CN109433268A - A kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter - Google Patents
A kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter Download PDFInfo
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- CN109433268A CN109433268A CN201810581427.3A CN201810581427A CN109433268A CN 109433268 A CN109433268 A CN 109433268A CN 201810581427 A CN201810581427 A CN 201810581427A CN 109433268 A CN109433268 A CN 109433268A
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- CN
- China
- Prior art keywords
- polyaniline
- solution
- silver orthophosphate
- preparation
- pani
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- 229920000767 polyaniline Polymers 0.000 title claims abstract description 49
- 239000013078 crystal Substances 0.000 title claims abstract description 25
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002245 particle Substances 0.000 title claims abstract description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 30
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910000397 disodium phosphate Inorganic materials 0.000 claims abstract description 5
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 14
- 239000003054 catalyst Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 229910000161 silver phosphate Inorganic materials 0.000 description 27
- 229910019142 PO4 Inorganic materials 0.000 description 12
- 238000006731 degradation reaction Methods 0.000 description 11
- 230000015556 catabolic process Effects 0.000 description 10
- 239000000178 monomer Substances 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 239000011941 photocatalyst Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- 239000004020 conductor Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 239000012901 Milli-Q water Substances 0.000 description 1
- AMHXQVUODFNFGR-UHFFFAOYSA-K [Ag+3].[O-]P([O-])([O-])=O Chemical group [Ag+3].[O-]P([O-])([O-])=O AMHXQVUODFNFGR-UHFFFAOYSA-K 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004770 highest occupied molecular orbital Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 229940019931 silver phosphate Drugs 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
-
- B01J35/33—
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of preparation methods using polyaniline control silver orthophosphate crystal particle diameter.The following steps are included: polyaniline is added in n,N-Dimethylformamide (DMF) solution by (1), it is ultrasonically treated 2~5h；(2) by AgNO3Solution is added dropwise in above-mentioned DMF solution, is protected from light 6~20h of stirring；(3) by Na2HPO4·12H2O solution is added dropwise in the solution that step (2) obtains, and is protected from light 1~6h of stirring, for several times with water and ethanol washing, is centrifugally separating to obtain solid portion, the silver orthophosphate crystal that partial size is 0.15-0.38 μm after being made polyaniline-modified after vacuum drying.Preparation process of the present invention is simple, the Ag that can be 20 μm by average grain diameter3PO4Crystal modification is little particle crystal of the average grain diameter in 0.15-0.38 μ m.The little particle Ag being prepared simultaneously3PO4@PANI composite catalyst shows excellent visible light catalytic performance.
Description
Technical field
The invention belongs to the preparation technical fields of conductor photocatalysis material, and in particular to brilliant with polyaniline control silver orthophosphate
The preparation method of body partial size.
Background technique
In recent decades, it is seen that photoactive catalyst-silver phosphate (Ag3PO4) because of its excellent organic pollutant degradation energy
Power and by extensive concern.Ag3PO4Unique position of energy band makes the photohole in its valence band have Strong oxdiative ability, can be direct
Oxidation and degradation of contaminant.But Ag3PO4Photocatalytic activity and its crystalline size size, pattern it is in close relations, in preparation process
In easily there is Ag3PO4Crystalline size is uncontrollable, the irregular defect of pattern, is particularly prone to generate that partial size is big, photocatalysis is living
The low Ag of property3PO4Crystal.This defect directly affects Ag3PO4Photocatalytic activity, and seriously hinder Ag3PO4Popularization
Using.
The present invention is directed to Ag3PO4The shortcomings that crystal grain that partial size is big, photocatalytic activity is low is easily formed in preparation process is led to
Overdoping electrically conductive polyaniline is modified silver orthophosphate, reaches control Ag3PO4Crystal particle diameter is in 0.15-0.38 μ m, together
The purpose of its photocatalytic activity of Shi Tigao.Using PANI as the characteristics of conductive long-chain polymer, pass through itself and Ag+Between it is quiet
Electro ultrafiltration, by Ag+The surface PANI is adsorbed and be uniformly distributed in, Ag is effectively prevent3PO4Crystal is reunited, and final preparation generates small size
Ag3PO4Particle.In addition, using the conjugated pi structure and unique electric conductivity of PANI, as the carrier of photohole, by light
Raw hole is rapidly migrated to catalyst surface, direct oxidation degradable organic pollutant by its HOMO track.Reach light induced electron-
The effect of hole quick separating, to improve the photocatalytic activity of catalyst.
Summary of the invention
The present invention provides a kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter, and preparation method is simple, easy
Operation, the Ag that can be 20 μm by average grain diameter3PO4Crystal modification is that little particle of the average grain diameter in 0.15-0.38 μ m is brilliant
Body.The little particle Ag being prepared simultaneously3PO4@PANI composite catalyst shows excellent visible light catalytic performance.
A kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter, comprising the following steps:
Polyaniline is added in n,N-Dimethylformamide (DMF) solution by step 1), is ultrasonically treated 2~5h；
Step 2) is by AgNO3Solution is added dropwise in above-mentioned DMF solution, is protected from light 6~20h of stirring；
Step 3) is by Na2HPO4·12H2O solution is added dropwise in the solution that step (2) obtains, and is protected from light 1~6h of stirring,
For several times with water and ethanol washing, it is centrifugally separating to obtain solid portion, partial size is 0.15- after being made polyaniline-modified after vacuum drying
0.38 μm of silver orthophosphate crystal.
Preferably, polyaniline described in the step 1) step 1) is conductivity type polyaniline (PANI), wherein add
The solid-to-liquid ratio of PANI and DMF solution is 0.4~2g/L.
Preferably, the step 2) AgNO3Mass ratio with PANI is 30:1~120:1.
Further, the step 3) Na2HPO4·12H2O and AgNO3Molar ratio be 1:3, vacuum drying temperature be 50~
60℃。
Compared with prior art, the invention has the following advantages:
(1) present invention is by Ag3PO4PANI is adulterated in preparation process, is successfully prepared crystal particle diameter in 0.15-0.38 μ
Efficient visible light catalyst Ag within the scope of m3PO4@PANI。
(2) PANI adulterated in the present invention, unique pi-conjugated backbone become the good carrier of photohole
And conductor, it can further promote the separation of photo-generated carrier.
(3) operation of the present invention is simple and easy, green non-pollution.
Detailed description of the invention
Fig. 1 is the Ag being prepared3PO4The electron-microscope scanning figure of monomer.
Fig. 2 is the silver phosphate composite photocatalyst Ag being prepared3PO4The electron-microscope scanning figure of@PANI, wherein Fig. 2 (a) be
The electron-microscope scanning figure in 10 μm of visuals field, Fig. 2 (b) are the electron-microscope scanning figure in 5 μm of visuals field.
Fig. 3 is the composite photo-catalyst Ag being prepared3PO4The XRD diagram of@PANI.
Fig. 4 is the composite photo-catalyst Ag being prepared3PO4The ultravioletvisible absorption figure of@PANI.
Fig. 5 is the Ag being prepared3PO4And Ag3PO4The degradation curve of@PANI degradation of phenol.
Fig. 6 is Ag3PO4And Ag3PO4The corresponding polymerization kinetics curves of degradation curve of@PANI degradation of phenol.
Specific embodiment
Below by drawings and examples, present invention is further described in detail:
Embodiment 1:
A kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter, steps are as follows:
(1) 0.0377g PANI is weighed in 40mL n,N-Dimethylformamide (DMF), is ultrasonically treated 3h.
(2) 1.53g AgNO is weighed3It is dissolved in 30mL ultrapure water, solution is added dropwise in above-mentioned solution, is persistently kept away
Light stirs 12h；
(3) 1.074gNa is weighed2HPO4·12H2O is dissolved in 30mL ultrapure water, and step is added dropwise in the solution
(2) in the solution obtained, it is protected from light stirring 6h.The solidliquid mixture is centrifuged, and with ethyl alcohol and milli-Q water 3~
It is 5 times, dry under 55 DEG C of vacuum conditions.Obtain the Ag that PANI load capacity is 3%3PO4@3%PANI composite material.As right
Than Ag3PO4Step (1) is saved in the preparation of monomer, is prepared under the same conditions by step (2) and step (3).By each
Kind characterization technique is to Ag3PO4@3%PANI composite material and Ag3PO4Monomer is characterized, is assessed.
Fig. 1 is the scanning electron microscope (SEM) photograph of silver orthophosphate monomer, and silver orthophosphate crystal size is different, and big silver orthophosphate crystal particle diameter is 20
μm or so, and polyhedron pattern is presented.
Fig. 2 is Ag3PO4The scanning electron microscope (SEM) photograph of@3%PANI composite material, under 10 μm of the Electronic Speculum visual field, without bulky grain
Occur.Silver orthophosphate crystal size is 0.15-0.38 μm, and silver orthophosphate crystal is orderly to be attached on PANI.
Fig. 3 is Ag3PO4The XRD spectrum of@3%PANI composite material, all diffraction maximums are and Ag3PO4Standard card
(JCPDS no.06-0505) is consistent.
Fig. 4 is Ag3PO4Monomer and Ag3PO4The ultraviolet-visible absorption spectroscopy of@3%PANI composite material, ABSORPTION EDGE are
520nm or so, Ag3PO4Light absorption of the monomer after 520nm is decreased obviously, and composite catalyst 520-800nm still have compared with
Strong light absorption.Show after adulterating PANI, the absorbing properties of composite material significantly increase.
