CN103934008B - A kind of preparation method of galapectite load silver phosphate photocatalyst - Google Patents
A kind of preparation method of galapectite load silver phosphate photocatalyst Download PDFInfo
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- CN103934008B CN103934008B CN201410156228.XA CN201410156228A CN103934008B CN 103934008 B CN103934008 B CN 103934008B CN 201410156228 A CN201410156228 A CN 201410156228A CN 103934008 B CN103934008 B CN 103934008B
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- galapectite
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- silver nitrate
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Abstract
The present invention discloses a kind of preparation method of galapectite load silver phosphate photocatalyst, concrete steps are as follows: joined by galapectite in salpeter solution, obtain acid-treated galapectite, acid-treated for 4 ~ 8g galapectite is placed in vacuum filtration bottle, under vacuum conditions with the mixing of silver nitrate ethanolic solution, allow silver nitrate fully enter in galapectite pipe, continue stirring 2 ~ 3h, Separation of Solid and Liquid, the oven dry of 70 ~ 80 DEG C, vacuum; Join 50mL by drying the product obtained, concentration is in the sodium dihydrogen phosphate of 0.5 ~ 1.5mol/L, stirs 4 ~ 5h, Separation of Solid and Liquid, and washing, dries and obtain a kind of galapectite load silver phosphate photocatalyst for 100 ~ 105 DEG C.Advantage of the present invention is: the ducted air of emptying galapectite and steam, allows silver nitrate enter into pipeline; Remove the aluminum oxide of galapectite inwall, increase light can be reached and thoroughly spend and increase the effect in aperture; It is inner that the silver orthophosphate particle obtained is present in galapectite pipe, avoids reuniting and coming off.
Description
Technical field
The present invention relates to novel environmental pollution control material field, particularly relate to a kind of preparation of galapectite load silver phosphate photocatalyst.
Background technology
Along with the development of science and technology, the health of environment and the mankind from the murder by poisoning organic pollution serious threat produced 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 Surface Physical Chemistry character and the efficient visible light photocatalysis performance of its uniqueness, one of focus becoming research.But nanoparticles is easily reunited, reunion rear surface is long-pending to be reduced greatly, decreased effectiveness.
Galapectite is again by title halloysite.Chemical composition is identical with kaolinite, has the SiO of identical 1: 1
2/ Al
2o
3ratio, lamellar structure has been curled into SiO
2at skin, Al
2o
3at internal layer, therefore dust trachelospermum jasminoide nanotube has the surface nature closely similar with SiO2, and Al
2o
3similar internal layer character.In general halloysite nanotubes forms by multiple kaolin lamella is curling, and be natural many wall-shaped nanotube, pipe external diameter is 20-100nm, and internal diameter is 5-30nm, and length is 150nm-2 μm.Galapectite and the kaolin main distinction on crystal structure, one is tubular structure, and one is sheet structure.Halloysite nanotubes, forms, in micro-tube shaped structure by kaolinic lamella is curling under natural endowment.Nano-Ag particles is loaded in the pipe of galapectite, can effectively control nano-Ag particles size.But existing technology is only outer surface nano-Ag particles being loaded to galapectite, and inner surface area is huge, has good adsorption effect, if made full use of by internal layer, then effectively can solve the problem of silver orthophosphate particle agglomeration simultaneously.
Summary of the invention
The object of the invention is for overcoming the deficiencies in the prior art, a kind of preparation method of galapectite load silver phosphate photocatalyst is provided.
