CN109110909A - A kind of preparation method of Ag doping modification biological filtrate - Google Patents
A kind of preparation method of Ag doping modification biological filtrate Download PDFInfo
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- CN109110909A CN109110909A CN201811014652.5A CN201811014652A CN109110909A CN 109110909 A CN109110909 A CN 109110909A CN 201811014652 A CN201811014652 A CN 201811014652A CN 109110909 A CN109110909 A CN 109110909A
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- 239000000706 filtrate Substances 0.000 title claims abstract description 32
- 230000004048 modification Effects 0.000 title claims abstract description 24
- 238000012986 modification Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000463 material Substances 0.000 claims abstract description 24
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 18
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 18
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 18
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 16
- 229960004853 betadex Drugs 0.000 claims abstract description 16
- 230000001699 photocatalysis Effects 0.000 claims abstract description 14
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 58
- 239000000243 solution Substances 0.000 claims description 23
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000000945 filler Substances 0.000 claims description 12
- 238000007146 photocatalysis Methods 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 9
- -1 chloropropionate Alkane Chemical class 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- 238000001746 injection moulding Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004743 Polypropylene Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 229920001155 polypropylene Polymers 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims 6
- 229910001923 silver oxide Inorganic materials 0.000 claims 1
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 238000005215 recombination Methods 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 230000004888 barrier function Effects 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000005672 electromagnetic field Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 9
- 230000001376 precipitating effect Effects 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 239000010865 sewage Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 235000015097 nutrients Nutrition 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 210000004081 cilia Anatomy 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
-
- 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
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Microbiology (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Biodiversity & Conservation Biology (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The present invention relates to a kind of preparation methods of Ag doping modification biological filtrate, belong to clean and environmental protection field of material technology.The present invention is using the effect of microwave electromagnetic field come heat medium, silver orthophosphate is prepared by microwave-assisted sluggish precipitation, and it is deposited on nano-titanium dioxide, manufactured silver orthophosphate is cubic four-footed shape, to being absorbed and utilized for visible light, photo-generate electron-hole is small to recombination probability, with titanium dioxide it is compound after embed through beta-cyclodextrin, so that it had both had the structure of beta-cyclodextrin cavity, there is stronger mechanical strength again, preferable translucency, biggish specific surface area, this characteristic, which can greatly improve, receives silver orthophosphate/composite titania material surface pollutant concentration, improve catalytic efficiency, simultaneously because the barrier action of beta-cyclodextrin, reduce electron-hole pair recombination probability, reduce electron-hole pair in crystals and, photocatalytic activity is improved.The present invention has a vast market foreground and application prospect.
Description
Technical field
The present invention relates to a kind of preparation methods of Ag doping modification biological filtrate, belong to clean and environmental protection field of material technology.
Background technique
The processing of city domestic sewage is an important component of efforts at environmental protection, handles the fine or not of quality and is made
Filtrate has direct relation, at present used in filter, be powdered such as to be built so that quartz sand is as the main component mostly
It builds with river sand or other such as by vitrified bond at short grained ceramic grain filter.These filtrates it is different degrees of there are one
A little problems, such as river sand are the graininess of very little, and filtrate itself does not have hole, and filtration is by the gap between filtrate
Come what is completed, suspended matter, the impurity being used for a long time in sewage are easy to the gap between blocking sand, lose filtration, make
With the time is short, replacement is inconvenient, while being also unfavorable for the formation and attachment of biomembrane；It is sintered little particle filtrate, porosity is low, raw
The adhesion property of object film is low, and filter effect is poor, and biochemical property cannot be met the requirements, and, sintering system high in sintering manufacturing cost
The gases such as great amount of carbon dioxide can be also generated during making, cause environmental pollution.
Biomembrane process due to using filtrate (carrier) can not only improve the microorganism aggregation degree in reaction tank, to mention
High disposal effect, and the superperformance of the anti-load impact of organic matter can be played, therefore be applied to a variety of sewage treatment process.
