CN105498815A - Preparation method of rod-like bismuth phosphate loaded biomass carbon aerogel material - Google Patents
Preparation method of rod-like bismuth phosphate loaded biomass carbon aerogel material Download PDFInfo
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- CN105498815A CN105498815A CN201510886395.4A CN201510886395A CN105498815A CN 105498815 A CN105498815 A CN 105498815A CN 201510886395 A CN201510886395 A CN 201510886395A CN 105498815 A CN105498815 A CN 105498815A
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- aerogel material
- bismuth phosphate
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- 239000002028 Biomass Substances 0.000 title claims abstract description 53
- SFOQXWSZZPWNCL-UHFFFAOYSA-K bismuth;phosphate Chemical compound [Bi+3].[O-]P([O-])([O-])=O SFOQXWSZZPWNCL-UHFFFAOYSA-K 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 title claims abstract description 34
- 239000004966 Carbon aerogel Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 45
- 239000011240 wet gel Substances 0.000 claims abstract description 18
- 235000011274 Benincasa cerifera Nutrition 0.000 claims abstract description 12
- 244000036905 Benincasa cerifera Species 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000007710 freezing Methods 0.000 claims description 14
- 230000008014 freezing Effects 0.000 claims description 14
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 239000002775 capsule Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 11
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 238000004043 dyeing Methods 0.000 abstract 2
- 238000003933 environmental pollution control Methods 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 239000002131 composite material Substances 0.000 description 7
- 238000001069 Raman spectroscopy Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- 230000010355 oscillation Effects 0.000 description 5
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000010926 purge Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 230000018199 S phase Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 229910003873 O—P—O Inorganic materials 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- 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
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A preparation method of a rod-like bismuth phosphate loaded biomass carbon aerogel material belongs to the technical field of material preparation and photocatalytic environmental pollution control. The preparation method comprises the following steps: removing skin and bladder of a white gourd, and preparing biomass carbon-based wet gel according to a hydrothermal method without adding any surfactant. The prepared rod-like bismuth phosphate loaded biomass carbon aerogel material is 0.3 to 0.5 [mu]m in diameter, and has such a photocatalytic degradation effect on a simulative dyeing wastewater methylene blue solution that the degradation rate of methylene blue in a 10 mg/L methylene blue solution can reach up to 90 percent when the bismuth phosphate loaded biomass carbon aerogel material is added into the methylene blue solution and the mixture is exposed in visible light for 3.5 hours, so that the rod-like bismuth phosphate loaded biomass carbon aerogel material can be applied to the field of dyeing wastewater treatment.
Description
Technical field
The invention belongs to the technical field of material preparation and photocatalysis environmental pollution improvement, be specifically related to a kind of preparation method and application of bar-shaped bismuth phosphate load biomass carbon aerogel material photochemical catalyst.
Background technology
The world today; global energy crisis and problem of environmental pollution day by day serious; the Faced In Sustainable Development of human society huge challenge; Photocatalitic Technique of Semiconductor is because of the important application prospect in field of environment pollution control; and traditional photochemical catalyst to there is quantum efficiency low; the shortcomings such as solar energy utilization ratio is not high, thus the photochemical catalyst of development of new has attracted the extensive concern of researcher.
Bismuth phosphate is a kind of conventional photochemical catalyst, and the compound about bismuth phosphate material also has relevant research, comprises the compound etc. of metal or nonmetal compound, semiconductor light-catalyst.Relevant document also reports and adopts new carbon such as Graphene, graphene aerogel etc. to form functional composite material with photochemical catalyst hydridization, enhances the photocatalysis performance of material to pollutant.Application number is 201310351384.5 preparation methods reporting bismuth phosphate and stannic oxide/graphene nano composite, application number is 201510007126.6 preparation methods reporting the composite of bismuth phosphate and silver bromide, and application number is respectively the preparation method that 201410208195.9,201410709028.2 report bismuth phosphate.But the pre-treatment more complicated of Graphene, often needs to use poisonous Oxidizing and Reducing Agents, needs to regulate solution ph, heating using microwave etc., add production cost, limit its practical application in other preparation methods.
