CN109772462A - A kind of natural sponge preparation method loading gold silver nanometer particle and its application in terms of catalytic degradation azobenzene pollutant - Google Patents
A kind of natural sponge preparation method loading gold silver nanometer particle and its application in terms of catalytic degradation azobenzene pollutant Download PDFInfo
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- CN109772462A CN109772462A CN201910070668.6A CN201910070668A CN109772462A CN 109772462 A CN109772462 A CN 109772462A CN 201910070668 A CN201910070668 A CN 201910070668A CN 109772462 A CN109772462 A CN 109772462A
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Abstract
The present invention relates to a kind of natural sponge preparation method for loading gold silver nanometer particle and its in the application of efficient catalytic azobenzene.Natural sponge first passes around the pretreatment hydrolysis of alkali, remove the tissue squame on sponge fiber surface, in favor of the load of nano particle and the stabilization of catalytic performance, then upper gold or silver nano-grain are loaded under optimum conditions, a kind of sponge composite material structure that novel injection-extrusion reaction form will load nano particle is used as a kind of deformable reaction vessel of included catalysis, also sponge composite material can be filled in continuous flow reaction system, realize the continuous catalysis conversion of reactant, to realize that the efficient catalytic to azobenzene pollutant in water environment is degraded.
Description
Technical field
The present invention relates to water pollution process fields, and in particular to a kind of natural sponge preparation side for loading gold silver nanometer particle
Method and its application in terms of catalytic degradation azobenzene pollutant.
Background technique
It is several most kinds, including acidity, mordant dyeing, activity, cation, neutral dye that azo dyes, which is in synthetic dyestuffs,
Material, disperse dyes etc..Account for the 80% of organic dyestuff product population.Chromatography is complete.Most azo dyes are aromatic amines through weight
It is coupled after nitridation with phenols, aromatic amine, active methylene compound.After absorption, make by the activation of human body
With the structure for changing DNA, causes the lesion of human body and induce cancer.Its chemical property is more stable, and waste component is complicated, therefore even
Nitrogen waste water from dyestuff is the high concentrated organic wastewater of generally acknowledged refractory reason.
There are mainly three types of method for treating wastewater of azo dye, physical method: natural sedimentation method, filtration method, absorption method, centrifugation point
From method, it is therefore an objective to remove big sand, solids Soft flocks；Chemical method: neutralisation, coacervation (flocking settling method, cohesion buoyance lift method),
Oxidizing process (aeration oxidation process, oxidizing method)；Biochemical method: activated sludge process, biological filter process, anaerobic digestion, oxidation
Useless Organic substance in water is decomposed by microorganism and is removed by pool method.Applying in physical treatment process at most is absorption method, at present work
It the use of more adsorbent is granular active carbon and activated silica diatomaceous earth and resin in industry.Studies have shown that active carbon is most of dye
The best adsorbent of material (containing azo dyes), but its regeneration is difficult, it is at high cost.Chemical method is always the main of dye wastewater treatment
Method, in recent years, the technologies such as photochemical catalytic oxidation, electrolytic oxidation, light electrolysis oxidation also have certain research, ferric trichloride and ferric sulfate
Mixture and aluminum sulfate can be used to handle containing even waste water from dyestuff.
Therefore, the nano-catalytic agent carrier with efficient mass transfer is developed, and is applied to azobenzene pollutant effluents
Improvement is of great significance.In addition, efficient mass transfer carrier is developed further into the packing type catalysis for continuous flow reaction system
Agent, it can be achieved that pollutant effluents continuous improvement.
Summary of the invention
It is an object of the present invention to provide a kind of natural sponge preparation method for loading gold silver nanometer particle, party's legal systems
Gold/silver nanoparticle catalyst carrier the resistance to mass tranfer obtained is low, replacement is convenient and nano particle can be fully used.
It is a further object of the present invention to provide a kind of gold/silver nanoparticle catalyst carriers of above method preparation in efficient catalytic
Application in water environment of degrading in terms of azobenzene pollutant.
The purpose of the present invention is realized by following scheme:
The present invention is with natural sponge for carrier loaded gold silver nanometer particle, comprising the following steps:
(1) natural sponge pre-processes, detailed process are as follows: take the sponge of certain mass several, at certain density NaOH
Reason liquid handles the different time respectively at a certain temperature, and after treatment is cleaned 5 times or more with ultrapure water.