It is easy to accomplish for removing the technique composition of organic matter and nutrient salts, therefore the prior art has developed a variety of biomembrane sides
Method, but existing product major part existing defects, photocatalysis performance is undesirable, can not effectively remove organic matter and nutrient salts.
Filtrate applied to above-mentioned biomembrane process by shape point there are many selection, including sponge-type, cilium shape, cast,
Ball-type etc.；Different materials can also be selected, organic material includes the macromolecule resin materials such as polyethanol, polyvinyl alcohol, polysulfones,
And inorganic material includes granular active carbon, volcanic ash, ceramics etc..With the difference of filtrate usage mode, technique constitute and
Drive manner different from, but its basic performance depends primarily on the formed biomembrane of filter material surface.Simultaneously as should be in filtrate
This precondition that surface is initially formed biomembrane is even more important more than durability, economy.Therefore, using how many upper limitation
Property.The said goods existing defects, photocatalysis performance is poor, and titanium dioxide is unevenly distributed.
Summary of the invention
The technical problems to be solved by the invention: existing existing product major part existing defects are directed to, photocatalysis performance is not
Ideal, provides a kind of preparation side of Ag doping modification biological filtrate at the problem of can not effectively removing organic matter and nutrient salts
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of Ag doping modification biological filtrate, specific preparation step are as follows:
(1) taking urea, silver nitrate, nano-titanium dioxide, that stirring in deionized water is added is mixed by 1:10 in mass ratio after mixing
Close, add phosphoric acid, be fitted into reaction kettle react after mixing evenly, after being cooled to room temperature filter, wash, dry, obtain silver orthophosphate/
Composite titania material；
(2) taking beta-cyclodextrin that mass fraction is added is to be stirred in 25% sodium hydroxide solution, then epoxychloropropane is added dropwise, after
1~2h of continuous stirring, obtains prepolymer；
(3) taking silver orthophosphate/composite titania material that mass fraction is added is in 25% sodium hydroxide solution, with 300W ultrasonic wave
15~20min of ultrasonic disperse, obtains dispersion liquid, and dispersion liquid is added in prepolymer and stirs 20~30min, adds epoxy chloropropionate
Alkane is stirred to react 2~3h at 60~70 DEG C, filters, washes after being cooled to room temperature, is dry, obtaining photocatalysis filler；
(4) it takes photocatalysis filler, polypropylene to be fitted into and melt blending in instrument is blended, mixture is packed into after being cooled to 40~50 DEG C and is infused
Injection molding in instrument is moulded, and under 1~2MPa pressure, heat preservation 1~2h of compacting, discharge to obtain Ag doping modification biological filtrate.
Step (1) urea, silver nitrate, nano-titanium dioxide, phosphoric acid molar ratio be 3:6:6:2.
Step (1) reaction process is microwave heating to 80~90 DEG C, 30~40min of insulation reaction.
Step (2) beta-cyclodextrin, sodium hydroxide solution, epoxychloropropane parts by weight be 3~6 parts of beta-cyclodextrins,
100~200 parts of sodium hydroxide solutions, 1.8~3.6 parts of epoxychloropropane.
Step (3) silver orthophosphate/composite titania material, sodium hydroxide solution, epoxychloropropane parts by weight be
10~20 parts of silver orthophosphate/composite titania materials, 100~200 parts of sodium hydroxide solutions, 1.8~3.6 parts of epoxychloropropane.
The mass ratio of the silver orthophosphate/composite titania material and beta-cyclodextrin is 5:3~20:3.
