CN110257311A - A kind of microorganism being used to prepare broccoli shape antimony trisulfide and its application - Google Patents

A kind of microorganism being used to prepare broccoli shape antimony trisulfide and its application Download PDF

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CN110257311A
CN110257311A CN201910743357.1A CN201910743357A CN110257311A CN 110257311 A CN110257311 A CN 110257311A CN 201910743357 A CN201910743357 A CN 201910743357A CN 110257311 A CN110257311 A CN 110257311A
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antimony trisulfide
broccoli
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CN110257311B (en
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张海坤
解静仪
孙延瑜
胡晓珂
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Yantai Institute of Coastal Zone Research of CAS
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    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G30/00—Compounds of antimony
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    • C—CHEMISTRY; METALLURGY
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C12R—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES C12C - C12Q, RELATING TO MICROORGANISMS
    • C12R2001/00—Microorganisms ; Processes using microorganisms
    • C12R2001/01—Bacteria or Actinomycetales ; using bacteria or Actinomycetales

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Abstract

The invention belongs to environmental project water-treatment technology field, specifically a kind of microorganism for being used to prepare broccoli shape antimony trisulfide and its applications.The present invention relates to microorganism be ocean salt single-cell bacteriaHalomonasSp.X3 is preserved in China typical culture collection center, address: Wuhan University, and the preservation time is on May 30th, 2019, deposit number are as follows: CCTCC M 2019409.Bacterial strain of the present invention is that indigenous microorganism is screened to obtain from marine sediment, can prepare nanometer antimony trisulfide using potassium pyroantimonate and sodium thiosulfate or sodium sulfite as precursor.The nanometer antimony trisulfide that microorganism obtains through the invention is in broccoli shape, can be used to accelerate the light degradation of azo dyes class compound as photochemical catalyst.The preparation of current antimony trisulfide mostly uses chemical method, and the present invention is prepared the antimony trisulfide of morphology controllable using microorganism for the first time, has stronger novelty.

Description

A kind of microorganism being used to prepare broccoli shape antimony trisulfide and its application
Technical field
The present invention relates to environmental project water-treatment technology fields, and in particular to a kind of broccoli shape antimony trisulfide of being used to prepare Microorganism and its application.
Background technique
In recent years, extensive concern of the binary metal chalcogenide because of its excellent photoelectric characteristic, by scientific research personnel.Gold The band gap for belonging to chalcogenide is all narrow, and relatively narrow band-gap energy makes it widely absorb visible light and near-infrared in sunlight Light has a good application prospect in photovoltaic and thermo-electric device.Wherein, antimonous sulfide (Sb2S3) band gap 1.6 eV a left side The right side is widely used to solar battery, semiconductor optoelectronic/volt device close to the best theoretical band gap magnitude of unijunction solar cell In part.In addition, Sb2S3Nano material specific surface area also with higher, it is also possible in the photo catalysis reactor based on visible light In.Therefore, Sb is studied2S3The efficient controlledly synthesis of nano material is the emphasis direction of this field.
The Sb to have registered at present2S3Synthetic method is mostly chemical method, as hydro-thermal method, wet chemistry method, microwave method, circumfluence method, Colloid reaction method and low-temperature solvent thermal method etc..These methods can synthesize the Sb of different-shape under certain condition2S3, such as rodlike, Dumbbell shaped, chrysanthemum shape, sea urchin shape and dandelion shape etc..But these methods have relative complex, the control of some conditions is more Harsh, some need adds a large amount of toxic chemical substance, has certain limitation in actual application.Therefore, pole It is necessary to develop a kind of Sb environmental-friendly, low in cost and easily operated2S3Synthetic method.
Biosynthesis nano material has the characteristics that low in cost, environmental-friendly, can targetedly develop Sb2S3Nanometer material The Microbe synthesis synthetic technology of material.Studies have reported that microorganism can be used to synthesize various metals chalcogenide such as CuS, ZnS, FeS etc..But since Sb (V) compound toxicity itself is big and hardly possible reduction, it there is no utilize Microbe synthesis Sb at present2S3It receives The report of rice material.
Summary of the invention
It is an object of that present invention to provide a kind of microorganism for being used to prepare broccoli shape antimony trisulfide and its applications.