Embodiment 2:
The Ag that will be prepared3PO4Monomer and Ag3PO4@3%PANI composite photo-catalyst is used for the degradation of phenol, to comment
Estimate its photocatalytic activity.The material 50mg being prepared is accurately weighed respectively in the phenol solution that 100mL concentration is 25mg/L,
Lasting stirring, and degradation reaction is carried out under 300W xenon lamp (λ > 420nm) irradiation condition.The solution of differential responses time is taken to carry out
Concentration mensuration, as a result as shown in Figure 5.This it appears that Ag3PO4The degradation capability of@PANI is significantly better than Ag3PO4Monomer.Fig. 6
For with Ag3PO4And Ag3PO4The corresponding polymerization kinetics curves of degradation curve of@PANI degradation of phenol.As shown, rate
Constant is by 0.016min-1It is increased to 0.18min-1, the photocatalytic speed of composite photocatalyst is 11.25 times of monomer.
Claims (4)
1. a kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter, comprising the following steps:
Polyaniline is added in n,N-Dimethylformamide (DMF) solution by step 1), is ultrasonically treated 2~5h；
Step 2) is by AgNO3Solution is added dropwise in above-mentioned DMF solution, is protected from light 6~20h of stirring；
Step 3) is by Na2HPO4·12H2O solution is added dropwise in the solution that step 2) obtains, and is protected from light 1~6h of stirring, is used water
For several times with ethanol washing, it is centrifugally separating to obtain solid portion, partial size is 0.15-0.38 after being made polyaniline-modified after vacuum drying
μm silver orthophosphate crystal.
2. a kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter according to right 1, it is characterised in that: step
It is rapid 1) described in polyaniline be conductivity type polyaniline (PANI), wherein the solid-to-liquid ratio of the PANI and DMF solution that add be 0.4~
2g/L。
3. a kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter according to right 1, it is characterised in that: step
Rapid 2) the described AgNO3Mass ratio with PANI is 30:1~120:1.
4. a kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter according to right 1, it is characterised in that: step
Rapid 3) the described Na2HPO4·12H2O and AgNO3Molar ratio be 1:3, vacuum drying temperature be 50~60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810581427.3A CN109433268A (en) | 2018-06-07 | 2018-06-07 | A kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810581427.3A CN109433268A (en) | 2018-06-07 | 2018-06-07 | A kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter |
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| Publication Number | Publication Date |
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| CN109433268A true CN109433268A (en) | 2019-03-08 |
Family
ID=65533040
Family Applications (1)
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| CN201810581427.3A Pending CN109433268A (en) | 2018-06-07 | 2018-06-07 | A kind of preparation method using polyaniline control silver orthophosphate crystal particle diameter |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110227557A (en) * | 2019-05-20 | 2019-09-13 | 湖南大学 | Silver orthophosphate and the pucherite Three-element composite photocatalyst of polyaniline modified synergic and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102935385A (en) * | 2012-11-02 | 2013-02-20 | 常州大学 | Efficient and stable visible light polyaniline group nanometer silver phosphate compound photocatalyst and preparation method thereof |
| KR101284610B1 (en) * | 2012-04-09 | 2013-07-17 | 한국과학기술원 | Nanofiber with elliptical pore structure, method for fabricating the same and articles comprising the same |
| CN107824207A (en) * | 2017-07-28 | 2018-03-23 | 湖南大学 | A kind of preparation method for the silver phosphate composite photocatalyst for handling water body Malachite Green |
-
2018
- 2018-06-07 CN CN201810581427.3A patent/CN109433268A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101284610B1 (en) * | 2012-04-09 | 2013-07-17 | 한국과학기술원 | Nanofiber with elliptical pore structure, method for fabricating the same and articles comprising the same |
| CN102935385A (en) * | 2012-11-02 | 2013-02-20 | 常州大学 | Efficient and stable visible light polyaniline group nanometer silver phosphate compound photocatalyst and preparation method thereof |
| CN107824207A (en) * | 2017-07-28 | 2018-03-23 | 湖南大学 | A kind of preparation method for the silver phosphate composite photocatalyst for handling water body Malachite Green |
Non-Patent Citations (1)
| Title |
|---|
| YUYU BU ET AL.: ""Role of Polyaniline on the Photocatalytic Degradation and Stability Performance of the Polyaniline/Silver/Silver Phosphate Composite under Visible Light"", 《ACS APPLIED MATERIALS & INTERFACES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110227557A (en) * | 2019-05-20 | 2019-09-13 | 湖南大学 | Silver orthophosphate and the pucherite Three-element composite photocatalyst of polyaniline modified synergic and its preparation method and application |
| CN110227557B (en) * | 2019-05-20 | 2021-04-20 | 湖南大学 | Silver phosphate and polyaniline synergistically modified bismuth vanadate ternary composite photocatalyst and preparation method and application thereof |
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Application publication date: 20190308 |