CN110064408A - A kind of preparation method for the alpha-crystal form FeOOH catalyst having loaded iron sulfide - Google Patents
A kind of preparation method for the alpha-crystal form FeOOH catalyst having loaded iron sulfide Download PDFInfo
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- CN110064408A CN110064408A CN201910480247.0A CN201910480247A CN110064408A CN 110064408 A CN110064408 A CN 110064408A CN 201910480247 A CN201910480247 A CN 201910480247A CN 110064408 A CN110064408 A CN 110064408A
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- Prior art keywords
- alpha
- iron sulfide
- crystal form
- feooh
- water
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Links
- 229910002588 FeOOH Inorganic materials 0.000 title claims abstract description 49
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000013078 crystal Substances 0.000 title claims abstract description 42
- 239000003054 catalyst Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910001868 water Inorganic materials 0.000 claims abstract description 43
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000011941 photocatalyst Substances 0.000 claims abstract description 27
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 26
- 229940101006 anhydrous sodium sulfite Drugs 0.000 claims abstract description 25
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims abstract description 25
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 31
- 239000000975 dye Substances 0.000 claims description 30
- 230000001699 photocatalysis Effects 0.000 claims description 28
- 238000007146 photocatalysis Methods 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 24
- 239000002131 composite material Substances 0.000 claims description 17
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 17
- 229940043267 rhodamine b Drugs 0.000 claims description 17
- 230000015556 catabolic process Effects 0.000 claims description 13
- 238000006731 degradation reaction Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 10
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 230000003197 catalytic effect Effects 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000010189 synthetic method Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 229910052603 melanterite Inorganic materials 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000012423 maintenance Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000006552 photochemical reaction Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 229940001482 sodium sulfite Drugs 0.000 claims description 4
- 235000010265 sodium sulphite Nutrition 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- -1 green vitriol ion Chemical class 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 238000009775 high-speed stirring Methods 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 229910001430 chromium ion Inorganic materials 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000011651 chromium Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 229910052683 pyrite Inorganic materials 0.000 description 5
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 5
- 239000011028 pyrite Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- SPSSULHKWOKEEL-UHFFFAOYSA-N 2,4,6-trinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O SPSSULHKWOKEEL-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- NFMAZVUSKIJEIH-UHFFFAOYSA-N bis(sulfanylidene)iron Chemical compound S=[Fe]=S NFMAZVUSKIJEIH-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- DCOPUUMXTXDBNB-UHFFFAOYSA-N diclofenac Chemical compound OC(=O)CC1=CC=CC=C1NC1=C(Cl)C=CC=C1Cl DCOPUUMXTXDBNB-UHFFFAOYSA-N 0.000 description 1
- 229960001259 diclofenac Drugs 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-N hydroperoxyl Chemical compound O[O] OUUQCZGPVNCOIJ-UHFFFAOYSA-N 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229960002415 trichloroethylene Drugs 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B01J35/39—
-
- B01J35/61—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention discloses a kind of preparation methods of alpha-crystal form FeOOH catalyst for having loaded iron sulfide, it is characterized in that, it is synthesized using one step hydro thermal method, anhydrous sodium sulfite deionized water solution is slowly added dropwise into green vitriol solion water, high-speed stirred, it is all put into again and autoclave is kept into high temperature constant temperature heating, loaded the alpha-crystal form FeOOH photocatalyst material of iron sulfide, the FeS synthesized by being centrifuged at a high speed after being cooled to room temperature2It is the molar ratio of nanometer materials, wherein green vitriol and anhydrous sodium sulfite in 1:8 ± 0.1 with alpha-feooh；The reaction temperature of green vitriol and anhydrous sodium sulfite in a high pressure reaction kettle is 160-200 degree, and the reaction time is 1-2 hours.FeOOH together with iron sulfide load, is improved efficiency by the present invention under the premise of economizing on resources, and plays the purpose that orientation goes heavy metal ion and macromolecular organic pollutant in water removal.
Description
Technical field
The present invention relates to chemical field, especially a kind of system for the alpha-crystal form FeOOH catalyst for having loaded iron sulfide
Preparation Method.
