CN103801341A - Method for preparing carbon fiber modified hydrotalcite lamella loaded silver phosphate - Google Patents
Method for preparing carbon fiber modified hydrotalcite lamella loaded silver phosphate Download PDFInfo
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- CN103801341A CN103801341A CN201410068737.7A CN201410068737A CN103801341A CN 103801341 A CN103801341 A CN 103801341A CN 201410068737 A CN201410068737 A CN 201410068737A CN 103801341 A CN103801341 A CN 103801341A
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- hydrotalcite
- lamella
- silver phosphate
- silver orthophosphate
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Abstract
The invention discloses a method for preparing carbon fiber modified hydrotalcite lamella loaded silver phosphate. The method comprises the following specific steps: adding hydrotalcite powder into a crylic acid solution, adding silver phosphate while stirring constantly, then adding ammonium persulfate, and after stirring, performing precipitation separation and stoving; putting in a vacuum furnace, calcining in vacuum, then stripping the hydrotalcite lamella off in a microwave oven; finally, adding into a phosphoric acid solution, stirring, separating, and stoving so as to obtain the carbon fiber modified hydrotalcite lamella loaded silver phosphate catalyst. Carbon fibers and silver phosphate particles cover the surface of the hydrotalcite layer, and due to the electrical conductivity of the carbon fibers, photoproduction electrons can be educed to be prevented from combining with a hole. As the hydrotalcite is in a stripped state, the huge inner surface area of the hydrotalcite becomes the outer surface area, and the silver phosphate loaded on the surface of the hydrotalcite is easy to illuminate by light during photocatalysis, and is likely to contact an organic substance to be processed so as to promote mass transfer.
Description
Technical field
The present invention relates to environmental pollution control field of new, relate in particular to the preparation of the fiber-modified hydrotalcite lamella load silver orthophosphate of a kind of carbonaceous.
Background technology
Along with scientific and technological development, environment and the mankind's health from the murder by poisoning organic pollution serious threat producing in industrial and agricultural production, seek a kind of new and effective environmental improvement technology and have great importance.Photocatalysis technology, because it is energy-conservation, efficient, contaminant degradation thorough, non-secondary pollution advantage, has become a kind of emerging environmental improvement technology with important application prospect at present.In recent years, the development of new and effective visible-light photocatalyst becomes an important research content in photocatalysis technology, wherein there is the catalysis material of surface plasma resonance effect, because of its unique Surface Physical Chemistry character and efficient visible light photocatalysis performance, become one of focus of research.
Hydrotalcite-based compound (LDHs) is to pile up by interlayer anion and positively charged laminate the compound forming.Hydrotalcite chemical structure of general formula is: [M
2+ 1-xm
3+x (OH)
2]
x+[(A
n-)
x/nmH
2o], wherein M
2+and M
3+be respectively the divalence and the trivalent metal cation that are positioned on main body laminate, as Mg
2+, Ni
2+, Zn
2+, Mn
2+, Cu
2+, Co
2+, Pd
2+, Fe
2+deng bivalent cation and Al
3+, Cr
3+, Co
3+, Fe
3+all can form hydrotalcite Deng Tricationic; A
n–for interlayer anion, can comprise inorganic anion, organic anion, complex anion, same many and heteropolyanion; X is M
3+/ (M
2++ M
3+) molar ratio, be approximately that 4:1 is to 2:1; M is the number of intermediary water molecule.Its structure is similar to shepardite Mg (OH)
2, share seamed edge and form main body laminate by octahedron.Be positioned at the divalent metal M on laminate
2+can be by the close trivalent metal cation M of ion half price in certain proportion
3+the isomorphous replace, make laminate positively charged, interlayer exist can exchange anion and laminate on positive charge balance, make the overall structure of LDHs be electroneutral.The anion of interlayer can be exchanged, and through a series of modifications, hydrotalcite material can obtain the many kinds of materials that performance is different.
Utilize the catalyst of hydrotalcite load, in current catalyticing research field, occupy important position.It has that preparation technology is simple, catalytic selectivity good, catalytic activity is high, pollution-free, the easy advantage that separates with reaction system and can be recycled etc.But in the application process of hydrotalcite supported catalyst, also there are some problems: such as hydrotalcite by catalyst cupport after interlayer, interlamellar spacing may some increase, but because hydrotalcite is a layer structure, be horizontal structure between layers, interlamellar spacing is less, and centre is also being mingled with catalyst crystal, also has in addition interlayer in conjunction with water, have a strong impact on the diffusion of pollutant to catalyst surface, caused catalyst surface not to be utilized completely, and reduced catalytic efficiency.