(2) prepared by gold silver nanometer particle, detailed process are as follows: the sponge of different pretreatments type is immersed in preference temperature one
Determine to place 1 hour in the chlorauric acid solution or silver nitrate solution of given volume concentration.Then with ultrapure water clean 3 times with
On, unbonded metal precursor is washed away, the sponge for having chelated metal precursor is placed on certain density sodium borohydride under stiring
In ten minutes, to grow gold silver nanometer particle in sponge fiber.It is cleaned later with ultrapure water and has loaded gold silver nanometer particle
Sponge 5 times or more with spare.
The concentration of NaOH treatment fluid is 0.1M in step (1), and preference temperature is 60 DEG C, is generally placed upon in insulating box and controls
60 DEG C of constant temperature.
The concentration of gold chloride is 2mM in step (2), and the concentration of silver nitrate is 5mM, and the concentration of sodium borohydride is 0.1mM,
Preference temperature is 30 DEG C, is generally placed upon in water bath with thermostatic control and controls 30 DEG C of constant temperature.
What it is the present invention also provides a kind of preparation of above scheme is carrier loaded gold silver nanometer particle to water ring with natural sponge
The application that azobenzene pollutant efficient catalytic is degraded in border.Wherein, the azobenzene pollutant is methyl orange.
In this application, the azobenzene pollutant solution is injected into load has gold/silver nano-grain natural
On sponge, the ratio of the two is 1:10~1:100 (volume: quality), stops reaction, extrusion solution after 10-30s.Wherein, described
Azobenzene pollutant solution concentration is 0.1-10mM.
In this application, also gold/silver nano-grain natural sponge is filled in chromatographic column, is compacted with quartz sand, it will
Azobenzene pollutant solution adds reaction system above chromatographic column, opens the vacuum filtration system of connection, allows azobenzene
Pollutant flows through load solution-stabilizedly has gold/silver nano-grain natural sponge to be reacted.Wherein, the azobenzene is dirty
Dye object solution concentration is 0.1-10mM.
Compared with existing supported nanoparticles, the present invention has the advantages that
(1) there is compression can restore in shape and have biocompatibility for natural sponge materials, and porous structure is conducive to
Reduce diffusional resistance；
(2) three dimensional scaffold structure of natural sponge is conducive to the growth of nano particle and making full use of for space；
(3) solution is filled in that natural sponge fiber extends and tubercle is built-up, among the micropore that interconnects, can be direct
It is contacted with the nanocatalyst on sponge fiber surface, to weaken influence of the diffusional resistance to rate of catalysis reaction.
Detailed description of the invention
Fig. 1 is the surface sweeping electron microscopic picture of the natural sponge of 5 alkali process of natural sponge and embodiment；
Fig. 2 is the transmission electron microscope picture of the gold nano grain of 2 natural sponge of embodiment load growth；
Fig. 3 is the transmission electron microscope picture of the gold nano grain of natural sponge load growth after 2 alkali process of embodiment；
Fig. 4 be embodiment 1 prepare Jenner's nano composite material in injection-extrusion reaction system to methyl orange continuous catalysis
The conversion ratio of reaction-cycle-index figure.
Specific embodiment
In the present invention, natural sponge first passes around alkali process hydrolysis, then loads upper gold or silver nanoparticle under optimum conditions
Particle uses the sponge composite material structure that the novel injection-extrusion reaction form of one kind will load nano particle as one
Sponge composite material, can also be filled in continuous flow reaction system by the deformable reaction vessel of the included catalysis of kind, realize
The continuous catalysis of reactant converts, to realize that the efficient catalytic to azobenzene pollutant in water environment is degraded.
Research object is prepared as with gold/silver nano-grain below, to method of the invention and is answered by specific embodiment
With being described in detail.
Embodiment 1:
Specific steps are as follows:
(1) natural sponge pre-processes:
Take 10mg natural sponge, with the NaOH treatment fluid of 0.1M at 60 DEG C by its respective pretreatment 0h, 1h, 2h, 3h,
4h, 5h are directly cleaned 5 times with ultrapure water after processing.
