CN103934008A - Preparation method of halloysite loading phosphoric acid Silverlight catalyst - Google Patents

Preparation method of halloysite loading phosphoric acid Silverlight catalyst Download PDF

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Publication number
CN103934008A
CN103934008A CN201410156228.XA CN201410156228A CN103934008A CN 103934008 A CN103934008 A CN 103934008A CN 201410156228 A CN201410156228 A CN 201410156228A CN 103934008 A CN103934008 A CN 103934008A
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halloysite
galapectite
separatory funnel
silver nitrate
vacuum filtration
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CN201410156228.XA
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CN103934008B (en
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马建锋
邹静
李良银
姚超
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Jiangyin Intellectual Property Operation Co., Ltd
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Changzhou University
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Abstract

The invention discloses a preparation method of a halloysite loading phosphoric acid Silverlight catalyst. The preparation method comprises the following specific steps of adding halloysite in a salpeter solution so as to obtain the halloysite after acid treatment, placing the 4-8g halloysite after acid treatment into a vacuum filtration bottle, mixing the halloysite and a silver nitrate ethanol solution under a vacuum state, enabling the silver nitrate to fully enter a halloysite pipe, sequentially stirring 2-5h, carrying out solid-liquid separation, and vacuum drying at 70-80 DEG C; adding the obtained product after drying in a 50 mL of sodium dihydrogen phosphate solution the concentration of which is 0.5-1.5mol/L, stirring for 4-5h, carrying out solid-liquid separation, washing, drying at 100-105 DEG C so as to obtain the halloysite loading phosphoric acid Silverlight catalyst. The preparation method provided by the invention has the advantages that the air and moisture in a halloysite pipeline are discharged, the silver nitrate enters a pipeline, an aluminum oxide of the inner wall of the halloysite is removed, the effects of increasing light penetrating degree and aperture property action can be achieved, the obtained silver phosphate particles are arranged in a halloysite pipe and are prevented from birdnesting and falling.

