CN108906041A - A kind of preparation method for the single layer golden film can be used for photocatalytic degradation 4- nitrophenol - Google Patents
A kind of preparation method for the single layer golden film can be used for photocatalytic degradation 4- nitrophenol Download PDFInfo
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- CN108906041A CN108906041A CN201810816809.XA CN201810816809A CN108906041A CN 108906041 A CN108906041 A CN 108906041A CN 201810816809 A CN201810816809 A CN 201810816809A CN 108906041 A CN108906041 A CN 108906041A
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- 239000002356 single layer Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000013033 photocatalytic degradation reaction Methods 0.000 title claims abstract description 14
- 239000010931 gold Substances 0.000 claims abstract description 57
- 229910052737 gold Inorganic materials 0.000 claims abstract description 57
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000011521 glass Substances 0.000 claims abstract description 46
- 239000004579 marble Substances 0.000 claims abstract description 33
- 240000008027 Akebia quinata Species 0.000 claims abstract description 31
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 31
- 235000007756 Akebia quinata Nutrition 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 239000002105 nanoparticle Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 24
- 235000013339 cereals Nutrition 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 9
- 238000007605 air drying Methods 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- 238000007654 immersion Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- BRSVJNYNWNMJKC-UHFFFAOYSA-N [Cl].[Au] Chemical compound [Cl].[Au] BRSVJNYNWNMJKC-UHFFFAOYSA-N 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 2
- 238000009790 rate-determining step (RDS) Methods 0.000 claims description 2
- 239000011260 aqueous acid Substances 0.000 claims 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims 1
- 238000001338 self-assembly Methods 0.000 claims 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims 1
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 abstract description 15
- 239000003638 chemical reducing agent Substances 0.000 abstract description 8
- 238000006467 substitution reaction Methods 0.000 abstract description 6
- 231100000252 nontoxic Toxicity 0.000 abstract description 5
- 230000003000 nontoxic effect Effects 0.000 abstract description 5
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 208000036142 Viral infection Diseases 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 231100000331 toxic Toxicity 0.000 description 5
- 230000002588 toxic effect Effects 0.000 description 5
- 238000004064 recycling Methods 0.000 description 4
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical class OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000009881 electrostatic interaction Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- CPJSUEIXXCENMM-UHFFFAOYSA-N phenacetin Chemical compound CCOC1=CC=C(NC(C)=O)C=C1 CPJSUEIXXCENMM-UHFFFAOYSA-N 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- OQUFOZNPBIIJTN-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;sodium Chemical compound [Na].OC(=O)CC(O)(C(O)=O)CC(O)=O OQUFOZNPBIIJTN-UHFFFAOYSA-N 0.000 description 1
- ZLCPKMIJYMHZMJ-UHFFFAOYSA-N 2-nitrobenzene-1,3-diol Chemical compound OC1=CC=CC(O)=C1[N+]([O-])=O ZLCPKMIJYMHZMJ-UHFFFAOYSA-N 0.000 description 1
- RTZZCYNQPHTPPL-UHFFFAOYSA-N 3-nitrophenol Chemical class OC1=CC=CC([N+]([O-])=O)=C1 RTZZCYNQPHTPPL-UHFFFAOYSA-N 0.000 description 1
- FYKHWKNFKLTGNX-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1.OC1=CC=C([N+]([O-])=O)C=C1 FYKHWKNFKLTGNX-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- NPAKNKYSJIDKMW-UHFFFAOYSA-N carvedilol Chemical compound COC1=CC=CC=C1OCCNCC(O)COC1=CC=CC2=NC3=CC=C[CH]C3=C12 NPAKNKYSJIDKMW-UHFFFAOYSA-N 0.000 description 1
- 229960004195 carvedilol Drugs 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- -1 gold ion Chemical class 0.000 description 1
- 230000000622 irritating effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 description 1
- 229960005489 paracetamol Drugs 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229960003893 phenacetin Drugs 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 210000001186 vagus nerve Anatomy 0.000 description 1
- 238000007740 vapor deposition Methods 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- B01J35/39—
-
- B01J35/59—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—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
-
- 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
Abstract
The invention discloses a kind of preparation methods of single layer golden film that can be used for photocatalytic degradation 4- nitrophenol, specifically comprise the following steps：First prepare the positively charged glass marble in surface, gold nano particle colloidal sols；Glass marble is soaked in electrostatic self-assembled in gold nano particle colloidal sols again；Glass marble is taken out later, is placed in fiveleaf akebia fruit extracting solution, aqueous solution of chloraurate is added and impregnates obtained single layer golden film；The present invention makes glass ball surface attachment gold nano grain form gold kind by the way that positively charged glass marble and electronegative gold nano grain attract each other；Using facilitate be easy to get, virose hydroxylamine hydrochloride that cheap, easily stored nontoxic fiveleaf akebia fruit extracting solution substitution is conventional as reducing agent prepares single layer golden film, single layer of gold film properties obtained are stable, adhesive ability is strong, uniform film thickness, reusable, new route of synthesis is provided for the preparation of other single layer metal firms, overcomes the shortcomings that molecule is easy to run off in use, hardly possible recycles.
