CN107175113A - A kind of multiporous biological gold doping zeroth order iron catalyst and preparation method and application - Google Patents
A kind of multiporous biological gold doping zeroth order iron catalyst and preparation method and application Download PDFInfo
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Abstract
The invention belongs to the technical field of environmental microorganism material, a kind of multiporous biological gold doping zeroth order iron catalyst and preparation method and application is disclosed.Methods described is：(1) it is collected by filtration, cleans after pycnoporus samguineus culture to stationary phase, freezes, freeze-dried powder is made；(2) freeze-dried powder is added in golden precursor solution, adjusts pH, be placed in constant temperature oscillator and cultivate, calcined, cleaned, drying obtains multiporous biological gold；(3) by multiporous biological gold, ferrous salt, ultrasonic disperse and it is dissolved in the water, obtains mixed solution；(4) under protection gas and stirring condition, sodium borohydride solution is added dropwise into mixed solution, continues to stir after dripping, stirring terminates to be cleaned, and dries, the golden doped magnetic zeroth order iron catalyst of multiporous biological is obtained.The preparation method of the present invention is simple, it is not necessary to introduce other chemical reagent, realizes the doping of gold and Zero-valent Iron, reduces the consumption of gold, and prepared catalyst particle size is homogeneous, and catalytic performance is good.
Description
Technical field
The invention belongs to environmental microorganism material and contaminant degradation technical field, more particularly to a kind of multiporous biological gold is mixed
Miscellaneous Zero-valent Iron and preparation method thereof, and multiporous biological gold doping Zero-valent Iron are applied in terms of environmental contaminants degraded.
Background technology
Nano-noble metal gold is because it possesses a variety of good characteristics and is widely used in every field, especially in catalysis neck
Domain is particularly important.The preparation method of traditional nanogold is Physical and chemical method, and these method requirement conditions are harsh, can
HTHP, and a variety of chemical reagent can be needed, high energy consumption, pollution is big.In recent years, microorganism is honest and clean due to its aboundresources
Valency is easy to get and is applied to noble metal synthesis field.
Because gold utensil has good catalytic capability, in catalytic environment pollutant very advantageous, but to be faced with yield few for gold,
Cost is high, so other catalysis materials that adulterate are required.But existing catalyst, particle diameter is uneven, and specific surface area is small, urges
Change activity to have much room for improvement.
The content of the invention
In order to overcome the shortcoming and defect of prior art, it is an object of the invention to provide a kind of multiporous biological gold doping zero
The preparation method of valency iron catalyst.The present invention using biotechnology with chemical technology be combined prepare one kind it is more larger than surface,
Catalytic activity is good, the nano material of uniform particle sizes.
Another object of the present invention is to provide the multiporous biological gold doping zeroth order iron catalyst obtained by the above method.
It is still another object of the present invention to provide the application of above-mentioned multiporous biological gold doping zeroth order iron catalyst.The catalysis
Agent is used for catalytic degradation environmental organic pollutant, particularly halogen contamination, specially tetrabromobisphenol A.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of multiporous biological gold doping zeroth order iron catalyst, comprises the following steps：
(1) it is collected by filtration after pycnoporus samguineus (Pycnoporus sanguineus) culture to stationary phase, cleans, freeze,
Freeze-dried powder is made；The pycnoporus samguineus (Pycnoporus sanguineus), buy in Chinese microorganism strain preservation management
Committee's common micro-organisms center, preserving number is CGMCC5.00815；
(2) pycnoporus samguineus freeze-dried powder in step (1) is mixed with golden precursor solution, pH is to 3~5 for regulation, obtains bacterium
Outstanding mixed liquor；Bacterium is hanged into mixed liquor constant-temperature shaking culture, collected, to containing in fungus plus alkali mixing for collection, is calcined, cleaning is obtained
To porous nano-Au；The golden precursor solution is compound solution containing gold element；
(3) by the porous nano-Au and ferrous salt of step (2), ultrasonic disperse and it is dissolved in the water, obtains mixed solution；Institute
It is more than one in frerrous chloride, ferrous sulfate or green vitriol to state ferrous salt；
(4) under protection gas and stirring condition, sodium borohydride solution is added dropwise into mixed solution, continues after dripping
Stirring, stirring terminates cleaned, dried, and obtains the golden doped magnetic zeroth order iron catalyst of multiporous biological.Described in step (4) after
The time of continuous stirring is 30~90min.