The technical solution used in the present invention in turn includes the following steps:
1) galapectite purity being not less than 80wt% joins in the salpeter solution of 1 ~ 5wt%, reaction system solid-to-liquid ratio is 5 ~ 10% by mass percentage, 4 ~ 8h is stirred under normal temperature, centrifugal dehydration is also dry, and obtain acid-treated galapectite, after process, the aluminum oxide of galapectite internal layer is dissolved, internal diameter of the pipeline becomes large, leave silicon dioxide layer, have transparent effect, catalyst effectively can receive illumination;
2) 2g silver nitrate is dissolved in 80 ~ 100mL ethanol, is mixed with silver nitrate ethanolic solution;
3) acid-treated for 4 ~ 8g galapectite is placed in vacuum filtration bottle, magnetic agitation rotor is put in vacuum filtration bottle, the thin neck in vacuum filtration bottle side connects vavuum pump, vacuum filtration bottle bottleneck connects separatory funnel by rubber stopper, rubber stopper plays sealing process, make compact siro spinning technology between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition;
4) silver nitrate ethanolic solution is loaded in separatory funnel, the vacuum filtration bottle of separatory funnel of ining succession is placed on magnetic stirring apparatus, open vavuum pump, vacuumize, open magnetic stirring apparatus, open separatory funnel cock, allow the silver nitrate ethanolic solution in separatory funnel drip, mix under vacuum conditions, when silver nitrate is soon added dropwise to complete, open separatory funnel cock completely rapidly, allow air enter completely, under the pressure of air, silver nitrate is allowed fully to enter in galapectite pipe, continue stirring 2 ~ 3h, Separation of Solid and Liquid, the oven dry of 70 ~ 80 DEG C, vacuum;
5) join 50mL by drying the product obtained, concentration is in the sodium dihydrogen phosphate of 0.5 ~ 1.5mol/L, stirs 4 ~ 5h, Separation of Solid and Liquid, and washing, dries and obtain a kind of galapectite load silver phosphate photocatalyst for 100 ~ 105 DEG C.
Advantage of the present invention is: 1. the ducted air of emptying galapectite and steam, enables galapectite fully contact with silver nitrate, particularly allows silver nitrate enter into pipeline.2. remove the aluminum oxide of galapectite inwall, increase light can be reached and thoroughly spend and increase the effect in aperture.3. it is inner that the silver orthophosphate particle obtained is present in galapectite pipe, avoids reuniting and coming off.
Detailed description of the invention
3 embodiments of the present invention are below provided further:
Embodiment 1
Galapectite purity being not less than 80wt% joins in the salpeter solution of 5wt%, and reaction system solid-to-liquid ratio is 10% by mass percentage, stirs 8h under normal temperature, and centrifugal dehydration is also dry, obtains acid-treated galapectite; 2g silver nitrate is dissolved in 100mL ethanol, is mixed with silver nitrate ethanolic solution; Acid-treated for 8g galapectite is placed in vacuum filtration bottle, magnetic agitation rotor is put in vacuum filtration bottle, the thin neck in vacuum filtration bottle side connects vavuum pump, vacuum filtration bottle bottleneck connects separatory funnel by rubber stopper, rubber stopper plays sealing process, make compact siro spinning technology between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition; Silver nitrate ethanolic solution is loaded in separatory funnel, the vacuum filtration bottle of separatory funnel of ining succession is placed on magnetic stirring apparatus, open vavuum pump, vacuumize, open magnetic stirring apparatus, open separatory funnel cock, allow the silver nitrate ethanolic solution in separatory funnel drip, mix under vacuum conditions, when silver nitrate is soon added dropwise to complete, open separatory funnel cock completely rapidly, allow air enter completely, under the pressure of air, silver nitrate is allowed fully to enter in galapectite pipe, continue to stir 3h, Separation of Solid and Liquid, the oven dry of 80 DEG C, vacuum; Join 50mL by drying the product obtained, concentration is in the sodium dihydrogen phosphate of 1.5mol/L, stirs 5h, Separation of Solid and Liquid, and washing, dries and obtain a kind of galapectite load silver phosphate photocatalyst for 105 DEG C.
By obtained galapectite load silver phosphate photocatalyst for the treatment of wastewater containing methylene blue: it is in the methylene blue waste water of 40mg/L that 0.5g galapectite load silver phosphate photocatalyst joins 300mL concentration, under 300w Metal halogen lamp irradiates, reaction 30min, percent of decolourization is 96.4%, after catalyst separation reuses 7 times, under similarity condition, reaction 30min, percent of decolourization is 92.5%.The silver orthophosphate particle of same quality at identical conditions, during 30min, percent of decolourization is 92.6%, compares exfoliated alta-mud load silver phosphate catalyst, and the silver amount contained by silver orthophosphate particle is relatively much bigger, therefore the product that obtains of the application is more economical, better effects if.
