CN103990455A - Preparation method of bentonite supported silver vanadate photo-catalyst - Google Patents
Preparation method of bentonite supported silver vanadate photo-catalyst Download PDFInfo
- Publication number
- CN103990455A CN103990455A CN201410258304.8A CN201410258304A CN103990455A CN 103990455 A CN103990455 A CN 103990455A CN 201410258304 A CN201410258304 A CN 201410258304A CN 103990455 A CN103990455 A CN 103990455A
- Authority
- CN
- China
- Prior art keywords
- bentonite
- solution
- silver
- catalyst
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses a preparation method of bentonite supported silver vanadate photo-catalyst. The preparation method comprises the following steps: adding vanadium pentoxide into nitrite acid solution, stirring to form a VO<2+> solution; adding dried bentonite powder into the VO<2+> solution, stirring, precipitating, separating, washing, drying at the temperature of 105 DEG C, then calcining by heating to 300-400 DEG C and thus preparing bentonite modified by V2O5; weighing 1-1.2mmol of silver nitrate and preparing into a 10-15mmol/L solution, dropwise adding diluted ammonia water into the solution, dropwise adding and vibrating simultaneously, carrying out solid-liquid separation after fully precipitating, pouring off supernatant liquor, continuously adding the diluted ammonia water into the solid dropwise till the primary sediment is just fully dissolved; adding the bentonite modified by V2O5 into a Tollen reagent , stirring for 4-6 hours, separating the sediment, washing the sediment with distilled water for 3-4 times, then drying at the temperature of 100-105 DEG C to obtain the bentonite supported silver vanadate photo-catalyst. By virtue of the method, silver vanadate is successfully fixed in bentonite layers, thereby facilitating the absorption and the catalysis, and fully the nanometer effect of the catalyst is fully exerted.
Description
Technical field
The invention belongs to water treatment field, relate to a kind of preparation method of alta-mud load vanadic acid silver photochemical catalyst, relate in particular to a kind of catalysis material for the treatment of organic wastewater and preparation method thereof.
Background technology
Current, follow the develop rapidly of industrial technology, the water resource that the mankind depend on for existence is all subject to pollution in various degree, and water resource pollution has become the problem demanding prompt solution that countries in the world face.The existence of the pollutant in water, particularly toxic organic pollutant, not only causes environmental pollution, ecological disruption, and serious harm human health.These organic pollutions comprise polycyclic aromatic hydrocarbon, Polychlorinated biphenyls, agricultural chemicals, environmental disturbances element, dyestuff etc.
Bentonite is a kind of clay rock that montmorillonite is that essential mineral forms of take, at field of environment protection also wide application prospect.The layer silicate mineral that montmorillonite is comprised of aluminum oxide octahedral sheet that limit connects altogether of two tetrahedral si-o film therebetween that top connects altogether, monolithic layer in its structure is the thin slice that asperratio is very large, diameter is about 100-200nm, and thickness is only 1nm.The such thin slice of 5-10 layer, by the interlayer cation formation basic granules that combines, form larger irregular group, thereby bentonite has layer structure by these basic granuleses.In structure, aluminium is to silicon and the magnesium ion exchange alternative to the isomorph of aluminium, can cause negative electrical charge (being layer charge) surplus in construction unit layer, for reaching the balance of positive and negative charge, needs the cation of some to compensate and is positioned at interlayer region.These cations are with ion bonding force connecting structure elementary layer, and are movable, and its key is more much bigger than molecular link or hydrogen bond by force.Therefore when smectite structure elementary layer internal charge does not reach balance, in the space between elementary layer, will carry out filling by a certain amount of cation, thereby (sun) ion exchange will occur.Montmorillonite is because isomorph in broken key, lattice replaces and to be adsorbed on its surperficial humus dissociation etc. former thereby electronegative, thereby cause between lattice layer in conjunction with loose, meet water and easily expand into fragment, particle decentralization is high, there is huge internal surface area and a large amount of exchangeable cations, make it have good absorption property and ion-exchange performance (unit bentonite cation exchange capacity is about 74～130mmol/100g).
