CN107983395A - Using flyash as silicon source and the class fenton catalyst of source of iron and application - Google Patents
Using flyash as silicon source and the class fenton catalyst of source of iron and application Download PDFInfo
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- CN107983395A CN107983395A CN201711234309.7A CN201711234309A CN107983395A CN 107983395 A CN107983395 A CN 107983395A CN 201711234309 A CN201711234309 A CN 201711234309A CN 107983395 A CN107983395 A CN 107983395A
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- flyash
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- hydrochloric acid
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- 239000010881 fly ash Substances 0.000 title claims abstract description 49
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 16
- 239000010703 silicon Substances 0.000 title claims abstract description 16
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 11
- 230000008025 crystallization Effects 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000002351 wastewater Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 230000000717 retained effect Effects 0.000 claims abstract description 6
- 230000020477 pH reduction Effects 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims 1
- 239000002808 molecular sieve Substances 0.000 abstract description 12
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 abstract description 12
- 239000010883 coal ash Substances 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 4
- 239000004411 aluminium Substances 0.000 abstract description 3
- 239000002910 solid waste Substances 0.000 abstract description 3
- 230000000593 degrading effect Effects 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000008267 milk Substances 0.000 description 6
- 210000004080 milk Anatomy 0.000 description 6
- 235000013336 milk Nutrition 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 2
- QPILZZVXGUNELN-UHFFFAOYSA-M sodium;4-amino-5-hydroxynaphthalene-2,7-disulfonate;hydron Chemical compound [Na+].OS(=O)(=O)C1=CC(O)=C2C(N)=CC(S([O-])(=O)=O)=CC2=C1 QPILZZVXGUNELN-UHFFFAOYSA-M 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- HMNPDEGBVWDHAR-UHFFFAOYSA-N 8-aminonaphthalen-1-ol Chemical class C1=CC(O)=C2C(N)=CC=CC2=C1 HMNPDEGBVWDHAR-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
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- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0316—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing iron group metals, noble metals or copper
- B01J29/0333—Iron group metals or copper
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
-
- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/041—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41
- B01J29/042—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41 containing iron group metals, noble metals or copper
- B01J29/044—Iron group metals or copper
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analytical Chemistry (AREA)
- Catalysts (AREA)
Abstract
Include the following steps the invention discloses a kind of by silicon source and the class fenton catalyst of source of iron and application, preparation method of flyash：(1) flyash carries out acidification with hydrochloric acid, and hydrochloric acid filtrate is spare；(2) flyash after acidification is uniformly mixed with sodium hydroxide, is added after roasting in deionized water, it is stand-by that supernatant is isolated after stirring；(3) it is uniformly mixed after template is dissolved in deionized water with dispersant with supernatant in step (2), it is 7 to adjust pH using the hydrochloric acid filtrate retained in step (1)；(4) above-mentioned solution is placed in crystallization in reaction kettle, and 41 molecular sieve carried iron catalysts of MCM containing aluminium are obtained after filtered, washing, dry and roasting.The preparation method can efficiently use the components such as silicon in flyash, aluminium, iron, the catalyst of preparation can fast and effeciently degrading waste water organic pollution, realize the higher value application of solid waste coal ash.
Description
Technical field
The invention belongs to changing rejected material to useful resource field, is related to a kind of using flyash as silicon source and the class fenton catalyst of source of iron
And application.
Background technology
Flyash is one of large solid waste of coal-burning power plant and coal-burning boiler generation.By the end of the year 2014, China's fire
For power generator installation total capacity up to 9.16 hundred million kilowatts, 41,73,100,000,000 kilowatt hour of generated energy, produces flyash up to 5.78 hundred million tons.Powder
The stacking of coal ash does not only take up a large amount of soils, and causes serious environmental pollution.At present, comprehensive utilization of the China to flyash
Rate alreadys exceed 70%, but is concentrated mainly on the fields such as the relatively low urban architecture of added value, road engineering, ecological backfill, agricultural,
Become more meticulous very low with higher value application ratio.