Carbon back aeroge is a kind of lightweight, three-dimensional net structure nano-porous materials, has a wide range of applications in fields such as solar cell, sensor, ultracapacitor, water treatment field, catalyst carriers.In recent years, development clean, continuable environmentally friendly be that raw material is prepared novel carbon back aeroge and become new study hotspot with natural biomass.Because it has, density is low, specific area is high, the three-dimensional net structure of porous, and the researchs such as rich surface is containing a large amount of apparent groups, as C=C, C=O ,-OH, C-O-C etc., thus further modifies it, compound, modification are had laid a good foundation; The preparation of this material simultaneously has the features such as with low cost, simple and easy to get, has widened its application prospect further.
Summary of the invention
The object of this invention is to provide a kind of preparation method of bismuth phosphate load biomass carbon aerogel material, first composite is applied to photocatalysis field of environment pollution control.
The present invention includes following steps:
1) after removing the peel, going the wax gourd of capsule, cut into bulk, at 180 DEG C, carry out a hydro-thermal reaction 12h after cleaning, obtain living beings carbon back wet gel;
2) by freezing, dry for living beings carbon back wet gel, biomass carbon aeroge is obtained;
3) intermediate water thermal response is carried out in the mixing of bismuth nitrate, biomass carbon aeroge and sodium dihydrogen phosphate, obtain hydrothermal product;
4) solid phase of hydrothermal product is alternately washed final vacuum through water and ethanol dry, obtain bar-shaped bismuth phosphate load biomass carbon aerogel material.
Raw material of the present invention is the wax gourd of natural plants tissue, removing skin and capsule, without the need to adding any surfactant, can obtain living beings carbon back wet gel by hydro-thermal method.The bar-shaped bismuth phosphate load biomass carbon aerogel material diameter obtained is 0.3 μm ~ 0.5 μm, photocatalytic Degradation to dye wastewater methylene blue solution: for 10mg/L aqueous solution of methylene blue, after adding appropriate bismuth phosphate/biomass carbon aerogel composite, through radiation of visible light 3.5h, the degradation rate of methylene blue reaches 90%, is expected to it to be applied in dye wastewater treatment field.
Advantage of the present invention:
1. the bismuth phosphate load biomass carbon aerogel material that prepared by the present invention has abundant raw material, with low cost; The advantages such as preparation technology is simple, easy and simple to handle.
2. the bismuth phosphate load biomass carbon aerogel material that the present invention obtains has good light degradation effect to dyestuffs such as methylene blues, and when 210min, degradation rate reaches 90%.
Further, lumpy sizes of the present invention is 2cm × 2cm × 4cm.Be cut into relatively uniform suitable size, be can participate in hydro-thermal reaction more fully after being conducive to it, generate biomass carbon aeroge.
Being the impurity in order to clean wax gourd surface, preventing it from having a negative impact to follow-up reaction, in described step 1), adopting the ultrasonic wax gourd to being cut into bulk to clean.
Described step 2) in, first living beings carbon back wet gel is refrigerated to internal moisture by evenly freezing solid, then solid is put into the dry 24h of freeze drier of-55 DEG C.Object is to ensure that the microcellular structure of its inside is not destroyed, and forms the material with three-dimensional network framework supporting structure.
In described step 3), after first bismuth nitrate being dissolved in ethylene glycol or water, add biomass carbon aeroge, after living beings carbon aerogels dissolves, then add NaH
2pO
42H
2o; The mass ratio that feeds intake of described bismuth nitrate and biomass carbon aeroge is 3 ~ 18: 1; Described NaH
2pO
42H
2the mass ratio that feeds intake of O and biomass carbon aeroge is 0.78 ~ 6: 1.By dividing a method of progressively dissolving to be to be more evenly dispersed in solution by mixture, be convenient to react more fully.