Step (4) melting temperature is 220~240 DEG C.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention using the effect of microwave electromagnetic field come heat medium, have heating speed fastly, homogeneous heating, it is energy-efficient,
The characteristics of convenient for controlling, prepares silver orthophosphate by microwave-assisted sluggish precipitation, and is deposited on nano-titanium dioxide, manufactured
Silver orthophosphate is cubic four-footed shape, small to recombination probability to being absorbed and utilized of visible light, photo-generate electron-hole, with dioxy
Change titanium it is compound after embedded through beta-cyclodextrin so that it had not only had a structure of beta-cyclodextrin cavity, but have stronger mechanical strength,
Preferable translucency, biggish specific surface area, this characteristic, which can greatly improve, receives silver orthophosphate/composite titania material surface
Pollutant concentration improves catalytic efficiency, simultaneously because the barrier action of beta-cyclodextrin, reduces electron-hole pair recombination probability, subtract
Few electron-hole pair in crystals and, improve photocatalytic activity；
(2) present invention is by increasing the contact area of titanium dioxide and silver orthophosphate, and then promotes the light that the excitation of silver orthophosphate light generates
The separative efficiency of raw electron-hole, while during light degradation, a small amount of Ag existing for phosphoric acid silver surface+It can gradually be reduced into
Simple substance Ag can increase the absorption transfer capability to photon by the plasma resonance effect of Ag, to further increase the life
Object filtrate Photocatalytic Degradation Property.
Specific embodiment
15~30mmol urea, 30~60mmol silver nitrate are taken, 30~60mmol nano-titanium dioxide is pressed after mixing
Mass ratio 1:10 is added in deionized water, stirs 20~30min with 300~400r/min, adds 10~20mmol phosphoric acid, stir
It is fitted into reaction kettle after mixing uniformly, and microwave heating, to 80~90 DEG C, 30~40min of insulation reaction is filtered after being cooled to room temperature
Filter residue is obtained, filter residue 2~3 times is washed with deionized and is placed in drying box, dries at 60~80 DEG C to constant weight, obtains phosphoric acid
Silver/titanium dioxide composite material, takes 3~6g beta-cyclodextrin, and 100~200g mass fraction is added and is in 25% sodium hydroxide solution,
20~30min is stirred with 200~300r/min, then 1.8~3.6g epoxychloropropane is added dropwise with 0.1~0.2g/min, continues to stir
1~2h is mixed, prepolymer is obtained, takes 10~20g silver orthophosphate/composite titania material, it is 25% that 100~200g mass fraction, which is added,
In sodium hydroxide solution, 15~20min is dispersed with 300W ultrasonic echography, obtains dispersion liquid, dispersion liquid is added in prepolymer and is stirred
20~30min is mixed, 1.8~3.6g epoxychloropropane is added, 2~3h is stirred to react at 60~70 DEG C, after being cooled to room temperature
It filters to obtain precipitating, is washed with deionized and is precipitated to cleaning solution and is in neutrality, then precipitating is placed in drying box, at 60~70 DEG C
It dries to constant weight, obtains photocatalysis filler, take 1.5~1.8g photocatalysis filler, 120~150g polypropylene, which is fitted into, to be blended in instrument,
Melting mixing is uniform at 220~240 DEG C, and mixture is fitted into injection molding in injection molding instrument after being cooled to 40~50 DEG C, and 1~
Under 2MPa pressure, heat preservation 1~2h of compacting, discharge to obtain Ag doping modification biological filtrate.
Example 1
15mmol urea is taken, 30mmol silver nitrate, 30mmol nano-titanium dioxide, 1:10 in mass ratio is added and goes after mixing
In ionized water, 20min is stirred with 300r/min, 10mmol phosphoric acid is added, is fitted into reaction kettle after mixing evenly, and microwave adds
For heat to 80 DEG C, insulation reaction 30min filters to obtain filter residue after being cooled to room temperature, and is washed with deionized filter residue 2 times and is placed on drying
It in case, dries at 60 DEG C to constant weight, obtains silver orthophosphate/composite titania material, take 3g beta-cyclodextrin, 100g mass point is added
Number is to stir 20min in 25% sodium hydroxide solution with 200r/min, then 1.8g epoxychloropropane is added dropwise with 0.1g/min, continue
1h is stirred, prepolymer is obtained, takes 10g silver orthophosphate/composite titania material, it is that 25% sodium hydroxide is molten that 100g mass fraction, which is added,
In liquid, 15min is dispersed with 300W ultrasonic echography, obtains dispersion liquid, dispersion liquid is added in prepolymer and stirs 20min, is added
1.8g epoxychloropropane is stirred to react 2h at 60 DEG C, and precipitating is filtered to obtain after being cooled to room temperature, is washed with deionized and is precipitated to
Cleaning solution is in neutrality, then precipitating is placed in drying box, is dried at 60 DEG C to constant weight, is obtained photocatalysis filler, 1.5g light is taken to urge
Change filler, 120g polypropylene, which is fitted into, to be blended in instrument, and melting mixing is uniform at 220 DEG C, mixture is packed into after being cooled to 40 DEG C
It is molded injection molding in instrument, and under 1MPa pressure, heat preservation compacting 1h, discharge to obtain Ag doping modification biological filtrate.
