollutant main source is the development that manufacturing industry and heavy industry are advanced by leaps and bounds.In all pollutions of China, water resource is dirty
Dye is particularly acute, and the toxicity and non-biodegradable of Organic Pollutants In Water easily cause cancer and mutation, so, in recent years
Come, research catalytic degradation organic pollution obtains the favor of scientific research personnel.
At present, the research on catalytic degradation organic pollution is more and more, there is absorption, filtering, and precipitation and photocatalysis are dropped
All multi-methods such as solution, compared to other method, photocatalytic degradation is many excellent due to its environmentally friendly and superpower detergent power etc.
One of point, the technology as research degradable organic pollutant.Light-catalysed core is completed using catalyst.And high activity
The design of catalyst will turn into the important research object of future studies photocatalytic degradation organic matter with synthesis.
The content of the invention
The purpose of the present invention is the high performance Pd/ZnO catalysis materials of exploitation, by four-footed shape ZnO nano material and Pd
Nanocomposites, prepare the Pd/ZnO composites with excellent photocatalysis degradation organic contaminant and anti-microbial property.
The technical scheme is that：A kind of Pd/ZnO composite nano materials with photocatalysis performance, preparation method bag
Include following steps：ZnO is scattered in absolute ethyl alcohol, Pd nano-particles are added, after stirring, is put in baking oven, in 100 DEG C
Lower drying, obtains target product.
A kind of above-mentioned Pd/ZnO composite nano materials with photocatalysis performance, described ZnO passes through chemical vapor deposition
Area method synthesizes：It is put into porcelain dish after zinc powder is ground, N is passed through when tube furnace is warming up into 700 DEG C -1000 DEG C2And O2, continue to rise
Temperature, after constant temperature 20-60min at 1000 DEG C -1300 DEG C, the porcelain dish that will be equipped with zinc powder is put into tube furnace, closes tube furnace,
Constant temperature 1-1.5h, is cooled to room temperature at 1000 DEG C -1300 DEG C, obtains ZnO.
A kind of above-mentioned Pd/ZnO composite nano materials with photocatalysis performance, described Pd nano-particles pass through liquid phase
Reducing process synthesizes：Ascorbic acid, polyvinylpyrrolidone and KBr are taken, distillation water dissolves are added, Na is added2PdCl4It is molten
Liquid, reacts 2-8h in 80 DEG C of oil baths, centrifugation, and vacuum drying obtains Pd nano-particles.
A kind of above-mentioned Pd/ZnO composite nano materials with photocatalysis performance, in mass ratio, ascorbic acid:Polyethylene
Pyrrolidones:KBr:Na2PdCl4=1:1.75:5:0.95.
A kind of above-mentioned Pd/ZnO composite nano materials with photocatalysis performance, in mass ratio, ZnO:Pd nano-particles
=50:1.
A kind of above-mentioned Pd/ZnO composite nano materials with photocatalysis performance are in photocatalysis degradation organic contaminant
Application.Method is as follows：In the solution containing organic pollution, above-mentioned Pd/ZnO composite nano materials, luminous intensity are added
It is 60-180mwcm-1, light application time is 40-70min.Preferably, the addition of Pd/ZnO composite nano materials is dense to end
It is 0.0125-0.450gL to spend-1。
A kind of application of the above-mentioned Pd/ZnO composite nano materials with photocatalysis performance in photocatalysis antibacterial.Method
It is as follows：Above-mentioned Pd/ZnO composite nano materials are added in bacteria suspension, 30-60min is irradiated under visible light.
Compared with prior art, the invention has the advantages that：
1) present invention, design synthesizes four-footed shape Pd/ZnO nano composite materials, and the catalyst has been obviously improved nano-ZnO
Catalytic performance.
2) present invention, the ZnO after doping Pd compared with being compared before undoped p, photo-catalytic degradation of methyl-orange improved efficiency.
3) present invention, after catalytic degradation, can be recycled, the catalytic degradation time with recycling catalyst by 5 times
70min or so is stilled remain in, there is preferable stability, high recycling rate.
4) present invention, compared with being compared before undoped p, photocatalysis sterilization performance is obviously improved the ZnO after doping Pd.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of ZnO prepared by embodiment 1.
Fig. 2 is the TEM figures of Pd nano-particles prepared by embodiment 1.
Fig. 3 is the TEM figures of Pd/ZnO composite nano materials prepared by embodiment 1.
Fig. 4 a are the ultraviolet visible absorption spectra figures of Pd/ZnO composite nano materials Photocatalytic Degradation On Methyl Orange Solutions.
Fig. 4 b are the ultraviolet visible absorption spectra figures of ZnO Photocatalytic Degradation On Methyl Orange Solutions.
