CN108404992A - A kind of preparation method of PVA sponges loading nano silvery material and application - Google Patents
A kind of preparation method of PVA sponges loading nano silvery material and application Download PDFInfo
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- CN108404992A CN108404992A CN201810201626.7A CN201810201626A CN108404992A CN 108404992 A CN108404992 A CN 108404992A CN 201810201626 A CN201810201626 A CN 201810201626A CN 108404992 A CN108404992 A CN 108404992A
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 73
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 34
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 19
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 19
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229960003638 dopamine Drugs 0.000 claims abstract description 17
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007983 Tris buffer Substances 0.000 claims abstract description 14
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 13
- 239000000975 dye Substances 0.000 claims abstract description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000006260 foam Substances 0.000 claims description 14
- 239000011265 semifinished product Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- WTDRDQBEARUVNC-UHFFFAOYSA-N L-Dopa Natural products OC(=O)C(N)CC1=CC=C(O)C(O)=C1 WTDRDQBEARUVNC-UHFFFAOYSA-N 0.000 claims description 3
- MHUWZNTUIIFHAS-CLFAGFIQSA-N dioleoyl phosphatidic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(COP(O)(O)=O)OC(=O)CCCCCCC\C=C/CCCCCCCC MHUWZNTUIIFHAS-CLFAGFIQSA-N 0.000 claims description 3
- 229960004502 levodopa Drugs 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 2
- 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 claims 2
- 229910052796 boron Inorganic materials 0.000 claims 2
- 239000001257 hydrogen Substances 0.000 claims 2
- 229910052708 sodium Inorganic materials 0.000 claims 2
- 239000011734 sodium Substances 0.000 claims 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- -1 be cleaned and dried Substances 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 239000010842 industrial wastewater Substances 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 63
- 229920002451 polyvinyl alcohol Polymers 0.000 description 63
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 63
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 6
- 230000003139 buffering effect Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 2
- JYCQQPHGFMYQCF-UHFFFAOYSA-N 4-tert-Octylphenol monoethoxylate Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(OCCO)C=C1 JYCQQPHGFMYQCF-UHFFFAOYSA-N 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 230000008953 bacterial degradation Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 description 1
- 229950004053 octoxinol Drugs 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance 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
- 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
-
- 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
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
-
- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- 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
-
- 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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of preparation methods of PVA sponges loading nano silvery material, specifically comprise the following steps：Prepare PVA sponges；PVA sponges are soaked in dopamine solution, Tris buffer solutions is used in combination to adjust pH value to 7.0~9.5；PVA sponges after being impregnated by dopamine solution and Tris buffer solutions are soaked in silver nitrate solution；PVA sponges after being impregnated by dopamine solution, Tris buffer solutions and silver nitrate solution are soaked in sodium borohydride solution, are cleaned and dried, PVA sponge loading nano silvery materials are made.PVA sponge loading nano silvery materials are applied to the reduction of p-nitrophenol organic dyestuff in industrial wastewater.Beneficial effects of the present invention are：PVA sponge loading nano silvery materials have excellent catalytic activity in sodium borohydride degradation p-nitrophenol organic dyestuff experiment, and do not cause secondary pollution after the completion of reacting；Good catalytic effect is still kept by being recycled for multiple times.
Description
Technical field
The present invention relates to the reduction technique field of p-nitrophenol organic dyestuff in industrial wastewater more particularly to a kind of PVA
The preparation method of sponge loading nano silvery material and application.
Background technology
P-nitrophenol is very intractable a kind of organic pollution containing phenols in industrial wastewater, under low concentration,
Human body and organism in water can be caused to seriously endanger.The degradation measure of p-nitrophenol includes phase autoclave electric discharge, biology
Bacterial degradation and catalytic degradation method etc..Wherein, p-nitrophenol is reduced into para-aminophenol using efficient different-phase catalyst,
Right and wrong are often with the method for having utility value.Because para-aminophenol is a kind of widely used industrial chemicals, chemical industry, medicine,
The industrial circles such as fuel, rubber and oil dope have critically important application.