Flyash main component includes SiO2、Al2O3、FeO、Fe2O3And CaO etc., using coal ash for manufacturing for high added value
Product can not only alleviate flyash heap and be rivals in a contest pressure caused by environment, can also realize the recycling of solid waste, therefore be subject to the country
The concern of outer experts and scholars.The a large amount of SiO of fly ash content2And Al2O3, it is expected to it and is closed as substituted for silicon, aluminum chemistry pure reagent
Into the suitable feedstock of sial mesopore molecular sieve.Such as Chinese invention patent CN102557063B《Prepared by raw material of fly ash in electric power plant
The method and molecular sieve of molecular sieve》Disclose it is a kind of using fly ash in electric power plant as raw material, W type molecular sieves are synthesized by alkaline agent of KOH
Method, the molecular sieve of preparation have unique preferential strong selectivity absorption property for polarity, unsaturation and easy polar molecule,
It is used to work well during the simultaneous removing of nitrogen phosphorus in water process.Chinese invention patent CN103787354B《One kind utilizes fine coal
Ash prepares the application of Cr (VI) ion in MCM-41 adsorbent solutions》Provide a kind of side that MCM-41 is prepared using Hydrothermal Synthesiss
Method, but HCl treatment flyash original powder is used in pretreatment process, the metal ion in flyash is removed in the lump, causes gold
Belong to the secondary pollution and waste of ion.Chinese invention patent CN103769045B《A kind of fly ash base high-performance sorbing material
Preparation method》The method that high-performance sorbing material is prepared using flyash as raw material is provided, can be by the silicon in flyash, aluminium etc.
Conversion is the active ingredient in sorbing material, and positive effect is played for absorption Pollutants in Wastewater.To sum up, existing profit
With coal ash for manufacturing for the method for molecular sieve using based on silicon source and silicon source, to fail effectively for the metal component in flyash
Utilize, cause the wasting of resources, while can also cause the secondary pollution of metal ion.So far, gold in flyash is directly utilized
The molecular sieve catalyst for belonging to component preparation assembling metal ion is rarely reported.
The content of the invention
It is an object of the invention to overcome the prior art to prepare molecular sieve using the silicon source in flyash and silicon source merely to inhale
Enclosure material, there is provided a kind of while prepare molecular sieve carried metal class Fenton using the silica in flyash and metal component and urge
The method of agent.Prepared catalyst also produces freely in addition to stronger adsorption capacity with active oxidation agent
The performance of base degrading waste water organic matter.
To achieve the above object, the present invention uses following technical scheme：
(1) by the dry flyash original powder hydrochloric acid acidification to constant weight, filter, wash, be dried for standby, hydrochloric acid filtrate
It is spare；
(2) flyash and sodium hydroxide ground and mixed obtained step (1) is uniform, and deionized water is added to after roasting
In, it is spare that supernatant is isolated after stirring；
(3) template CTAB and dispersant PEG are dissolved in deionized water, are mixed with above-mentioned supernatant, after stirring evenly,
It is 7 to adjust pH value of solution using the hydrochloric acid filtrate retained in step (1)；
(4) solution obtained in step (3) is placed in reaction kettle after carrying out crystallization and taken out, filtered, washing, do
Dry and roasting obtains Fe/Al-MCM-41 class fenton catalysts.
The concentration of hydrochloric acid is 5~8mol/L in the step (1).
The mass ratio of flyash and sodium hydroxide is 1 in the step (2):(1.0~2.0).
Step (2) roasting carries out in Muffle furnace, and temperature is 550 DEG C, roasting time 5h.
Template in the step (3)：Dispersant：The mass ratio of water is 1:1:20.
Mixed liquor pH value is adjusted using the hydrochloric acid filtrate obtained in step (1) in the step (3), wherein containing flyash
The metal ion of dissolution.
Crystallization temperature is 110 DEG C, crystallization time 12h in the step (4), and calcination temperature is 400 DEG C, and roasting time is
4h, heating rate are 1 DEG C/min.
Using technical solution provided by the invention, compared with existing known technology, there is following remarkable result：
(1) while using the silica in flyash and metal component molecular sieve carried metal class fenton catalyst is prepared,
Both realize the recycling of flyash, and turn avoid the secondary pollution and waste of metal ion in utilization of fly ash；
(2) keeping the stronger absorption property of molecular sieve at the same time, having by metallic iron active oxidation agent in catalyst to waste water
Machine thing carries out efficient degradation.