Description
Technical field
The present invention is to be related to a kind of preparation method of single layer golden film that can be used for photocatalytic degradation 4- nitrophenol, belongs to and receives
Rice grain catalyst preparation technical field.
Background technique
Paranitrophenol (p-nitrophenol) also known as 4- nitrophenol (4-nitrophenol), there are three same altogether for nitrophenols
Enantiomers, i.e., o-, m-, p- nitrophenols.It is colourless or pale yellow crystals under paranitrophenol room temperature, hot water, second can be dissolved in
Alcohol, ether, are soluble in caustic alkali, are in yellow in the carbonate solution of alkali metal.It is oxidizable in air, make to darken.It is high
It is unstable under temperature, start to decompose when being heated to 273 DEG C.Paranitrophenol is inflammable, toxic, absorbs through skin, can cause allergy.It is right
The toxic effect of people is also imperfectly understood.Results of animal：Central nervous and the irritating effect of vagus nerve ending and suppression
Production is used, and there is also ferrihemochrome disease and expiratory dyspnea.The toxicity intensity sequence of nitrophenol：Align body>Meta position body>It is adjacent
Position body.It is commonly used for the intermediate of the fine chemicals such as pesticide, medicine, dyestuff；Also serve as manufacture phenacetin, paracetamol, agriculture
Medicine 1605, developer rice Carvedilol, paranitrophenol sulphur grass-green GN, the black CL of reversion, the black CLB of reversion, reversion are blue
RNX, sulfur red brown b3r also serve as leather fungicide and acid value indicator.Paranitrophenol is a kind of organic pollutant, is had
High stability, solubility and accumulating effect easily generates serious pollution to environment and is difficult to remove.
Photocatalytic degradation method is a kind of more effective method for handling 4- nitrophenol in sewage, and degradation efficiency depends on
In the performance of photochemical catalyst used.The photocatalysis efficiency of gold nano grain Yin Qigao is by extensive concern.However, in practical application
In, the recycling of gold nano grain difficulty causes cost raising, limits further applying for photocatalytic degradation method.
Currently, gold is supported on substrate be prepared into golden film be realize gold recycling, reduce photocatalytic degradation reaction at
This effective way.So far, the preparation method of golden film mainly has physical method and chemical method.Physical method include pulse laser deposition,
Vacuum vapor deposition method and magnetron sputtering method etc..This method operating process is simple, but to the more demanding of equipment, at high cost.Chemistry
Method includes chemical vapour deposition technique, laser chemistry decomposition method and electrostatic self-assembled method etc..Wherein, electrostatic self-assembled method is because of its method
Simply, at low cost, controllability is good, film obtained have many advantages, such as quality is stable, adhesive ability is strong, uniform film thickness and by pass
Note.During film, hydroxylamine hydrochloride generallyd use as reducing agent realize the quick reduction of gold ion.However, hydrochloric acid
Azanol is toxic, easily pollutes the environment.The present invention realizes single layer golden film using green plants extracting solution substitution hydroxylamine hydrochloride
Quickly preparation, the selection for reducing agent in metallic film preparation process provide new thinking.Based on the present invention, golden film institute is prepared
The cost needed is low, and preparation process is pollution-free, and the structure of golden film is uniform, and photocatalytic activity is high, reusable, will be photocatalysis
The practical application of degradation 4- nitrophenol technology is laid a good foundation.