Nano-Ag particles are the catalyst of good catalysis sodium borohydride reduction p-nitrophenol.On the one hand, due to quantum
The redox ability of dimensional effect, nano-Ag particles greatly enhances；In addition, since its size is small, large specific surface area, nano silver
Particle has very strong adsorption capacity to organic dyestuff.But nano-Ag particles are easy to reunite, it is difficult to obtain the silver nanoparticle being evenly distributed
Particle；Cause to pollute in addition, silver nano-grain is easy to leak into environment when treating wastewater.For this purpose, usually by nano silver
Grain surface is modified and loads to and prevents it to reunite in various carriers and limit its leakage.But this way can reduce silver nanoparticle
The surface-active and catalytic performance or preparation process of grain are complicated, of high cost, are unfavorable for being generalized to industrial practical application.
Patent CN103460243A discloses a kind of preparation of Temperature-Sensitive Microgel asymmetry supported nano-silver catalyst
Method.Temperature-Sensitive Microgel asymmetry supported nano-silver catalyst prepared by this method shows good Thermo-sensitive, is urging
During changing reduction p-nitrophenol, catalysis reaction efficiency is simultaneously by the common regulation and control of temperature and microgel Thermo-sensitive, table
Reveal good catalytic activity.But the raw material n-isopropyl acrylamide that this method uses is expensive, limits this method
Industrial applications.
Invention content
Technical problem to be solved by the invention is to provide a kind of preparation method of PVA sponges loading nano silvery material with answer
With to overcome above-mentioned deficiency in the prior art.
The technical solution that the present invention solves above-mentioned technical problem is as follows：A kind of preparation of PVA sponges loading nano silvery material
Method specifically comprises the following steps：
S100, PVA sponges are prepared；
S200, PVA sponges are soaked in dopamine solution, Tris buffer solutions is used in combination to adjust pH value to 7.0~9.5；
S300, the PVA sponges after being impregnated by dopamine solution and Tris buffer solutions are soaked in silver nitrate solution；
S400, the PVA sponges after being impregnated by dopamine solution, Tris buffer solutions and silver nitrate solution are soaked in
Sodium borohydride solution is cleaned and dried, and PVA sponge loading nano silvery materials are made.
The specific preparation process of the PVA sponges is as follows：
S110,3~9 parts of PVA, 54 parts of water are added into container, are heated to 85 DEG C~95 DEG C, mechanical agitation, until PVA is complete
Dissolving；
S120,5~15 parts of formaldehyde and 2.5~7.5 parts of 30wt.% triton x-100s are added, stir 5min~30min；
S130,10~15 parts of 50wt.%H are added2SO4, 5min~15min is stirred, foam solution is obtained；
S140, by foam solution transfer empty in container, then by container be put into 45 DEG C~75 DEG C baking ovens cure 2h~
5h obtains sponge semi-finished product；
S150, sponge semi-finished product are washed into 15min~45min with clear water, removes extra sulfuric acid, be put into baking oven and do
It is dry, obtain PVA sponges.The PVA is one kind in PVA-1788, PVA-2088 or PVA-2488.The PVA sponges are in DOPA
The time impregnated in amine aqueous solution is 12h~36h.A concentration of 1g/L~8g/L of the dopamine solution.The PVA sponges are in nitre
The time impregnated in sour silver solution is 6h~18h.A concentration of 0.001mol/L~0.010mol/L of the silver nitrate solution.Institute
It is 1h~5h to state the time that PVA sponges are impregnated in sodium borohydride solution.A concentration of 0.1mol/L of the sodium borohydride solution
~1.0mol/L.
The beneficial effects of the invention are as follows：The invention firstly uses physical blowing, the crosslinked methods of sulfuric acid catalysis, and the seas PVA are made
Then silk floss utilizes the amine-modified PVA sponges of DOPA, and using the reproducibility of dopamine and sodium borohydride that nano-Ag particles are uniform
It loads to inside matrix and the duct of PVA sponges, polyvinylalcohol sponge loading nano silvery material of the present invention is degraded in sodium borohydride
There is excellent catalytic activity in the experiment of p-nitrophenol organic dyestuff, and secondary pollution is not caused after the completion of reacting, pass through
It is recycled for multiple times and still keeps good catalytic effect, prepare simply, it is at low cost.