(2) prepared by silver nano-grain:
Above-mentioned pretreated natural sponge is separately immersed in the chlorauric acid solution of 20ml, 3mM or the nitre of 20ml, 6mM
In sour silver solution, places 1 hour, kept for 30 DEG C of constant temperature.Then it is cleaned 3 times with ultrapure water, washes away unbonded metal precursor,
The sponge for having chelated metal precursor is placed in the sodium borohydride of 0.1mM 10 minutes under stiring, to be grown in sponge fiber
Gold/silver nano-grain.It is cleaned gold-supported/silver nano-grain sponge 5 times with ultrapure water later, it is spare.
For the present embodiment effect picture as shown in figure 4, after alkali process 4h, the natural sponge performance of load gold nano grain is more steady
Fixed, catalytic degradation effect is more preferably.
Embodiment 2:
Specific steps are as follows:
(1) natural sponge pre-processes:
10mg natural sponge is taken, pre-processes 4h at 60 DEG C with the NaOH treatment fluid of 0.01M, 0.1M, 0.2M respectively, is handled
It is directly cleaned 6 times with ultrapure water afterwards.
(2) prepared by silver nano-grain:
Natural sponge after above-mentioned pretreatment 4h is separately immersed in the chlorauric acid solution or 20ml, 6mM of 20ml, 3mM
It in silver nitrate solution, places 1 hour, is kept for 30 DEG C of constant temperature.Then it is cleaned 3 times with ultrapure water, washes away unbonded metal precursor,
The sponge for having chelated metal precursor is placed in the sodium borohydride solution of 0.1mM 10 minutes under stiring, in sponge fiber
Grow gold silver nanometer particle.Sponge 6 times for having loaded gold silver nanometer particle are cleaned with ultrapure water later.
The present embodiment effect picture is as shown in Figures 2 and 3, the gold nano grain partial size that natural sponge loads after alkali process point
Cloth is relatively narrow, average grain diameter is also smaller, shows that natural sponge after alkali process is more advantageous to the growth of nano particle.
Embodiment 3:
Specific steps are as follows:
(1) natural sponge pre-processes:
10mg natural sponge is taken, is pre-processed 4h at 40 DEG C, 60 DEG C, 80 DEG C respectively with the NaOH treatment fluid of 0.1M,
It is directly cleaned 5 times with ultrapure water after processing.
(2) prepared by silver nano-grain:
Natural sponge after pretreatment 4h is separately immersed in the chlorauric acid solution of 20ml, 3mM or the nitric acid of 20ml, 6mM
It in silver-colored solution, places 1 hour, is kept for 30 DEG C of constant temperature.Then it is cleaned 3 times with ultrapure water, washes away unbonded metal precursor, it will
The sponge for having chelated metal precursor is placed in the sodium borohydride of 0.1mM 10 minutes under stiring, to grow gold in sponge fiber
Silver nano-grain.Sponge 5 times for having loaded gold silver nanometer particle are cleaned with ultrapure water later.
The present embodiment has inquired into the influence that NaOH treatment temperature grows gold silver nanometer particle, the results showed that 60 DEG C of processing temperature
The growth of degree treated natural sponge is more advantageous to nano particle.
Embodiment 4:
Specific steps are as follows:
(1) natural sponge pre-processes:
10mg natural sponge is taken, handles 4h at 60 DEG C with the NaOH treatment fluid of 0.1M, it is directly clear with ultrapure water after processing
It washes 5 times.
(2) prepared by silver nano-grain:
By pre-process 4h after natural sponge be immersed in 20ml, 3mM chlorauric acid solution or 20ml, 6mM silver nitrate it is molten
1 hour in liquid, control disposition temperature is 20 DEG C, 30 DEG C, 40 DEG C respectively.Then it is cleaned 3 times with ultrapure water, washes away unbonded gold
Belong to precursor, the sponge for having chelated metal precursor is placed in the sodium borohydride of 0.1mM 10 minutes under stiring, in sponge fiber
Upper growth gold silver nanometer particle.Sponge 6 times for having loaded gold silver nanometer particle are cleaned with ultrapure water later.
The present embodiment has inquired into the influence that load temperature grows gold silver nanometer particle, the results showed that under 30 DEG C of load temperatures
Natural sponge is more advantageous to the growth of nano particle.