Brief description of the drawings
Fig. 1 is Fe/Al-MCM-41 catalyst X-ray diffractograms prepared in the embodiment of the present invention 1.
Fig. 2 is Fe/Al-MCM-41 catalyst SEM-EDS figures prepared in the embodiment of the present invention 1.
Fig. 3 is the Fe/Al-MCM-41 catalysts ammonium persulfate-sodium bisulfate degraded H prepared in the embodiment of the present invention 1
The removal effect tendency chart of acid.
Embodiment
Technical scheme is described in further detail below in conjunction with the drawings and specific embodiments, the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1
A kind of Fe/Al-MCM-41 class fenton catalyst preparation and application using flyash as silicon source and source of iron：
(1) 20.0g flyash original powders are weighed, 80 DEG C that drying to constant weight is spare, by above-mentioned flyash original powder and 80mL concentration
To handle 3h in 60 DEG C of water-baths after 6mol/L mixed in hydrochloric acid, then it is separated by filtration, reservation filtrate is spare, after Washing of Filter Cake
Drying.
(2) weigh respectively in step (1) the flyash 10.0g of pretreatment and 15.0g sodium hydroxides in agate mortar into
Row grinding, is placed in Muffle kiln roasting 5h, and calcination temperature is 550 DEG C, is mixed after natural cooling with 50mL deionized waters, magnetic force stirs
12h is mixed, takes supernatant spare.
(3) 0.75g templates are weighed respectively and 0.75g dispersants are dissolved in 15mL deionized waters, magnetic agitation to solution
Uniformly, while by the supernatant obtained in step (2) it is slowly added in solution, continues to stir 1h, with the salt retained in step (1)
It is 7 that acid solution, which adjusts pH value of solution, continues to stir 2h acquisition milk yellow colloidal sols.Yellow sol is transferred to 100mL polytetrafluoroethylene (PTFE)
In reaction kettle, 110 DEG C of crystallization 12h, question response kettle cooled to room temperature after the completion of crystallization, obtains milk yellow suspension, filtering
Washing is 400 DEG C after Muffle kiln roasting 5h, calcination temperature for 7,80 DEG C of dryings to pH, and heating rate is 1 DEG C/min, to obtain the final product
Fe/Al-MCM-41 catalyst.
The XRD spectra of Fe/Al-MCM-41 catalyst manufactured in the present embodiment is as shown in Figure 1, SEM-EDS is analyzed such as Fig. 2 institutes
Show.As seen from Figure 1, sample is about to have a diffraction maximum at 1.95 in 2 θ, which is mesostructured material
Characteristic peak.The catalyst that Fig. 2 EDS characterization results illustrate to prepare contains metallic element Fe.
The Fe/Al-MCM-41 prepared using embodiment 1 be the H that class fenton catalyst is degraded in simulated wastewater it is sour (1- amino-
8- naphthols -3,6- disulfonic acid).50mL concentration be 20mg/L H acid solutions in add 0.01gFe/Al-MCM-41 catalyst and
1mL concentration is 0.06mol/L oxidants Oxone (ammonium persulfate-sodium bisulfate), reacts 1h, H acid degradations under 60 DEG C of water bath conditions
Situation is as shown in Figure 3.With the experimental result contrast for being individually added into oxidant as can be seen that being urged using the class Fenton of this programme preparation
Agent has stronger active oxidation agent ability.
Using Fe/Al-MCM-41 prepared by embodiment 1 as the o-chlorphenol in class fenton catalyst degraded simulated wastewater.
0.01gFe/Al-MCM-41 catalyst is added in the ortho-chloro phenol solution that 50mL concentration is 20mg/L and 1mL concentration is
3min is reacted under 0.06mol/L oxidants Oxone, 385W microwave condition, o-chlorophenol degradation rate reaches 86.1%.