PVA sponge loading nano silvery materials are applied to the reduction of p-nitrophenol organic dyestuff in industrial wastewater.
Description of the drawings
Fig. 1 is the SEM pictures for the PVA sponge loading nano silvery materials that in the present invention prepared by embodiment 5；
Fig. 2 be the present invention in embodiment 5 prepare PVA sponges nano silver material to sodium borohydride catalyzing p-nitrophenol also
Former design sketch；
Fig. 3 be the present invention in embodiment 5 prepare PVA sponges by 200 times extruding absorb water step after to sodium borohydride
It is catalyzed p-nitrophenol reduction effect figure.
Specific implementation mode
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
A kind of preparation method of PVA sponges loading nano silvery material, specifically comprises the following steps：
It is prepared by S100, PVA sponge：3 parts of PVA-1788 are added into three-necked flask, 54 parts of water are heated to 85 DEG C, machinery stirs
It mixes, until PVA-1788 is completely dissolved；Cooling solution is added 5 parts of formaldehyde and 2.5 parts of 30wt.% triton x-100s is (bent to room temperature
It draws and leads to X-100：Octoxinol), stir 5min；Add 10 parts of 50wt.%H2SO4, 5min is stirred, foam solution is obtained；At once
Obtained foam solution is placed in beaker, then beaker is put into 45 DEG C of baking ovens and cures 2h, obtains sponge semi-finished product；By institute
Sponge semi-finished product obtained wash 15min with clear water, remove extra sulfuric acid, are placed in oven and dried, and obtain PVA sponges
(PVA：Polyvinyl alcohol)；
S200,70 parts of dry PVA sponges are taken, is soaked in 100 parts of 1g/L dopamine solution 12h, be used in combination Tris bufferings molten
Liquid (trishydroxymethylaminomethane) adjusts pH value to 7.5；
S300, cleaning-drying, then PVA sponges are soaked in 140 parts of 0.001mol/L silver nitrate solutions 6h；
S400, PVA sponges are soaked in 140 parts of 0.1mol/L sodium borohydride solution 1h, be cleaned and dried, PVA sponges are made
Loading nano silvery material.
Embodiment 2
A kind of preparation method of PVA sponges loading nano silvery material, specifically comprises the following steps：
It is prepared by S100, PVA sponge：6 parts of PVA-2088 are added into three-necked flask, 54 parts of water are heated to 90 DEG C, machinery stirs
It mixes, until PVA-2088 is completely dissolved；10 parts of formaldehyde and 5 parts of 30wt.% triton x-100s, stirring is added to room temperature in cooling solution
10min；Add 30 parts of 50wt.%H2SO4, 5min is stirred, foam solution is obtained；Obtained foam solution is placed in burning at once
In cup, then beaker is put into 55 DEG C of baking ovens and cures 3h, obtains sponge semi-finished product；By obtained sponge semi-finished product clear water
30min is washed, extra sulfuric acid is removed, is placed in oven and dried, obtain PVA sponges；
S200,70 parts of dry PVA sponges are taken, is soaked in 100 parts of 4g/L dopamine solutions for 24 hours, be used in combination Tris bufferings molten
Liquid adjusts pH value to 8.5；
S300, cleaning-drying, then PVA sponges are soaked in 140 parts of 0.002mol/L silver nitrate solutions 12h；
S400, PVA sponges are soaked in 140 parts of 0.60mol/L sodium borohydride solution 3h, be cleaned and dried, PVA sponges are made
Loading nano silvery material.