Embodiment 5:
Specific steps are as follows:
(1) natural sponge pre-processes:
10mg natural sponge is taken, 4h is processed at 60 DEG C with the NaOH treatment fluid of 0.1M, directly with ultrapure after processing
Water cleans 5 times.
(2) prepared by gold nano grain:
Natural sponge after pretreatment 4h is separately immersed in the chlorauric acid solution that 20ml concentration is respectively 1mM, 3mM, 5mM
Or concentration is to place 1 hour in the silver nitrate solution of 6mM, is kept for 30 DEG C of constant temperature.Then it is cleaned 4 times, is washed away not with ultrapure water
In conjunction with metal precursor, the sponge for having chelated metal precursor is placed in the sodium borohydride of 0.1mM 10 minutes under stiring, with
Gold silver nanometer particle is grown in sponge fiber.Sponge 5 times for having loaded gold silver nanometer particle are cleaned with ultrapure water later.
The present embodiment effect picture is as shown in Figure 1, after alkali process, and the three dimensional scaffold structure and surface chemical composition of sponge are simultaneously
Do not change significantly, by from the elemental analysis of XPS it is known that O constituent content increase F constituent content subtracts after alkali process
It is few, to be more advantageous to the load of gold/silver nano-grain.
Embodiment 6:
Specific steps are as follows:
(1) natural sponge pre-processes:
10mg natural sponge is taken, 4h is processed at 60 DEG C with the NaOH treatment fluid of 0.1M, directly with ultrapure after processing
Water cleans 5 times.
(2) prepared by silver nano-grain:
By pre-process 4h after natural sponge be separately immersed in the chlorauric acid solution of 20ml, 3mM or concentration be respectively 3mM,
It in the silver nitrate solution of 6mM, 8mM, places 1 hour, is kept for 30 DEG C of constant temperature.Then it is cleaned 3 times, is washed away unbonded with ultrapure water
Metal precursor, the sponge for having chelated metal precursor is placed in the sodium borohydride of 0.1mM 10 minutes under stiring, in sponge
Gold silver nanometer particle is grown on fiber.Sponge 5 times for having loaded gold silver nanometer particle are cleaned with ultrapure water later.
The present embodiment has inquired into the influence that silver nitrate concentration grows gold silver nanometer particle, the results showed that the silver nitrate of 6mM
Natural sponge is more advantageous to the growth of nano particle after solution processing.
Embodiment 7:
Specific steps are as follows:
(1) natural sponge pre-processes:
10mg natural sponge is taken, 4h is processed at 60 DEG C with the NaOH treatment fluid of 0.1M, directly with ultrapure after processing
Water cleans 5 times.
(2) prepared by silver nano-grain:
By pre-process 4h after natural sponge be immersed in 20ml, 3mM chlorauric acid solution or 20ml, 6mM silver nitrate it is molten
It is placed respectively in liquid 0.5h, 1,2h, 3h, 5h hours, is kept for 30 DEG C of constant temperature.Then it is cleaned 3 times, is washed away unbonded with ultrapure water
Metal precursor, the sponge for having chelated metal precursor is placed in the sodium borohydride of 0.1mM 10 minutes under stiring, in sponge
Gold silver nanometer particle is grown on fiber.Sponge 5 times for having loaded gold silver nanometer particle are cleaned with ultrapure water later.
The present embodiment has inquired into the influence grown to gold silver nanometer particle the load liquid processing time, the results showed that at load liquid
Natural sponge after reason 5h is more advantageous to the growth of nano particle.
Embodiment 8:
Specific steps are as follows:
(1) natural sponge pre-processes:
10mg natural sponge is taken, 4h is processed at 60 DEG C with the NaOH treatment fluid of 0.1M, directly with ultrapure after processing
Water cleaning 5 times or more.
(2) prepared by silver nano-grain:
Natural sponge after pretreatment 4h is separately immersed in the chlorauric acid solution of 20ml, 3mM or the nitric acid of 20ml, 6mM
It in silver-colored solution, places 1 hour, is kept for 30 DEG C of constant temperature.Then it is cleaned 3 times with ultrapure water, washes away unbonded metal precursor, by chela
The sponge for having closed metal precursor is individually placed in the sodium borohydride of 0.01mM, 0.1mM, 0.2mM 10 minutes under stiring, in sea
Gold silver nanometer particle is grown on cotton fiber.Sponge 6 times for having loaded gold silver nanometer particle are cleaned with ultrapure water later.