Fig. 5 a are recycling ultraviolet visible absorption spectras figure (circulation primary) of Pd/ZnO composite nano materials.
Fig. 5 b are recycling ultraviolet visible absorption spectras figure (circulation secondary) of Pd/ZnO composite nano materials.
Fig. 5 c are the recycling ultraviolet visible absorption spectra figures (circulation three times) of Pd/ZnO composite nano materials.
Fig. 5 d are the recycling ultraviolet visible absorption spectra figures (circulation four times) of Pd/ZnO composite nano materials.
Fig. 5 e are the recycling ultraviolet visible absorption spectra figures (circulation five times) of Pd/ZnO composite nano materials.
Fig. 6 is the antibacterial effect figure of ZnO and Pd/ZnO under visible light conditions；
Wherein, A：Non- illumination ZnO；A1：Visible ray ZnO；B：Non- illumination Pd/ZnO；B1：Visible ray Pd/ZnO；C：Non- illumination
Blank；C1：Visible ray blank.
Specific embodiment
Technical scheme for a better understanding of the present invention, spy is described in further detail with specific embodiment, but side
Case not limited to this.
Embodiment 1 has the Pd/ZnO composite nano materials of photocatalysis performance
1. chemical vapour deposition technique (CVD) synthesizes nano-ZnO：Take 5.0012g zinc powders, be put into after grinding it is standby in porcelain dish,
The temperature programming condition of tube furnace is set, it is 3 that velocity ratio is passed through when being warming up to 800-900 DEG C:2 N2And O2, then heat to
1100-1200 DEG C, after constant temperature 30-40min, the porcelain dish equipped with zinc powder is put into, closes tube furnace, in calcining at 1100-1200 DEG C
1h, is cooled to room temperature, obtains white product, as nano-ZnO.
Product is through SEM characterization results as shown in figure 1, as seen from Figure 1, the ZnO synthesized by CVD is in four-footed shape, explanation
The ZnO of four-footed shape can be largely prepared by simple CVD.
2. liquid phase reduction synthesizes Pd nano-particles：Take 60mg ascorbic acid, 105mg polyvinylpyrrolidones (PVP) and
300mg KBrs, add 10mL distillation water dissolves, add 3mL Na2PdCl4Solution (contains Na2PdCl457mg), 80
6h is reacted in DEG C oil bath, is centrifuged, product is put in vacuum drying chamber and is dried, obtain the solid powder of bright black, as Pd receives
Rice corpuscles.
The synthesis of 3.Pd/ZnO composite nano materials：10mg ZnO are scattered in 3mL absolute ethyl alcohols, addition is scattered in
0.2mg Pd nano-particles in 2mL ethanol, and stir, after reaction 6h, it is put in baking oven, dried at 100 DEG C, obtain grey and consolidate
Body powder, as Pd/ZnO composite nano materials.
It is as shown in Figure 3 that product characterizes structure through TEM.From the figure 3, it may be seen that cubical Pd nano-particles are successfully supported on four-footed
On the ZnO of shape, from figure 3, it can be seen that Pd nano-particles are uniformly supported on ZnO, and Pd of the surrounding without free state
Nano-particle, this is due to there is certain interaction force between nanoscale Pd and ZnO so that metal nanoparticle easily with
ZnO is combined.
The Pd/ZnO composite nano materials photocatalysis degradation organic contaminants of embodiment 2
In 40mL concentration be 20.0mgL-1Methyl orange solution in, add embodiment 1 prepare Pd/ZnO composite Nanos
Material, makes the final concentration of 0.200gL of Pd/ZnO composite nano materials-1, dispersion liquid is transferred to photolytic cell by ultrasonic disperse
In, dispersion liquid is placed in dark place stirring 30min by magnetic agitation, reaches adsorption equilibrium, is then 100mwcm in light intensity-1
Under carry out photocatalytic degradation, every 10min sampling once, centrifugation, take supernatant liquor, determine the UV absorption light at its 463nm
Spectrum.
Comparative example：Ibid, Pd/ZnO composite nano materials are replaced with the chemical vapour deposition technique of embodiment 1 to method by difference
(CVD) nano-ZnO of synthesis.
From Fig. 4 a and Fig. 4 b, Pd/ZnO composite nano materials of the invention, at 40 minutes, degraded reached
Entirely, without the ZnO for loading, degradable needs are reached 60 minutes.It can be seen that the present invention has loaded the composite of the ZnO of Pd,
Photocatalysis performance is significantly improved, and degradation time shortens 20min, because Pd makes the photoproduction that ZnO is produced in photocatalytic process
The rate of departure in electronics and hole is accelerated, and strengthens the oxidative degradation ability in hole.