Pycnoporus samguineus (Pycnoporus sanguineus) described in step (1), buys and is protected in Chinese microorganism strain
Administration committee's common micro-organisms center is hidden, preserving number is CGMCC5.00815.
Cleaning described in step (1) is decompression suction filtration, is cleaned using deionized water, and the number of times of the cleaning is 3~5 times.
Drying described in step (1) is dry 48~72h at freeze-drying, -60~-80 DEG C.
The concentration that bacterium described in step (2) hangs golden presoma in mixed liquor is 0.5~2.0mmolL-1, the use of freeze-dried powder
Measure as 1~7gL-1。
Golden presoma is preferably gold chloride described in step (2).
The condition cultivated described in step (2) is that 24~72h is cultivated at 20~40 DEG C.
Filtered through gauze collection is collected as described in step (2).
Calcining described in step (2) is calcined under protection gas, and calcining heat is 420~500 DEG C, and calcination time is
2~4h.The protection gas is nitrogen or argon gas, preferably argon gas.
Alkali described in step (2) is (1~2) with pycnoporus samguineus freeze-dried powder mass ratio：1, be preferably (1~1.5)：1；
The alkali is more than one in sodium hydroxide or potassium hydroxide, preferably potassium hydroxide.
Cleaning refers to first be cleaned with 3wt%~5wt% hydrochloric acid described in step (2), then is cleaned with deionized water into
Property.
Ferrous salt consumption described in step (3) is 10~45 times of porous nano-Au mole dosage.
It is nitrogen that gas is protected described in step (4).
The consumption of sodium borohydride described in step (4) is 8~12 times of the mole dosage of ferrous salt.
Cleaning described in step (4) refers to carry out suction filtration cleaning using water, until the water of filtering is neutrality.
Step (4) drying is vacuum drying, and condition is dry 8~24h at 60~80 DEG C.
The multiporous biological gold doping zeroth order iron catalyst is obtained by above-mentioned preparation method.
The multiporous biological gold doping zeroth order iron catalyst is used for catalytic degradation environmental organic pollutant, particularly containing halogen
Pollutant.
The present invention has advantages below and technique effect
(1) preparation method of the present invention is simple, need not introduce other chemical reagent, realizes mixing for porous golden and Zero-valent Iron
It is miscellaneous；
(2) present invention obtains nanogold using biological recovering method gold, by firing, is formed on the supported porous carbon of nanogold
Form, is evenly distributed, bigger than surface；
(3) the porous gold doping Zero-valent Iron catalyst particle size that the present invention is obtained is homogeneous, and size is 10nm or so particle, is urged
Change performance is good, and (when applied to catalysis tetrabromobisphenol A, the clearance of tetrabromobisphenol A is 99.7% in 120min, is shown good
Catalytic performance).
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of the porous nano-Au prepared in embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of the porous nano-Au doping zeroth order iron catalyst prepared in embodiment 1；
Fig. 3 is the XRD of the porous nano-Au doping zeroth order iron catalyst prepared in embodiment 1；
Fig. 4 be embodiment 1 in prepare porous nano-Au (i.e. porous gold), porous nano-Au adulterate zeroth order iron catalyst
Under the catalysis of (i.e. porous gold doping Zero-valent Iron), porous carbon prepared by embodiment 2 and Zero-valent Iron, the degradation rate of tetrabromobisphenol A is bent
Line chart；
Fig. 5 is the curve map of the catalyst degrading tetrabromobisphenol A of different gold contents prepared by embodiment 3；
Fig. 6 be embodiment 3 prepare gold content be 2% catalyst under condition of different pH, catalytic degradation tetrabromobisphenol A
Curve map.
Embodiment
With reference to specific embodiments and the drawings, the present invention is described in further detail, but embodiments of the present invention
Not limited to this.