To achieve the above object, the invention adopts a technical scheme as:
A kind of microorganism being used to prepare broccoli shape antimony trisulfide, microorganism are marine bacteriaHalomonasSp. X3, to protect Be hidden in China typical culture collection center, address: China, Wuhan, Wuhan University, preservation time are on May 30th, 2019, are protected Hiding number are as follows: CCTCC M 2019409.
The strain growth condition is 10-50oIt is grown under the conditions of C, salinity 1-7%, pH 4-10.
A kind of application of microorganism, the microorganism are preparing the application in broccoli shape antimony trisulfide.
It is described to be inoculated in dry weight containing Sb (V) and S for 0.1-1 g/L marine bacteria2O3 2-(or SO3 2-) inorganic salts training It supports in base, in 10-50oC, under the conditions of 1-7% salinity and pH 4-10, the carbon source for adding 0.5-2 g/L carries out reduction reaction, Again up to broccoli shape Sb after processed by hot bath2S3；The carbon source sodium lactate, glucose, sodium formate or sucrose.
Further
1) by the marine bacteria in the Sb of mM containing 0.01-2 (V) and 0.5-2 mM S2O3 2- (or SO3 2-) inorganic salts training It supports in base in 10-50oC, the mixture of 1-10 d is protected from light under the conditions of 1-7% salinity and pH 4-10；
2) mixture obtained in step (1) is centrifuged, obtained precipitating is placed in deionized water and is ultrasonically treated, be centrifuged The precipitating anionic surfactant (dodecyl sodium sulfate) of 0.2-5% is resuspended afterwards, 70-100oC processed by hot bath 1-45 Min, then centrifugation are simultaneously dry to get the as biological broccoli shape Sb prepared of powdered granule by pellet frozen2S3。
The temperature is 20-40oC, 1-3% salinity and pH 6-8.
A kind of broccoli shape Sb2S3Preparation, by the dry weight be 0.1-1 g/L marine bacteria be inoculated in containing Sb (V) and S2O3 2-(or SO3 2-) minimal medium in, in 10-50oC, under the conditions of 1-7% salinity and pH 4-10,0.5-2 is added The carbon source of g/L carries out reduction reaction, then up to broccoli shape Sb after processed by hot bath2S3；The carbon source sodium lactate, glucose, Sodium formate or sucrose.
Further,
1) by marine bacteria described in claim 1 in Sb containing 0.01-2mM (V) and 0.5-2mM S2O3 2- (or SO3 2-) nothing In 10-50 in machine salt culture mediumoC, under the conditions of 1-7% salinity and pH 4-10, the carbon source of 0.5-2 g/L is added, is then protected from light Reaction 1-10 d obtains mixture；
2) mixture obtained in step (1) is centrifuged, obtained precipitating is placed in deionized water and is ultrasonically treated, be centrifuged The precipitating cationic surfactant (dodecyl sodium sulfate) of 0.2-5% is resuspended afterwards, 70-100oC processed by hot bath 1- 45min, then centrifugation are simultaneously dry to get the as biological broccoli shape Sb prepared of powdered granule by pellet frozen2S3。
One kind preparing broccoli shape Sb2S3Application, the antimony trisulfide light degradation catalysis waste water from dyestuff in azo Application in compound.
Xiang Jingshui ultrasonic disperse concentration is the nanometer Sb of 1-100 mg/L2S3Dispersion liquid is added useless to dyestuff to be processed In water, in room temperature, the lower progress photocatalytic degradation of xenon long-arc lamp (500W) irradiation, and then realize to azo chemical combination in waste water from dyestuff The degradation of object；Wherein, nanometer Sb in every liter of waste water2S3Additional amount be 1-100 mg.
The invention has the advantages that:
The present invention screens to obtain indigenous microorganism from marine sediment, can be with potassium pyroantimonate and sodium thiosulfate or sulfurous acid Sodium is that precursor prepares nanometer antimony trisulfide.The nanometer antimony trisulfide that microorganism obtains through the invention is in broccoli shape, is that pattern can The antimony trisulfide of control is synthesized by microbial method, and technical costs is cheap and environmental-friendly, and industrialization valence is had more compared with chemical method Value.The nanometer antimony trisulfide that microorganism obtains through the invention, can be as photochemical catalyst for accelerating azo dyes class compound Light degradation.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 1 mentionsHalomonasSp. X3 generates the color change after antimony trisulfide in 5 d Figure.Wherein, 1 bacterium+Sb (V)+SO3 2-；2 bacterium+Sb (V)+S2O3 2-；3 bacterium+Sb (V).
