CN108636136B - A kind of Pd/C3N4The preparation method and application of@biomass carbon composite fiber membrane - Google Patents
A kind of Pd/C3N4The preparation method and application of@biomass carbon composite fiber membrane Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 239000012528 membrane Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000835 fiber Substances 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 19
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium on carbon Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 20
- 239000004917 carbon fiber Substances 0.000 claims abstract description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 230000015556 catabolic process Effects 0.000 claims abstract description 9
- 238000006731 degradation reaction Methods 0.000 claims abstract description 9
- 238000007146 photocatalysis Methods 0.000 claims abstract description 8
- 230000001699 photocatalysis Effects 0.000 claims abstract description 8
- 239000002028 Biomass Substances 0.000 claims abstract description 7
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 7
- 239000011941 photocatalyst Substances 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 239000004098 Tetracycline Substances 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 9
- 239000012279 sodium borohydride Substances 0.000 claims description 9
- 229960002180 tetracycline Drugs 0.000 claims description 9
- 229930101283 tetracycline Natural products 0.000 claims description 9
- 235000019364 tetracycline Nutrition 0.000 claims description 9
- 150000003522 tetracyclines Chemical class 0.000 claims description 9
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 210000002268 wool Anatomy 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000005030 aluminium foil Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- UXGNZZKBCMGWAZ-UHFFFAOYSA-N dimethylformamide dmf Chemical compound CN(C)C=O.CN(C)C=O UXGNZZKBCMGWAZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001523 electrospinning Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 229910052573 porcelain Inorganic materials 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 240000001398 Typha domingensis Species 0.000 claims 1
- 230000000593 degrading effect Effects 0.000 claims 1
- 238000006197 hydroboration reaction Methods 0.000 claims 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 11
- 239000002105 nanoparticle Substances 0.000 abstract description 7
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- -1 by C3N4 Substances 0.000 abstract 1
- 239000000356 contaminant Substances 0.000 abstract 1
- 238000009987 spinning Methods 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 241000233948 Typha Species 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 206010014979 Epidemic typhus Diseases 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 208000028104 epidemic louse-borne typhus Diseases 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007952 growth promoter Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
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- 238000001228 spectrum Methods 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/08—Polysaccharides
- B01D71/12—Cellulose derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- 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
- B01J35/39—Photocatalytic 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
- C02F2101/38—Organic compounds containing nitrogen
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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Abstract
The invention belongs to material preparation and the technical fields of environmental pollution improvement, provide a kind of Pd/C3N4The preparation method of@biomass carbon composite fiber membrane, the preparation method is as follows: step 1, preparation Pd/C3N4@biomass carbon fiber composite photochemical catalyst；Step 2, method of electrostatic spinning prepare Pd/C3N4@biomass carbon fiber composite photocatalysis membrana.The present invention utilizes the high adsorption of biomass carbon fiber, by C3N4, Pd nano particle be uniformly supported on its surface, improve the separative efficiency of photo-generate electron-hole, in combination with the structure of the intrinsic high porosity of static spinning membrane, realize and degrade to the efficient catalytic of target contaminant, have many advantages, such as synthesis simply, degradation efficiency is high.
Description
Technical field
The invention belongs to material preparation and the technical fields of environmental pollution improvement, and in particular to a kind of Pd/C3N4@biomass
The preparation method and application of carbon fiber composite membrane.
Background technique
Tetracycline is a kind of efficient broad-spectrum antibiotic, is a part for maintaining human and animal's health indispensable, it
It can treat a variety of diseases, including Eaton agent pneumonia and epidemic typhus.In addition, some countries including the U.S.,
Tetracycline is also widely used as growth promoter and feeds to animal.This results in the sustained release of tetracycline and environmental accumulation causes
The extensive concern of society.Certain micro-organisms is killed to the tetracycline residue object property of can choose in environment, and can be induced
The generation of some drug-fast bacterias, to endanger the balance of human health and aquatic ecosystem.Therefore in effective removal water environment
Remaining tetracycline is extremely urgent.In current numerous processing methods, photocatalysis technology is considered maximally efficient and to environment
Harmless method.
Photocatalysis technology and membrane separation technique are coupled, the catalysis film system of building is a kind of great application prospect
Water treatment system.It is to be realized using membrane material as reaction medium in conjunction with chemical reaction process, on the one hand utilizes film
Specific function realizes that the control input of the quick separating, reactant of reaction product, reactive separation process are integrated etc., on the other hand
Using catalyst as functional material, solve the problems, such as fouling membrane, realize the practical application of membrane material, be used repeatedly,
The purpose of extending catalyst service life.