The recycling of the Pd/ZnO composite nano materials photocatalysis degradation organic contaminants of embodiment 3
Method：Method with embodiment 2, after photocatalysis terminates, by the methyl orange solution containing Pd/ZnO composite nano materials
It is centrifuged, and water washing 3 times, catalyst is put in 40 DEG C of baking oven and is dried, tested as second photocatalysis
Photochemical catalyst, the rest may be inferred, investigates the stability of Pd/ZnO composite nano materials.It is analyzed using same characterizing method, is tied
Fruit such as Fig. 5 a- Fig. 5 e.
From Fig. 5 a- Fig. 5 e：Using nano-ZnO experiment condition light intensity be 100mwcm-1, catalyst concn is
0.200g·L-1Under the conditions of when proceeding to the 5th degradation experiment to methyl orange solution, when degradation rate reaches 100%, the time is still
70min or so is maintained at, the excellent recycling performance of Pd/ZnO composite nano materials is embodied.
The Pd/ZnO composite nano materials photocatalysis antibacterials of embodiment 4
The preparation of LB culture mediums：Sodium chloride 2.5012g, peptone 2.5015g, yeast extract 1.2519g are weighed, is added water to
250mL, its pH=7.2~7.4 is adjusted with NaOH solution, obtains LB fluid nutrient mediums；To adding 2% fine jade in fluid nutrient medium
Fat, you can obtain solid medium, the 30min that sterilized in 121 DEG C of high-pressure steam sterilizing pans is placed in by culture medium, is refrigerated standby.
Antibacterial experiment：
1) with oese picking strain Escherichia coli (E.coli ATCC 15597), rule on solid medium, 37
24h is cultivated in DEG C incubator, picking single bacterium is fallen within fluid nutrient medium, and 11h is cultivated in 37 DEG C of constant temperature oscillator, obtains OD values
It is 1.820 bacteria suspension.
2) 5mL bacteria suspensions are taken in 20min is centrifuged on centrifuge, with the phosphate buffer solution of pH=7.0 (hereinafter referred to as
" PBS ") washing after, add PBS, obtain PBS bacteria suspensions；Stepwise dilution is carried out to bacteria suspension with phosphate buffer solution, makes it
Final diluted concentration is 102cfu·mL-1。
3) ZnO the and Pd/ZnO composites for weighing 5.0mg respectively are put in centrifuge tube, add PBS ultrasonic disperses, then
It is 10 to add 0.5mL concentration2cfu·mL-1Bacteria suspension, fully shake up, take 100 μ L spread plates, remaining dispersion liquid is put in
After irradiating 60min under xenon source, 100 μ L spread plates are taken, flat board is put in 37 DEG C of constant incubators and cultivates 24h, observed
Colony growth situation, while counting and calculating sterilizing rate, does blank assay.
Compare the anti-microbial property of the ZnO catalyst under illumination condition of load Pd and unsupported Pd, as a result as shown in fig. 6,
As shown in Figure 6：Contrast A and A1 understands, it is seen that light has certain facilitation, non-illumination bar to four-footed shape ZnO antibacterial effects
The antibiotic rate of four-footed shape ZnO can reach 30% under part, and the antibiotic rate of four-footed shape ZnO can reach 50% under illumination condition.Contrast B
Understood with B1, it is seen that light has to the antibacterial effect of four-footed shape Pd/ZnO and is obviously promoted effect, four-footed shape Pd/ under non-illumination condition
The antibiotic rate of ZnO can reach 54.3%, and the antibiotic rate of four-footed shape Pd/ZnO can reach 93.6% under illumination condition.Contrast A1 and
B1 can be further characterized by, it is seen that light is better than ZnO to the facilitation of four-footed shape Pd/ZnO antibacterial effects, because your gold supported
After category Pd, reduce light and excite lower ZnO to produce the compound probability in light induced electron and hole, increased the sky with strong oxidizing property
Cave and the generation of living radical, so as to destroy the cell membrane of bacterium, cause a series of hydrolysis to breed bacterial growth
It is suppressed.Contrast A1, B1, C1 understand, it is seen that antibacterial effect is four-footed shape Pd/ZnO under light>Four-footed shape ZnO, contrasts A, B, C
Understand, antibacterial effect is four-footed shape Pd/ZnO under non-illumination>Four-footed shape ZnO.
Obviously, be obviously improved the catalytic performance of ZnO after Pd doping in the present invention, in Photocatalytic Degradation On Methyl Orange Solution and
There is good effect in the anti-Escherichia coli reaction of photocatalysis, this method is simple to operate, it is easy to prepare.
Claims (10)
1. a kind of Pd/ZnO composite nano materials with photocatalysis performance, it is characterised in that preparation method comprises the following steps：
ZnO is scattered in absolute ethyl alcohol, Pd nano-particles are added, after stirring, is put in baking oven, in being dried at 100 DEG C, obtain mesh
Mark product.