Embodiment 1
A kind of preparation method of multiporous biological gold doping zeroth order iron catalyst, comprises the following steps：
(1) by pycnoporus samguineus after PDA cultivates 3.5d, it is collected by filtration and is cleaned with deionized water at 3 times, -60 DEG C and frozen
Dry 48h, is made freeze-dried powder；0.2g freeze-dried powders are taken into container, chlorauric acid solution are added, regulation pH is 5, obtains bacteria suspension, bacterium
The concentration of gold chloride is 1mmolL in suspension-1, the concentration of freeze-dried powder is 4gL-1；Bacteria suspension is put into isothermal vibration device
It is collected by filtration after 40 DEG C of culture 48h, adds potassium hydroxide 0.3g and stir, is put into tube furnace to calcine and calcines 2h at 420 DEG C,
First cleaned with 4wt% hydrochloric acid, after cleaned with deionized water to neutrality, obtain porous nano-Au；The porous nano-Au obtained
Scanning electron microscope (SEM) photograph (SEM) as shown in Figure 1；
(2) porous nano-Au 0.05g, green vitriol 2.48g is taken to be added in 80mL deionized water, ultrasound point
Dissolving is dissipated, mixed solution is made；Under conditions of nitrogen is protected and is stirred, 200gL is added dropwise dropwise-1Sodium borohydride solution 20ml
Into mixed solution, after after completion of dropwise addition, continue stirring reaction 1h, cleaned with anaerobic deionized water 4 times rapidly, at 80 DEG C of vacuum
12h is dried, porous nano-Au doping zeroth order iron catalyst i.e. multiporous biological gold doping zeroth order iron catalyst is obtained.The present embodiment system
The SEM (ESEM) of standby porous nano-Au doping zeroth order iron catalyst is as shown in Fig. 2 it is observed that on porous carbon structure
Nanogold, Zero-valent Iron are loaded with, particle diameter is 10~20nm, is come in every shape.Porous nano-Au doping zeroth order manufactured in the present embodiment
The XRD of iron catalyst is as shown in Figure 3.
Embodiment 2
(1) preparation of porous C catalyst：
By pycnoporus samguineus after PDA cultures 4d, it is collected by filtration and clean with deionized water 3 times, it is lyophilized at latter -60 DEG C
Freeze-dried powder is made in 48h；0.4g freeze-dried powders are taken into container, addition potassium hydroxide 0.4g stirs to be put into tube furnace and calcined
At 460 DEG C calcine 2h after, first cleaned with 4wt% hydrochloric acid, after cleaned with deionized water to neutrality, obtain porous carbon；
(2) preparation of zeroth order iron catalyst:
Green vitriol 2.48g is taken to be added in 80mL deionized water, mixed solution is made in ultrasonic disperse；
Under under conditions of nitrogen protection and stirring, 200mgL is added dropwise dropwise-1Sodium borohydride solution 20mL is treated into copperas solution
After completion of dropwise addition, continue stirring reaction 1h, cleaned afterwards with anaerobic deionized water 4 times rapidly, 12h is dried at 80 DEG C of vacuum, is obtained
Zero-valent Iron.
Embodiment 3
The preparation of the multiporous biological gold doping zeroth order iron catalyst of different gold contents：
Take 0 respectively, 0.012,0.025, the porous nano-Au and four parts of water of 2.48g seven that prepare in 0.05g embodiment 1
Ferrous sulfate is closed, 80mL deionized water is added to together by every a porous nano-Au and per a green vitriol
In, four parts of mixed solutions are made in ultrasonic disperse；Under conditions of nitrogen is protected and is stirred, into every a mixed solution dropwise
200gL is added dropwise-1Sodium borohydride solution 20ml is rapid clear with anaerobic deionized water after after completion of dropwise addition, continuing stirring reaction 1h
Wash 4 times, 12h is dried at 80 DEG C of vacuum, respectively obtain the multiporous biological gold doping Zero-valent Iron that gold content is 0,0.5%, 1%, 2%
Catalyst.
The measure of merit of multiporous biological gold doping Zero-valent Iron catalyst degrading tetrabromobisphenol A：
Under A, different catalysts, the degraded test of tetrabromobisphenol A：
From 100mL centrifuge tube as reaction vessel, weigh the porous nano-Au (i.e. porous gold) of the preparation of embodiment 1
0.1g, embodiment 1 prepares porous nano-Au doping zeroth order iron catalyst 0.1g (i.e. porous gold doping Zero-valent Iron), and embodiment 2 is made
Zeroth order iron catalyst (0.1g) prepared by standby porous C catalyst (0.1g) (i.e. porous carbon) and embodiment 2 (i.e. zeroth order
Iron), it is added to respectively in 50mL 10mg/L tetrabromobisphenol A solution, i.e., porous gold doping Zero-valent Iron+tetrabromobisphenol A, porous
Gold+tetrabromobisphenol A, Zero-valent Iron+tetrabromobisphenol A, the four groups of experiments of porous carbon+tetrabromobisphenol A, regulation pH are 7, and ultrasonic (180W) is molten
2min is solved, 30 DEG C of reactions in constant temperature oscillator, three parallel laboratory tests of every group of experiment, interval 20min samplings, when always sampling is placed into
Between be 2h.It is measured after being filtered during sampling with 0.5 μm of needle tubing filter with high performance liquid chromatograph rapidly.