Background technique
With the fast development of dyeing and metal industry, a large amount of dyeing waste waters and high chemical valence heavy metal wastewater thereby
Discharge causes a large amount of water pollution in violation of rules and regulations, seriously threatens natural environment and the life and health safety of the mankind, how quickly to have
The degradation macromolecular dyestuff and reducing heavy metal ion of effect become the problem of present environmental area is studied extensively, water-soluble azo
Dyestuff contains phenyl ring mostly, and property is stablized, and traditional chemistry and bioanalysis are difficult to obtain better effects.It is urged using photochemical catalyst light
Changing degradation water pollutant is present more common method, generates strong oxidizer for organic pollutant exhaustive oxidation using light and is
H2O, CO2Equal inorganic molecules, it is applied widely, increasingly it is valued by people.
Pyrite (FeS2) it is a kind of pyrite widely present on the earth, itself value is lower, still, pyrite
It is gradually concerned by people as a kind of semiconductor with attraction electronic capability and good optical properties.Pyrite has
The ability of harmful heavy metal ions and larger molecular organics pollutant difficult to degrade in environment is removed, accordingly toward experimental data table
Bright, pyrite can effectively remove the organic contaminations such as trichloro ethylene, 2,4,6-trinitrotoluene, Diclofenac and macromolecular dyestuff
Object.At the same time it can also remove some higher toxic heavy metals of valence state, hexavalent chromium Cr(VI using pyrite) etc. dirts
Contaminate object.Under normal conditions, Pyrite-type FeS is synthesized2The main method of powder is high pressure hydro-thermal and solvent-thermal method, and such methods are closed
Simple at means, synthetic effect is good, can pass through the methods of regulation pH value, reaction temperature, heating time and raw material proportioning
Obtain good crystal form.
FeOOH microparticle possesses good photocatalysis performance based on its special structure, and can effectively degrade water
In heavy metal and larger molecular organics, and due to the substance have be readily synthesized, specific surface area is higher, with pollutant contact surface
Product is big, raw material abundance prepares the advantages that cheap and utilized extensively by people.FeOOH semiconductor catalysis technique passes through sunlight
A series of important chemical reactions are driven, generate electrons and holes pair, target stains substance in further redox water will too
Sun can be converted into utilizable chemical energy, effectively solution problem of environmental pollution.
Therefore, the compound of iron sulfide and FeOOH has photocatalytic more higher than iron sulfide and FeOOH
Can, synthetic method is simple, and photocatalysis efficiency is high, however, the compound for how efficiently synthesizing iron sulfide and FeOOH extremely closes
It is important, a set of feasible efficient synthetic method currently not yet.
Summary of the invention
One of contents of the present invention are to provide a kind of alpha-crystal form FeOOH composite wood for having loaded iron sulfide of simplicity
One one-step hydro-thermal synthesis method of material has and prepares that material is cheap, the simple feature of production process.To solve existing dyeing waste water
With heavy metal containing wastewater treatment problem.
The two of the contents of the present invention provide a kind of using the alpha-crystal form FeOOH composite material drop for having loaded iron sulfide
Xie Shuizhong macromolecular dyestuff rhodamine B and heavy metal Cr6+Method.
One of contents of the present invention implementation method is:
A kind of preparation method for the alpha-crystal form FeOOH catalyst having loaded iron sulfide, which is characterized in that use a step hydro-thermal
Method synthesis, anhydrous sodium sulfite deionized water solution is slowly added dropwise into green vitriol solion water, high-speed stirred,
It is all put into again and autoclave is kept into high temperature constant temperature heating, loaded after being cooled to room temperature by being centrifuged at a high speed
The alpha-crystal form FeOOH photocatalyst material of iron sulfide, the FeS synthesized2It is nanometer materials with alpha-feooh,
The molar ratio of middle green vitriol and anhydrous sodium sulfite is in 1:8 ± 0.1；Green vitriol and anhydrous sulfurous acid
The reaction temperature of sodium in a high pressure reaction kettle is 160-200 degree, and the reaction time is 1-2 hours.
