CN114534516B - Preparation method of filtering and photocatalytic degradation integrated composite membrane layer - Google Patents
Preparation method of filtering and photocatalytic degradation integrated composite membrane layer Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims abstract description 26
- 238000001914 filtration Methods 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000013033 photocatalytic degradation reaction Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000012876 carrier material Substances 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 230000008878 coupling Effects 0.000 claims description 22
- 238000010168 coupling process Methods 0.000 claims description 22
- 238000005859 coupling reaction Methods 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 229910001220 stainless steel Inorganic materials 0.000 claims description 17
- 239000010935 stainless steel Substances 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012634 fragment Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 230000001939 inductive effect Effects 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 11
- 239000010865 sewage Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 6
- 238000004887 air purification Methods 0.000 abstract description 5
- 239000000969 carrier Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 4
- 230000005284 excitation Effects 0.000 abstract description 3
- 238000009616 inductively coupled plasma Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 238000004506 ultrasonic cleaning Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 10
- 230000006872 improvement Effects 0.000 description 9
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 6
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
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- 238000006731 degradation reaction Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000005373 porous glass Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000012465 retentate Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- 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
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0044—Inorganic membrane manufacture by chemical reaction
-
- 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
- B01D71/02—Inorganic material
-
- 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
- B01J27/06—Halogens; Compounds thereof
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- 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
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- 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
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- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0217—Pretreatment of the substrate before coating
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/349—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of flames, plasmas or lasers
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
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- 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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Abstract
The invention discloses a preparation method of a filtering and photocatalytic degradation integrated composite membrane layer in the fields of air purification and sewage treatment, which comprises the following steps: selecting porous carriers with different pore diameters, different thicknesses and different materials; putting the porous carrier material into acetone or ethanol solution for ultrasonic cleaning, repeatedly washing with deionized water, and drying; pretreating the porous carrier by low-pressure low-temperature plasma; the growth of the film layer is mainly controlled by a hydrothermal synthesis method, and a precursor substance for preparing the film layer material is added into a hydrothermal reaction kettle; the surface film layer of the porous carrier is subjected to post-treatment by using atmospheric low-temperature plasma, and the surface film layer of the porous carrier is mainly treated by using a radio frequency inductively coupled plasma instrument, wherein the adjustable parameters of the plasma instrument comprise the power of an excitation power supply, the type of plasma gas and the treatment time. The composite membrane layer prepared by the invention can be used for air purification and sewage treatment.
Description
Technical Field
The invention belongs to the field of air purification and sewage treatment, and particularly relates to a preparation method of a filtering and photocatalytic degradation integrated composite membrane layer.
Background
At present, sewage treatment is taken as the most important environmental engineering in the present stage in China, which is beneficial to maintaining the water body environment of rivers, lakes and seas, and polluted water bodies which are harmful to the environment are degraded into reclaimed water harmless to the environment through a good treatment process, and the reclaimed water can be provided for various municipal or industrial purposes such as public water spraying, cooling circulating water and the like, so that the recycling of water resources is realized, and the problem of water resource shortage is relieved to a certain extent.
Microporous filtration can be used to retain particulates, bacteria, contaminants, etc. from gas and liquid phases, and is a necessary means to ensure product quality in the modern industry. The driving force of microfiltration is to pass a suspension through a membrane, where liquid and small solutes permeate the membrane to collect as permeate. Suspended particles are trapped by the membrane and collected as a concentrated retentate. The mechanism by which particles are trapped depends on the properties of the membrane (physical and chemical properties) and the nature of the interactions between the membrane and the particles.
The photocatalysis technology has excellent performance in water treatment, and has the characteristics of green and safe performance, high degradation efficiency, mild condition, low economic cost and the like. Can completely mineralize pollutants in the organic wastewater into non-toxic and harmless inorganic micromolecules.
However, the prior art does not combine the technologies of microporous filtration and photocatalytic degradation to manufacture a composite sewage purification membrane layer.
Disclosure of Invention
The invention mainly solves the problems of application expansion and efficiency improvement of a filtering catalytic material, and aims to develop a novel high-efficiency bismuth-based/doped semiconductor visible light catalytic solid-supported film layer by utilizing a comprehensive innovation process of combining a hydrothermal controllable synthesis technology with a low-temperature plasma modification and deposition technology.