Tetrabromobisphenol A concentration mensuration：Agilent -1200, C18 separation column, mobile phase：Methanol:Water=90:10, flow velocity
1.0mL·min-1, Detection wavelength 220nm, the μ L of sampling volume 20,30 DEG C of column oven temperature.Test result is as shown in Figure 4.Fig. 4 is
Porous gold doping Zero-valent Iron, porous gold, Zero-valent Iron and porous carbon carry out the degradation rate curve of catalytic degradation to tetrabromobisphenol A
Figure.
Under B, different nanogold/Zero-valent Iron ratios (i.e. different gold contents), the degraded test of tetrabromobisphenol A：
The catalyst 0.1g that the gold content that respectively prepared by Example 3 is 0,0.5%, 1%, 2%, is added to 50mL respectively
Concentration is in 10mg/L tetrabromobisphenol A, regulation pH is 7, and ultrasonic (180W) dissolving 2min places into constant temperature oscillator 30 DEG C
Reaction, interval 20min samplings, total sample time is 2h.Efficient liquid phase is used after being filtered during sampling with 0.5 μm of needle tubing filter rapidly
Chromatograph is measured.Tetrabromobisphenol A concentration mensuration：Agilent -1020, C18 separation column, mobile phase：Methanol:Water=90:
10, flow velocity 1.0mLmin-1, Detection wavelength 220nm, the μ L of sampling volume 20,30 DEG C of column oven temperature.Test result such as Fig. 5 institutes
Show.Fig. 5 is the curve map of the catalyst degrading tetrabromobisphenol A of different gold contents prepared by embodiment 3.
C, investigation are under different pH, the removal efficiency of tetrabromobisphenol A：
The catalyst that gold content prepared by embodiment 3 is 2% is added in the tetrabromobisphenol A that 50mL concentration is 10mg/L,
It is 3,5,7,9,11 to adjust pH, ultrasonic (180W) dissolving 2min, places into 30 DEG C of reactions in constant temperature oscillator, and interval 20min takes
Sample, total sample time is 2h.It is measured after being filtered during sampling with 0.5 μm of needle tubing filter with high performance liquid chromatograph rapidly.
Tetrabromobisphenol A concentration mensuration：Agilent -1020, C18 separation column, mobile phase：Methanol:Water=90:10, flow velocity 1.0mL
min-1, Detection wavelength 220nm, the μ L of sampling volume 20,30 DEG C of column oven temperature.Test result is as shown in Figure 6.Fig. 6 is embodiment 3
The catalyst that the gold content of preparation is 2% is under condition of different pH, the curve map of catalytic degradation tetrabromobisphenol A.Ordinate is four
The ratio of bromine bisphenol A concentration and initial concentration.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not limited by examples detailed above
System, it is other it is any without departing from spirit of the invention and the change made under principle, modification, replacement, combine, simplification is
Effect.
Claims (10)
1. a kind of preparation method of multiporous biological gold doping zeroth order iron catalyst, it is characterised in that：Comprise the following steps：
(1) it is collected by filtration, cleans after pycnoporus samguineus culture to stationary phase, freezes, pycnoporus samguineus freeze-dried powder is made；
(2) pycnoporus samguineus freeze-dried powder in step (1) is mixed with golden precursor solution, pH is to 3~5 for regulation, obtains bacterium outstanding mixed
Close liquid；Bacterium is hanged into mixed liquor and is placed in culture in constant temperature oscillation, is collected, adds alkali to mix to containing in fungus for collection, calcining, cleaning,
Obtain porous nano-Au；The golden precursor solution is compound solution containing gold element；The condition of the culture is 20~40
24~72h is cultivated at DEG C；
(3) by the porous nano-Au and ferrous salt of step (2), ultrasonic disperse and it is dissolved in the water, obtains mixed solution；
(4) under protection gas and stirring condition, sodium borohydride solution is added dropwise into mixed solution, continues to stir after dripping
Mix, stirring terminates to be cleaned, and dries, obtain the golden doped magnetic zeroth order iron catalyst of multiporous biological.
2. according to claim 1 multiporous biological gold doping zeroth order iron catalyst preparation method, it is characterised in that：Step
(2) golden presoma is gold chloride described in；
Ferrous salt described in step (3) is more than one in green vitriol, ferrous sulfate or frerrous chloride；
Alkali described in step (2) is more than one in sodium hydroxide or potassium hydroxide.