Embodiment 2
Galapectite purity being not less than 80wt% joins in the salpeter solution of 1wt%, and reaction system solid-to-liquid ratio is 5% by mass percentage, stirs 4h under normal temperature, and centrifugal dehydration is also dry, obtains acid-treated galapectite; 2g silver nitrate is dissolved in 80mL ethanol, is mixed with silver nitrate ethanolic solution; Acid-treated for 4g galapectite is placed in vacuum filtration bottle, magnetic agitation rotor is put in vacuum filtration bottle, the thin neck in vacuum filtration bottle side connects vavuum pump, vacuum filtration bottle bottleneck connects separatory funnel by rubber stopper, rubber stopper plays sealing process, make compact siro spinning technology between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition; Silver nitrate ethanolic solution is loaded in separatory funnel, the vacuum filtration bottle of separatory funnel of ining succession is placed on magnetic stirring apparatus, open vavuum pump, vacuumize, open magnetic stirring apparatus, open separatory funnel cock, allow the silver nitrate ethanolic solution in separatory funnel drip, mix under vacuum conditions, when silver nitrate is soon added dropwise to complete, open separatory funnel cock completely rapidly, allow air enter completely, under the pressure of air, silver nitrate is allowed fully to enter in galapectite pipe, continue to stir 2h, Separation of Solid and Liquid, the oven dry of 70 DEG C, vacuum; Join 50mL by drying the product obtained, concentration is in the sodium dihydrogen phosphate of 0.5mol/L, stirs 4h, Separation of Solid and Liquid, and washing, dries and obtain a kind of galapectite load silver phosphate photocatalyst for 100 DEG C.
By obtained galapectite load silver phosphate photocatalyst for the treatment of containing acid scarlet waste water: it is in the acid scarlet waste water of 40mg/L that 0.5g galapectite load silver phosphate photocatalyst joins 300mL concentration, under 300w Metal halogen lamp irradiates, reaction 30min, percent of decolourization is 96.3%, after catalyst separation reuses 7 times, under similarity condition, reaction 30min, percent of decolourization is 93.0%.At identical conditions, during 30min, percent of decolourization is 91.1% to the silver orthophosphate particle of same quality.
Embodiment 3
Galapectite purity being not less than 80wt% joins in the salpeter solution of 3wt%, and reaction system solid-to-liquid ratio is 10% by mass percentage, stirs 8h under normal temperature, and centrifugal dehydration is also dry, obtains acid-treated galapectite; 2g silver nitrate is dissolved in 100mL ethanol, is mixed with silver nitrate ethanolic solution; Acid-treated for 8g galapectite is placed in vacuum filtration bottle, magnetic agitation rotor is put in vacuum filtration bottle, the thin neck in vacuum filtration bottle side connects vavuum pump, vacuum filtration bottle bottleneck connects separatory funnel by rubber stopper, rubber stopper plays sealing process, make compact siro spinning technology between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition; Silver nitrate ethanolic solution is loaded in separatory funnel, the vacuum filtration bottle of separatory funnel of ining succession is placed on magnetic stirring apparatus, open vavuum pump, vacuumize, open magnetic stirring apparatus, open separatory funnel cock, allow the silver nitrate ethanolic solution in separatory funnel drip, mix under vacuum conditions, when silver nitrate is soon added dropwise to complete, open separatory funnel cock completely rapidly, allow air enter completely, under the pressure of air, silver nitrate is allowed fully to enter in galapectite pipe, continue to stir 3h, Separation of Solid and Liquid, the oven dry of 75 DEG C, vacuum; Join 50mL by drying the product obtained, concentration is in the sodium dihydrogen phosphate of 1mol/L, stirs 4h, Separation of Solid and Liquid, and washing, dries and obtain a kind of galapectite load silver phosphate photocatalyst for 100 DEG C.
By obtained galapectite load silver phosphate photocatalyst for the treatment of containing acid scarlet waste water: it is in the acid scarlet waste water of 40mg/L that 0.5g galapectite load silver phosphate photocatalyst joins 300mL concentration, under 300w Metal halogen lamp irradiates, reaction 30min, percent of decolourization is 96.8%, after catalyst separation reuses 7 times, under similarity condition, reaction 30min, percent of decolourization is 92.4%.At identical conditions, during 30min, percent of decolourization is 93.3% to the silver orthophosphate particle of same quality.
