CN104357485B - A kind of method that utilization sulfate reducing bacteria prepares Ag/AgCl visible light catalysts - Google Patents
A kind of method that utilization sulfate reducing bacteria prepares Ag/AgCl visible light catalysts Download PDFInfo
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- CN104357485B CN104357485B CN201410642288.2A CN201410642288A CN104357485B CN 104357485 B CN104357485 B CN 104357485B CN 201410642288 A CN201410642288 A CN 201410642288A CN 104357485 B CN104357485 B CN 104357485B
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- reducing bacteria
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Abstract
A kind of method that utilization sulfate reducing bacteria prepares Ag/AgCl visible light catalysts, is related to a kind of preparation method of Ag/AgCl visible light catalysts.The present invention is to solve the Ag/AgCl photochemical catalysts of existing chemical method synthesis very big, the problem of stability is poor that there is grain diameter.Method：First, sulfate reducing bacteria is inoculated into the anaerobism of the Starkey culture mediums containing improvement bottle, nutrient solution is cultivated to obtain in 37 DEG C of constant incubator；2nd, AgNO is added into nutrient solution3Solution lucifuge culture under the conditions of 37 DEG C；3rd, ultrasonication is carried out to cultured mixed-culture medium；4th, the mixed-culture medium centrifugation after ultrasonication, takes the supernatant after centrifugation to centrifuge again, collects precipitation, that is, obtain Ag/AgCl visible light catalysts.Visible light catalyst shape prepared by the inventive method is homogeneous, and particle diameter distribution is narrow, is difficult to reunite.For preparing Ag/AgCl visible light catalysts.
Description
Technical field
The present invention relates to a kind of preparation method of Ag/AgCl visible light catalysts.
Background technology
Conductor photocatalysis material has the ability that catalytic oxidation-reduction reacts, being capable of fully oxidized decomposition organic contamination
Thing, reducing heavy metal ion, are usually used in organic pollution in processing waste water, waste gas.Therefore, conductor photocatalysis degradation technique is
Solve the effective way of problem of environmental pollution.In different semiconductor light-catalysts, titanium dioxide due to good optics and
Characteristic electron has been widely studied.However, titanium dioxide is a kind of wide bandgap semiconductor materials, ultraviolet light can only be absorbed, is caused
Solar spectrum utilization rate is low.Therefore a kind of semiconductor light-catalyst with high visible light catalytic activity is searched out as a weight
The research topic wanted.
It has recently been demonstrated that metal composite nano particle is due to its unique surface plasma resonance (Surface
Plasmon resonance, SPR) effect, with excellent visible light catalytic performance, it can be used as high efficiency photocatalyst.At present,
The research of silver and silver halide composite nanometer particle (such as Ag/AgCl) is widely paid close attention to, and has successfully developed a variety of Ag/
AgCl photochemical catalysts.The conventional preparation method of Ag/AgCl visible light catalysts is generally chemical method, in chemical reaction process, Ag+
AgCl precipitations are quickly generated with Cl-, the nano particle diameter of gained is very big, and stability is poor, and pattern also is difficult to control.And bioanalysis
Simple to operate, reaction is gentle, environmental protection, and the nano particle shape synthesized is homogeneous, and particle diameter is small, and stability is good.It is reported that
Some bacteriums, fungi or plant powder can synthesize Ag/AgCl visible light catalysts.However, synthesizing Ag/AgCl on anaerobic bacteria
The research of visible light catalyst is domestic, and there is not been reported.
The content of the invention
There is grain diameter the present invention is to solve the Ag/AgCl photochemical catalysts of existing chemical method synthesis very big, it is stable
Property difference the problem of there is provided a kind of method that utilization sulfate reducing bacteria prepares Ag/AgCl visible light catalysts.
The method that the present invention prepares Ag/AgCl visible light catalysts using sulfate reducing bacteria, is carried out according to the following steps：
First, sulfate reducing bacteria Garciella sp.wxz01 are inoculated into detesting for the Starkey culture mediums containing improvement
In oxygen bottle, quiescent culture 5 days, obtain nutrient solution in 37 DEG C of constant incubator；
2nd, 0.1M AgNO is added into nutrient solution3Solution lucifuge culture 15 days under the conditions of 37 DEG C；
Three then using ultrasonic cell disruption instrument to cultured mixed-culture medium carry out ultrasonication, running parameter
Ultrasonic 15s is set to, 5s, 0 DEG C of temperature, power 80% is spaced；
4th, the mixed-culture medium after ultrasonication centrifuges 4~6min under conditions of 4000~6000rpm, takes after centrifugation
Supernatant centrifuge 9~11min again under 13000~15000rpm, collect precipitation, that is, obtain Ag/AgCl visible light catalytics
Agent.
Ag/AgCl visible light catalyst shapes prepared by the inventive method are homogeneous, and particle diameter distribution is narrow, are difficult to reunite.This hair
It is bright that there is low cost, efficiency high, be simple to operate and friendly to environment, suitable for industrialized production.The present invention is in preparation process
Any surfactant, protective agent and crosslinking agent are not used.The present invention prepares Ag/AgCl visible light catalysts and can be used in preparing
Various catalysis materials, applied to solar cell, photocatalytic degradation field etc..