Embodiment 3
A kind of preparation method of PVA sponges loading nano silvery material, specifically comprises the following steps：
It is prepared by S100, PVA sponge：9 parts of PVA-2488 are added into three-necked flask, 54 parts of water are heated to 95 DEG C, machinery stirs
It mixes, until PVA-2488 is completely dissolved；Cooling solution is added 15 parts of formaldehyde and 7.5 parts of 30wt.% triton x-100s, stirs to room temperature
Mix 30min；Add 15 parts of 50wt.%H2SO4, 15min is stirred, foam solution is obtained；Foam solution is placed in beaker at once
In, then beaker is put into 75 DEG C of baking ovens and cures 5h, obtains sponge semi-finished product；Obtained sponge semi-finished product are washed with clear water
45min is washed, extra sulfuric acid is removed, is placed in oven and dried, obtains PVA sponges；
S200,70 parts of dry PVA sponges are taken, is soaked in 100 parts of 8g/L dopamine solution 36h, be used in combination Tris bufferings molten
It is 9.5 that liquid, which adjusts pH value,；
S300, cleaning-drying, then sponge is soaked in 140 parts of 0.010mol/L silver nitrate solutions 18h；
S400, PVA sponges are soaked in 140 parts of 1.0mol/L sodium borohydride solution 5h, be cleaned and dried, PVA sponges are made
Loading nano silvery material.
Embodiment 4
A kind of preparation method of PVA sponges loading nano silvery material, specifically comprises the following steps：
It is prepared by S100, PVA sponge：6 parts of PVA-1788 are added into three-necked flask, 54 parts of water are heated to 90 DEG C, machinery stirs
It mixes, until PVA-1788 is completely dissolved；Cooling solution is added 10 parts of formaldehyde and 7.5 parts of 30wt.% triton x-100s, stirs to room temperature
Mix 20min；Add 10 parts of 50wt.%H2SO4, 10min is stirred, foam solution is obtained；Obtained foam solution is placed at once
In beaker, then beaker is put into 60 DEG C of baking ovens and cures 4h, obtains sponge semi-finished product；By obtained sponge semi-finished product with clearly
Water washing 30min removes extra sulfuric acid, is placed in oven and dried, and obtains PVA sponges；
S200,70 parts of dry PVA sponges are taken, is soaked in 100 parts of 5g/L dopamine solutions for 24 hours, be used in combination Tris bufferings molten
It is 9.0 that liquid, which adjusts pH value,；
S300, cleaning-drying, then sponge is soaked in 140 parts of 0.006mol/L silver nitrate solutions 12h；
S400, PVA sponges are soaked in 140 parts of 0.5mol/L sodium borohydride solution 3h, be cleaned and dried, PVA sponges are made
Loading nano silvery material.
Embodiment 5
A kind of preparation method of PVA sponges loading nano silvery material, specifically comprises the following steps：
It is prepared by S100, PVA sponge：6 parts of PVA-1788 are added into three-necked flask, 54 parts of water are heated to 95 DEG C, machinery stirs
It mixes, until PVA-1788 is completely dissolved；Cooling solution is added 10 parts of formaldehyde and 5.0 parts of 30wt.% triton x-100s, stirs to room temperature
Mix 30min；Add 15 parts of 50wt.%H2SO4, 15min is stirred, foam solution is obtained；Obtained foam solution is placed at once
In beaker, then beaker is put into 70 DEG C of baking ovens and cures 5h, obtains sponge semi-finished product；By obtained sponge semi-finished product with clearly
Water washing 45min removes extra sulfuric acid, is placed in oven and dried, and obtains PVA sponges；
S200,70 parts of dry PVA sponges are taken, is soaked in 100 parts of 4g/L dopamine solution 12h, be used in combination Tris bufferings molten
It is 8.5 that liquid, which adjusts pH value,；
S300, cleaning-drying, then sponge is soaked in 140 parts of 0.008mol/L silver nitrate solutions 12h；
S400, sponge is soaked in 140 parts of 0.5mol/L sodium borohydride solution 5h, be cleaned and dried, PVA sponge loads are made
Nano silver material.