Vanadic acid silver is that a class has visible light-responded novel photocatalyst, and its monoclinic phase energy gap is lower than 2.7eV, has higher visible light-respondedly, and stable in properties, becomes study hotspot in recent years.Vanadic acid silver has multiple preparation method, as solid-phase synthesis, coprecipitation, chemical deposition, metalorganic decomposition, hydro-thermal method, sonochemical method etc.Vanadic acid silver prepared by these methods is nano particle, although have higher specific area, easily reunites, and reduces treatment effect, and is difficult to and aqueous phase separation after processing waste water, and its practicality is reduced greatly.
Summary of the invention
The object of the invention is for overcoming the deficiencies in the prior art, a kind of preparation method of alta-mud load vanadic acid silver photochemical catalyst is provided.
Object of the present invention can be achieved through the following technical solutions:
A kind of preparation method of alta-mud load vanadic acid silver photochemical catalyst adopts following methods to make:
1) 5～8g vanadic anhydride is joined in the salpeter solution that 25mL concentration is 0.1～0.5mol/L, stir 20～40min, generate VO
2 +solution;
2) to VO
2 +in solution, add 8～10g to be dried, to pulverize the bentonite of 100 mesh sieves, stir 4～8h, VO
2 +with the cation between bentonite bed exchanges, precipitate and separate, with distilled water washing 2～3 times, makes VO
2 +pillared bentonite, by VO
2 +pillared bentonite is warmed up to 300～400 ℃ of calcinings after drying at 105 ℃, by the VO in bentonite bed
2 +be converted into V
2o
5, make V
2o
5the bentonite of modification;
3) take 1～1.2mmol silver nitrate and be configured to 10～15mmol/L solution, in this solution, drip weak aqua ammonia, the vibration of dropping limit, limit, after complete to precipitation, Separation of Solid and Liquid, after supernatant is outwelled, continues to drip weak aqua ammonia in solid, until the initial precipitation occurring is dissolved just completely, obtain silver ammino solution;
4) by V
2o
5the bentonite of modification joins in silver ammino solution, stirs 4-6h, under alkali condition, and V
2o
5form vanadate, vanadate and silver ion reaction generate vanadic acid silver between bentonite bed, precipitate and separate, and after distilled water washing 3～4 times, 100～105 ℃ of oven dry, obtain a kind of alta-mud load vanadic acid silver photochemical catalyst.
Described bentonite is commercially available calcium base or sodium bentonite.
The invention has the beneficial effects as follows:
1, bentonite is after modification, there is very bigger serface, can be used for adsorb organic compound, the catalytic action of recycling vanadic acid silver, can directly the organic pollution of absorption be decomposed into harmless material (as carbon dioxide, water etc.), after decomposition, this water treatment agent can reuse.
2, vanadic acid silver is fixed between bentonite bed, and between its particle, reuniting may be less, can remain nano effect, strengthens adsorption effect.
The specific embodiment
Embodiment 1
8g vanadic anhydride is joined in the salpeter solution that 25mL concentration is 0.5mol/L, stir 40min, generate VO
2 +solution; To VO
2 +in solution, add 10g to be dried, to pulverize the commercially available calcium-base bentonite of 100 mesh sieve, stir 8h, VO
2 +with the cation between bentonite bed exchanges, precipitate and separate, with distilled water washing 3 times, makes VO
2 +pillared bentonite, by VO
2 +pillared bentonite is warmed up to 400 ℃ of calcinings after drying at 105 ℃, by the VO in bentonite bed
2 +be converted into V
2o
5, make V
2o
5the bentonite of modification; Take 1.2mmol silver nitrate and be configured to 15mmol/L solution, in this solution, drip weak aqua ammonia, the vibration of dropping limit, limit, after complete to precipitation, Separation of Solid and Liquid, after supernatant is outwelled, continues to drip weak aqua ammonia in solid, until the initial precipitation occurring is dissolved just completely, obtain silver ammino solution; By V
2o
5the bentonite of modification joins in silver ammino solution, stirs 6h, under alkali condition, and V
2o
5form vanadate, vanadate and silver ion reaction generate vanadic acid silver between bentonite bed, precipitate and separate, and after distilled water washing 4 times, 105 ℃ of oven dry, obtain a kind of alta-mud load vanadic acid silver photochemical catalyst.
The catalyst 0.75g obtaining is joined in the Orange II waste water that 550mL concentration is 50mg/L, under 300w iodine-tungsten lamp irradiates, react 80 minutes, percent of decolourization is 90.2%.