The purpose of the invention is realized in the following way: a preparation method of a filtering and photocatalytic degradation integrated composite membrane layer comprises the following steps:
(1) Selecting a porous carrier with the aperture of 1-500 um and the thickness of 1-5 mm;
(2) Pretreatment of a porous carrier: placing the porous carrier into an acetone or ethanol solution, ultrasonically cleaning for 5-20 minutes, repeatedly washing with deionized water for 3-8 times, and then placing in a drying oven at 50-100 ℃ for drying for 30-120 minutes;
(3) Pretreatment of the porous support by low pressure low temperature plasma: applying a radio frequency inductively coupled low pressure low temperature plasma instrument to treat the surface of the porous carrier with low pressure low temperature plasma;
(4) Growth of a film layer: adding a precursor substance for preparing a BiOBr film material into a hydrothermal reaction kettle, then placing a porous carrier into the reaction kettle filled with the precursor for sealing, controlling the hydrothermal synthesis time to be 3-10 h, controlling the hydrothermal synthesis temperature to be 100-200 ℃, and generating a photocatalytic film layer on the surface of the porous carrier;
(5) Carrying out post-treatment on the surface film layer of the porous carrier by using atmospheric pressure low-temperature plasma: a radio frequency inductively coupled atmospheric pressure low temperature plasma instrument is used to treat the surface film layer of the porous carrier with the atmospheric pressure low temperature plasma.
The method comprises the steps of firstly preprocessing a selected porous carrier, then preprocessing the porous carrier by using low-pressure low-temperature plasma, then generating a photocatalytic film layer on the preprocessed porous carrier by using a hydrothermal synthesis method, and finally performing post-processing on the photocatalytic film layer by using atmospheric pressure low-temperature plasma. Compared with the prior art, the invention has the beneficial effects that: the prepared photocatalysis immobilized membrane layer not only has a bismuth-based/doped semiconductor hierarchical porous (mesoporous and hollow) micro-nano structure membrane layer with high specific surface area, but also can construct a multiple high-efficiency surface interface structure in the membrane layer, and is a novel air purification and sewage treatment product; the high-efficiency surface interface structure is a close contact interface which is connected by chemical bonds, can effectively reduce the transfer resistance of carriers, shortens the migration path of the carriers, and prolongs the service life of the carriers to the greatest extent. Therefore, the material can enhance the absorption of sunlight or simulated sunlight and promote the separation of photo-generated carriers, thereby further improving the photocatalysis performance.
As a further improvement of the invention, the porous carrier is made of metal, and the metal porous carrier is made of nickel, copper or stainless steel. Porous nickel, porous copper or stainless steel mesh may be used as the porous support.
As a further improvement of the invention, the porous carrier is made of inorganic nonmetal, and the inorganic nonmetal porous carrier is made of ceramic or glass. Porous ceramics or porous glass may be used as the porous support.
As a further improvement of the invention, the porous carrier is made of organic materials, and the porous carrier made of organic materials is made of plastics, rubber or resin. Porous plastics, porous rubbers or porous resins may be used as the porous support.
As a further improvement of the invention, the low-pressure low-temperature plasma is gas, the working pressure is 0.5-2 Pa, and the working temperature is 30-100 ℃. The surface of the porous carrier is pretreated by low-pressure low-temperature plasma.
As a further improvement of the invention, the power of the excitation power supply of the radio frequency inductance coupling low-pressure low-temperature plasma instrument is 100-500W, the treatment time is 50-500 seconds, and the low-pressure low-temperature plasma gas is N 2 、H 2 Ar or C 2 H 4 . And determining the adjustable parameters of the radio frequency inductively coupled low-pressure low-temperature plasma processor.
As a further improvement of the invention, the precursor substance is Bi (NO) with the mass of 1-3 g 3 ) 3 ·5H 2 The O is completely dissolved in 50-80 mL of deionized water to form a solution, and the mass of KBr is 0.2-1 g. Bi (NO) 3 ) 3 ·5H 2 O solution and KBr are used as reactants of hydrothermal synthesis, namely precursor substances for preparing the BiOBr film layer on the surface of the porous carrier, so that the preparation of the BiOBr film layer on the surface of the porous carrier is realized.
As a further improvement of the invention, the atmospheric pressure low-temperature plasma is gas, the working pressure is 1 atmosphere, and the working temperature is 30-100 ℃. And (3) carrying out post-treatment on the BiOBr photocatalytic film layer generated on the surface of the porous carrier through atmospheric pressure low-temperature plasma.