However, nano catalytic material will lead to the reunion of catalysis material, dispersion by way of blending in conjunction with membrane technology
Not high and with organic polymer films incompatibility is spent, this results in the decline of catalytic performance and degradation efficiency.Meanwhile tradition
The porosity and specific surface area of the catalytic membrane of the method preparation of plate knifing are smaller, this is also a weight for limiting catalytic performance
Want factor.
Summary of the invention
Using cattail wool, as biomass carbon source, the height of biomass carbon fiber (Carbon fiber, CF) is utilized in the present invention
Absorption property, by C3N4, Pd nano particle be uniformly supported on its surface and can be improved the separative efficiency of photo-generate electron-hole, from
And construct the composite material of high absorption, high catalytic activity；Then composite film material is prepared using simple electrostatic spinning technique, made
Membrane material has biggish surface area.Compared with the blend film of traditional phase inversion preparation, this method utilizes to the greatest extent
The high adsorption and high activity of catalysis material, to achieve the effect that improve photocatalysis performance.This method provides a kind of structures
The new approaches for integrating the catalytic membrane of efficient absorption, catalytic degradation are built, realize the purpose of efficiently removal environmental wastewater.
A kind of Pd/C3N4The preparation method of@biomass carbon composite fiber membrane, cattail wool and urea are obtained through one step carbonization
C3N4@CF composite material, Pd nano particle in situ homoepitaxial is in C3N4@CF composite material surface obtains Pd/C3N4@CF is compound
Photochemical catalyst, the Pd/C3N4@CF composite photo-catalyst is prepared into Pd/C using electrostatic spinning process3N4@biomass carbon fiber
Composite membrane, the specific steps are as follows:
Step 1, preparation Pd/C3N4@biomass carbon fiber composite photochemical catalyst:
A weighs a certain amount of cattail wool as biomass carbon source, is immersed in urea liquid after clean dry, is put into after dry
In porcelain boat, it is then transferred to tube furnace, under conditions of nitrogen protection, certain time is calcined under certain temperature, to naturally cold
But it takes out afterwards, obtains C3N4@CF composite photo-catalyst, for use；
The C that b takes step a to prepare3N4@CF composite photo-catalyst is dispersed in water, and obtains C3N4@CF dispersion liquid；Then by chlorination
Palladium PdCl2Solution is added to C3N4It is uniformly mixed in@CF dispersion liquid, adds sodium borohydride NaBH4Solution obtains mixed liquor A, stirs
It mixes and stands after a certain period of time, be finally centrifuged, wash, is dry, obtaining Pd/C3N4@CF composite photo-catalyst.
Step 2, preparation Pd/C3N4@biomass carbon composite fiber membrane:
Take gained Pd/C in step 13N4@CF composite photo-catalyst is distributed in n,N-Dimethylformamide DMF, is added
PAN simultaneously stirs to get casting solution；Prepared film is all made of electrostatic spinning process preparation, and casting solution loading is mounted on syringe pump
On syringe in, make syringe needle point and collector maintained a certain distance and applied a voltage on syringe needle；It adjusts
After saving casting film flow velocity, electrospinning fibre is deposited on the non-woven substrate being placed on ground connection aluminium foil, obtain Pd/C3N4@CF is compound
Film.
In step 1a, the temperature of the drying is 60~80 DEG C, drying time is 12~for 24 hours；It is described to be forged in tube furnace
Burning temperature is 550~580 DEG C, calcination time 2h.
In step 1b, the C3N4The concentration of@CF dispersion liquid is 0.01~0.02g/mL；The PdCl2The concentration of solution is
0.001g/mL；The NaBH4The concentration of solution is 0.05g/mL；In the mixed liquor A, C3N4/ CF composite photo-catalyst,
PdCl2And NaBH4Mass ratio be (1~2): (0.01~0.2): 1.
In step 1b, the mixing time is 30min, time of repose 2h.
In step 2, Pd/C3N4The amount ratio of@CF composite photo-catalyst, PAN and DMF are 0.05~0.3g:1~3g:
20mL；Mixing time is 4h.