2. a kind of Pd/ZnO composite nano materials with photocatalysis performance according to claim 1, it is characterised in that institute
The ZnO for stating is synthesized by chemical vapour deposition technique：It is put into porcelain dish after zinc powder is ground, tube furnace is warming up to 700 DEG C -1000
DEG C when be passed through N2And O2, continue to heat up, after constant temperature 20-60min at 1000 DEG C -1300 DEG C, the porcelain dish that will be equipped with zinc powder is put into pipe
In formula stove, tube furnace is closed, constant temperature 1-1.5h, is cooled to room temperature at 1000 DEG C -1300 DEG C, obtains ZnO.
3. a kind of Pd/ZnO composite nano materials with photocatalysis performance according to claim 1, it is characterised in that institute
The Pd nano-particles stated are synthesized by liquid phase reduction：Ascorbic acid, polyvinylpyrrolidone and KBr are taken, distilled water is added
Dissolving, adds Na2PdCl4Solution, reacts 2-8h in 80 DEG C of oil baths, centrifugation, and vacuum drying obtains Pd nano-particles.
4. a kind of Pd/ZnO composite nano materials with photocatalysis performance according to claim 3, it is characterised in that press
Mass ratio, ascorbic acid:Polyvinylpyrrolidone:KBr:Na2PdCl4=1:1.75:5:0.95.
5. a kind of Pd/ZnO composite nano materials with photocatalysis performance according to claim 1, it is characterised in that press
Mass ratio, ZnO:Pd nano-particle=50:1.
6. a kind of Pd/ZnO composite nano materials with photocatalysis performance described in claim 1 are in the organic dirt of photocatalytic degradation
Application in dye thing.
7. application according to claim 6, it is characterised in that method is as follows：In the solution containing organic pollution, plus
Enter the Pd/ZnO composite nano materials described in claim 1, luminous intensity is 60-180mwcm-1, light application time is 40-70min.
8. application according to claim 7, it is characterised in that the addition of Pd/ZnO composite nano materials is to final concentration
It is 0.0125-0.450gL-1。
9. a kind of Pd/ZnO composite nano materials with photocatalysis performance described in claim 1 in photocatalysis antibacterial should
With.
10. application according to claim 9, it is characterised in that method is as follows：Claim 1 institute is added in bacteria suspension
The Pd/ZnO composite nano materials stated, irradiate 30-60min under visible light.
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| CN109046344A (en) * | 2018-07-18 | 2018-12-21 | 辽宁大学 | A kind of preparation method and application of high performance Pd-Zn alloy@C/ZnO composite material |
| CN111514931A (en) * | 2020-04-21 | 2020-08-11 | 东华大学 | Preparation method of high polymer and palladium-gold nanorod fiber film with photocatalytic performance |
| CN113499773A (en) * | 2021-07-08 | 2021-10-15 | 辽宁大学 | Nano enzyme of nano zinc oxide supported palladium nanoparticles and preparation method and application thereof |
| CN115414931A (en) * | 2022-08-31 | 2022-12-02 | 北京工业大学 | Preparation method of Pd/ZnO catalyst for hydrogen production by methanol steam reforming |
| CN116058385A (en) * | 2022-11-18 | 2023-05-05 | 辽宁大学 | Palladium zinc oxide nano enzyme material with double enzyme activities, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109046344A (en) * | 2018-07-18 | 2018-12-21 | 辽宁大学 | A kind of preparation method and application of high performance Pd-Zn alloy@C/ZnO composite material |
| CN109046344B (en) * | 2018-07-18 | 2021-06-01 | 辽宁大学 | Preparation method and application of high-performance Pd-Zn alloy @ C/ZnO composite material |
| CN111514931A (en) * | 2020-04-21 | 2020-08-11 | 东华大学 | Preparation method of high polymer and palladium-gold nanorod fiber film with photocatalytic performance |
| CN113499773A (en) * | 2021-07-08 | 2021-10-15 | 辽宁大学 | Nano enzyme of nano zinc oxide supported palladium nanoparticles and preparation method and application thereof |
| CN115414931A (en) * | 2022-08-31 | 2022-12-02 | 北京工业大学 | Preparation method of Pd/ZnO catalyst for hydrogen production by methanol steam reforming |
| CN115414931B (en) * | 2022-08-31 | 2024-01-05 | 北京工业大学 | Preparation method of Pd/ZnO catalyst for preparing hydrogen by methanol steam reforming |
| CN116058385A (en) * | 2022-11-18 | 2023-05-05 | 辽宁大学 | Palladium zinc oxide nano enzyme material with double enzyme activities, and preparation method and application thereof |
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