Claims (1)
1. a preparation method for galapectite load silver phosphate photocatalyst, is characterized in that in turn including the following steps:
1) galapectite purity being not less than 80wt% joins in the salpeter solution of 1 ~ 5wt%, reaction system solid-to-liquid ratio is 5 ~ 10% by mass percentage, 4 ~ 8h is stirred under normal temperature, centrifugal dehydration is also dry, and obtain acid-treated galapectite, after process, the aluminum oxide of galapectite internal layer is dissolved, internal diameter of the pipeline becomes large, leave silicon dioxide layer, have transparent effect, catalyst effectively can receive illumination;
2) 2g silver nitrate is dissolved in 80 ~ 100mL ethanol, is mixed with silver nitrate ethanolic solution;
3) acid-treated for 4 ~ 8g galapectite is placed in vacuum filtration bottle, magnetic agitation rotor is put in vacuum filtration bottle, the thin neck in vacuum filtration bottle side connects vavuum pump, vacuum filtration bottle bottleneck connects separatory funnel by rubber stopper, rubber stopper plays sealing process, make compact siro spinning technology between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition;
4) silver nitrate ethanolic solution is loaded in separatory funnel, the vacuum filtration bottle of separatory funnel of ining succession is placed on magnetic stirring apparatus, open vavuum pump, vacuumize, open magnetic stirring apparatus, open separatory funnel cock, allow the silver nitrate ethanolic solution in separatory funnel drip, mix under vacuum conditions, when silver nitrate is soon added dropwise to complete, open separatory funnel cock completely rapidly, allow air enter completely, under the pressure of air, silver nitrate is allowed fully to enter in galapectite pipe, continue stirring 2 ~ 3h, Separation of Solid and Liquid, the oven dry of 70 ~ 80 DEG C, vacuum;
5) join 50mL by drying the product obtained, concentration is in the sodium dihydrogen phosphate of 0.5 ~ 1.5mol/L, stirs 4 ~ 5h, Separation of Solid and Liquid, and washing, dries and obtain a kind of galapectite load silver phosphate photocatalyst for 100 ~ 105 DEG C.
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| CN104624213B (en) * | 2015-02-10 | 2016-09-28 | 济南大学 | A kind of silver/silver phosphate improved silica composite particles and preparation method thereof |
| CN107308964A (en) * | 2017-07-11 | 2017-11-03 | 柳州若思纳米材料科技有限公司 | A kind of preparation method of galapectite load indium phosphate catalyst |
| CN107349924B (en) * | 2017-08-07 | 2019-10-18 | 浙江工业大学 | BiVO4/ galapectite composite nano catalysis material and preparation method thereof |
| CN108031467B (en) * | 2017-12-08 | 2019-10-18 | 浙江工业大学 | A kind of Bi2MoO6Coat halloysite nanotubes composite material and preparation method and application |
| 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 |
| CN110639589B (en) * | 2019-10-11 | 2022-06-24 | 常州纳欧新材料科技有限公司 | Carbon nitride material with one-dimensional nano structure and preparation method and application thereof |
| CN112662168B (en) * | 2020-12-04 | 2022-09-09 | 株洲时代工程塑料实业有限公司 | Antibacterial mildew preventive, halogen-free flame-retardant antibacterial mildew-proof nylon composite material, and preparation method and application thereof |
| CN113019312B (en) * | 2021-03-03 | 2022-07-15 | 中国科学院地球化学研究所 | Halloysite-based composite material for removing radioactive iodide ions and preparation method thereof |
| CN113041992B (en) * | 2021-04-08 | 2022-07-26 | 中国科学院地球化学研究所 | Halloysite-based efficient adsorbent for removing radioactive I-and preparation method thereof |
| CN113956473B (en) * | 2021-08-16 | 2023-12-12 | 丽水学院 | Halloysite nanotube composite material for adsorbing and degrading antibiotics in wastewater by photocatalysis and preparation method thereof |
| CN114471732A (en) * | 2022-03-03 | 2022-05-13 | 北京服装学院 | Photocatalytic composite nanofiber membrane and preparation method and application thereof |
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Effective date of registration: 20201130 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 |