Further, synthetic method is as follows:
(1) by green vitriol (FeSO4·7H2O it) is made it completely dissolved in deionized water by stirring；Molar concentration
For 0.15mol/L；
(2) by anhydrous sodium sulfite (Na2SO3) made it completely dissolved in deionized water by stirring；Molar concentration is
1.2mol/L；
(3) anhydrous sodium sulfite deionized water solution is slowly added dropwise under stirring water-soluble into green vitriol ion
In liquid, rate of addition 1ml/s, and be sufficiently stirred under the revolving speed of 300 ± 50r/min 1 ± 0.1 hour；
(4) after the completion of stirring, slurries are slowly poured into autoclave, control compactedness is no more than 70%；
(5) in a high pressure reaction kettle, heated at constant temperature 1-2 hours at a temperature of being kept for 160-200 degrees Celsius；
(6) it is centrifugally separating to obtain the alpha-crystal form hydroxyl for having loaded iron sulfide after being cooled to room temperature for 4000 ± 100r/min by revolving speed
Base iron oxide photocatalyst material；
(7) it is washed 4 ± 1 times with deionized water and ethyl alcohol, and is dried in vacuo 12 ± 1 hours at 35 ± 5 DEG C repeatedly, loaded
The alpha-crystal form FeOOH photocatalyst material powder of iron sulfide.
Further, specific synthetic method is as follows:
(1) accurate weighing 0.84g green vitriol (FeSO4·7H2O), made it completely dissolved by stirring and gone in 35ml
In ionized water；
(2) accurate weighing 2.92g anhydrous sodium sulfite (Na2SO3), it is made it completely dissolved by stirring in 25ml deionized water
In；
(3) sodium sulfite solution dissolved is slowly added dropwise into ferrous sulfate solution under stirring, rate of addition is
1ml/s, and be sufficiently stirred under the revolving speed of 300r/min 1 hour；
(4) after the completion of stirring, slurries are slowly poured into autoclave, control compactedness is 70%；
(5) in a high pressure reaction kettle, heated at constant temperature 1-2 hours at a temperature of being maintained at 160-200 degrees Celsius；
(6) it is controlled after being cooled to room temperature by revolving speed and has been loaded the α crystalline substance of iron sulfide in being centrifuged at a high speed for 4000r/min
Type FeOOH photocatalyst material；
(7) washed repeatedly 4 times with deionized water and ethyl alcohol, and 35 degrees Celsius at a temperature of be dried in vacuo 12 hours, made
Standby successful solid photocatalysts material powder.
Two implementation method of the contents of the present invention is: having loaded the alpha-crystal form FeOOH catalyst degradation of iron sulfide
Macromolecular dyestuff rhodamine B and/or heavy metal Cr in water6+。
Macromolecular dyestuff rhodamine B or heavy metal in the alpha-crystal form FeOOH catalyst degradation water of iron sulfide are loaded
Cr6+Method, heavy metal Cr 6+ or macromolecular dyestuff rhodamine B in liquid to be processed of effectively degrading in acid condition pass through
Dilute hydrochloric acid adjusts the pH value in liquid to be processed between 2-4；
(1), by treated, liquid to be processed is added in photo catalysis reactor, then nanoscale load is added into photo catalysis reactor
The alpha-crystal form FeOOH catalyst of iron sulfide forms mixture in photo catalysis reactor；In the revolving speed of 200 ± 20r/min
Lower agitating solution, forms it into homogeneous slurry, covers photo catalysis reactor with dark reaction hood, stirs under non-illuminated conditions
For a period of time, composite photo-catalyst is allowed sufficiently to adsorb dye, rhodamine B or heavy metal Cr in liquid to be processed6+；It is taken after absorption
Top solution measures dye, rhodamine B and/or heavy metal Cr in solution6+Concentration simultaneously records；
(2), it gives photo catalysis reactor to increase ultraviolet light condition, increases light-blocking fence on the outside of photo catalysis reactor, allow light
Catalytic reactor carries out photochemical reaction under the irradiation of ultraviolet light, and maintenance stirring rate is 200 ± 20r/min, and every mistake 30 ±
3min takes top solution measurement concentration and to record, dye, rhodamine B and/or heavy metal in water after 150 ± 10min reaction
Cr6+Basic removal；
(3), stop stirring, the alpha-crystal form FeOOH composite photo-catalyst for having loaded iron sulfide is allowed in water slowly to precipitate, pass through
120 ± 10min precipitating completely, then passes through filtering, filtrate discharge or recycling；Filtered recycling precipitate, precipitating
Alpha-crystal form FeOOH composite photo-catalyst is loaded containing iron sulfide in object, is reused, water quality is directly arranged after reaching standard
It puts.