Brief description of the drawings
The Ag/AgCl nano particle transmission electron microscope figures that Fig. 1 is prepared for experiment 1；The Ag/ that Fig. 2 is prepared for experiment 1
The X-ray diffractogram of AgCl nano particles.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition between each embodiment
Any combination.
Embodiment one：Present embodiment prepares the side of Ag/AgCl visible light catalysts using sulfate reducing bacteria
Method, is carried out according to the following steps：
First, sulfate reducing bacteria Garciella sp.wxz01 are inoculated into detesting for the Starkey culture mediums containing improvement
In oxygen bottle, quiescent culture 5 days, obtain nutrient solution in 37 DEG C of constant incubator；
2nd, 0.1M AgNO is added into nutrient solution3Solution lucifuge culture 15 days under the conditions of 37 DEG C；
Three then using ultrasonic cell disruption instrument to cultured mixed-culture medium carry out ultrasonication, running parameter
Ultrasonic 15s is set to, 5s, 0 DEG C of temperature, power 80% is spaced；
4th, the mixed-culture medium after ultrasonication centrifuges 4~6min under conditions of 4000~6000rpm, takes after centrifugation
Supernatant centrifuge 9~11min again under 13000~15000rpm, collect precipitation, that is, obtain Ag/AgCl visible light catalytics
Agent.
Embodiment two：Present embodiment from unlike embodiment one：Sulfate described in step one
Reducing bacteria Garciella sp.wxz01 are isolated from Daqing oil field oil recovery factory oil-polluted water, are deposited in Chinese micro- life
Thing culture presevation administration committee common micro-organisms center, preservation address is the institute 3 of Chaoyang District, Beijing City Beichen Lu 1, preservation
Date is on July 3rd, 2014, and deposit number is CGMCC No：9410.It is other identical with embodiment one.
Embodiment three：Present embodiment from unlike embodiment one or two：Added in step 2
AgNO3The volume ratio of solution and nutrient solution is 1:100.It is other identical with embodiment one or two.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Surpass in step 4
Mixed-culture medium after sound is broken centrifuges 5min under conditions of 5000rpm.Other phases one of with embodiment one to three
Together.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Take after centrifugation
Supernatant centrifuges 10min again under 14000rpm.It is other identical with one of embodiment one to four.
Experiment 1：
The method that this experiment prepares Ag/AgCl visible light catalysts using sulfate reducing bacteria, is carried out according to the following steps：
The first, sulfate reducing bacteria Garciella sp.wxz01 are inoculated into the Starkey culture mediums improved containing 100mL
Anaerobism bottle in, quiescent culture 5 days, obtain nutrient solution in 37 DEG C of constant incubator；
2nd, 1mL 0.1M AgNO is added into nutrient solution3Solution lucifuge culture 15 days under the conditions of 37 DEG C；
3rd, ultrasonication is carried out to cultured mixed-culture medium using ultrasonic cell disruption instrument, running parameter is set
For ultrasonic 15s, 5s, 0 DEG C of temperature, power 80% are spaced；
4th, the mixed-culture medium after ultrasonication centrifuges 5min under conditions of 5000rpm, takes the supernatant after centrifugation to exist
10min is centrifuged under 14000rpm again, precipitation is collected, that is, obtains Ag/AgCl visible light catalysts.
Sulfate reducing bacteria Garciella sp.wxz01 described in step one are from Daqing oil field oil recovery factory oil-polluted water
In it is isolated, be deposited in China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC), preservation address
It is the institute 3 of Chaoyang District, Beijing City Beichen Lu 1, preservation date is on July 3rd, 2014, and deposit number is CGMCC No：9410.
The mixed-culture medium of lucifuge culture 15 days in step 2 is centrifuged into 10min under conditions of 7000r/min, collected
The bacterial sediment arrived, it is right in the acetone that concentration is respectively 50%, 70%, 90%, 100% after fixing 2h through 2.5% glutaraldehyde
Sample is dehydrated.Then, sample is placed on 37 DEG C of oven overnights.By sample, taking-up is repaired with treating block machine from incubator, exposure
Go out tissue, then exposed tissue accomplished 45 degree of angles with treating block machine.After being embedded in epoxy resin medium, what is trimmed
Tissue block is cut into thickness for 0.5~1.0 μm, maximum section area 2mm2Ultra-thin section.Section is positioned in the coated copper of carbon
On the net.Ultra-thin section is dyed with 3% acetic acid uranium, and with lead citrate detect cell ultra microstructure.Utilize H-7650
Type transmission electron microscope (Japanese HITACHI companies) observes pattern, and accelerating potential is 80KV.As shown in figure 1, the Ag/ of synthesis
AgCl visible light catalysts are in spherical substantially, are dispersed in around thalline, and particle diameter is in 10~50nm.