3. according to claim 1 multiporous biological gold doping zeroth order iron catalyst preparation method, it is characterised in that：Step
(2) concentration of pycnoporus samguineus freeze-dried powder described in bacterium hangs mixed liquor is 1~7g/L；
The concentration that bacterium described in step (2) hangs golden presoma in mixed liquor is 0.5~2.0mmolL-1；
Alkali described in step (2) is 1 with pycnoporus samguineus freeze-dried powder mass ratio：(1~2)；
Ferrous salt consumption described in step (3) is 10~45 times of porous nano-Au mole dosage；
The consumption of sodium borohydride described in step (4) is 8~12 times of the mole dosage of ferrous salt.
4. according to claim 1 multiporous biological gold doping zeroth order iron catalyst preparation method, it is characterised in that：Step
(1) pycnoporus samguineus described in, buy in China Committee for Culture Collection of Microorganisms's common micro-organisms center, preserving number is
CGMCC5.00815。
5. according to claim 1 multiporous biological gold doping zeroth order iron catalyst preparation method, it is characterised in that：Step
(2) calcining described in is calcined under protection gas, and calcining heat is 420~500 DEG C, and calcination time is 2~4h.
6. according to claim 5 multiporous biological gold doping zeroth order iron catalyst preparation method, it is characterised in that：It is described to protect
It is nitrogen or argon gas to protect gas.
7. according to claim 1 multiporous biological gold doping zeroth order iron catalyst preparation method, it is characterised in that：Step
(1) cleaning described in is decompression suction filtration, is cleaned using deionized water；
Cleaning refers to first be cleaned with 3wt%~5wt% hydrochloric acid described in step (2), then is cleaned with deionized water to neutrality；
It is nitrogen that gas is protected described in step (4)；The time for continuing stirring described in step (4) is 30~90min；Step (4)
Described in cleaning refer to using water carry out suction filtration cleaning, until filtering water for neutrality；
The condition of step (4) described drying is dry 8~24h at 60~80 DEG C.
8. a kind of multiporous biological gold doping zeroth order iron catalyst prepared according to any one of claim 1~7 methods described.
9. the application of multiporous biological gold doping zeroth order iron catalyst according to claim 8, it is characterised in that：The porous life
Thing gold doping zeroth order iron catalyst is used for catalytic degradation environmental organic pollutant.
10. application according to claim 9, it is characterised in that：The organic pollution is tetrabromobisphenol A.
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| PCT/CN2017/116393 WO2018205610A1 (en) | 2017-05-12 | 2017-12-15 | Porous biogold-doped zero-valent iron catalyst, preparation method therefor and use thereof |
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| WO2018205610A1 (en) * | 2017-05-12 | 2018-11-15 | 华南理工大学 | Porous biogold-doped zero-valent iron catalyst, preparation method therefor and use thereof |
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| WO2020031090A1 (en) * | 2018-08-06 | 2020-02-13 | King Abdullah University Of Science And Technology | Single metal atom or bimetallic alloy heterogeneous catalysts on a carbonaceous support produced by metal precursor deposition on exoelectrogen bacteria and pyrolyzing |
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| WO2018205610A1 (en) * | 2017-05-12 | 2018-11-15 | 华南理工大学 | Porous biogold-doped zero-valent iron catalyst, preparation method therefor and use thereof |
| CN108793377A (en) * | 2018-06-08 | 2018-11-13 | 湖南农业大学 | One Yeasts load the preparation method of Nanoscale Iron metal/composite material |
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| CN108940310A (en) * | 2018-07-20 | 2018-12-07 | 华南理工大学 | A kind of Pd/Fe@Fe3O4Composite catalyst and the preparation method and application thereof |
| CN108940310B (en) * | 2018-07-20 | 2021-01-19 | 华南理工大学 | Pd/Fe @ Fe3O4Composite catalyst and preparation method and application thereof |
| WO2020031090A1 (en) * | 2018-08-06 | 2020-02-13 | King Abdullah University Of Science And Technology | Single metal atom or bimetallic alloy heterogeneous catalysts on a carbonaceous support produced by metal precursor deposition on exoelectrogen bacteria and pyrolyzing |
| US11701639B2 (en) | 2018-08-06 | 2023-07-18 | King Abdullah University Of Science And Technology | Single metal atom or bimetallic alloy heterogeneous catalysts on a carbonaceous support produced by metal precursor deposition on exoelectrogen bacteria and pyrolyzing |
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