Example 2
22mmol urea is taken, 45mmol silver nitrate, 45mmol nano-titanium dioxide, 1:10 in mass ratio is added and goes after mixing
In ionized water, 25min is stirred with 350r/min, 15mmol phosphoric acid is added, is fitted into reaction kettle after mixing evenly, and microwave adds
For heat to 85 DEG C, insulation reaction 35min filters to obtain filter residue after being cooled to room temperature, and is washed with deionized filter residue 2 times and is placed on drying
It in case, dries at 70 DEG C to constant weight, obtains silver orthophosphate/composite titania material, take 5g beta-cyclodextrin, 150g mass point is added
Number is to stir 25min in 25% sodium hydroxide solution with 250r/min, then 2.7g epoxychloropropane is added dropwise with 0.15g/min, after
Continuous stirring 1h, obtains prepolymer, takes 15g silver orthophosphate/composite titania material, and addition 150g mass fraction is 25% sodium hydroxide
In solution, 17min is dispersed with 300W ultrasonic echography, obtains dispersion liquid, dispersion liquid is added in prepolymer and stirs 25min, then plus
Enter 2.7g epoxychloropropane, be stirred to react 2h at 65 DEG C, precipitating is filtered to obtain after being cooled to room temperature, precipitating is washed with deionized
It is in neutrality to cleaning solution, then precipitating is placed in drying box, dried at 65 DEG C to constant weight, obtain photocatalysis filler, take 1.7g light
Catalytic filler, 135g polypropylene, which is fitted into, to be blended in instrument, and melting mixing is uniform at 230 DEG C, fills mixture after being cooled to 45 DEG C
Enter to be molded injection molding in instrument, and under 1MPa pressure, heat preservation compacting 1h, discharge to obtain Ag doping modification biological filtrate.
Example 3
30mmol urea is taken, 60mmol silver nitrate, 60mmol nano-titanium dioxide, 1:10 in mass ratio is added and goes after mixing
In ionized water, 30min is stirred with 400r/min, 20mmol phosphoric acid is added, is fitted into reaction kettle after mixing evenly, and microwave adds
For heat to 90 DEG C, insulation reaction 40min filters to obtain filter residue after being cooled to room temperature, and is washed with deionized filter residue 3 times and is placed on drying
It in case, dries at 80 DEG C to constant weight, obtains silver orthophosphate/composite titania material, take 6g beta-cyclodextrin, 200g mass point is added
Number is to stir 30min in 25% sodium hydroxide solution with 300r/min, then 3.6g epoxychloropropane is added dropwise with 0.2g/min, continue
2h is stirred, prepolymer is obtained, takes 20g silver orthophosphate/composite titania material, it is that 25% sodium hydroxide is molten that 200g mass fraction, which is added,
In liquid, 20min is dispersed with 300W ultrasonic echography, obtains dispersion liquid, dispersion liquid is added in prepolymer and stirs 30min, is added
3.6g epoxychloropropane is stirred to react 3h at 70 DEG C, and precipitating is filtered to obtain after being cooled to room temperature, is washed with deionized and is precipitated to
Cleaning solution is in neutrality, then precipitating is placed in drying box, is dried at 70 DEG C to constant weight, is obtained photocatalysis filler, 1.8g light is taken to urge
Change filler, 150g polypropylene, which is fitted into, to be blended in instrument, and melting mixing is uniform at 240 DEG C, mixture is packed into after being cooled to 50 DEG C
It is molded injection molding in instrument, and under 2MPa pressure, heat preservation compacting 2h, discharge to obtain Ag doping modification biological filtrate.