The syringe needle point is kept at a distance from 20.5cm with collector, and the voltage is 12.5kv；The casting film liquid stream
Speed is 0.8mLh-1。
The DMF in the above technical solution, it acts as solvents, dissolve PAN to prepare casting solution.
The PAN in the above technical solution, it acts as membrane matrixs.
Pd/C prepared by the present invention3N4@CF composite photocatalysis membrane is applied to degradation tetracycline.
Technological merit of the invention:
(1) cattail wool chosen has fibre structure, after cattail wool is impregnated in urea liquid, is formed after step carbonization
C3N4@CF is able to maintain fibre structure and possesses biggish specific surface area, the adsorbed target pollutant of energy rapid, high volume；
Make Pd nano particle in situ homoepitaxial in C using the method for sodium borohydride reduction3N4/ CF composite photo-catalyst table
Face is quickly transferred to the light induced electron of composite material on Pd nano particle, electron hole separative efficiency is improved, to improve light
Catalytic efficiency.
(2) there is biggish membrane aperture and membrane flux using the catalytic membrane that the method for electrostatic spinning constructs, this is dynamic
The process of absorption degradation provides the basis of quick adsorption, and entire synthetic method is simple and convenient.
(3) film after the degradation of long-time Dynamic Adsorption can mitigate membrane pollution problem by illumination, to membrane separation technique
Provide a kind of new opinion.
Detailed description of the invention
Fig. 1 is Pd/C3N4The transmission electron microscope picture of@CF composite material.
Fig. 2 is CF, C3N4@CF、Pd/C3N4The XRD spectrum of@CF composite material.
Specific embodiment
Embodiment 1:
(1)Pd/C3N4The preparation of@biomass carbon fiber composite photochemical catalyst
It weighs and is immersed in after 2g cattail wool is cleaned and dried in saturation urea liquid, be transferred to tube furnace after dry, protected in nitrogen
2h is calcined under shield at 550 DEG C, heating rate is 2.3 DEG C/min, takes out after natural cooling and obtains C3N4@CF, for use；
Take 1g C3N4@CF composite photo-catalyst is dispersed in 100ml water for use, takes 0.01g PdCl2It is dissolved in 10ml water
And be added in above-mentioned dispersion liquid and stir 2h, then 1g sodium borohydride is dissolved in 20ml water, and is added into above-mentioned dispersion liquid,
Stirring stood 2h after 30 minutes, i.e. acquisition Pd load C3N4@CF composite photo-catalyst.
(2)Pd/C3N4The preparation of@biomass carbon composite fiber membrane
It chooses above-mentioned composite material 0.05g to be dispersed in 20ml DMF, 2g PAN is then dissolved in the solution, and stir 4h
Obtain casting solution；10ml casting solution is transferred in syringe, prepares composite membrane using typical electrostatic spinning technique, it is specific to join
Number are as follows: syringe needle point is kept at a distance from 20.5cm with collector, and it is 12.5kv that needle point, which applies voltage, and casting film flow velocity is
0.8mL h-1。
Embodiment 2:
Prepare C3N4When@CF, in the case where guaranteeing that other conditions are constant, C is studied by changing urea concentration3N4
Influence to biomass carbon material catalytic performance；Prepare Pd load C3N4When@CF composite photo-catalyst, weighed C is selected3N4@CF
And PdCl2Quality be respectively as follows: 1g/0.2g and 2g/0.2g, by adjusting the mass ratio of the two come investigate Pd load capacity for
C3N4The influence of@CF composite catalyzing material catalytic activity.
Embodiment 3:
Prepare Pd load C3N4When@CF composite photocatalysis membrane (other conditions are constant), by the addition for changing composite catalyst
(0.1g, 0.2g, 0.3g) is measured to investigate influence of the dosage of composite catalyst to absorption degradation effect, screens optimal amount；Guarantee
Other conditions are constant, adjust the viscosity of casting solution by changing the additional amount (1g, 3g) of PAN, so that it is poly- to control composite membrane
Close the size of fiber diameter, adjustment aperture.Final choice most has proportion, so that the Pd/C of building3N4@CF composite photocatalysis membrane
90% or more is reached to the degradation effect of tetracycline in visible light (λ > 420nm) irradiation 120min.
As shown in Figure 1, Pd nano particle homoepitaxial is in C3N4The load on the surface@CF, CN can be carried out further with XRD
Characterization proves.