Embodiment 2
5g vanadic anhydride is joined in the salpeter solution that 25mL concentration is 0.1mol/L, stir 20min, generate VO
2 +solution; To VO
2 +in solution, add 8g to be dried, to pulverize the commercially available sodium bentonite of 100 mesh sieve, stir 4h, VO
2 +with the cation between bentonite bed exchanges, precipitate and separate, with distilled water washing 2 times, makes VO
2 +pillared bentonite, by VO
2 +pillared bentonite is warmed up to 300 ℃ of calcinings after drying at 105 ℃, by the VO in bentonite bed
2 +be converted into V
2o
5, make V
2o
5the bentonite of modification; Take 1mmol silver nitrate and be configured to 10mmol/L solution, in this solution, drip weak aqua ammonia, the vibration of dropping limit, limit, after complete to precipitation, Separation of Solid and Liquid, after outwelling supernatant, continuation drips weak aqua ammonia in solid, until the initial precipitation occurring is dissolved just completely, obtains silver ammino solution; By V
2o
5the bentonite of modification joins in silver ammino solution, stirs 4h, under alkali condition, and V
2o
5form vanadate, vanadate and silver ion reaction generate vanadic acid silver between bentonite bed, precipitate and separate, and after distilled water washing 3 times, 100 ℃ of oven dry, obtain a kind of alta-mud load vanadic acid silver photochemical catalyst.
The catalyst 0.75g obtaining is joined in the Orange II waste water that 550mL concentration is 50mg/L, under 300w iodine-tungsten lamp irradiates, react 80 minutes, percent of decolourization is 91.4%.
Embodiment 3
7g vanadic anhydride is joined in the salpeter solution that 25mL concentration is 0.4mol/L, stir 30min, generate VO
2 +solution; To VO
2 +in solution, add 10g to be dried, to pulverize the commercially available calcium-base bentonite of 100 mesh sieve, stir 6h, VO
2 +with the cation between bentonite bed exchanges, precipitate and separate, with distilled water washing 3 times, makes VO
2 +pillared bentonite, by VO
2 +pillared bentonite is warmed up to 400 ℃ of calcinings after drying at 105 ℃, by the VO in bentonite bed
2 +be converted into V
2o
5, make V
2o
5the bentonite of modification; Take 1.2mmol silver nitrate and be configured to 15mmol/L solution, in this solution, drip weak aqua ammonia, the vibration of dropping limit, limit, after complete to precipitation, Separation of Solid and Liquid, after supernatant is outwelled, continues to drip weak aqua ammonia in solid, until the initial precipitation occurring is dissolved just completely, obtain silver ammino solution; By V
2o
5the bentonite of modification joins in silver ammino solution, stirs 5h, under alkali condition, and V
2o
5form vanadate, vanadate and silver ion reaction generate vanadic acid silver between bentonite bed, precipitate and separate, and after distilled water washing 4 times, 105 ℃ of oven dry, obtain a kind of alta-mud load vanadic acid silver photochemical catalyst.
The catalyst 0.75g obtaining is joined in the methylene blue waste water that 550mL concentration is 50mg/L, under 300w iodine-tungsten lamp irradiates, react 80 minutes, percent of decolourization is 94.3%.