Ag doping modification biological filtrate prepared by the present invention is detected, specific detection is as follows:
Using the biofilter material of Guangzhou company production as comparative example, sanitary sewage is taken, by dosage 100mg/L, the present invention is made
Standby Ag doping modification biological filtrate is handled sanitary sewage with the filtering velocity of 20n/h, specific testing result such as following table table 1.
1 Ag doping modification biological media performance of table characterization
Ag doping modification biological media performance prepared by the present invention as shown in Table 1, COD removal rate is high, NH3- N removal rate is high, should
Biofilter material Photocatalytic Degradation Property is good, and Ag doping modification biological filtrate prepared by the present invention has a vast market foreground and answers
Use prospect.
Claims (7)
1. a kind of preparation method of Ag doping modification biological filtrate, which is characterized in that specific preparation step are as follows:
(1) taking urea, silver nitrate, nano-titanium dioxide, that stirring in deionized water is added is mixed by 1:10 in mass ratio after mixing
Close, add phosphoric acid, be fitted into reaction kettle react after mixing evenly, after being cooled to room temperature filter, wash, dry, obtain silver orthophosphate/
Composite titania material；
(2) taking beta-cyclodextrin that mass fraction is added is to be stirred in 25% sodium hydroxide solution, then epoxychloropropane is added dropwise, after
1~2h of continuous stirring, obtains prepolymer；
(3) taking silver orthophosphate/composite titania material that mass fraction is added is in 25% sodium hydroxide solution, with 300W ultrasonic wave
15~20min of ultrasonic disperse, obtains dispersion liquid, and dispersion liquid is added in prepolymer and stirs 20~30min, adds epoxy chloropropionate
Alkane is stirred to react 2~3h at 60~70 DEG C, filters, washes after being cooled to room temperature, is dry, obtaining photocatalysis filler；
(4) it takes photocatalysis filler, polypropylene to be fitted into and melt blending in instrument is blended, mixture is packed into after being cooled to 40~50 DEG C and is infused
Injection molding in instrument is moulded, and under 1~2MPa pressure, heat preservation 1~2h of compacting, discharge to obtain Ag doping modification biological filtrate.
2. a kind of preparation method of Ag doping modification biological filtrate as described in claim 1, which is characterized in that step (1) institute
State urea, silver nitrate, nano-titanium dioxide, phosphoric acid molar ratio be 3:6:6:2.
3. a kind of preparation method of Ag doping modification biological filtrate as described in claim 1, which is characterized in that step (1) institute
Stating reaction process is microwave heating to 80~90 DEG C, 30~40min of insulation reaction.
4. a kind of preparation method of Ag doping modification biological filtrate as described in claim 1, which is characterized in that step (2) institute
State beta-cyclodextrin, sodium hydroxide solution, epoxychloropropane parts by weight be 3~6 parts of beta-cyclodextrins, 100~200 parts of sodium hydroxides
Solution, 1.8~3.6 parts of epoxychloropropane.
5. a kind of preparation method of Ag doping modification biological filtrate as described in claim 1, which is characterized in that step (3) institute
State silver orthophosphate/composite titania material, sodium hydroxide solution, epoxychloropropane parts by weight be 10~20 parts of silver orthophosphate/bis-
Titanium oxide composite material, 100~200 parts of sodium hydroxide solutions, 1.8~3.6 parts of epoxychloropropane.
6. a kind of preparation method of Ag doping modification biological filtrate as described in claim 1, which is characterized in that the phosphoric acid
The mass ratio of silver/titanium dioxide composite material and beta-cyclodextrin is 5:3~20:3.
7. a kind of preparation method of Ag doping modification biological filtrate as described in claim 1, which is characterized in that step (4) institute
Stating melting temperature is 220~240 DEG C.
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| CN116059739A (en) * | 2023-03-06 | 2023-05-05 | 山东华城工程技术有限公司 | Silver-doped surface-modified multifunctional filter material and preparation method and application thereof |
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