Summary of the invention
In view of the above-mentioned problems existing in the prior art and demand, the object of the present invention is to provide one kind can be used for photocatalysis drop
The preparation method for solving the single layer golden film of 4- nitrophenol realizes single layer using green plants fiveleaf akebia fruit extracting solution substitution hydroxylamine hydrochloride
The quick preparation of golden film overcomes the shortcomings that molecule is easy to run off in use, hardly possible recycles.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method for the single layer golden film can be used for photocatalytic degradation 4- nitrophenol, it is characterised in that：Specific packet
Include following steps：
(1) the mixed liquid dipping glass marble for utilizing 3- aminopropyl triethoxysilane and dehydrated alcohol, stands 24 hours, makes
Glass ball surface is positively charged；
(2) deionized water mixed with aqueous solution of chloraurate, be heated to boiling, reinject sodium citrate aqueous solution, obtained
Gold nano particle colloidal sols；
(3) glass marble positively charged in step (1) is soaked in step (2) in gold nano particle colloidal sols obtained, into
Row electrostatic self-assembled；
(4) glass marble for completing electrostatic self-assembled in step (3) is taken out, is placed in fiveleaf akebia fruit extracting solution, is then added
Aqueous solution of chloraurate obtains single layer golden film after carrying out immersion treatment.
Preferably, the glass bulb diameter is 2.5mm~5.5mm.
Preferably, 3- aminopropyl triethoxysilane described in step (1) and the dehydrated alcohol are according to volume
Than 1:100 mixing.
Preferably, the electrostatic self-assembled time is 1 hour~2 hours in rate-determining steps (3).
Preferably, the aqueous solution of chloraurate amount being added in step (4) is the 20 μ L of μ L~80, described in step (4)
The immersion treatment time is 1 hour~2 hours.
Preferably, glass marble described in step (1) passes through steps of processing before experiment：Glass marble is put into
It is cleaned 3 times, each 10min in vessel, natural air drying is spare after cleaning.
Preferably, the fiveleaf akebia fruit extracting solution during the preparation process, mix by the dosage of fiveleaf akebia fruit and deionized water
Composition and division in a proportion example is 1g：(75~150) mL.
Preferably, the preparation of the fiveleaf akebia fruit extracting solution includes the following steps：
S1：By fiveleaf akebia fruit and deionized water according to mixed proportion 1g：(75~150) mL is mixed, and is heated to boiling simultaneously
It is kept for fluidized state 10 minutes~30 minutes；
S2：After liquid natural cooling in step S1, with 10000rpm centrifugal treating 10min, obtained supernatant is eight
Month letter extracting solution.
Preferably, the preparation of the gold nano particle colloidal sols includes the following steps：Take 100mL deionized water with
It after the aqueous solution of chloraurate mixing of 290uL0.1mol/L, is heated to boiling, after reacting 10min, injects 3mL 1wt% citric acid
Sodium water solution continues to keep fluidized state reaction 15min, is centrifuged after liquid is cooling, obtains gold nano particle colloidal sols.
Compared with prior art, the present invention has the advantages that：
The present invention is allowed to by the way that glass marble to be immersed in the mixed liquor of 3- aminopropyl triethoxysilane and dehydrated alcohol
Positively charged, by electrostatic interaction, positively charged glass marble attracts each other with electronegative gold nano grain, keeps glass ball surface attached
Gold nano grain formed gold kind；Toxic hydroxylamine hydrochloride is substituted with nontoxic fiveleaf akebia fruit extracting solution and makees reducing agent, with Jin Zhongwei
Activated centre continues under room temperature to restore gold chloride；The gold restored forms a film in gold kind surface deposition, growth, list obtained
Layer golden film performance is stable, adhesive ability is strong, uniform film thickness, reusable；The present invention by with facilitate be easy to get, it is cheap,
The conventional virose hydroxylamine hydrochloride of easily stored nontoxic fiveleaf akebia fruit extracting solution substitution prepares single layer golden film as reducing agent,
So that cost is relatively low and will not generate any environmental pollution for single layer of gold film preparation, provided for the preparation of other single layer metal firms
New route of synthesis；In addition, preparation method simple process of the present invention, single layer of gold membrane structure obtained are uniform, repeatable sharp
With property is good, raw material fiveleaf akebia fruit is conveniently easy to get, photocatalytic activity compared with gold nano grain activity quite；Molecule is overcome to exist
It is easy to run off in use process, difficult the shortcomings that recycling, has effectively facilitated the development of photocatalytic degradation 4- nitrophenol technology.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of gold nano grain made from the embodiment of the present invention 1；
Fig. 2 is the X-ray diffraction spectrogram of gold nano grain made from the embodiment of the present invention 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of gold nano grain made from the embodiment of the present invention 2；
Fig. 4 is the X-ray diffraction spectrogram of gold nano grain made from the embodiment of the present invention 2；
Fig. 5 is the scanning electron microscope (SEM) photograph of gold nano grain made from the embodiment of the present invention 3；
Fig. 6 is the X-ray diffraction spectrogram of gold nano grain made from the embodiment of the present invention 3.