The XRD analysis of Ag/AgCl visible light catalysts：
Step 4 is centrifuged into 10min again under 14000rpm, obtained precipitation sterile water wash 2-3 times is collected, puts
In air dry oven drying.After being completely dried, collect desciccate and be put into Muffle furnace, 400 DEG C of calcinings 1h, burning-off Ag/AgCl
The biomass on visible light catalyst surface simultaneously grinds to form fine powder.Using Bruker D8 types x-ray diffractometer (Germany
Bruker companies) carry out XRD signs.X-ray powder diffraction instrument is using CuKa as radiation source, and X-ray is 1.6KW by power
The copper X-ray pipe of (40KV, 40mM) is produced.Measured between 2 θ are 25-90 degree.As shown in Fig. 2 the θ values of gained spectrum 2
Peak value is at 38.116 °, 44.277 °, 64.426 ° and 77.472 °, and Ag is observed in correspondence (111), (200), (220) and (311) face
The presence of diffraction pattern；At 27.831 °, 32.243 °, 46.233 °, 54.828 °, 57.478 °, 67.471 °, 74.471 ° and
Observe AgCl diffraction maximums in 76.734 ° of correspondence (111), (200), (220), (311), (222), (400), (311) and (420) faces
Presence.This further demonstrates synthesized Ag/AgCl visible light catalysts using bacterial strain Garciella sp.wxz01.
Claims (4)
1. a kind of method that utilization sulfate reducing bacteria prepares Ag/AgCl visible light catalysts, it is characterised in that this method press with
Lower step is carried out：
The first, sulfate reducing bacteria Garciella sp.wxz01 are inoculated into the anaerobism bottle of the Starkey culture mediums containing improvement
In, quiescent culture 5 days, obtain nutrient solution in 37 DEG C of constant incubator；
2nd, 0.1M AgNO is added into nutrient solution3Solution lucifuge culture 15 days under the conditions of 37 DEG C；
Three then using ultrasonic cell disruption instrument to cultured mixed-culture medium carry out ultrasonication, running parameter set
For ultrasonic 15s, 5s, 0 DEG C of temperature, power 80% are spaced；
4th, the mixed-culture medium after ultrasonication centrifuges 4~6min under conditions of 4000~6000rpm, takes upper after centrifugation
Clear liquid centrifuges 9~11min again under 13000~15000rpm, collects precipitation, that is, obtains Ag/AgCl visible light catalysts；
Sulfate reducing bacteria Garciella sp.wxz01 wherein described in step one are deposited in Chinese microorganism strain preservation pipe
Reason committee common micro-organisms center, preservation address is the institute 3 of Chaoyang District, Beijing City Beichen Lu 1, and preservation date is 2014 7
The moon 3, deposit number is CGMCC No：9410.
2. the method that a kind of utilization sulfate reducing bacteria according to claim 1 prepares Ag/AgCl visible light catalysts, its
It is characterised by the AgNO added in step 23The volume ratio of solution and nutrient solution is 1:100.
3. the method that a kind of utilization sulfate reducing bacteria according to claim 1 prepares Ag/AgCl visible light catalysts, its
It is characterised by step 4 that the mixed-culture medium after ultrasonication centrifuges 5min under conditions of 5000rpm.
4. the method that a kind of utilization sulfate reducing bacteria according to claim 1 prepares Ag/AgCl visible light catalysts, its
It is characterised by taking the supernatant after centrifugation to centrifuge 10min again under 14000rpm.
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Citations (3)
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|---|---|---|---|---|
| CN101602109A (en) * | 2009-06-15 | 2009-12-16 | 中北大学 | A kind of preparation method of silver nano material |
| CN102888428A (en) * | 2011-07-21 | 2013-01-23 | 中国科学院过程工程研究所 | Method for synthesizing nano silver by utilizing Bacillus amyloliquefaciensBacillus amyloliquefaciens LSSE-62 |
| CN103642844A (en) * | 2013-12-13 | 2014-03-19 | 东北林业大学 | Method for preparing nano silver particles by reducing in bacillus thallus |
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2014
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602109A (en) * | 2009-06-15 | 2009-12-16 | 中北大学 | A kind of preparation method of silver nano material |
| CN102888428A (en) * | 2011-07-21 | 2013-01-23 | 中国科学院过程工程研究所 | Method for synthesizing nano silver by utilizing Bacillus amyloliquefaciensBacillus amyloliquefaciens LSSE-62 |
| CN103642844A (en) * | 2013-12-13 | 2014-03-19 | 东北林业大学 | Method for preparing nano silver particles by reducing in bacillus thallus |
Non-Patent Citations (3)
| Title |
|---|
| Nitrate reductase-mediated synthesis of silver nanoparticles from AgNO3;S. Anil Kumar等;《Biotechnology Letters》;Springer;20070331;第29卷(第3期);第439页摘要，第440页第1及最后1段，第441页左栏第4段-第442页右栏第3段 * |
| Nitrite reductase activity of sulphate-reducing bacteria prevents their inhibition by nitrate-reducing, sulphideoxidizing bacteria;E. A. Greene等;《Environmental Microbiology》;Wiley;20030731;第5卷(第7期);第607页摘要倒数第4行 * |
| 大庆油田地面***的硫酸盐还原菌的分离与鉴定;魏利等;《湖南科技大学学报（自然科学版）》;20060331;第21卷(第1期);第83页第2段 * |
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