In described step 3), the temperature conditions of intermediate water thermal response is 160 DEG C.Temperature is the value be relatively fixed of synthetic chemical.
In described step 3), the mass ratio that feeds intake of described bismuth nitrate and biomass carbon aeroge is 3 ~ 18: 1, all can obtain bar-shaped bismuth phosphate load biomass carbon aerogel material.Further, under the mass ratio that feeds intake of bismuth nitrate and biomass carbon aeroge is the condition of 8.43: 1, the bar-shaped bismuth phosphate load biomass carbon aerogel material made has excellent characteristic and is: for 10mg/L aqueous solution of methylene blue, after adding appropriate bismuth phosphate/biomass carbon aerogel composite, through radiation of visible light 3.5h, the degradation rate of methylene blue reaches 90%.
Prove through test: in described step 3), at NaH
2pO
42H
2the mass ratio that feeds intake of O and biomass carbon aeroge is under the condition of 2.74: 1, the bar-shaped bismuth phosphate load biomass carbon aerogel material made has following excellent characteristic: for 10mg/L aqueous solution of methylene blue, after adding appropriate bismuth phosphate/biomass carbon aerogel composite, through radiation of visible light 3.5h, the degradation rate of methylene blue reaches 90%.
In described step 4), vacuum drying temperature conditions is 60 DEG C, and the time is 12h.By making sample obtain better drying condition to the control of temperature and time.
Accompanying drawing explanation
The XRD spectra of Fig. 1 sample prepared by example 1,2,3,4,5 of the present invention.
Fig. 2 is the FTIR spectrogram of the present invention's sample prepared by example 1,2,3,4,5 of the present invention.
The Raman spectrogram of the sample of Fig. 3 prepared by example 3 of the present invention.
The scanning electron microscope (SEM) photograph of the sample of Fig. 4 prepared by example 3 of the present invention.
The scanning electron microscope (SEM) photograph of the sample of Fig. 5 prepared by example 4 of the present invention.
The scanning electron microscope (SEM) photograph of the sample of Fig. 6 prepared by example 5 of the present invention.
Detailed description of the invention
One, below in conjunction with embodiment, the invention will be further described, but protection scope of the present invention is not only confined to embodiment.
Embodiment 1:
Wax gourd is cleaned, remove the peel, remove capsule, cut into 2cm × 2cm × 4cm size, put it into reactor, then add water, under the temperature of mixed system is 180 DEG C of conditions, carries out hydro-thermal reaction 12h, carbon back wet gel is obtained after having reacted, carbon back wet gel is carried out freezing processing 24h in refrigerator, obtains internal moisture by evenly freezing solid sample, namely sample is obtained biomass carbon aerogel material after dry 24h in freeze drier.
Take 0.1201gBi (NO
3)
25H
2o is dissolved in the solvent (volume ratio is 2:1) of 30mL glycol/water, and sonic oscillation dissolves completely to it, is then added in above-mentioned solution by 0.04g biomass carbon aeroge, stirs 30min and dissolves to it, then add 0.03901gNaH
2pO
42H
2o, proceeds to the polytetrafluoroethylene (PTFE) stainless steel cauldron of 50mL, constant temperature 18h at 160 DEG C after stirring 6h, naturally obtain hydrothermal product after cooling.The sample obtained is used respectively distilled water and ethanol purge 3 times, then sample is placed on 12h in 60 DEG C of vacuum drying chambers, be i.e. obtained bismuth phosphate load biomass carbon aerogel material.