Description

A kind of preparation of galapectite load silver orthophosphate photochemical catalyst
Technical field
The present invention relates to environmental pollution control field of new, relate in particular to a kind of preparation of galapectite load silver orthophosphate photochemical catalyst.
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.But nanoparticles is easily reunited, reunion rear surface is long-pending to be reduced greatly, and effect weakens.
Galapectite is claimed halloysite again.Chemical composition is identical with kaolinite, has the identical SiO of 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, by curling the forming of multiple kaolin lamellas, is natural many walls type nanotube, and pipe external diameter is 20-100nm, and internal diameter is 5-30nm, and length is 150nm-2 μ m.Galapectite and the kaolin main distinction on crystal structure, the one, tubular structure, the one, sheet structure.Halloysite nanotubes, by kaolinic lamella curling forming under natural endowment, is micro-tube shaped structure.Nano-Ag particles is loaded in the pipe of galapectite, can effectively control nano-Ag particles size.But existing technology is only the outer surface that nano-Ag particles is loaded to galapectite, and inner surface area is huge, has good adsorption effect simultaneously, if internal layer is made full use of, can effectively solve the problem of silver orthophosphate particle agglomeration.
Summary of the invention
The object of the invention is, for overcoming the deficiencies in the prior art, provides a kind of preparation of galapectite load silver orthophosphate photochemical catalyst.
The technical solution used in the present invention is in turn include the following steps:
1) galapectite that purity is not less than to 80wt% joins in the salpeter solution of 1~5wt%, reaction system solid-to-liquid ratio is 5~10% by mass percentage, under normal temperature, stir 4~8h, centrifugal dehydration is also dry, obtains acid-treated galapectite, after processing the aluminum oxide of galapectite internal layer dissolved fall, it is large that internal diameter of the pipeline becomes, leave silicon dioxide layer, have transparent effect, catalyst can effectively receive illumination;
2) 2g silver nitrate is dissolved in 80~100mL ethanol, is mixed with silver nitrate ethanolic solution;
3) acid-treated 4~8g galapectite is placed in to vacuum filtration bottle, in vacuum filtration bottle, put into magnetic agitation rotor, 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 closely to connect between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition;
4) silver nitrate ethanolic solution is packed in separatory funnel, the vacuum filtration bottle of the 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, under vacuum state, mix, in the time that silver nitrate is soon added dropwise to complete, open rapidly separatory funnel cock completely, allow air enter completely, under the pressure of air, allow silver nitrate fully enter in galapectite pipe, continue to stir 2~3h, Separation of Solid and Liquid, 70~80 DEG C of oven dry of vacuum;
5) product oven dry being obtained joins 50mL, in the sodium dihydrogen phosphate that concentration is 0.5~1.5mol/L, stirs 4~5h, Separation of Solid and Liquid, and washing, 100~105 DEG C of oven dry obtain a kind of galapectite load silver orthophosphate photochemical catalyst.
Advantage of the present invention is: 1. the ducted air of emptying galapectite and steam, and galapectite can fully be contacted with silver nitrate, particularly allow silver nitrate can enter into pipeline.2. remove the aluminum oxide of galapectite inwall, can reach the effect that increases the saturating degree of light and increase aperture.3. the silver orthophosphate particle obtaining is present in galapectite pipe inside, avoids reuniting and coming off.
Detailed description of the invention
3 embodiment of the present invention are below further provided:
Embodiment 1
The galapectite that purity is not less than to 80wt% joins in the salpeter solution of 5wt%, and reaction system solid-to-liquid ratio is 10% by mass percentage, under normal temperature, stirs 8h, 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 8g galapectite is placed in to vacuum filtration bottle, in vacuum filtration bottle, put into magnetic agitation rotor, 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 closely to connect between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition; Silver nitrate ethanolic solution is packed in separatory funnel, the vacuum filtration bottle of the 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, under vacuum state, mix, in the time that silver nitrate is soon added dropwise to complete, open rapidly separatory funnel cock completely, allow air enter completely, under the pressure of air, allow silver nitrate fully enter in galapectite pipe, continue to stir 3h, Separation of Solid and Liquid, 80 DEG C of oven dry of vacuum; The product that oven dry is obtained joins 50mL, in the sodium dihydrogen phosphate that concentration is 1.5mol/L, stirs 5h, Separation of Solid and Liquid, and washing, 105 DEG C of oven dry obtain a kind of galapectite load silver orthophosphate photochemical catalyst.
By the galapectite load silver orthophosphate photochemical catalyst making for the treatment of wastewater containing methylene blue: 0.5g galapectite load silver orthophosphate photochemical catalyst joins in the methylene blue waste water that 300mL concentration is 40mg/L, under 300w Metal halogen lamp irradiates, reaction 30min, percent of decolourization is 96.4%, after catalyst separation recycling 7 times, under similarity condition, reaction 30min, percent of decolourization is 92.5%.The silver orthophosphate particle of same quality is under identical condition, when 30min, percent of decolourization is 92.6%, compares exfoliated alta-mud load silver orthophosphate catalyst, 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
The galapectite that purity is not less than to 80wt% joins in the salpeter solution of 1wt%, and reaction system solid-to-liquid ratio is 5% by mass percentage, under normal temperature, stirs 4h, 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 4g galapectite is placed in to vacuum filtration bottle, in vacuum filtration bottle, put into magnetic agitation rotor, 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 closely to connect between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition; Silver nitrate ethanolic solution is packed in separatory funnel, the vacuum filtration bottle of the 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, under vacuum state, mix, in the time that silver nitrate is soon added dropwise to complete, open rapidly separatory funnel cock completely, allow air enter completely, under the pressure of air, allow silver nitrate fully enter in galapectite pipe, continue to stir 2h, Separation of Solid and Liquid, 70 DEG C of oven dry of vacuum; The product that oven dry is obtained joins 50mL, in the sodium dihydrogen phosphate that concentration is 0.5mol/L, stirs 4h, Separation of Solid and Liquid, and washing, 100 DEG C of oven dry obtain a kind of galapectite load silver orthophosphate photochemical catalyst.
By the galapectite load silver orthophosphate photochemical catalyst making for the treatment of containing acid scarlet waste water: 0.5g galapectite load silver orthophosphate photochemical catalyst joins in the acid scarlet waste water that 300mL concentration is 40mg/L, under 300w Metal halogen lamp irradiates, reaction 30min, percent of decolourization is 96.3%, after catalyst separation recycling 7 times, under similarity condition, reaction 30min, percent of decolourization is 93.0%.The silver orthophosphate particle of same quality is under identical condition, and when 30min, percent of decolourization is 91.1%.
Embodiment 3
The galapectite that purity is not less than to 80wt% joins in the salpeter solution of 3wt%, and reaction system solid-to-liquid ratio is 10% by mass percentage, under normal temperature, stirs 8h, 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 8g galapectite is placed in to vacuum filtration bottle, in vacuum filtration bottle, put into magnetic agitation rotor, 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 closely to connect between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition; Silver nitrate ethanolic solution is packed in separatory funnel, the vacuum filtration bottle of the 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, under vacuum state, mix, in the time that silver nitrate is soon added dropwise to complete, open rapidly separatory funnel cock completely, allow air enter completely, under the pressure of air, allow silver nitrate fully enter in galapectite pipe, continue to stir 3h, Separation of Solid and Liquid, 75 DEG C of oven dry of vacuum; The product that oven dry is obtained joins 50mL, in the sodium dihydrogen phosphate that concentration is 1mol/L, stirs 4h, Separation of Solid and Liquid, and washing, 100 DEG C of oven dry obtain a kind of galapectite load silver orthophosphate photochemical catalyst.
By the galapectite load silver orthophosphate photochemical catalyst making for the treatment of containing acid scarlet waste water: 0.5g galapectite load silver orthophosphate photochemical catalyst joins in the acid scarlet waste water that 300mL concentration is 40mg/L, under 300w Metal halogen lamp irradiates, reaction 30min, percent of decolourization is 96.8%, after catalyst separation recycling 7 times, under similarity condition, reaction 30min, percent of decolourization is 92.4%.The silver orthophosphate particle of same quality is under identical condition, and when 30min, percent of decolourization is 93.3%.