Further, the photo catalysis reactor is the glass container of translucency.
Further, the concentration of dye, rhodamine B is 30mg/L or heavy metal Cr in liquid to be processed6+Concentration be 30mg/L,
Corresponding catalyst amounts are 0.7 ± 0.05g/L；The mixing time of homogeneous slurry is 2 ± 0.01min；Dark reaction mixing time
For 40 ± 2min；Ultraviolet light condition is the ultraviolet lamp that wavelength is 400 ± 20nm.
The method of the measurement processing liquid concentration is that the solution of acquirement is first passed through supercentrifuge 4000r/min's
It is centrifuged under revolving speed, separates the catalyst granules in water, retell supernatant and pour into cuvette, use UV-vis spectroscopy
Dye strength in photometer measurement water；
The above experiment photochemical catalyst catalytic efficiency is 85% or more.
The invention has the benefit that realizing two kinds of photochemical catalyst phases of iron sulfide and FeOOH in the 1, present invention
Mutually auxiliary, not only increases the photocatalysis efficiency of iron sulfide, also improves the catalytic efficiency of FeOOH, by FeOOH
Together with iron sulfide load, efficiency is improved under the premise of economizing on resources, and is played orientation and is gone heavy metal ion in water removal
With the purpose of macromolecular organic pollutant；
2, raw material used in the invention is common cheap, rich reserves, and the catalyst of preparation has large specific surface area, easily recycling point
From etc. outstanding feature, improve independent FeOOH be not readily separated, it is difficult collect, the small disadvantage of specific surface area；
3, process for synthetic catalyst preparation process described in the invention is simple, and reaction process is easy to control, and the catalysis generated
Agent has very high catalytic capability.
Detailed description of the invention
Fig. 1 is the XRD spectrum of invention gained iron sulfide load alpha-crystal form FeOOH composite photo-catalyst；
Fig. 2 is degradation effect of the invention gained iron sulfide load alpha-crystal form FeOOH composite photo-catalyst to heavy metal ion
Figure；
Fig. 3 is degradation effect of the invention gained iron sulfide load alpha-crystal form FeOOH composite photo-catalyst to macromolecular dyestuff
Figure.
Specific embodiment
Embodiment 1:
Iron sulfide load crystal form FeOOH catalyst is prepared first.
As shown in Figure 1, being synthesized using one step hydro thermal method, the FeS synthesized2For nanoscale, alpha-feooh is nanoscale,
Specific synthetic method is as follows:
(1) accurate weighing 0.84g green vitriol (FeSO4·7H2O), made it completely dissolved by stirring and gone in 35ml
In ionized water；Molar concentration is 0.15mol/L.
(2) accurate weighing 2.92g anhydrous sodium sulfite (Na2SO3), it is made it completely dissolved by stirring in 25ml deionization
In water；Molar concentration is 1.2mol/L
(3) sodium sulfite solution dissolved is slowly added dropwise into ferrous sulfate solution under stirring, and 300 ±
A hour is sufficiently stirred under the revolving speed of 30r/min；
(4) after the completion of stirring, slurries are slowly poured into the stainless steel autoclave of polytetrafluoroethyllining lining, control filling
Degree is 70%；
(5) by autoclave 160-200 degrees Celsius at a temperature of heated at constant temperature 1-2 hours；
(6) the iron sulfide photochemical catalyst of alpha-crystal form FeOOH has been loaded by being centrifuged at a high speed after being cooled to room temperature
Material (supercentrifuge rotating speed is controlled in 4000r/min)；
(7) it is washed repeatedly 4 ± 1 times with deionized water and ethyl alcohol, and small in 35 ± 5 degrees Celsius of at a temperature of vacuum drying 12 ± 1
When, the solid photocatalysts material powder that is successfully prepared.
In reactant allocation ratio, the molar ratio of two kinds of materials of strict control green vitriol and anhydrous sodium sulfite
Example, is accurately controlled in 1:8；
When the molar ratio of two kinds of materials of green vitriol and anhydrous sodium sulfite is 1:5, product is bloodstone
(Fe2O3)；
When the molar ratio of two kinds of materials of green vitriol and anhydrous sodium sulfite is 1:8, product is alpha-crystal form hydroxyl oxygen
Change the iron sulfide of iron load；
When the molar ratio of two kinds of materials of green vitriol and anhydrous sodium sulfite is 1:10, product is magnetic iron ore
(Fe3O4).