Embodiment 2
It is a kind of to be prepared by the Fe/Al-MCM-41 classes fenton catalyst of silicon source and source of iron of flyash, substantially with embodiment 1,
Preparation process is as follows：
(1) 20.0g flyash original powders are weighed, 80 DEG C that drying to constant weight is spare, by above-mentioned flyash original powder and 80mL concentration
To handle 3h in 60 DEG C of water-baths after 6mol/L mixed in hydrochloric acid, then it is separated by filtration, reservation filtrate is spare, after Washing of Filter Cake
Drying.
(2) weigh respectively in step (1) the flyash 10.0g of pretreatment and 10.0g sodium hydroxides in agate mortar into
Row grinding, is placed in Muffle kiln roasting 5h, and calcination temperature is 550 DEG C, is mixed after natural cooling with 50mL deionized waters, magnetic force stirs
12h is mixed, takes supernatant spare.
(3) 0.75g templates are weighed respectively and 0.75g dispersants are dissolved in 15mL deionized waters, magnetic agitation to solution
Uniformly, while by the supernatant obtained in step (2) it is slowly added in solution, continues to stir 1h, with the salt retained in step (1)
It is 7 that acid solution, which adjusts pH value of solution, continues to stir 2h acquisition milk yellow colloidal sols.Yellow sol is transferred to 100mL polytetrafluoroethylene (PTFE)
In reaction kettle, 110 DEG C of crystallization 12h, question response kettle cooled to room temperature after the completion of crystallization, obtains milk yellow suspension, filtering
Washing is 400 DEG C after Muffle kiln roasting 5h, calcination temperature for 7,80 DEG C of dryings to pH, and heating rate is 1 DEG C/min, to obtain the final product
Fe/Al-MCM-41 catalyst.
Embodiment 3
It is a kind of to be prepared by the Fe/Al-MCM-41 classes fenton catalyst of silicon source and source of iron of flyash, substantially with embodiment 1,
Preparation process is as follows：
(1) 20.0g flyash original powders are weighed, 80 DEG C that drying to constant weight is spare, by above-mentioned flyash original powder and 80mL concentration
To handle 3h in 60 DEG C of water-baths after 8mol/L mixed in hydrochloric acid, then it is separated by filtration, reservation filtrate is spare, after Washing of Filter Cake
Drying.
(2) weigh respectively in step (1) the flyash 10.0g of pretreatment and 20.0g sodium hydroxides in agate mortar into
Row grinding, is placed in Muffle kiln roasting 5h, and calcination temperature is 550 DEG C, is mixed after natural cooling with 50mL deionized waters, magnetic force stirs
12h is mixed, takes supernatant spare.
(3) 0.75g templates are weighed respectively and 0.75g dispersants are dissolved in 15mL deionized waters, magnetic agitation to solution
Uniformly, while by the supernatant obtained in step (2) it is slowly added in solution, continues to stir 1h, with the salt retained in step (1)
It is 7 that acid solution, which adjusts pH value of solution, continues to stir 2h acquisition milk yellow colloidal sols.Yellow sol is transferred to 100mL polytetrafluoroethylene (PTFE)
In reaction kettle, 110 DEG C of crystallization 12h, question response kettle cooled to room temperature after the completion of crystallization, obtains milk yellow suspension, filtering
Washing is 400 DEG C after Muffle kiln roasting 5h, calcination temperature for 7,80 DEG C of dryings to pH, and heating rate is 1 DEG C/min, to obtain the final product
Fe/Al-MCM-41 catalyst.
Claims (7)
- It is 1. a kind of using flyash as silicon source and the class fenton catalyst of source of iron, it is characterised in that the catalyst passes through following step It is rapid to prepare：(1) by the dry flyash original powder hydrochloric acid acidification to constant weight, filtering, wash to neutrality, spare after drying, hydrochloric acid Filtrate A is spare；(2) it is the flyash after acidification and sodium hydroxide ground and mixed is uniform, added after roasting in deionized water, stirring It is spare that supernatant B is isolated after 12h；(3) template CTAB and dispersant PEG are dissolved in deionized water, are mixed with supernatant B, adjusted using hydrochloric acid filtrate A PH value of solution is 7, continues to stir 2h, obtains solution C；(4) solution C is placed in reaction kettle after 110 DEG C of crystallization 12h and taken out, filtered, washing, dry and roasting obtain Fe/Al- MCM-41 class fenton catalysts.