Fig. 2 is the x-ray photoelectron spectroscopy figure for the biological nano antimony trisulfide that the embodiment of the present invention 2 is mentioned.Wherein, (a) It is the swarming figure of antimony with oxygen difference chemical valence；(b) be sulphur different valence state swarming figure.
Fig. 3 a-b is 1 μm of electron scanning electron microscope (a) of the biological nano antimony trisulfide that the embodiment of the present invention 2 is mentioned；(b) 500 nm；50 nm of electronic transmission electron microscope (c) for the biological nano antimony trisulfide that Fig. 3 c-d embodiment of the present invention 2 is mentioned；(d) 100 nm。
Fig. 4 is surface sweeping electro microscope energy spectrum (EDS) figure for the biological nano antimony trisulfide that the embodiment of the present invention 3 is mentioned.
Fig. 5 is the catalytic effect diagram for the biological nano antimony trisulfide that the embodiment of the present invention 4 is mentioned, wherein biological nano antimony trisulfide Ultrasonic treatment is first passed through before use 1 hour.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with Any mode limits the present invention.
The present invention screens one plant of ocean native bacterium, is named as using the ocean bed mud in the middle part of Bohai Haixia as bacterium source X3, can be spread cultivation proliferation with the classical culture medium such as modified version LB and ocean 2216E, and the bacterial strain is in temperature 10-50oC, salinity 1- It can also be in minimal medium with several kinds of carbon source (such as sodium lactate, glucose, sodium formate and sucrose) under the conditions of 7%, pH 4-10 For growth.The modified version LB culture medium is every liter, and 10 g peptones, 5 g yeast extracts, 20 g NaCl, surplus is deionization Water；The ocean 2216E culture medium is every liter, 5 g peptones, 1 g yeast extract, 0.01 g high ferric phosphate, surplus Chen Haishui； Minimal medium described in the minimal medium is every liter, 1 g NH4Cl, 0.8 g Na2HPO4, 0.2 g KH2PO4, 0.2 g MgCl2·7H2O, 0.1 g CaCl2·2H2O, 20 g NaCl, surplus is deionized water.
X3 is Gram-negative bacteria, and bacterium colony is in light brown, irregular cycle, surface are smooth, edge is without flash, is swept through electronics It retouches Electronic Speculum identification and finds the bacterium in Dan Sheng, rod-shaped, shown in 16s rRNA, through comparing and Bolivia's Halomonas (Halomonas boliviensis LC1 similarity highest (96.85%)), therefore be named asHalomonasSp. X3, China typical culture collection center has been preserved in it, address is Wuhan City, Hubei Province Wuchang District Bayi Road Luo Jia Shan, when preservation Between be on May 30th, 2019, deposit number are as follows: CCTCC M 2019405.It is identified,HalomonasSp. X3 can produce west Orchid shape antimony trisulfide, subsequent embodiment is based on the studies above.
Halomonas Sp. the 16srRNA sequence of X3:
CGAGCGGTAACAGATCCAGCTTGCTGGATGCTGACGAGCGGCGGACGGGTGAGTAATGCATAGGAATCTGCC CGNTAGTGGGGGATAACCTGGGGAAACCCAGGCTAATACCGCATACGTCCTACGGGAGAAAGGGGGCTTCGGCTCC CGCTATCGGATGAGCCTATGTCGGATTAGCTAGTTGGTGAGGTAACGGCTCACCAAGGCCACGATCCGTAGCTGGT CTGAGAGGATGATCAGCCACATCGGGACTGAGACACGGCCCGAACTCCTACGGGAGGCAGCAGTGGGGAATATTGG ACAATGGGGGGAACCCTGATCCAGCCATGCCGCGTGTGTGAAGAAGGCCCTCGGGTTGTAAAGCACTTTCAGCGAG GAAGAACGCCTAGCGGTTAATACCCGCTAGGAAAGACATCACTCGCAGAAGAAGCACCGGCTAACTCCGTGCCAGC AGCCGCGGTAATACGGAGGGTGCAAGCGTTAATCGGAATTACTGGGCGTAAAGCGCGCGTAGGTGGCTTGATAAGC CGGTTGTGAAAGCCCCGGGCTCAACCTGGGAACGGCATCCGGAACTGTCAAGCTAGAGTGCAGGAGAGGAAGGTAG AATTCCCGGTGTAGCGGTGAAATGCGTAGAGATCGGGAGGAATACCAGTGGCGAAGGCGGCCTTCTGGACTGACAC TGACACTGAGGTGCGAAAGCGTGGGTAGCAAACAGGATTAGATACCCTGGTAGTCCACGCCGTAAACGATGTCGAC CAGCCGTTGGGTGCCTAGCGCACTTTGTGGCGAAGTTAACGCGATAAGTCGACCGCCTGGGGAGTACGGCCGCAAG GTTAAAACTCAAATGAATTGACGGGGGCCCGCACAAGCGGTGGAGCATGTGGTTTAATTCGATGCAACGCGAAGAA CCTTACCTACTCTTGACATCCTGCGAATTNGGTAGAGATACCTTAGTGCCTTCGGGAACGCAGAGACAGGTGCTGC ATGGCTGTCGTCAGCTCGTGTTGTGAAATGTTGGGTTAAGTCCCGTAACGAGCGCAACCCTTGTCCTTATTTGCCA GCGCGTAATGGCGGGAACTCTAAGGAGACTGCCGGTGACAAACCGGAGGAAGGTGGGGACGACGTCAAGTCATCAT GGCCCTTACGAGTAGGGCTACACACGTGCTACAATGGTCGGTACAAAGGGTTGCCAACTCGCGAGAGTGAGCCAAT CCCGAAAAGCCGATCTCAGTCCGGATCGGAGTCTGCAACTCGACTCCGTGAAGTCGGAATCGCTAGTAATCGTAGA TCAGAATGCTACGGTGAATACGTTCCCGGGCCTTGTACACACCGCCCGTCACACCATGGGAGTGGACTGCACCAGA AGTGGTTAGCCTAACGCAAGAGGGCGATCACCA。
Embodiment 1
By above-mentioned acquisition strain X 3 (dry weight is 0.5 g/L), Sb (V) (0.1 mM) and 1 mM S2O3 2-(or SO3 2-) in It is mixed in 100 mL minimal mediums, salinity is 2 %, and pH is adjusted to 7, adds the sodium lactate of 18 mM, exposes nitrogen 15 Min, 30o5 d are protected from light in the anaerobic culture box of C, color change is referring to Fig. 1.
The minimal medium is every liter, 1 g NH4Cl, 0.8 g Na2HPO4, 0.2 g KH2PO4, 0.2 g MgCl2·7H2O, 0.1 g CaCl2·2H2O, 20 g NaCl, surplus is deionized water.
As seen from Figure 1, it will become under the conditions of X3 can be existing for the antimony and thiosulfate or sulphite orange Color, verified is Sb2S3, wherein the deeper reduction effect of color is better.The result shows that adding sulfurous in current reaction system The reaction system of hydrochlorate is more shallower (referring to Fig. 1) in same time point color than the reaction system for adding thiosulfate, shows sulphur Thiosulfate effect is more prominent than sulphite effect.
Embodiment 2
By above-mentioned acquisition strain X 3 (0.5 g/L), Sb (V) (0.2 mM) and 1 mM S2O3 2-In 100 mL inorganic salts cultures It is mixed in base, salinity is 2 %, and pH is adjusted to 7, adds the sodium lactate of 18 mM, 15 min of nitrogen is exposed, 30oThe anaerobism of C is trained It supports in case and is protected from light 5 d, obtained mixture is centrifuged (10000 rpm, 5 min), collect precipitating and be placed in deionized water Middle ultrasonic treatment 1h 1% anionic surfactant dodecyl sodium sulfate of precipitating is resuspended after centrifugation, 90oC hot bath 45 min are handled, then centrifugation (10000 rpm, 10 min) is dry by pellet frozen again, as Sb2S3(referring to fig. 2).
The minimal medium is every liter, 1 g NH4Cl, 0.8 g Na2HPO4, 0.2 g KH2PO4, 0.2 g MgCl2·7H2O, 0.1 g CaCl2·2H2O, 20 g NaCl, surplus is deionized water.