Embodiment 2:
Wax gourd is cleaned, remove the peel, remove capsule, cut into 2cm × 2cm × 4cm size, put it into reactor, then add water, under the temperature of mixed system is 180 DEG C of conditions, carries out hydro-thermal reaction 12h, carbon back wet gel is obtained after having reacted, carbon back wet gel is carried out freezing processing 24h in refrigerator, obtains internal moisture by evenly freezing solid sample, namely sample is obtained biomass carbon aerogel material after dry 24h in freeze drier.
Take 0.2403gBi (NO
3)
25H
2o is dissolved in the solvent (volume ratio is 2:1) of 30mL glycol/water, and sonic oscillation dissolves completely to it, is then added in above-mentioned solution by 0.04g biomass carbon aeroge, stirs 30min and dissolves to it, then add 0.07801gNaH
2pO
42H
2o, proceeds to the polytetrafluoroethylene (PTFE) stainless steel cauldron of 50mL, constant temperature 18h at 160 DEG C after stirring 6h, naturally obtain hydrothermal product after cooling.The sample obtained is used respectively distilled water and ethanol purge 3 times, then sample is placed on 12h in 60 DEG C of vacuum drying chambers, be i.e. obtained bismuth phosphate load biomass carbon aerogel material.
Embodiment 3:
Wax gourd is cleaned, remove the peel, remove capsule, cut into 2cm × 2cm × 4cm size, put it into reactor, then add water, under the temperature of mixed system is 180 DEG C of conditions, carries out hydro-thermal reaction 12h, carbon back wet gel is obtained after having reacted, carbon back wet gel is carried out freezing processing 24h in refrigerator, obtains internal moisture by evenly freezing solid sample, namely sample is obtained biomass carbon aerogel material after dry 24h in freeze drier.
Take 0.3372gBi (NO
3)
25H
2o is dissolved in the solvent (volume ratio is 2:1) of 30mL glycol/water, and sonic oscillation dissolves completely to it, is then added in above-mentioned solution by 0.04g biomass carbon aeroge, stirs 30min and dissolves to it, then add 0.1096gNaH
2pO
42H
2o, proceeds to the polytetrafluoroethylene (PTFE) stainless steel cauldron of 50mL, constant temperature 18h at 160 DEG C after stirring 6h, naturally obtain hydrothermal product after cooling.The sample obtained is used respectively distilled water and ethanol purge 3 times, then sample is placed on 12h in 60 DEG C of vacuum drying chambers, be i.e. obtained bismuth phosphate load biomass carbon aerogel material.
Embodiment 4:
Wax gourd is cleaned, remove the peel, remove capsule, cut into 2cm × 2cm × 4cm size, put it into reactor, then add water, under the temperature of mixed system is 180 DEG C of conditions, carries out hydro-thermal reaction 12h, carbon back wet gel is obtained after having reacted, carbon back wet gel is carried out freezing processing 24h in refrigerator, obtains internal moisture by evenly freezing solid sample, namely sample is obtained biomass carbon aerogel material after dry 24h in freeze drier.
Take 0.4817gBi (NO
3)
25H
2o is dissolved in the solvent (volume ratio is 2:1) of 30mL glycol/water, and sonic oscillation dissolves completely to it, is then added in above-mentioned solution by 0.04g biomass carbon aeroge, stirs 30min and dissolves to it, then add 0.1565gNaH
2pO
42H
2o, proceeds to the polytetrafluoroethylene (PTFE) stainless steel cauldron of 50mL, constant temperature 18h at 160 DEG C after stirring 6h, naturally obtain hydrothermal product after cooling.The sample obtained is used respectively distilled water and ethanol purge 3 times, then sample is placed on 12h in 60 DEG C of vacuum drying chambers, be i.e. obtained bismuth phosphate load biomass carbon aerogel material.
Embodiment 5:
Wax gourd is cleaned, remove the peel, remove capsule, cut into 2cm × 2cm × 4cm size, put it into reactor, then add water, under the temperature of mixed system is 180 DEG C of conditions, carries out hydro-thermal reaction 12h, carbon back wet gel is obtained after having reacted, carbon back wet gel is carried out freezing processing 24h in refrigerator, obtains internal moisture by evenly freezing solid sample, namely sample is obtained biomass carbon aerogel material after dry 24h in freeze drier.