Specific embodiment
Technical solution of the present invention is described in further detail below in conjunction with drawings and examples.
Being extracted by following step for fiveleaf akebia fruit extracting solution used in following embodiments is made：
S1：By fiveleaf akebia fruit (g) and deionized water (mL) according to mixed proportion 1g：(75~150) mL is mixed, and is heated to
It boils and keeps fluidized state 10 minutes~30 minutes；
S2：After liquid natural cooling in step S1, with 10000rpm centrifugal treating 10min, obtained supernatant is eight
Month letter extracting solution.
Being extracted by following step for gold nano particle colloidal sols used in following embodiments is made：
It is 1wt% sodium citrate aqueous solution as reducing agent using concentration and prepares gold nano grain, takes 100mL deionized water
After being mixed with the aqueous solution of chloraurate of 290uL 0.1mol/L, it is heated to 100 DEG C and is allowed to boil, be added after boiling reaction 10min
The sodium citrate aqueous solution of 3mL 1wt% continues to keep fluidized state reaction 15min, is centrifuged after liquid is cooling, obtains gold
Nano particle colloidal sol.
Embodiment 1
A kind of preparation method of single layer golden film can be used for photocatalytic degradation 4- nitrophenol provided in this embodiment, specifically
Include the following steps：
(1) glass marble that diameter is 2.5mm is put into vessel and is cleaned 3 times, each 10min, natural air drying is standby after cleaning
With；
(2) using 3- aminopropyl triethoxysilane and dehydrated alcohol according to volume ratio 1:100 mixed mixed liquor leachings
Glass marble made from step (1) is steeped, 24 hours is stood, keeps glass ball surface positively charged；
(3) with above-mentioned positively charged glass marble 3 times of 20mL dehydrated alcohol resonance cleaning, every subresonance cleaning 10min is gone
Except extra 3- aminopropyl triethoxysilane, and natural air drying；
(4) glass marble will be made in step (3) to be immersed in gold nano particle colloidal sols 1 hour, carries out electrostatic self-assembled, makes
Glass ball surface uniform adsorption gold kind；
(5) the glass marble taking-up that electrostatic self-assembled is completed in step (4) is placed in fiveleaf akebia fruit extracting solution, the fiveleaf akebia fruit
Extracting solution is mixed to prepare by the way that 75mL deionized water is added in 1g fiveleaf akebia fruit, adds 20 μ L aqueous solution of chloraurate, at immersion
Reason stands 1 hour, obtains single layer golden film.
The golden film that the above method is prepared using the field emission scanning electron microscope of Japanese NERCN-TC-006 model
Surface carries out morphology analysis, as shown in Figure 1；Fig. 1 can be seen that the golden film of preparation is single layer structure and film forming is uniform.
The golden film above method prepared using the D/max-2600PC type x-ray diffractometer of Amada Co., Ltd. into
Row constituent analysis, as shown in Figure 2；Fig. 2 can be seen that the x-ray diffraction pattern of golden film matches with the standard drawing of elemental gold, explanation
The ingredient for the golden film prepared is elemental gold, and other impurities are not present.
Embodiment 2
A kind of preparation method of single layer golden film can be used for photocatalytic degradation 4- nitrophenol provided in this embodiment, specifically
Include the following steps：
(1) glass marble that diameter is 4mm is put into vessel and is cleaned 3 times, each 10min, natural air drying is spare after cleaning；
(2) using 3- aminopropyl triethoxysilane and dehydrated alcohol according to volume ratio 1:100 mixed mixed liquor leachings
Glass marble made from step (1) is steeped, 24 hours is stood, keeps glass ball surface positively charged；
(3) with above-mentioned positively charged glass marble 3 times of 20mL dehydrated alcohol resonance cleaning, every subresonance cleaning 10min is gone
Except extra 3- aminopropyl triethoxysilane, and natural air drying；
(4) glass marble will be made in step (3) to be immersed in gold nano particle colloidal sols 1.5 hours, carries out electrostatic self-assembled,
Make glass ball surface uniform adsorption gold kind；
(5) the glass marble taking-up that electrostatic self-assembled is completed in step (4) is placed in fiveleaf akebia fruit extracting solution, the fiveleaf akebia fruit
Extracting solution is mixed to prepare by the way that 110mL deionized water is added in 1g fiveleaf akebia fruit, adds 50 μ L aqueous solution of chloraurate, at immersion
Reason stands 1.5 hours, obtains single layer golden film.