Silver orthophosphate is a kind of novel visible light catalyst, and this catalyst activity is high, and application is wide, can be for various organic substance decomposings.But this poor catalyst stability, the hole producing under light action and light induced electron are easily compound, cause its recycling rate of waterused low.
Summary of the invention
The object of the invention is for overcoming the deficiencies in the prior art, the preparation of the fiber-modified hydrotalcite lamella load silver orthophosphate of a kind of carbonaceous is provided.
The technical solution used in the present invention is in turn include the following steps:
1) be that 10g, the drying water talcum powder of crossing 80-100 mesh sieve join in the acrylic acid solution that 50mL, concentration are 200～400mmol/L by weight, stir 1h, when stirring, add again 20mL, concentration is the silver orthophosphate of 100～180mmol/L, continue to stir 3h, by acrylate ionomer and Ag ion exchange to hydrotalcite layers;
2) in above-mentioned system, add initator 5～15mmol ammonium persulfate, stir 4-5h at 60～80 ℃, polymerization occurs, form macromolecular fibre polymer, precipitate and separate, 60～75 ℃ of oven dry in hydrotalcite layers;
3) material obtaining is placed in to vacuum drying oven, isolated air calcination 2～3h at 400～600 ℃, by macromolecular fibre carbonization wherein, forms carbonaceous fiber;
4) product after calcining is placed in to 700w micro-wave oven, microwave irradiation 15～25min, utilizes the effect of micro-wave oven, and part carbon is burnt formation carbon dioxide by local heat, and hydrotalcite lamella is peeled off;
5) it is 50mL that the product of microwave irradiation being crossed joins volume, in the phosphoric acid solution that concentration is 20～40mmol/L, stirs 2～4h, precipitate and separate, and 80～105 ℃ of oven dry obtain the fiber-modified hydrotalcite lamella load silver orthophosphate catalyst of a kind of carbonaceous.
Hydrotalcite described in step 1) can be commercially available commodity, also can prepare according to prior art, and its technology of preparing is commonly known.Hydrotalcite chemical structure of general formula is: [M
2+ 1-xm
3+x (OH)
2]
x+[(A
n-)
x/nmH
2o], wherein M
2+for Mg
2+, Ni
2+, Mn
2+, Zn
2+, Ca
2+, Fe
2+, Cu
2+deng any in divalent metal; M
3+for Al
3+, Cr
3+, F
e 3+, C
o 3+deng any in trivalent metal cation; An-is anion, as CO
3 2-, NO
3 -, Cl
-, OH
-, SO
4 2-, PO
4 3-deng any in inorganic ions; X=0.5～0.15; M
2+/ M
3+=1～5.
First the anion exchange effect that utilizes hydrotalcite will have the monomer of polymerization and Ag ion exchange to hydrotalcite layers, then polymerization, carbonization, peel off, last phosphoric acid and silver oxide effect generate silver orthophosphate.In this process, owing to suitably controlling the exchange capacity of polymerization single polymerization monomer, can control monomer polymerization is the fibrous hydrotalcite layers that is present in, and through after carbonization, forms carbonaceous fiber.
There is silver orthophosphate particle in carbonaceous fiber surface, silver orthophosphate can excite and form hole and light induced electron after illumination, due to the electric conductivity of carbonaceous fiber, light induced electron can be derived to the reduction reaction participating in solution, thereby avoided compound with hole.Hole participates in oxidation reaction.
Because partial organic substances is decomposed in the heating using microwave that utilizes micro-wave oven, in decomposable process, produce a large amount of carbon dioxide, by the layer structural deterioration of hydrotalcite, the hydrotalcite that obtains peeling off, due in peeling off state, huge hydrotalcite internal surface area becomes external surface area, and the silver orthophosphate of its area load is more acceptant to illumination in photocatalytic process, be easier to contact with pending organic matter, promote mass transfer.