Take 0.7226gBi (NO
3)
25H
2o is dissolved in the solvent (volume ratio is 2:1) of 30mL glycol/water, and sonic oscillation dissolves completely to it, is then added in above-mentioned solution by 0.04g biomass carbon aeroge, stirs 30min and dissolves to it, then add 0.2348gNaH
2pO
42H
2o, proceeds to the polytetrafluoroethylene (PTFE) stainless steel cauldron of 50mL, constant temperature 18h at 160 DEG C after stirring 6h, naturally obtain hydrothermal product after cooling.The sample obtained is used respectively distilled water and ethanol purge 3 times, then sample is placed on 12h in 60 DEG C of vacuum drying chambers, be i.e. obtained bismuth phosphate load biomass carbon aerogel material.
Two, X-ray single crystal diffraction (XRD), Raman spectrometer (Raman), transmission electron microscope (TEM) etc. are utilized to analyze the crystalline phase of the sample that above five embodiments are made and structure.
The XRD spectra of Fig. 1 sample prepared by example 1,2,3,4,5 of the present invention, the diffraction maximum of sample prepared as shown in Figure 1 and six side phase BiPO
4(JCPDSNO.16-0766) diffraction maximum position is completely corresponding, and peak shape is very sharp-pointed, is six pure side's phases that degree of crystallinity is high, shows that the sample prepared is the bismuth phosphate of six side's phases.
Fig. 2 is the FTIR spectrogram of the present invention's sample prepared by example 1,2,3,4,5 of the present invention, and the sample of preparation is at 540cm
-1, 590cm
-1, 1029cm
-1belong to δ (O-P-O), ν respectively
4(PO
4), ν
3(PO
4) stretching vibration, show that prepared sample is bismuth phosphate.
The Raman spectrogram of the sample of Fig. 3 prepared by example 3 of the present invention, shows that from spectrogram bismuth phosphate composite is 127,166,230,280,967 and 1036cm
-1place's Raman peaks, wherein 127,166,230,280cm
-1belong to the flexural vibrations of Bi-O key, 408,554cm
-1belong to PO respectively
4 3-v
2and v
4flexural vibrations, 967cm
-1belong to PO
4 3-v
1symmetrical stretching vibration, 1036cm
-1belong to PO
4 3-antisymmetric stretching vibration; At 1356cm
-1and 1596cm
-1there are D peak and the G peak of obvious material with carbon element in place, and this shows the characteristic peak simultaneously comprising bismuth phosphate and carbon aerogels in prepared sample.
The scanning electron microscope (SEM) photograph of the sample of Fig. 4 prepared by example 3 of the present invention.As seen from Figure 4: prepared sample has regular and that pattern is homogeneous bar-like shape.
The scanning electron microscope (SEM) photograph of the sample of Fig. 5 prepared by example 4 of the present invention.As seen from Figure 5: prepared sample has regular and that pattern is homogeneous bar-like shape.
The scanning electron microscope (SEM) photograph of the sample of Fig. 6 prepared by example 5 of the present invention.As seen from Figure 6: prepared sample has regular and that pattern is homogeneous bar-like shape.
Claims (9)
1. a preparation method for bar-shaped bismuth phosphate load biomass carbon aerogel material, is characterized in that comprising the following steps:
1) after removing the peel, going the wax gourd of capsule, cut into bulk, at 180 DEG C, carry out a hydro-thermal reaction 12h after cleaning, obtain living beings carbon back wet gel;
2) by freezing, dry for living beings carbon back wet gel, biomass carbon aeroge is obtained;
3) intermediate water thermal response is carried out in the mixing of bismuth nitrate, biomass carbon aeroge and sodium dihydrogen phosphate, obtain hydrothermal product;
4) solid phase of hydrothermal product is alternately washed final vacuum through water and ethanol dry, obtain bar-shaped bismuth phosphate load biomass carbon aerogel material.