The SEM pictures of PVA sponge loading nano silvery materials prepared by embodiment 5- from electromicroscopic photograph as shown in Figure 1, analyze
Know that Ag nano particles are evenly distributed in the surface and duct of PVA sponges.
By the PVA sponge loading nano silvery materials catalysis reduction p-nitrophenol of the preparation of embodiment 5-, the load of PVA sponges
Nano silver material is shown in that Fig. 2, reaction temperature are room temperature to sodium borohydride catalyzing p-nitrophenol reduction effect.Fig. 3 is PVA sponges warp
After crossing 200 extruding water suction steps, to sodium borohydride catalyzing p-nitrophenol reduction effect, reaction temperature is room temperature.Fig. 3 knots
Fruit shows：PVA sponge loading nano silvery materials prepared by the present invention are in sodium borohydride degradation p-nitrophenol organic dyestuff experiment
In have excellent catalytic activity, and react after the completion of do not cause secondary pollution, still keep good by being recycled for multiple times
Catalytic effect.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification.
Claims (10)
1. a kind of preparation method of PVA sponges loading nano silvery material, which is characterized in that specifically comprise the following steps：
S100, PVA sponges are prepared；
S200, PVA sponges are soaked in dopamine solution, Tris buffer solutions is used in combination to adjust pH value to 7.0~9.5；
S300, the PVA sponges after being impregnated by dopamine solution and Tris buffer solutions are soaked in silver nitrate solution；
S400, the PVA sponges after being impregnated by dopamine solution, Tris buffer solutions and silver nitrate solution are soaked in boron hydrogen
Change sodium solution, be cleaned and dried, PVA sponge loading nano silvery materials are made.
2. the preparation method of PVA sponges loading nano silvery material according to claim 1, which is characterized in that the S100
In, the specific preparation process of the PVA sponges is as follows：
S110,3~9 parts of PVA, 54 parts of water are added into container, are heated to 85 DEG C~95 DEG C, mechanical agitation, until PVA is completely molten
Solution；
S120,5~15 parts of formaldehyde and 2.5~7.5 parts of 30wt.% triton x-100s are added, stir 5min~30min；
S130,10~15 parts of 50wt.%H are added2SO4, 5min~15min is stirred, foam solution is obtained；
S140, foam solution transfer is emptied in container, container is then put into solidification 2h~5h in 45 DEG C~75 DEG C baking ovens, is obtained
To sponge semi-finished product；
S150, sponge semi-finished product are washed into 15min~45min with clear water, removes extra sulfuric acid, be placed in oven and dried, obtains
To PVA sponges.
3. the preparation method of PVA sponges loading nano silvery material according to claim 2, which is characterized in that the S110
In, the PVA is one kind in PVA-1788, PVA-2088 or PVA-2488.
4. the preparation method of PVA sponges loading nano silvery material according to claim 1, which is characterized in that the S200
In, the time that the PVA sponges are impregnated in dopamine solution is 12h~36h.
5. the preparation method of PVA sponges loading nano silvery material according to claim 4, which is characterized in that the DOPA
A concentration of 1g/L~8g/L of amine aqueous solution.
6. the preparation method of PVA sponges loading nano silvery material according to claim 1, which is characterized in that the S300
In, the time that the PVA sponges are impregnated in silver nitrate solution is 6h~18h.
7. the preparation method of PVA sponges loading nano silvery material according to claim 6, which is characterized in that the nitric acid
A concentration of 0.001mol/L~0.010mol/L of silver-colored solution.
8. the preparation method of PVA sponges loading nano silvery material according to claim 1, which is characterized in that the S400
In, the time that the PVA sponges are impregnated in sodium borohydride solution is 1h~5h.
9. the preparation method of PVA sponges loading nano silvery material according to claim 8, which is characterized in that the boron hydrogen
Change a concentration of 0.1mol/L~1.0mol/L of sodium solution.
10. the PVA sponge loading nano silvery materials obtained by any one of the claim 1-9 preparation methods are applied to work
The reduction of p-nitrophenol organic dyestuff in industry waste water.
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Application publication date: 20180817 |