The products therefrom known to passing through the verifying of X-ray diffraction power spectrum in Fig. 2 is powdery Sb2S3, wherein by above-mentioned Fig. 2 a It records, the 3d of Sb (V)5/2In conjunction with can position appear in 531 eV, and the 3d of Sb (III)5/2It is appeared in conjunction with energy position 528.2 eV, thus infer, most Sb (V) is reduced to Sb (III).Meanwhile (Fig. 2 b) is schemed according to the XPS of S, S2O3 2-Substantially it is reduced to S2-, a portion and Sb (III) combination generation antimony trisulfide, another part are free in system.
With electronics scanning electron microscope and transmission electron microscope verifying resulting materials shape (referring to Fig. 3 a-d).By Fig. 3 a-b it is found that arrow It is the nanometer antimony trisulfide material generated that head, which is directed toward position, is in broccoli shape.By Fig. 3 c-d it is found that it is to produce that arrow, which is directed toward position, Raw nanometer antimony trisulfide material, is consistent with the resulting shape of scanning electron microscope.
Embodiment 3
By above-mentioned acquisition strain X 3 (0.7 g/L), Sb (V) (1 mM) and 2 mM SO3 2-In 100 mL minimal mediums Middle mixing, salinity are 3 %, and pH is adjusted to 7.2, add the glucose of 18 mM, 15 min of nitrogen are exposed, 30oThe anaerobism of C is trained It supports in case and is protected from light 7 d, obtained mixture is centrifuged (10000 rpm, 5 min), precipitating is placed in deionized water It is ultrasonically treated 1h, 1.5% anionic surfactant dodecyl sodium sulfate of precipitating is resuspended after centrifugation, 95oC hot bath 60 min are handled, then centrifugation (10000 rpm, 10 min) is dry by pellet frozen again, as Sb2S3。
The element contained with energy disperse spectroscopy verifying resulting materials, according to power spectrum, material is mainly by Sb and S element as the result is shown Composition, in addition there are the salt (such as Na, Cl, P) and biology prime element (such as C, N, O, P) (Fig. 4) of some remainings in surface.
Embodiment 4
Methyl orange in biological nano antimony trisulfide azo dyes, which is obtained, with above-described embodiment 2 carries out light degradation detection:
Control group and experimental group are set, and experimental group adds above-described embodiment 2 and obtains biological nano antimony trisulfide, using it as catalysis Agent, control group are the system for not adding catalyst: wherein experimental group reaction system is 50 mL deionized waters, 10 mg/L methyl oranges The biological nano antimony trisulfide of ultrasonic treatment is prepared with above-described embodiment of 30 mg/L, control systems are 50 mL deionized waters With 10 mg/L methyl oranges.Then (irradiation distance is about 10 cm) carries out photocatalysis under room temperature, xenon long-arc lamp (500W) irradiation Degradation, and 3 mL are sampled from above-mentioned experimental group and the reaction system of control group respectively, using spectrophotometer at 462 nm The concentration for monitoring methyl orange changes (referring to Fig. 5).
The degradation rate of the experimental group azo dyes containing material is significantly increased than control group as seen from Figure 5, in the reaction of 3h In time, the methyl orange degradation rate of blank control system is only 5% or so, and the degradation rate of the experimental group methyl orange of added material can Up to 82%.
Sequence table
<110>Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences
<120>a kind of microorganism for being used to prepare broccoli shape antimony trisulfide and its application
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<170> SIPOSequenceListing 1.0
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<211> 1397
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<213>marine bacteria (Halomonas sp. X3)
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cgagcggtaa cagatccagc ttgctggatg ctgacgagcg gcggacgggt gagtaatgca 60
taggaatctg cccgntagtg ggggataacc tggggaaacc caggctaata ccgcatacgt 120
cctacgggag aaagggggct tcggctcccg ctatcggatg agcctatgtc ggattagcta 180
gttggtgagg taacggctca ccaaggccac gatccgtagc tggtctgaga ggatgatcag 240