As shown in Fig. 2, the peak of Pd nano particle appears in 40 ° or so, and C3N4Characteristic peak be overlapped with the peak of CF, still
It can be, it is evident that introducing C3N4Afterwards, 20-30 ° or so of broad peak moves to right and intensity increases, this illustrates C3N4Successfully load
Onto CF.
Claims (8)
1. a kind of Pd/C3N4The preparation method of@biomass carbon composite fiber membrane, which comprises the steps of:
Step 1, preparation Pd/C3N4@biomass carbon fiber composite photochemical catalyst:
A weighs a certain amount of cattail wool as biomass carbon source, is immersed in urea liquid after clean dry, is put into porcelain boat after dry
In, it is then transferred to tube furnace, under conditions of nitrogen protection, certain time is calcined under certain temperature, after natural cooling
It takes out, obtains C3N4@biomass carbon fiber composite photochemical catalyst, for use；
The C that b takes step a to prepare3N4@biomass carbon fiber composite photochemical catalyst is dispersed in water, and obtains C3N4@biomass carbon fiber point
Dispersion liquid；Then by palladium chloride PdCl2Solution is added to C3N4It is uniformly mixed in@biomass carbon fiber dispersion, adds hydroboration
Sodium NaBH4Solution obtains mixed liquor A, and stirring is stood after a certain period of time, is finally centrifuged, washes, is dry, obtaining Pd/C3N4@biomass
Carbon fiber composite photo-catalyst；
Step 2, preparation Pd/C3N4@biomass carbon fiber composite photocatalysis membrana:
Take gained Pd/C in step 13N4@biomass carbon fiber composite photochemical catalyst is distributed in n,N-Dimethylformamide DMF,
PAN is added and stirs to get casting solution；Prepared film is all made of electrostatic spinning process preparation, and casting solution loading is mounted on note
It penetrates in the syringe on pump, syringe needle point and collector is made to maintain a certain distance and apply a voltage to syringe needle
On；After adjusting casting film flow velocity, electrospinning fibre is deposited on the non-woven substrate being placed on ground connection aluminium foil, obtain Pd/C3N4@
Biomass carbon composite fiber membrane.
2. a kind of Pd/C as described in claim 13N4The preparation method of@biomass carbon composite fiber membrane, which is characterized in that step
In rapid 1a, the temperature of the drying is 60~80 DEG C, drying time is 12~for 24 hours.
3. a kind of Pd/C as described in claim 13N4The preparation method of@biomass carbon composite fiber membrane, which is characterized in that step
In rapid 1a, the temperature of the calcining is 550~580 DEG C, and the time of calcining is 2h.
4. a kind of Pd/C as described in claim 13N4The preparation method of@biomass carbon composite fiber membrane, which is characterized in that step
In rapid 1b, the C3N4The concentration of@biomass carbon fiber dispersion is 0.01~0.02g/mL；The PdCl2The concentration of solution is
0.001g/mL；The NaBH4The concentration of solution is 0.05g/mL；In the mixed liquor A, C3N4/ biomass carbon fiber composite light
Catalyst, PdCl2And NaBH4Mass ratio be (1~2): (0.01~0.2): 1.
5. a kind of Pd/C as described in claim 13N4The preparation method of@biomass carbon composite fiber membrane, which is characterized in that step
In rapid 1b, the mixing time is 30min, time of repose 2h.
6. a kind of Pd/C as described in claim 13N4The preparation method of@biomass carbon composite fiber membrane, which is characterized in that step
In rapid 2, Pd/C3N4The amount ratio of@biomass carbon fiber composite photochemical catalyst, PAN and DMF is 0.05~0.3g:1~3g:
20mL。
7. a kind of Pd/C as described in claim 13N4The preparation method of@biomass carbon composite fiber membrane, which is characterized in that step
In rapid 2, mixing time 4h.
8. Pd/C made from the preparation method as described in claim 1~7 any one3N4The use of@biomass carbon composite fiber membrane
On the way, which is characterized in that by Pd/C3N4@biomass carbon composite fiber membrane is used as photocatalyst for degrading tetracycline, it is seen that light irradiation
90% or more is reached to the degradation effect of tetracycline after 120min.
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| CN110694661A (en) * | 2019-10-12 | 2020-01-17 | 台州学院 | g-C based on electrostatic spinning process3N4Preparation method and application of composite nanofiber membrane |
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