The specific embodiment
3 embodiment of the present invention are below further provided:
Embodiment 1
Weight is 10g, crosses the drying water talcum powder of 100 mesh sieves and join in the acrylic acid solution that 50mL, concentration are 400mmol/L, stir 1h, when stirring, add 20mL, the silver orthophosphate that concentration is 180mmol/L, continues to stir 3h again, add again initator 15mmol ammonium persulfate, at 80 ℃, stir 5h, precipitate and separate, 75 ℃ of oven dry; The material obtaining is placed in to vacuum drying oven, isolated air calcination 3h at 600 ℃; Product after calcining is placed in to 700w micro-wave oven, and microwave irradiation 25min, peels off hydrotalcite lamella; It is 50mL that product is joined to volume, in the phosphoric acid solution that concentration is 40mmol/L, stirs 4h, precipitate and separate, and 105 ℃ of oven dry obtain the fiber-modified hydrotalcite lamella load silver orthophosphate catalyst of a kind of carbonaceous.
By hydrotalcite lamella load silver orthophosphate the catalyst fiber-modified carbonaceous making for the treatment of wastewater containing methylene blue: 0.5g exfoliated hydrotalcite load silver orthophosphate catalyst joins in the methylene blue waste water that 300mL concentration is 50mg/L, under 300w Metal halogen lamp irradiates, reaction 30min, percent of decolourization is 97.1%, after catalyst separation recycling 5 times, under similarity condition, reaction 30min, percent of decolourization is 92.9%.The silver orthophosphate particle of same quality is under identical condition, when 30min, percent of decolourization is 91.2%, compares the fiber-modified hydrotalcite lamella load silver orthophosphate catalyst of carbonaceous, and the contained silver amount of silver orthophosphate particle is relatively much bigger, therefore the product that the application obtains is more economical, better effects if.
Embodiment 2
Weight is 10g, crosses the drying water talcum powder of 80 mesh sieves and join in the acrylic acid solution that 50mL, concentration are 200mmol/L, stir 1h, when stirring, add 20mL, the silver orthophosphate that concentration is 100mmol/L, continues to stir 3h again, add again initator 5mmol ammonium persulfate, at 60 ℃, stir 4h, precipitate and separate, 60 ℃ of oven dry; The material obtaining is placed in to vacuum drying oven, isolated air calcination 2h at 400 ℃; Product after calcining is placed in to 700w micro-wave oven, and microwave irradiation 15min, peels off hydrotalcite lamella; It is 50mL that product is joined to volume, in the phosphoric acid solution that concentration is 20mmol/L, stirs 2h, precipitate and separate, and 80 ℃ of oven dry obtain the fiber-modified hydrotalcite lamella load silver orthophosphate catalyst of a kind of carbonaceous.
By hydrotalcite lamella load silver orthophosphate the catalyst fiber-modified carbonaceous making for the treatment of containing acid scarlet waste water: 0.5g exfoliated hydrotalcite load silver orthophosphate catalyst joins in the acid scarlet waste water that 300mL concentration is 50mg/L, under 300w Metal halogen lamp irradiates, reaction 30min, percent of decolourization is 96.1%, after catalyst separation recycling 5 times, under similarity condition, reaction 30min, percent of decolourization is 93.2%.The silver orthophosphate particle of same quality is under identical condition, and when 30min, percent of decolourization is 90.1%.
Embodiment 3
Weight is 10g, crosses the drying water talcum powder of 80 mesh sieves and join in the acrylic acid solution that 50mL, concentration are 300mmol/L, stir 1h, when stirring, add 20mL, the silver orthophosphate that concentration is 100mmol/L, continues to stir 3h again, add again initator 5mmol ammonium persulfate, at 60 ℃, stir 4h, precipitate and separate, 60 ℃ of oven dry; The material obtaining is placed in to vacuum drying oven, isolated air calcination 3h at 500 ℃; Product after calcining is placed in to 700w micro-wave oven, and microwave irradiation 25min, peels off hydrotalcite lamella; It is 50mL that product is joined to volume, in the phosphoric acid solution that concentration is 40mmol/L, stirs 4h, precipitate and separate, and 105 ℃ of oven dry obtain the fiber-modified hydrotalcite lamella load silver orthophosphate catalyst of a kind of carbonaceous.