In reactant heating temperature, reaction when the two kinds of material reactions of green vitriol and anhydrous sodium sulfite is controlled
Temperature is 160-200 degree；
When the reaction temperature of two kinds of materials of green vitriol and anhydrous sodium sulfite is 150 degree, product is magnetic iron ore；
When the reaction temperature of two kinds of materials of green vitriol and anhydrous sodium sulfite is spent for 160-200, product is product
For the alpha-crystal form FeOOH for having loaded iron sulfide.
In reactant heating time, when two kinds of materials of strict control green vitriol and anhydrous sodium sulfite react
Reaction time is 1-2 hours；
When the reaction time of two kinds of materials of green vitriol and anhydrous sodium sulfite is 1-2 small, product is to have loaded sulphur
Change the alpha-crystal form FeOOH of iron；
When the reaction time of two kinds of materials of green vitriol and anhydrous sodium sulfite is 4-6 small, product is alpha-crystal form hydroxyl
Iron oxide；
When the reaction time of two kinds of materials of green vitriol and anhydrous sodium sulfite is 10-12 small, product is bloodstone.
Embodiment 2
Iron sulfide loads heavy metal Cr in crystal form FeOOH catalyst degradation water6+Method:
Heavy metal ion, the chromium ion solution for preparing 100mg/L using potassium bichromate are standby effectively in degradation water in acid condition
With, take 15mL to prepare solution, then take 35mL deionized water, prepare 50mL concentration be 30mg/L chromium ion solution, pass through dilute salt
PH value in acid-conditioning solution is between 2-4.
1, by treated, chromium ion solution is added in photo catalysis reactor, then nanometer half is added into photo catalysis reactor
Conductor photochemical catalyst forms mixture in photo catalysis reactor；The agitating solution under the revolving speed of 200 ± 20r/min, forms it into
Homogeneous slurry covers photo catalysis reactor with dark reaction hood, provides dark reaction environment, one section is stirred under non-illuminated conditions
Time allows composite photo-catalyst sufficiently to adsorb chromium ion in water.Chromium ion concentration in the solution measurement water of top is taken after absorption
And it records.
2, on-response device increases ultraviolet light condition, increases light-blocking fence on the outside of Photoreactor, allows Photoreactor
Photochemical reaction is carried out under the irradiation of ultraviolet light, and maintenance stirring rate is 200 ± 20r/min, and every 30 ± 3min of mistake takes top
Solution measurement chromium ion concentration simultaneously records, and chromium ion removes substantially in water after 150 ± 10min reaction.
3, stop stirring, the alpha-crystal form FeOOH composite photo-catalyst for having loaded iron sulfide is allowed in water slowly to precipitate, pass through
120 ± 10min precipitating is crossed completely, then by filtering, filtrate (water outlet) discharge or reuse.Filtered recycling precipitate,
It containing the alpha-crystal form FeOOH composite photo-catalyst for having loaded iron sulfide in sediment, may be reused 46 times, be discharged
Chromium ion concentration reach water standard, can be with direct emission.
Wherein, photo catalysis reactor is the good glass container of translucency；Catalyst amounts are 0.7g/L；
The mixing time for allowing it to become homogeneous slurry is 2 ± 0.1min；Dark reaction mixing time is 40 ± 2min；
The ultraviolet light condition is that wavelength is 400 ± 10nm ultraviolet lamp below；
The method for measuring chromium ion concentration is ultraviolet-visible spectrophotometer；Degradation effect as shown in Fig. 2, more than experiment described in
Photochemical catalyst catalytic efficiency be 90% or more.
Embodiment 3:
In acid condition effectively degradation water in macromolecular dyestuff rhodamine B method:
Specifically: the dye solution for preparing 100mg/L using rhodamine B is spare, takes 15mL to prepare solution, then take 35mL deionization
Water prepares the dye solution that 50mL concentration is 30mg/L, adjusts the pH value in solution between 2-4 by dilute hydrochloric acid.