2. preparation method according to claim 1, is characterized in that described lumpy sizes is 2cm × 2cm × 4cm.
3. preparation method according to claim 1, is characterized in that in described step 1), adopts ultrasonicly to clean being cut into block wax gourd.
4. preparation method according to claim 1, is characterized in that described step 2) in, first living beings carbon back wet gel is refrigerated to internal moisture by evenly freezing solid, then solid is put into the dry 24h of freeze drier of-55 DEG C.
5. preparation method according to claim 1, is characterized in that in described step 3), after first bismuth nitrate being dissolved in ethylene glycol or water, adds biomass carbon aeroge, after living beings carbon aerogels dissolves, then adds NaH
2pO
42H
2o; The mass ratio that feeds intake of described bismuth nitrate and biomass carbon aeroge is 3 ~ 18: 1; Described NaH
2pO
42H
2the mass ratio that feeds intake of O and biomass carbon aeroge is 0.78 ~ 6: 1.
6. preparation method according to claim 1 or 5, is characterized in that in described step 3), and the temperature conditions of intermediate water thermal response is 160 DEG C.
7. preparation method according to claim 5, it is characterized in that in described step 3), the mass ratio that feeds intake of described bismuth nitrate and biomass carbon aeroge is 8.43: 1.
8. preparation method according to claim 5, is characterized in that in described step 3), described NaH
2pO
42H
2the mass ratio that feeds intake of O and biomass carbon aeroge is 2.74: 1.
9. preparation method according to claim 1, it is characterized in that in described step 4), vacuum drying temperature conditions is 60 DEG C, the time is 12h.
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| CN107486152A (en) * | 2017-08-23 | 2017-12-19 | 江苏大学 | A kind of preparation method and application of leaf based biomass carbon aerogels |
| CN110420653A (en) * | 2019-09-02 | 2019-11-08 | 上海市农业科学院 | A kind of silver orthophosphate/hydro-thermal charcoal composite photo-catalyst and the preparation method and application thereof |
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| CN106111167A (en) * | 2016-06-21 | 2016-11-16 | 江苏大学 | A kind of preparation method of three-dimensional silver halide biomass carbon aerogel composite |
| CN106179408A (en) * | 2016-07-14 | 2016-12-07 | 扬州天辰精细化工有限公司 | A kind of Argentous sulfide. load Radix Raphani derives the preparation method of carbon aerogel material |
| CN107159111A (en) * | 2017-05-25 | 2017-09-15 | 江苏大学 | A kind of preparation method and applications of hydrophobic low-density pomelo peel carbon aerogels |
| CN107029763A (en) * | 2017-05-26 | 2017-08-11 | 桂林理工大学 | A kind of preparation method of bismuth phosphate/carbon composite photocatalyst |
| CN107486152A (en) * | 2017-08-23 | 2017-12-19 | 江苏大学 | A kind of preparation method and application of leaf based biomass carbon aerogels |
| CN107486152B (en) * | 2017-08-23 | 2019-08-02 | 江苏大学 | A kind of preparation method and application of leaf based biomass carbon aerogels |
| CN112110431A (en) * | 2019-06-19 | 2020-12-22 | 清华大学 | Graphene-bismuth phosphate aerogel and preparation method thereof |
| CN110420653A (en) * | 2019-09-02 | 2019-11-08 | 上海市农业科学院 | A kind of silver orthophosphate/hydro-thermal charcoal composite photo-catalyst and the preparation method and application thereof |
| CN114259989A (en) * | 2022-01-07 | 2022-04-01 | 云南中烟工业有限责任公司 | Biological carbon aerogel loaded hydrotalcite material, and synthesis method and application thereof |
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