Claims (1)

1. a preparation for galapectite load silver orthophosphate photochemical catalyst, is characterized in that in turn including the following steps:
1) galapectite that purity is not less than to 80wt% joins in the salpeter solution of 1~5wt%, reaction system solid-to-liquid ratio is 5~10% by mass percentage, under normal temperature, stir 4~8h, centrifugal dehydration is also dry, obtains acid-treated galapectite, after processing the aluminum oxide of galapectite internal layer dissolved fall, it is large that internal diameter of the pipeline becomes, leave silicon dioxide layer, have transparent effect, catalyst can effectively receive illumination;
2) 2g silver nitrate is dissolved in 80~100mL ethanol, is mixed with silver nitrate ethanolic solution;
3) acid-treated 4~8g galapectite is placed in to vacuum filtration bottle, in vacuum filtration bottle, put into magnetic agitation rotor, 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 closely to connect between separatory funnel and vacuum filtration bottle, separatory funnel cock is in closed condition;
4) silver nitrate ethanolic solution is packed in separatory funnel, the vacuum filtration bottle of the 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, under vacuum state, mix, in the time that silver nitrate is soon added dropwise to complete, open rapidly separatory funnel cock completely, allow air enter completely, under the pressure of air, allow silver nitrate fully enter in galapectite pipe, continue to stir 2~3h, Separation of Solid and Liquid, 70~80 DEG C of oven dry of vacuum;
5) product oven dry being obtained joins 50mL, in the sodium dihydrogen phosphate that concentration is 0.5~1.5mol/L, stirs 4~5h, Separation of Solid and Liquid, and washing, 100~105 DEG C of oven dry obtain a kind of galapectite load silver orthophosphate photochemical catalyst.
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CN104624213A (en) * 2015-02-10 2015-05-20 济南大学 Silver/silver phosphate modified silicon dioxide composite particle 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
CN107349924A (en) * 2017-08-07 2017-11-17 浙江工业大学 BiVO4/ galapectite composite nano catalysis material and preparation method thereof
CN108031467A (en) * 2017-12-08 2018-05-15 浙江工业大学 A kind of Bi2MoO6Coat halloysite nanotubes composite material and preparation method and application
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
CN110639589A (en) * 2019-10-11 2020-01-03 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
CN112662168A (en) * 2020-12-04 2021-04-16 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
CN113019312A (en) * 2021-03-03 2021-06-25 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
CN113041992A (en) * 2021-04-08 2021-06-29 中国科学院地球化学研究所 Halloysite-based efficient adsorbent for removing radioactive I-and preparation method thereof
CN113956473A (en) * 2021-08-16 2022-01-21 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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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
CN104624213A (en) * 2015-02-10 2015-05-20 济南大学 Silver/silver phosphate modified silicon dioxide composite particle 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
CN107349924A (en) * 2017-08-07 2017-11-17 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
CN108031467A (en) * 2017-12-08 2018-05-15 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
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
CN110639589A (en) * 2019-10-11 2020-01-03 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
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
CN112662168A (en) * 2020-12-04 2021-04-16 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
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
CN113019312A (en) * 2021-03-03 2021-06-25 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
CN113041992A (en) * 2021-04-08 2021-06-29 中国科学院地球化学研究所 Halloysite-based efficient adsorbent for removing radioactive I-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
CN113956473A (en) * 2021-08-16 2022-01-21 丽水学院 Halloysite nanotube composite material for adsorbing and degrading antibiotics in wastewater by photocatalysis 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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