By hydrotalcite lamella load silver orthophosphate the catalyst fiber-modified carbonaceous making for the treatment of containing acid scarlet waste water: 0.5g exfoliated hydrotalcite load silver orthophosphate catalyst joins in the acid scarlet waste water that 300mL concentration is 50mg/L, under 300w Metal halogen lamp irradiates, reaction 30min, percent of decolourization is 97.6%, after catalyst separation recycling 5 times, under similarity condition, reaction 30min, percent of decolourization is 94.6%.The silver orthophosphate particle of same quality is under identical condition, and when 30min, percent of decolourization is 91.9%.
Claims (1)
1. a preparation for the fiber-modified hydrotalcite lamella load silver orthophosphate of carbonaceous, is characterized in that in turn including the following steps:
1) be that 10g, the drying water talcum powder of crossing 80-100 mesh sieve join in the acrylic acid solution that 50mL, concentration are 200～400mmol/L by weight, stir 1h, when stirring, add again 20mL, concentration is the silver orthophosphate of 100～180mmol/L, continue to stir 3h, by acrylate ionomer and Ag ion exchange to hydrotalcite layers;
2) in above-mentioned system, add initator 5～15mmol ammonium persulfate, stir 4-5h at 60～80 ℃, polymerization occurs, form macromolecular fibre polymer, precipitate and separate, 60～75 ℃ of oven dry in hydrotalcite layers;
3) material obtaining is placed in to vacuum drying oven, isolated air calcination 2～3h at 400～600 ℃, by macromolecular fibre carbonization wherein, forms carbonaceous fiber;
4) product after calcining is placed in to 700w micro-wave oven, microwave irradiation 15～25min, utilizes the effect of micro-wave oven, and part carbon is burnt formation carbon dioxide by local heat, and hydrotalcite lamella is peeled off;
5) it is 50mL that the product of microwave irradiation being crossed joins volume, in the phosphoric acid solution that concentration is 20～40mmol/L, stirs 2～4h, precipitate and separate, and 80～105 ℃ of oven dry obtain the fiber-modified hydrotalcite lamella load silver orthophosphate catalyst of a kind of carbonaceous.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325543A (en) * | 2018-02-02 | 2018-07-27 | 华北理工大学 | A kind of synthetic method of activated carbon supported petal-shaped silver orthophosphate complex phase catalysis material |
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| CN102796215A (en) * | 2012-08-09 | 2012-11-28 | 福建师范大学 | Preparation method of peeled-up yellow-light hydrotalcite like/polymer nanocomposite |
| CN102910622A (en) * | 2012-10-25 | 2013-02-06 | 常州大学 | Preparation method of two-dimensional nano-graphene |
| WO2013169126A2 (en) * | 2012-05-09 | 2013-11-14 | Uniwersytet Jagielloński | Method for obtaining oxide catalysts on the base of exfoliated layered aluminosilicates |
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2014
- 2014-02-27 CN CN201410068737.7A patent/CN103801341B/en active Active
Patent Citations (3)
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| WO2013169126A2 (en) * | 2012-05-09 | 2013-11-14 | Uniwersytet Jagielloński | Method for obtaining oxide catalysts on the base of exfoliated layered aluminosilicates |
| CN102796215A (en) * | 2012-08-09 | 2012-11-28 | 福建师范大学 | Preparation method of peeled-up yellow-light hydrotalcite like/polymer nanocomposite |
| CN102910622A (en) * | 2012-10-25 | 2013-02-06 | 常州大学 | Preparation method of two-dimensional nano-graphene |
Non-Patent Citations (1)
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|---|
| JIAN FENG MA ET AL.: "Synthesis and characterization of Ag3PO4 immobilized in bentonite for the sunlight-driven degradation of Orange II", 《APPLIED CATALYSIS B: ENVIRONMENTAL》, vol. 134135, 2 January 2013 (2013-01-02) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325543A (en) * | 2018-02-02 | 2018-07-27 | 华北理工大学 | A kind of synthetic method of activated carbon supported petal-shaped silver orthophosphate complex phase catalysis material |
| CN108325543B (en) * | 2018-02-02 | 2021-02-02 | 华北理工大学 | Synthetic method of activated carbon-loaded petal-shaped silver phosphate complex-phase photocatalytic material |
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Effective date of registration: 20171205 Address after: Daitou town of Liyang City Ferry Street 213311 Jiangsu city of Changzhou province 8-2 No. 7 Patentee after: Liyang Chang Technology Transfer Center Co., Ltd. Address before: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Patentee before: Changzhou University |
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