Claims (1)
1. the preparation method of alta-mud load vanadic acid silver photochemical catalyst adopts a following methods, it is characterized in that in turn including the following steps:
1) 5～8g vanadic anhydride is joined in the salpeter solution that 25mL concentration is 0.1～0.5mol/L, stir 20～40min, generate VO
2 +solution;
2) to VO
2 +in solution, add 8～10g to be dried, to pulverize the bentonite of 100 mesh sieves, stir 4～8h, VO
2 +with the cation between bentonite bed exchanges, precipitate and separate, with distilled water washing 2～3 times, makes VO
2 +pillared bentonite, by VO
2 +pillared bentonite is warmed up to 300～400 ℃ of calcinings after drying at 105 ℃, by the VO in bentonite bed
2 +be converted into V
2o
5, make V
2o
5the bentonite of modification;
3) take 1～1.2mmol silver nitrate and be configured to 10～15mmol/L solution, in this solution, drip weak aqua ammonia, the vibration of dropping limit, limit, after complete to precipitation, Separation of Solid and Liquid, after supernatant is outwelled, continues to drip weak aqua ammonia in solid, until the initial precipitation occurring is dissolved just completely, obtain silver ammino solution;
4) by V
2o
5the bentonite of modification joins in silver ammino solution, stirs 4-6h, under alkali condition, and V
2o
5form vanadate, vanadate and silver ion reaction generate vanadic acid silver between bentonite bed, precipitate and separate, and after distilled water washing 3～4 times, 100～105 ℃ of oven dry, obtain a kind of alta-mud load vanadic acid silver photochemical catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410258304.8A CN103990455B (en) | 2014-06-11 | 2014-06-11 | A kind of preparation method of alta-mud load silver vanadate photochemical catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410258304.8A CN103990455B (en) | 2014-06-11 | 2014-06-11 | A kind of preparation method of alta-mud load silver vanadate photochemical catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103990455A true CN103990455A (en) | 2014-08-20 |
| CN103990455B CN103990455B (en) | 2015-12-30 |
Family
ID=51304934
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410258304.8A Active CN103990455B (en) | 2014-06-11 | 2014-06-11 | A kind of preparation method of alta-mud load silver vanadate photochemical catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103990455B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104998639A (en) * | 2015-08-05 | 2015-10-28 | 常州市长润石油有限公司 | Method for preparing silver oxide and carbon composite catalyst by means of industrial wastewater |
| CN110496624A (en) * | 2019-08-22 | 2019-11-26 | 四川建筑职业技术学院 | A kind of composite material and preparation method for sewage treatment |
| CN112661165A (en) * | 2020-12-10 | 2021-04-16 | 北京机械力化学研究院有限公司 | High-energy grinding preparation of rare earth-loaded bentonite and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19705326A1 (en) * | 1997-02-12 | 1998-08-13 | Basf Ag | Selective oxidation of non-cyclic unsaturated hydrocarbon |
| CN101069846A (en) * | 2006-05-09 | 2007-11-14 | 北京化工大学 | Preparation of high-activity silver-carried/titanium dioxide pillar braced montomorillonite composite nano catalyst |
| EP2436439A1 (en) * | 2010-10-01 | 2012-04-04 | Council of Scientific and Industrial Research | Ruthenium complex intercalated N-doped or N,S-codoped titania pillared montmorillonite and a process for the preparation thereof |
| CN102600869A (en) * | 2012-02-23 | 2012-07-25 | 常州水木环保科技有限公司 | Synthetic method of supported silver phosphate photocatalyst |
-
2014
- 2014-06-11 CN CN201410258304.8A patent/CN103990455B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19705326A1 (en) * | 1997-02-12 | 1998-08-13 | Basf Ag | Selective oxidation of non-cyclic unsaturated hydrocarbon |
| CN101069846A (en) * | 2006-05-09 | 2007-11-14 | 北京化工大学 | Preparation of high-activity silver-carried/titanium dioxide pillar braced montomorillonite composite nano catalyst |
| EP2436439A1 (en) * | 2010-10-01 | 2012-04-04 | Council of Scientific and Industrial Research | Ruthenium complex intercalated N-doped or N,S-codoped titania pillared montmorillonite and a process for the preparation thereof |
| CN102600869A (en) * | 2012-02-23 | 2012-07-25 | 常州水木环保科技有限公司 | Synthetic method of supported silver phosphate photocatalyst |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104998639A (en) * | 2015-08-05 | 2015-10-28 | 常州市长润石油有限公司 | Method for preparing silver oxide and carbon composite catalyst by means of industrial wastewater |
| CN110496624A (en) * | 2019-08-22 | 2019-11-26 | 四川建筑职业技术学院 | A kind of composite material and preparation method for sewage treatment |