- 2. preparation method according to claim 1, it is characterised in that：In the step (1) concentration of hydrochloric acid for 5~ 8mol/L。
- 3. preparation method according to claim 1, it is characterised in that：Flyash and sodium hydroxide in the step (2) Mass ratio is 1:(1.0~2.0).
- 4. preparation method according to claim 1, it is characterised in that：Template in the step (3):Dispersant:Water Mass ratio is 1:1:20.
- 5. preparation method according to claim 1, it is characterised in that：The salt retained in the step (3) using step (1) Acidleach liquid A adjusts pH of mixed, wherein containing the metal ion separated out in flyash original powder.
- 6. preparation method according to claim 1, it is characterised in that：Calcination temperature in the step (4) is 400 DEG C, Roasting time is 4h, and heating rate is 1 DEG C/min.
- 7. the application using flyash as silicon source and the class fenton catalyst of source of iron as described in claim 1~6 is any, its feature It is：The catalyst can activate persulfate and degrade to wastewater through organic matter.
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Cited By (7)
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| CN108993457A (en) * | 2018-07-27 | 2018-12-14 | 河北科技大学 | A method of adsorbent is prepared by raw material of flyash |
| CN109592776A (en) * | 2019-02-02 | 2019-04-09 | 常熟理工学院 | A kind of preparation method of the waste water renovation agent based on flying ash |
| CN110639599A (en) * | 2019-10-19 | 2020-01-03 | 青岛科技大学 | Copper-iron bimetal doped modified fly ash-molecular sieve composite catalyst and preparation method and application thereof |
| CN113578260A (en) * | 2021-07-23 | 2021-11-02 | 宁夏大学 | Preparation method of fly ash-based MCM-41 mesoporous molecular sieve and product thereof |
| CN113649061A (en) * | 2021-08-25 | 2021-11-16 | 华能(福建漳州)能源有限责任公司 | Method for synthesizing denitration catalyst by coal-fired power plant fly ash self-digestion |
| CN114534772A (en) * | 2022-01-17 | 2022-05-27 | 西华大学 | Catalyst for antibiotic wastewater treatment and application thereof |
| CN115770609A (en) * | 2022-11-17 | 2023-03-10 | 华电电力科学研究院有限公司 | Preparation method of fly ash-based Fe/ZSM-5 mesoporous molecular sieve catalyst |
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| CN108993457A (en) * | 2018-07-27 | 2018-12-14 | 河北科技大学 | A method of adsorbent is prepared by raw material of flyash |
| CN109592776A (en) * | 2019-02-02 | 2019-04-09 | 常熟理工学院 | A kind of preparation method of the waste water renovation agent based on flying ash |
| CN109592776B (en) * | 2019-02-02 | 2021-04-27 | 常熟理工学院 | Preparation method of waste water repairing agent based on incineration fly ash |
| CN110639599A (en) * | 2019-10-19 | 2020-01-03 | 青岛科技大学 | Copper-iron bimetal doped modified fly ash-molecular sieve composite catalyst and preparation method and application thereof |
| CN113578260A (en) * | 2021-07-23 | 2021-11-02 | 宁夏大学 | Preparation method of fly ash-based MCM-41 mesoporous molecular sieve and product thereof |
| CN113649061A (en) * | 2021-08-25 | 2021-11-16 | 华能(福建漳州)能源有限责任公司 | Method for synthesizing denitration catalyst by coal-fired power plant fly ash self-digestion |
| CN114534772A (en) * | 2022-01-17 | 2022-05-27 | 西华大学 | Catalyst for antibiotic wastewater treatment and application thereof |
| CN115770609A (en) * | 2022-11-17 | 2023-03-10 | 华电电力科学研究院有限公司 | Preparation method of fly ash-based Fe/ZSM-5 mesoporous molecular sieve catalyst |
| CN115770609B (en) * | 2022-11-17 | 2024-04-19 | 华电电力科学研究院有限公司 | Preparation method of fly ash-based Fe/ZSM-5 mesoporous molecular sieve catalyst |
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Application publication date: 20180504 |