The present embodiment has inquired into the influence that NaBH4 concentration grows gold silver nanometer particle, the results showed that the NaBH4 of 0.1mM
Natural sponge is more advantageous to the growth of nano particle after concentration processing.
Embodiment 9:
Specific steps are as follows:
(1) natural sponge pre-processes:
10mg natural sponge is taken, 4h is processed at 60 DEG C with the NaOH treatment fluid of 0.1M, directly with ultrapure after processing
Water cleans 6 times.
The surface sweeping electron microscopic picture of natural sponge (a) and the natural sponge (b) of alkali process is as shown in Figure 1, it can be seen that at alkali
The three dimensional scaffold structure of sponge changes there is no apparent after reason.
(2) prepared by gold nano grain:
Natural sponge after pretreatment 4h is separately immersed in the chlorauric acid solution or 20ml concentration point that 20ml concentration is 3mM
It Wei not place 1 hour in the silver nitrate solution of 3mM, 6mM, 8mM, be kept for 30 DEG C of constant temperature.Then it is cleaned 4 times, is washed with ultrapure water
Unbonded metal precursor is removed, the sponge for having chelated metal precursor is placed in the sodium borohydride solution of 0.1mM under stiring and is divided
Other places are managed 5,10,20,30 minutes, to grow gold silver nanometer particle in sponge fiber.Gold-supported is cleaned with ultrapure water later
The sponge of silver nano-grain 5 times, it is spare.
The present embodiment has inquired into the influence grown to gold silver nanometer particle the NaBH4 processing time, the results showed that NaBH4 processing
Time does not have much affect to the load growth of nano particle.
It is characterized with pattern of the high power transmission electron microscope to load nano particle, the table with XPS and FTIR to nano material
Face physicochemical properties are characterized, measure golden or silver element content in composite material with ICP-OES, and a series of tables are passed through
Sign means can be known handle natural sponge 4h at 60 DEG C with 0.1M concentration NaOH treatment fluid after, the gold silver nanometer particle of preparation
Pattern, performance and gold and silver load capacity are best.
The surface sweeping electron microscopic picture of natural sponge and the natural sponge of alkali process is as shown in Figure 1；Natural sponge load growth
The transmission electron microscope picture of gold nano grain is as shown in Figure 2；Natural sponge after alkali process loads the saturating of the gold nano grain of growth
It is as shown in Figure 3 to penetrate electron microscopic picture, it can be seen that the gold nano grain particle diameter distribution that natural sponge loads after alkali process is relatively narrow, flat
Equal partial size is also smaller, and the pretreatment for showing alkali plays in nano particle forming process adjusts nucleation simultaneously as stabilizer
Conducive to the growth of nano particle.
Alkali process natural sponge gold-supported/silver nano-grain composite material catalytic performance see the table below compared with reported in the literature:
Gold/silver changes of contents in (injection-extrusion molding the repeats 20 times) composite material of reaction front and back:
As seen from the above table, the present invention, on the one hand can more preferably more using natural sponge as gold/silver nano-grain load
Gold/silver nano-grain in stable load, on the other hand its to the catalytic degradation effect of azobenzene pollutant more preferably.
The application of load type gold silver nano-grain efficient catalytic degradation azobenzene pollutant of the present invention, concrete operations are such as
Under:
(1) repeated injection-extrusion Catalysis experiments
In the Catalysis experiments of methyl orange, 1mL reaction solution, which is injected into load prepared by 50mg embodiment 8, gold/silver
In the natural sponge of nano particle, extrusion solution after 60s tests its UV-vis absorption spectrum.
Reaction solution is by 750mL methyl orange (3mM) and 1mL sodium borohydride (0.3M) and 7mL water mixed preparing；
(2) filtration catalytic is tested
By (natural sponge pre-processes 4h, and loads the sponge of upper gold or silver nano-grain) on 500mg advanced composite material (ACM)
It is filled in chromatographic column, is compacted with quartz sand.It include 2.25mL methyl orange (3mM), 3mL sodium borohydride (0.3M) and 21mL water
Reaction solution reaction system is added above chromatographic column, open the vacuum filtration system of connection, the stream of reaction solution, that is, stable
The advanced composite material (ACM) for crossing filling starts to react.After each filtration catalytic, take filtered fluid test ultraviolet-visible absorption spectroscopy in terms of
Calculate the conversion ratio of 4-NP.