1. by treated, dye solution is added in photo catalysis reactor, then is added nanometer into photo catalysis reactor and partly led
Body photochemical catalyst forms mixture in photo catalysis reactor；The agitating solution under the revolving speed of 200 ± 20r/min forms it into
Homogenate, covers photo catalysis reactor with dark reaction hood, provides dark reaction environment, when stirring one section under non-illuminated conditions
Between, allow composite photo-catalyst sufficiently to adsorb chromium ion in water.Dye strength in the solution measurement water of top is taken after absorption and is remembered
Record；
2. on-response device increases ultraviolet light condition, increases light-blocking fence on the outside of Photoreactor, allow Photoreactor in purple
Photochemical reaction is carried out under the irradiation of outer light, maintenance stirring rate is 200 ± 20r/min, and every 30min that crosses takes top solution measurement
Dye strength simultaneously records, and dyestuff removes substantially in water after 150min reacts.
3. stopping stirring, the alpha-crystal form FeOOH composite photo-catalyst for having loaded iron sulfide is allowed in water slowly to precipitate, passed through
120 ± 10min precipitating is crossed completely, then by filtering, filtrate (water outlet) discharge or reuse.Filtered recycling precipitate,
It containing the alpha-crystal form FeOOH composite photo-catalyst for having loaded iron sulfide in sediment, may be reused 46 times, be discharged
Dye strength reach water standard, can be with direct emission.The photo catalysis reactor is the good glass container of translucency；
Wherein, catalyst amounts 0.7g/L；Allowing it to become the mixing time of homogeneous slurry is 2min；
The dark reaction mixing time is 40 ± 5min；Ultraviolet light condition is that wavelength is 400 ± 20nm below ultraviolet
Lamp；
The method of measurement dye strength is that the solution of acquirement is first passed through supercentrifuge under the revolving speed of 4000 ± 100r/min
It is centrifuged, separates the catalyst granules in water, retell supernatant and pour into cuvette, use ultraviolet-visible spectrophotometer
Measure dye strength in water；Degradation effect as shown in figure 3, more than to test the photochemical catalyst catalytic efficiency be 90% or more.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its
Equivalent defines.
Claims (7)
1. a kind of preparation method for the alpha-crystal form FeOOH catalyst for having loaded iron sulfide, which is characterized in that use a step water
Thermal method synthesis, anhydrous sodium sulfite deionized water solution is slowly added dropwise into green vitriol solion water, high-speed stirring
It mixes, then is all put into and autoclave is kept into high temperature constant temperature heating, born after being cooled to room temperature by being centrifuged at a high speed
The alpha-crystal form FeOOH photocatalyst material of iron sulfide, the FeS synthesized are carried2It is nanoscale material with alpha-feooh
Material, wherein the molar ratio of green vitriol and anhydrous sodium sulfite is in 1:8 ± 0.1；Green vitriol and anhydrous
The reaction temperature of sodium sulfite in a high pressure reaction kettle is 160-200 degree, and the reaction time is 1-2 hours.
2. a kind of preparation method of alpha-crystal form FeOOH catalyst for having loaded iron sulfide according to claim 1,
It is characterized in that, synthetic method is as follows:
(1) by green vitriol (FeSO4·7H2O it) is made it completely dissolved in deionized water by stirring；Molar concentration
For 0.15 ± 0.01mol/L；
(2) by anhydrous sodium sulfite (Na2SO3) made it completely dissolved in deionized water by stirring；Molar concentration be 1.2 ±
0.05mol/L；
(3) anhydrous sodium sulfite deionized water solution is slowly added dropwise under stirring water-soluble into green vitriol ion
In liquid, and it is sufficiently stirred under the revolving speed of 300 ± 50r/min 1 ± 0.1 hour；
(4) after the completion of stirring, slurries are slowly poured into autoclave, control compactedness is no more than 70%；
(5) in a high pressure reaction kettle, heated at constant temperature 1-2 hours at a temperature of being kept for 160-200 degrees Celsius；
(6) it is centrifugally separating to obtain the alpha-crystal form hydroxyl for having loaded iron sulfide after being cooled to room temperature for 4000 ± 100r/min by revolving speed
Base iron oxide photocatalyst material；
(7) it is washed 4 ± 1 times with deionized water and ethyl alcohol, and is dried in vacuo 12 ± 1 hours at 35 ± 5 DEG C repeatedly, loaded
The alpha-crystal form FeOOH photocatalyst material powder of iron sulfide.