ccacatcggg actgagacac ggcccgaact cctacgggag gcagcagtgg ggaatattgg 300
acaatggggg gaaccctgat ccagccatgc cgcgtgtgtg aagaaggccc tcgggttgta 360
aagcactttc agcgaggaag aacgcctagc ggttaatacc cgctaggaaa gacatcactc 420
gcagaagaag caccggctaa ctccgtgcca gcagccgcgg taatacggag ggtgcaagcg 480
ttaatcggaa ttactgggcg taaagcgcgc gtaggtggct tgataagccg gttgtgaaag 540
ccccgggctc aacctgggaa cggcatccgg aactgtcaag ctagagtgca ggagaggaag 600
gtagaattcc cggtgtagcg gtgaaatgcg tagagatcgg gaggaatacc agtggcgaag 660
gcggccttct ggactgacac tgacactgag gtgcgaaagc gtgggtagca aacaggatta 720
gataccctgg tagtccacgc cgtaaacgat gtcgaccagc cgttgggtgc ctagcgcact 780
ttgtggcgaa gttaacgcga taagtcgacc gcctggggag tacggccgca aggttaaaac 840
tcaaatgaat tgacgggggc ccgcacaagc ggtggagcat gtggtttaat tcgatgcaac 900
gcgaagaacc ttacctactc ttgacatcct gcgaattngg tagagatacc ttagtgcctt 960
cgggaacgca gagacaggtg ctgcatggct gtcgtcagct cgtgttgtga aatgttgggt 1020
taagtcccgt aacgagcgca acccttgtcc ttatttgcca gcgcgtaatg gcgggaactc 1080
taaggagact gccggtgaca aaccggagga aggtggggac gacgtcaagt catcatggcc 1140
cttacgagta gggctacaca cgtgctacaa tggtcggtac aaagggttgc caactcgcga 1200
gagtgagcca atcccgaaaa gccgatctca gtccggatcg gagtctgcaa ctcgactccg 1260
tgaagtcgga atcgctagta atcgtagatc agaatgctac ggtgaatacg ttcccgggcc 1320
ttgtacacac cgcccgtcac accatgggag tggactgcac cagaagtggt tagcctaacg 1380
caagagggcg atcacca 1397

Claims (8)

1. a kind of microorganism for being used to prepare broccoli shape antimony trisulfide, it is characterised in that: microorganism is marine bacteriaHalomonas Sp. X3, to be preserved in China typical culture collection center, address: China, Wuhan, Wuhan University, preservation time are 2019 On May 30, in, deposit number are as follows: CCTCC M 2019409.
2. the microorganism according to claim 1 for being used to prepare broccoli shape antimony trisulfide, it is characterised in that: the strain growth Condition is 10-50oIt is grown under the conditions of C, salinity 1-7%, pH 4-10.
3. a kind of application of microorganism described in claim 1, it is characterised in that: the microorganism is preparing the vulcanization of broccoli shape Application in antimony.
4. a kind of broccoli shape Sb2S3Preparation method, it is characterised in that: by dry weight described in claim 1 be 0.1-1 g/L sea Foreign microbionation is in containing Sb (V) and S2O3 2-(or SO3 2-) minimal medium in, in 10-50oC, 1-7% salinity and pH Under the conditions of 4-10, the carbon source for adding 0.5-2 g/L carries out reduction reaction, then up to broccoli shape after processed by hot bath Sb2S3。
5. preparation method according to claim 4, it is characterised in that:
1) by the marine bacteria in the Sb of mM containing 0.01-2 (V) and 0.5-2 mM S2O3 2- (or SO3 2-) inorganic salts culture In 10-50 in baseoC, the mixture of 1-10 d is protected from light under the conditions of 1-7% salinity and pH 4-10；
2) mixture obtained in step (1) is centrifuged, obtained precipitating is placed in deionized water and is ultrasonically treated, be centrifuged The precipitating anionic surfactant dodecyl sodium sulfate of 0.2-5% is resuspended afterwards, 70-100oC processed by hot bath 1-45 Min, then centrifugation are simultaneously dry to get the as biological broccoli shape Sb prepared of powdered granule by pellet frozen2S3。
6. pressing preparation method described in claim 4 or 5, it is characterised in that: the temperature is 20-40oC, 1-3% salinity and pH 6-8。
7. preparing broccoli shape Sb described in a kind of claim 52S3Application, it is characterised in that: the antimony trisulfide is in light Application in degradation catalysis waste water from dyestuff in azo compound.
8. application according to claim 7, it is characterised in that: Xiang Jingshui ultrasonic disperse concentration is that the described of 1-100 mg/L receives Rice Sb2S3Dispersion liquid is added into waste water from dyestuff to be processed, carries out photocatalytic degradation under room temperature, xenon long-arc lamp (500W) irradiation, And then degradation of the realization to azo compound in waste water from dyestuff；Wherein, nanometer Sb in every liter of waste water2S3Additional amount be 1-100 mg。
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