As a further improvement of the invention, the power of the excitation power supply of the radio frequency inductive coupling atmospheric pressure low temperature plasma instrument is 300-800W, the treatment time is 60-150 seconds, and the atmospheric pressure low temperature plasma gas is NH 3 3-aminopropyl triethoxysilane (APTES) or Hexamethyldisiloxane (HMDSO). And determining the adjustable parameters of the radio frequency inductively coupled atmospheric pressure low temperature plasma processor.
Drawings
FIG. 1 is a schematic diagram of the technical route of the present invention.
Fig. 2 is an SEM image of a composite membrane layer prepared on the surface of porous nickel as a porous support.
Fig. 3 is a partial enlarged view of fig. 2.
Fig. 4 is a partial enlarged view of fig. 3.
Detailed Description
Example 1
The preparation method of the filtration and photocatalytic degradation integrated composite membrane layer of the embodiment comprises the following steps: (1) Selecting porous nickel with the aperture of 200um and the thickness of 3mm as a porous carrier;
(2) Pretreatment of a porous carrier: placing the porous carrier into a beaker filled with 30ml of ethanol solution, washing for 15min by ultrasonic waves, repeatedly washing for 5 times by deionized water to remove redundant organic matters and impurity fragments, then placing the porous carrier into a drying oven (drying oven), drying at 60 ℃ for 60min, and then naturally cooling to room temperature;
(3) Pretreatment of the porous support by low pressure low temperature plasma: using a radio frequency inductance coupling low-pressure low-temperature plasma instrument to treat the surface of the porous carrier by using low-pressure low-temperature plasma, wherein the low-pressure low-temperature plasma is N 2 ，N 2 The working pressure of the low-pressure low-temperature plasma is 2Pa, the working temperature is 30 ℃, the porous carrier material is pretreated under the condition that the power supply of the radio frequency inductance coupling low-pressure low-temperature plasma instrument is 100W, and the porous carrier material is pretreated by N 2 The plasma atmosphere is opposite to the porous carrierTreating for 50s;
(4) Growth of a film layer: under normal temperature, 1g of Bi (NO 3 ) 3 ·5H 2 O was completely dissolved in 80ml of deionized water, and the dissolved Bi (NO 3 ) 3 ·5H 2 Adding O solution and 0.72g KBr into 60ml of ethylene glycol sequentially, stirring, transferring the uniform solution into a stainless steel high-pressure reaction kettle (hydrothermal reaction kettle) with 200ml of volume and polytetrafluoroethylene lining after stirring, filling a precursor for preparing a BiOBr film layer into the stainless steel high-pressure reaction kettle, then placing a porous carrier material into the stainless steel high-pressure reaction kettle filled with the precursor for sealing, keeping the temperature at 100 ℃, keeping the temperature at 6 h, naturally cooling to room temperature after the reaction is finished, filtering and washing the surface film layer of the porous carrier by absolute ethyl alcohol for 5 times, and drying the porous carrier material for 4 hours at 60 ℃ to obtain a cleaned porous carrier material film layer;
(5) Post-treating the porous carrier film layer by using atmospheric pressure low-temperature plasma: using radio frequency inductance coupling atmospheric pressure low temperature plasma instrument to treat the surface film layer of porous carrier with atmospheric pressure low temperature plasma, wherein the atmospheric pressure low temperature plasma is NH 3 ，NH 3 The working pressure of the atmospheric pressure low-temperature plasma is 1 atmosphere, the working temperature is 30 ℃, the surface film layer of the porous carrier is subjected to post-treatment under the condition that the power of a power supply of a radio frequency inductance coupling atmospheric pressure low-temperature plasma instrument is 300W, and NH is used for the surface film layer 3 And treating the surface film layer of the porous carrier in the plasma atmosphere for 70s to finally obtain the surface film layer of the porous carrier, wherein the surface film layer is shown in figures 2-4.