Be Jenner's nano composite material prepared by the present invention in injection-extrusion reaction system to K2Cr2O7Continuous catalytic reaction
Conversion ratio-cycle-index figure it is as shown in Figure 4, it can be seen that gold nano composite material continuous use 20 times after still maintain steady
Fixed catalytic activity.
Reaction condition, gold/silver nano-grain load capacity and the rate of catalysis reaction respectively reacted in above-described embodiment 1-9 see the table below:
NaOH treatment fluid concentration, NaOH treatment temperature, NaOH processing time, load temperature, chlorine gold from the data in the table
The conditions such as acid concentration, silver nitrate concentration, load liquid processing time, NaBH4 concentration, NaBH4 processing time are for gold/silver nanoparticle
Load capacity and rate of catalysis reaction of the grain on natural sponge have a degree of influence, and the present invention is found by control variable
To the optimum process condition of gold/silver nano-grain growth, and by designing novel catalytic reaction form, to verify it efficient steady
Determine the performance of catalytic degradation azobenzene pollutant.
Above specific embodiment has carried out specific description, but content of the present invention to method of the invention
Be not restricted to the above case study on implementation, if in without departing from main scope of the invention, can to experiment condition and method into
The flexible change of row, these are all within the scope of protection of the present invention.Therefore, the invention patent and protection scope should be with appended rights
Subject to claim.
Claims (8)
1. a kind of natural sponge preparation method for loading gold silver nanometer particle, it is characterised in that the following steps are included:
(1) natural sponge pre-processes: the natural sponge of certain mass is taken, with the NaOH solution of 0.01~0.2M at 40~80 DEG C
0~5h is managed, after treatment cleaned at least 5 times with ultrapure water, wherein the quality of the natural sponge is with can be molten by the NaOH
Subject to liquid did not had；
(2) gold-supported/silver nano-grain: at 20~40 DEG C, by the chlorine gold of step (1) treated sponge is immersed in 1~5mM
Then 0.5~5 hour in the silver nitrate solution of acid solution or 3~8mM is cleaned at least 3 times with ultrapure water, is washed away unbonded
Metal precursor, the sponge for having chelated metal precursor is placed on 5 in the sodium borohydride solution of 0.01~0.2mM under agitation
~30 minutes, to grow gold silver nanometer particle in sponge fiber, gold-supported/silver nano-grain was cleaned with ultrapure water later
Sponge at least 5 times.
2. according to the method described in claim 1, it is characterized by: in step (1), the concentration of the NaOH solution is
0.1M, treatment temperature are 60 DEG C, and the processing time is 4h.
3. according to the method described in claim 1, it is characterized by: in step (2), the concentration of the chlorauric acid solution is
2mM, the concentration of the silver nitrate solution are 5mM, and the concentration of the sodium borohydride solution is 0.1mM, and treatment temperature is 30 DEG C.
4. the load of method preparation according to any one of claim 1-3 has gold/silver nano-grain natural sponge to exist
Application in efficient catalytic degradation water environment in terms of azobenzene pollutant.
5. application according to claim 4, it is characterised in that: the azobenzene pollutant solution is injected into load
Have on gold/silver nano-grain natural sponge, the ratio of the two is 1:10~1:100 (volume: quality), is stopped after 10-30s anti-
It answers, extrusion solution.
6. application according to claim 5, it is characterised in that: the azobenzene pollutant solution concentration is 0.1-
10mM。
7. application according to claim 4, it is characterised in that: gold/silver nano-grain natural sponge is filled in chromatography
It in column, is compacted with quartz sand, azobenzene pollutant solution is added into reaction system above chromatographic column, opens the vacuum of connection
Suction filtration system, allowing azobenzene pollutant to flow through load solution-stabilizedly has gold/silver nano-grain natural sponge to be reacted.
8. application according to claim 7, it is characterised in that: the azobenzene pollutant solution concentration is 0.1-
10mM。
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Application publication date: 20190521 |