The golden film that the above method is prepared using the field emission scanning electron microscope of Japanese NERCN-TC-006 model
Surface carries out morphology analysis, as shown in Figure 3；Fig. 3 can be seen that the golden film of preparation is single layer structure and film forming is uniform.
The golden film above method prepared using the D/max-2600PC type x-ray diffractometer of Amada Co., Ltd. into
Row constituent analysis, as shown in Figure 4；Fig. 4 can be seen that the x-ray diffraction pattern of golden film matches with the standard drawing of elemental gold, explanation
The ingredient for the golden film prepared is elemental gold, and other impurities are not present.
Embodiment 3
A kind of preparation method of single layer golden film can be used for photocatalytic degradation 4- nitrophenol provided in this embodiment, specifically
Include the following steps：
(1) glass marble that diameter is 5.5mm is put into vessel and is cleaned 3 times, each 10min, natural air drying is standby after cleaning
With；
(2) using 3- aminopropyl triethoxysilane and dehydrated alcohol according to volume ratio 1:100 mixed mixed liquor leachings
Glass marble made from step (1) is steeped, 24 hours is stood, keeps glass ball surface positively charged；
(3) with above-mentioned positively charged glass marble 3 times of 20mL dehydrated alcohol resonance cleaning, every subresonance cleaning 10min is gone
Except extra 3- aminopropyl triethoxysilane, and natural air drying；
(4) glass marble will be made in step (3) to be immersed in gold nano particle colloidal sols 2 hours, carries out electrostatic self-assembled, makes
Glass ball surface uniform adsorption gold kind；
(5) the glass marble taking-up that electrostatic self-assembled is completed in step (4) is placed in fiveleaf akebia fruit extracting solution, the fiveleaf akebia fruit
Extracting solution is mixed to prepare by the way that 150mL deionized water is added in 1g fiveleaf akebia fruit, adds 80 μ L aqueous solution of chloraurate, at immersion
Reason stands 2 hours, obtains single layer golden film.
The golden film that the above method is prepared using the field emission scanning electron microscope of Japanese NERCN-TC-006 model
Surface carries out morphology analysis, as shown in Figure 5；Fig. 5 can be seen that the golden film of preparation is single layer structure and film forming is uniform.
The golden film above method prepared using the D/max-2600PC type x-ray diffractometer of Amada Co., Ltd. into
Row constituent analysis, as shown in Figure 6；Fig. 6 can be seen that the x-ray diffraction pattern of golden film matches with the standard drawing of elemental gold, explanation
The ingredient for the golden film prepared is elemental gold, and other impurities are not present.
It is visible in summary：The present invention is by being immersed in 3- aminopropyl triethoxysilane and dehydrated alcohol for glass marble
In mixed liquor, it is allowed to positively charged, by electrostatic interaction, positively charged glass marble attracts each other with electronegative gold nano grain,
Glass ball surface attachment gold nano grain is set to form gold kind；Toxic hydrochloric acid is substituted with nontoxic green plants fiveleaf akebia fruit extracting solution
Azanol makees reducing agent, and the ratio for crossing control fiveleaf akebia fruit (g) and deionized water (mL) is 1:20 μ of μ L~80 L are added in (75~150)
Aqueous solution of chloraurate, control soaking time is 1 hour~2 hours, with gold kind for activated centre, continues to restore chlorine gold under room temperature
Acid；The gold restored forms a film in gold kind surface deposition, growth, single layer of gold film properties obtained are stable, adhesive ability is strong,
Uniform film thickness, it is reusable；The present invention by with facilitate be easy to get, cheap, easily stored nontoxic fiveleaf akebia fruit extracting solution
The conventional virose hydroxylamine hydrochloride of substitution prepares single layer golden film as reducing agent so that single layer of gold film preparation cost is relatively low and
Any environmental pollution will not be generated, provides new route of synthesis for the preparation of other single layer metal firms；In addition, institute of the present invention
State that preparation method simple process, single layer of gold membrane structure obtained are uniform, reusable property is good, raw material fiveleaf akebia fruit is conveniently easy to get,
Its photocatalytic activity is suitable compared with the activity of gold nano grain；Overcome molecule be easy to run off in use, difficult recycling
Disadvantage has effectively facilitated the development of photocatalytic degradation 4- nitrophenol technology.