Example 2
The preparation method of the filtration and photocatalytic degradation integrated composite membrane layer of the embodiment comprises the following steps: (1) Selecting porous copper with the aperture of 1um and the thickness of 5mm as a porous carrier;
(2) Pretreatment of a porous carrier: placing the porous carrier into a beaker filled with 30ml of ethanol solution, washing for 5min by ultrasonic waves, repeatedly washing for 8 times by deionized water to remove redundant organic matters and impurity fragments, then placing the porous carrier into a drying oven (drying oven), drying for 30min at 50 ℃, and then naturally cooling to room temperature;
(3) Pretreatment of the porous support by low pressure low temperature plasma: the surface of the porous carrier is treated by using a radio frequency inductance coupling low-pressure low-temperature plasma instrument by using low-pressure low-temperature plasma, wherein the low-pressure low-temperature plasma is H 2 ，H 2 The working air pressure of the low-pressure low-temperature plasma is 0.5Pa, the working temperature is 50 ℃, the porous carrier material is pretreated under the condition that the power supply of the radio frequency inductance coupling low-pressure low-temperature plasma instrument is 300W, and the porous carrier material is pretreated by H 2 Treating the porous carrier for 90s in the plasma atmosphere;
(4) Growth of a film layer: under normal temperature conditions, 3g of Bi (NO 3 ) 3 ·5H 2 O was completely dissolved in 50ml of deionized water, and the dissolved Bi (NO 3 ) 3 ·5H 2 Adding O solution and 0.36g KBr into 60ml of ethylene glycol sequentially, stirring, transferring the uniform solution into a stainless steel high-pressure reaction kettle (hydrothermal reaction kettle) with 200ml of volume and polytetrafluoroethylene lining after stirring, filling a precursor for preparing a BiOBr film layer into the stainless steel high-pressure reaction kettle, then placing a porous carrier material into the stainless steel high-pressure reaction kettle filled with the precursor for sealing, keeping the reaction kettle at 200 ℃ for 3 hours, naturally cooling to room temperature after the reaction is finished, then filtering and washing the surface film layer of the porous carrier by absolute ethyl alcohol for 5 times, and drying the porous carrier material at 60 ℃ for 4 hours to obtain a cleaned porous carrier material film layer;
(5) Post-treating the porous carrier film layer by using atmospheric pressure low-temperature plasma: the surface film layer of the porous carrier is treated by using an atmospheric pressure low-temperature plasma by using a radio frequency inductive coupling atmospheric pressure low-temperature plasma instrument, wherein the atmospheric pressure low-temperature plasma is 3-aminopropyl triethoxysilane, the working pressure of the 3-aminopropyl triethoxysilane atmospheric pressure low-temperature plasma is 1 atmosphere, the working temperature is 60 ℃, the surface film layer of the porous carrier is subjected to post treatment under the condition that the power of the radio frequency inductive coupling atmospheric pressure low-temperature plasma instrument is 500W, and the surface film layer of the porous carrier is treated for 60s by using the 3-aminopropyl triethoxysilane plasma atmosphere, so that the surface film layer of the porous carrier is finally obtained.
Example 3
The preparation method of the filtration and photocatalytic degradation integrated composite membrane layer of the embodiment comprises the following steps: (1) Selecting a stainless steel mesh with the aperture of 300um and the thickness of 1mm as a porous carrier;
(2) Pretreatment of a porous carrier: placing the porous carrier into a beaker filled with 30ml of ethanol solution, washing for 20min by ultrasonic waves, repeatedly washing for 3 times by deionized water to remove redundant organic matters and impurity fragments, then placing the porous carrier into a drying oven (drying oven), drying for 120min at 100 ℃, and then naturally cooling to room temperature;
(3) Pretreatment of the porous support by low pressure low temperature plasma: using a radio frequency inductance coupling low-pressure low-temperature plasma instrument to treat the surface of the porous carrier by using low-pressure low-temperature plasma, wherein the low-pressure low-temperature plasma is Ar, the working pressure of the Ar low-pressure low-temperature plasma is 1.5Pa, the working temperature is 100 ℃, the radio frequency inductance coupling low-pressure low-temperature plasma instrument is used for carrying out pretreatment on the porous carrier material under the condition that the power supply power is 500W, and the porous carrier is treated for 130s by using Ar plasma atmosphere;
(4) Growth of a film layer: under normal temperature, 2g of Bi (NO 3 ) 3 ·5H 2 O was completely dissolved in 60ml of deionized water, and the dissolved Bi (NO 3 ) 3 ·5H 2 Adding O solution and 1g KBr into 60ml of ethylene glycol sequentially, stirring to obtain a uniform solution, transferring the uniform solution into a stainless steel high-pressure reaction kettle (hydrothermal reaction kettle) with 200ml of volume and polytetrafluoroethylene lining, filling a precursor for preparing a BiOBr film layer into the stainless steel high-pressure reaction kettle, then placing a porous carrier material into the stainless steel high-pressure reaction kettle filled with the precursor for sealing, keeping the porous carrier material at 150 ℃ for 10 hours, naturally cooling to room temperature after the reaction is finished, filtering and washing the surface film layer of the porous carrier for 5 times by absolute ethyl alcohol, and drying the porous carrier material at 60 ℃ for 4 hours to obtain a cleaned porous carrier material film layer;
(5) Post-treating the porous carrier film layer by using atmospheric pressure low-temperature plasma: the surface film layer of the porous carrier is treated by using an atmosphere pressure low-temperature plasma by using a radio frequency inductance coupling atmosphere low-temperature plasma instrument, wherein the atmosphere pressure low-temperature plasma is hexamethyldisiloxane, the working pressure of the hexamethyldisiloxane atmosphere low-temperature plasma is 1 atmosphere, the working temperature is 100 ℃, the surface film layer of the porous carrier is subjected to post treatment under the condition that the power of the radio frequency inductance coupling atmosphere low-temperature plasma instrument is 800W, and the surface film layer of the porous carrier is treated for 150s by using the hexamethyldisiloxane plasma atmosphere, so that the surface film layer of the porous carrier is finally obtained.