| CN112661165A (en) * | 2020-12-10 | 2021-04-16 | 北京机械力化学研究院有限公司 | High-energy grinding preparation of rare earth-loaded bentonite and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103990455B (en) | 2015-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | Visible light photocatalytic degradation of MB using UiO-66/g-C3N4 heterojunction nanocatalyst | |
| Xu et al. | Catalytic degradation of sulfamethoxazole through peroxymonosulfate activated with expanded graphite loaded CoFe2O4 particles | |
| Yuan et al. | Self-assembled hierarchical and bifunctional MIL-88A (Fe)@ ZnIn2S4 heterostructure as a reusable sunlight-driven photocatalyst for highly efficient water purification | |
| Li et al. | TiO2 nanoparticles anchored onto the metal–organic framework NH2-MIL-88B (Fe) as an adsorptive photocatalyst with enhanced fenton-like degradation of organic pollutants under visible light irradiation | |
| Zhang et al. | Synthesis of flower-like MoS2/g-C3N4 nanosheet heterojunctions with enhanced photocatalytic reduction activity of uranium (VI) | |
| Chen et al. | Layered photocatalytic nanomaterials for environmental applications | |
| Zou et al. | β-Cyclodextrin modified graphitic carbon nitride for the removal of pollutants from aqueous solution: experimental and theoretical calculation study | |
| Zhang et al. | Super adsorption capability of rhombic dodecahedral Ca-Al layered double oxides for Congo red removal | |
| Wang et al. | Porous BiOBr/Bi2MoO6 heterostructures for highly selective adsorption of methylene blue | |
| Li et al. | Solar light-responsive CdS/UiO-66-NH2 for ultrafast uranium reduction from uranium-containing mine wastewater without external sacrificial agents | |
| CN102407117B (en) | Photocatalysis water-treating material as well as preparation method and application thereof | |
| Zhang et al. | Green recovery of titanium and effective regeneration of TiO2 photocatalysts from spent selective catalytic reduction catalysts | |
| Kumar et al. | Two dimensional S-scheme Bi2WO6–TiO2–Ti3C2 nanocomposites for efficient degradation of organic pollutants under natural sunlight | |
| Sun et al. | Self-assembly of tungstophosphoric acid/acidified carbon nitride hybrids with enhanced visible-light-driven photocatalytic activity for the degradation of imidacloprid and acetamiprid | |
| Guo et al. | Ag3PO4/rectorite nanocomposites: Ultrasound-assisted preparation, characterization and enhancement of stability and visible-light photocatalytic activity | |
| Ren et al. | In situ synthesis of gC 3 N 4/TiO 2 heterojunction nanocomposites as a highly active photocatalyst for the degradation of Orange II under visible light irradiation | |
| Xu et al. | Sonocatalytic degradation of tetracycline by BiOBr/FeWO4 nanomaterials and enhancement of sonocatalytic effect | |
| Meng et al. | Effects of inter/intralayer adsorption and direct/indirect reaction on photo-removal of pollutants by layered g-C3N4 and BiOBr | |
| Hussein et al. | Mesoporous spongy Ni–Co oxides@ wheat straw-derived SiO2 for adsorption and photocatalytic degradation of methylene blue pollutants | |
| Xu et al. | Heterojunction material BiYO3/g-C3N4 modified with cellulose nanofibers for photocatalytic degradation of tetracycline | |
| Chen et al. | Preparation of nano-Fe0 modified coal fly-ash composite and its application for U (VI) sequestration | |
| Sun et al. | Facile preparation of hydroxyl‑rich mesoporous magnesium silicate with excellent adsorption performance | |
| Yang et al. | Removing low concentration of Cr (III) from wastewater: using titanium dioxide surface modified montmorillonite as a selective adsorbent | |
| CN104801308A (en) | NiFe2O4/TiO2/sepiolite composite photocatalyst and preparation method thereof | |
| Song et al. | Modifying MOF-derived hollow BiVO4 architecture with copper tetraphenylphorphyrin as high-efficiency wide-visible-light Z-scheme heterojunction photocatalyst for 2-chlorophenol degradation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201118 Address after: No. 159, Chengjiang Middle Road, Jiangyin City, Wuxi City, Jiangsu Province Patentee after: Jiangyin Intellectual Property Operation Co.,Ltd. Address before: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Patentee before: CHANGZHOU University |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220915 Address after: No. 118, Xiji Avenue, Nanyue Village, Xinjie Street, Yixing City, Wuxi City, Jiangsu Province, 214200 Patentee after: Wuxi Wisdom Xingyi Information Technology Co.,Ltd. Address before: No. 159, Chengjiang Middle Road, Jiangyin City, Wuxi City, Jiangsu Province Patentee before: Jiangyin Intellectual Property Operation Co.,Ltd. |
|
| TR01 | Transfer of patent right |