Although above-described embodiment is the reaction for listing laboratory scale, it will be understood by those skilled in the art that this
Invention is not limited to the degradation of 4- nitrophenol, it may also be used for other organic pollutants, such as 2- nitrophenols, 3- nitrophenols, 2- nitro
Resorcinol, methyl red, methyl orange etc..
It is last it is necessarily pointed out that：The foregoing is merely the preferable specific embodiment of the present invention, but the present invention
Protection scope be not limited thereto, anyone skilled in the art in the technical scope disclosed by the present invention,
Any changes or substitutions that can be easily thought of, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method for the single layer golden film that can be used for photocatalytic degradation 4- nitrophenol, it is characterised in that：It specifically includes
Following steps：
(1) the mixed liquid dipping glass marble for utilizing 3- aminopropyl triethoxysilane and dehydrated alcohol, stands 24 hours, makes glass
Ball surface is positively charged；
(2) deionized water mixed with aqueous solution of chloraurate, be heated to boiling, reinject sodium citrate aqueous solution, obtain Jenner
Rice grain colloidal sol；
(3) glass marble positively charged in step (1) is soaked in step (2) in gold nano particle colloidal sols obtained, is carried out quiet
Electric self assembly；
(4) glass marble for completing electrostatic self-assembled in step (3) is taken out, is placed in fiveleaf akebia fruit extracting solution, chlorine gold is then added
Aqueous acid obtains single layer golden film after carrying out immersion treatment.
2. the preparation method of single layer golden film according to claim 1, it is characterised in that：The glass bulb diameter is 2.5mm
~5.5mm.
3. the preparation method of single layer golden film according to claim 1, it is characterised in that：3- aminopropyl described in step (1)
Triethoxysilane and the dehydrated alcohol are according to volume ratio 1:100 mixing.
4. the preparation method of single layer golden film according to claim 1, it is characterised in that：Electrostatic is from group in rate-determining steps (3)
ETL estimated time of loading is 1 hour~2 hours.
5. the preparation method of single layer golden film according to claim 1, it is characterised in that：The gold chloride being added in step (4)
Water-soluble liquid measure is 20 μ of μ L~80 L.
6. the preparation method of single layer golden film according to claim 1, it is characterised in that：Immersion treatment described in step (4)
Time is 1 hour~2 hours.
7. the preparation method of single layer golden film according to claim 1, it is characterised in that：Glass marble described in step (1) exists
Pass through steps of processing before experiment：Glass marble is put into vessel and is cleaned 3 times, each 10min, natural air drying is standby after cleaning
With.
8. the preparation method of single layer golden film according to claim 1, it is characterised in that：It is prepared by the fiveleaf akebia fruit extracting solution
In the process, the mixed proportion of the dosage of fiveleaf akebia fruit and deionized water is 1g：(75~150) mL.
9. the preparation method of single layer golden film described in -8 any claims according to claim 1, it is characterised in that：The August
The preparation of letter extracting solution includes the following steps：
S1：By fiveleaf akebia fruit and deionized water according to mixed proportion 1g：(75~150) mL is mixed, and is heated to boiling and be kept
Fluidized state 10 minutes~30 minutes；
S2：After liquid natural cooling in step S1, with 10000rpm centrifugal treating 10min, obtained supernatant is fiveleaf akebia fruit
Extracting solution.
10. the preparation method of single layer golden film described in -8 any claims according to claim 1, it is characterised in that：The gold
The preparation of nano particle colloidal sol includes the following steps：Take 100mL deionized water and 290 μ L 0.1mol/L aqueous solution of chloraurate mixed
It closes, is heated to boiling, after reacting 10min, inject 3mL 1wt% sodium citrate aqueous solution, continue to keep fluidized state reaction
15min is centrifuged after liquid is cooling, obtains gold nano particle colloidal sols.
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