Example 4
The preparation method of the filtration and photocatalytic degradation integrated composite membrane layer of the embodiment comprises the following steps: (1) Selecting porous nickel with the aperture of 500um and the thickness of 4mm as a porous carrier;
(2) Pretreatment of a porous carrier: placing the porous carrier into a beaker filled with 30ml of ethanol solution, washing for 10min by ultrasonic waves, repeatedly washing for 6 times by deionized water to remove redundant organic matters and impurity fragments, then placing the porous carrier into a drying oven (drying oven), drying for 90min at 80 ℃, and then naturally cooling to room temperature;
(3) Pretreatment of the porous support by low pressure low temperature plasma: using a radio frequency inductance coupling low-pressure low-temperature plasma instrument to treat the surface of the porous carrier by using low-pressure low-temperature plasma, wherein the low-pressure low-temperature plasma is C 2 H 4 ，C 2 H 4 The working pressure of the low-pressure low-temperature plasma is 1Pa, the working temperature is 80 ℃, the porous carrier material is pretreated under the condition that the power supply of the radio frequency inductance coupling low-pressure low-temperature plasma instrument is 400W, and the porous carrier material passes through C 2 H 4 Treating the porous carrier in the plasma atmosphere for 500s;
(4) Growth of a film layer: under normal temperature, 2g of Bi (NO 3 ) 3 ·5H 2 O was completely dissolved in 70ml of deionized water, and the dissolved Bi (NO 3 ) 3 ·5H 2 The O solution and 0.2g KBr were added to 60ml of ethylene glycol in succession and stirred to give a homogeneous solution which was then transferred to a volume of 200ml and had a polymerFilling a precursor for preparing a BiOBr film layer in a stainless steel high-pressure reaction kettle (hydrothermal reaction kettle) with a tetrafluoroethylene lining, then putting a porous carrier material into the stainless steel high-pressure reaction kettle filled with the precursor for sealing, keeping the porous carrier material at 120 ℃ for 8 hours, naturally cooling to room temperature after the reaction is finished, then filtering and washing the surface film layer of the porous carrier with absolute ethyl alcohol for 5 times, and drying the porous carrier material at 60 ℃ for 4 hours to obtain a washed porous carrier material film layer;
(5) Post-treating the porous carrier film layer by using atmospheric pressure low-temperature plasma: the surface film layer of the porous carrier is treated by using an atmosphere pressure low-temperature plasma by using a radio frequency inductance coupling atmosphere low-temperature plasma instrument, wherein the atmosphere pressure low-temperature plasma is hexamethyldisiloxane, the working pressure of the hexamethyldisiloxane atmosphere low-temperature plasma is 1 atmosphere, the working temperature is 80 ℃, the surface film layer of the porous carrier is subjected to post treatment under the condition that the power of the radio frequency inductance coupling atmosphere low-temperature plasma instrument is 600W, and the surface film layer of the porous carrier is treated for 120s by using the hexamethyldisiloxane plasma atmosphere, so that the surface film layer of the porous carrier is finally obtained.
The porous carrier composite membrane layers prepared in the examples 1-4 have good photocatalysis effect and filtering performance, and can be used for air purification and sewage treatment.
Example 5
The difference from example 1 is that: in the step (3): through N 2 The porous support is treated in a low pressure low temperature plasma atmosphere for 90s.
Example 6
The difference from example 1 is that: in the step (3): through N 2 The porous support is treated in a low pressure low temperature plasma atmosphere for 110s.
Example 7
The difference from example 1 is that: in the step (3): through N 2 The porous support is treated in a low pressure low temperature plasma atmosphere for 130s.