3. a kind of preparation method of alpha-crystal form FeOOH catalyst for having loaded iron sulfide according to claim 2,
It is characterized in that, specific synthetic method is as follows:
(1) accurate weighing 0.84g green vitriol (FeSO4·7H2O), by stirring make it completely dissolved in 35ml go from
In sub- water；
(2) accurate weighing 2.92g anhydrous sodium sulfite (Na2SO3), it is made it completely dissolved in 25ml deionized water by stirring；
(3) sodium sulfite solution dissolved is slowly added dropwise into ferrous sulfate solution under stirring, rate of addition is
1ml/s, and be sufficiently stirred under the revolving speed of 300r/min 1 hour；
(4) after the completion of stirring, slurries are slowly poured into autoclave, control compactedness is 70%；
(5) in a high pressure reaction kettle, heated at constant temperature 1-2 hours at a temperature of being maintained at 160-200 degrees Celsius；
(6) it is controlled after being cooled to room temperature by revolving speed and has been loaded the α crystalline substance of iron sulfide in being centrifuged at a high speed for 4000r/min
Type FeOOH photocatalyst material；
(7) washed repeatedly 4 times with deionized water and ethyl alcohol, and 35 degrees Celsius at a temperature of be dried in vacuo 12 hours, made
Standby successful solid photocatalysts material powder.
4. the alpha-crystal form FeOOH catalyst degradation water for having loaded iron sulfide prepared using method described in claim 1
Middle macromolecular dyestuff rhodamine B and/or heavy metal Cr6+。
5. the alpha-crystal form FeOOH catalyst degradation water for having loaded iron sulfide prepared using method described in claim 1
Middle macromolecular dyestuff rhodamine B and/or heavy metal Cr6+Method, which is characterized in that effectively degrade in acid condition to be processed
Heavy metal Cr in liquid6+And/or macromolecular dyestuff rhodamine B, by dilute hydrochloric acid adjust the pH value in liquid to be processed be 2-4 it
Between；
(1), by treated, liquid to be processed is added in photo catalysis reactor, then nanoscale load is added into photo catalysis reactor
The alpha-crystal form FeOOH catalyst of iron sulfide forms mixture in photo catalysis reactor；In the revolving speed of 200 ± 20r/min
Lower agitating solution, forms it into homogeneous slurry, covers photo catalysis reactor with dark reaction hood, stirs under non-illuminated conditions
For a period of time, composite photo-catalyst is allowed sufficiently to adsorb dye, rhodamine B and/or heavy metal Cr in liquid to be processed6+；After absorption
Take dye, rhodamine B and/or heavy metal Cr in the solution measurement solution of top6+Concentration simultaneously records；
(2), it gives photo catalysis reactor to increase ultraviolet light condition, increases light-blocking fence on the outside of photo catalysis reactor, allow light
Catalytic reactor carries out photochemical reaction under the irradiation of ultraviolet light, and maintenance stirring rate is 200 ± 20r/min, and every mistake 30 ±
3min takes top solution measurement concentration and to record, dye, rhodamine B and/or heavy metal in water after 150 ± 10min reaction
Cr6+Basic removal；
(3), stop stirring, the alpha-crystal form FeOOH composite photo-catalyst for having loaded iron sulfide is allowed in water slowly to precipitate, pass through
120 ± 10min precipitating completely, then passes through filtering, filtrate discharge or recycling；Filtered recycling precipitate, precipitating
Alpha-crystal form FeOOH composite photo-catalyst is loaded containing iron sulfide in object, is reused, water quality is directly arranged after reaching standard
It puts.
6. according to the method described in claim 5, it is characterized in that, the glass that the photo catalysis reactor is translucency holds
Device.
7. according to the method described in claim 5, it is characterized in that, the concentration of dye, rhodamine B is 30mg/L in liquid to be processed
Or heavy metal Cr6+Concentration be 30mg/L, corresponding catalyst amounts are 0.7 ± 0.05g/L；The mixing time of homogeneous slurry is
2±0.01min；Dark reaction mixing time is 40 ± 2min；Ultraviolet light condition is the ultraviolet lamp that wavelength is 400 ± 10nm.
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