Example 8
The difference from example 1 is that: step (a)(3) In (a): through N 2 The porous carrier is treated for 150s in a low-pressure low-temperature plasma atmosphere.
Example 9
The difference from example 1 is that: in the step (3): through N 2 The porous support is treated in a low pressure low temperature plasma atmosphere for 170s.
Example 10
The difference from example 1 is that: in the step (3): through N 2 The porous support was treated with a low pressure low temperature plasma atmosphere for 300s.
Example 11
The difference from example 1 is that: in the step (3): through N 2 The porous carrier is treated in a low pressure low temperature plasma atmosphere for 450s.
The porous support composite membrane layers prepared in example 1 and examples 5-11 were tested, example 7, by N 2 The porous carrier composite membrane layer prepared by treating the porous carrier for 130s in the low-pressure low-temperature plasma atmosphere has better photocatalysis effect and filtering performance.
Example 12
The difference from example 1 is that: in the step (3): by H 2 The porous support was treated with a low pressure low temperature plasma atmosphere for 50s.
Example 13
The difference from example 1 is that: in the step (3): the porous support was treated with an Ar low pressure low temperature plasma atmosphere for 50s.
Example 14
The difference from example 1 is that: in the step (3): through C 2 H 4 The porous support was treated with a low pressure low temperature plasma atmosphere for 50s.
The porous support composite membrane layers prepared in example 1 and examples 12-14 were tested, example 7, by H 2 The porous carrier composite membrane layer prepared by treating the porous carrier in the low-pressure low-temperature plasma atmosphere has better photocatalysis effect and filtering performance.
Claims (1)
1. The preparation method of the integrated composite membrane layer for filtering and photocatalytic degradation is characterized by comprising the following steps of:
(1) Selecting porous nickel with the aperture of 200um and the thickness of 3mm as a porous carrier;
(2) Pretreatment of a porous carrier: placing the porous carrier into a beaker filled with 30ml of ethanol solution, washing for 15min by ultrasonic waves, repeatedly washing for 5 times by deionized water to remove redundant organic matters and impurity fragments, placing the porous carrier into a drying box, drying at 60 ℃ for 60min, and naturally cooling to room temperature;
(3) Pretreatment of the porous support by low pressure low temperature plasma: using a radio frequency inductance coupling low-pressure low-temperature plasma instrument to treat the surface of the porous carrier by using low-pressure low-temperature plasma, wherein the low-pressure low-temperature plasma is N2, the working pressure of the N2 low-pressure low-temperature plasma is 2Pa, the working temperature is 30 ℃, the pretreatment is carried out on the porous carrier material under the condition that the power of the radio frequency inductance coupling low-pressure low-temperature plasma instrument is 100W, and the porous carrier is treated for 50s by using the atmosphere of H2 plasma;
(4) Growth of a film layer: under normal temperature, 1g of Bi (NO 3) 3.5H2O is completely dissolved in 80ml of deionized water, the dissolved Bi (NO 3) 3.5H2O solution and 0.72g of KBr are sequentially added into 60ml of ethylene glycol and stirred, after uniform solution is obtained by stirring, the uniform solution is transferred into a stainless steel high-pressure reaction kettle with 200ml of volume and polytetrafluoroethylene lining, so that a precursor for preparing a BiOBr film layer is filled into the stainless steel high-pressure reaction kettle, then the porous carrier material is put into the stainless steel high-pressure reaction kettle filled with the precursor for sealing, the temperature is kept at 6H under the temperature of 100 ℃, after the reaction is finished, the porous carrier material is naturally cooled to the room temperature, then the surface film layer of the porous carrier material is subjected to absolute ethyl alcohol filtration washing for 5 times, and the porous carrier material is dried for 4 hours under the temperature of 60 ℃ to obtain the cleaned porous carrier material film layer;
(5) Post-treating the porous carrier film layer by using atmospheric pressure low-temperature plasma: the surface film layer of the porous carrier is treated by using an atmosphere low-temperature plasma by using a radio frequency inductive coupling atmosphere low-temperature plasma instrument, wherein the atmosphere low-temperature plasma is NH3, the working pressure of the NH3 atmosphere low-temperature plasma is 1 atmosphere, the working temperature is 30 ℃, the surface film layer of the porous carrier is subjected to post treatment under the condition that the power of the radio frequency inductive coupling atmosphere low-temperature plasma instrument is 300W, and the surface film layer of the porous carrier is treated for 70 seconds by using the NH3 plasma atmosphere, so that the surface film layer of the porous carrier is finally obtained.
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