CN106757483A - Standby electret PEI boehmite composite fibre filtering material of a kind of electro-spinning and preparation method thereof - Google Patents
Standby electret PEI boehmite composite fibre filtering material of a kind of electro-spinning and preparation method thereof Download PDFInfo
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- CN106757483A CN106757483A CN201610998682.9A CN201610998682A CN106757483A CN 106757483 A CN106757483 A CN 106757483A CN 201610998682 A CN201610998682 A CN 201610998682A CN 106757483 A CN106757483 A CN 106757483A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/80—Type of catalytic reaction
- B01D2255/802—Photocatalytic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/91—Bacteria; Microorganisms
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- General Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Textile Engineering (AREA)
- Biomedical Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Analytical Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Filtering Materials (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention discloses a kind of standby electret PEI boehmite composite fibre filtering material of electro-spinning, by the raw material components of following weight portion：75 85 parts of PEI, 5 10 parts of silicon monoxide, 8 15 parts of Powdered Activated Carbon, 313 parts of aminopropyl triethoxysilane coupling agents, 0.8 2 parts of glacial acetic acid, appropriate deionized water, 36 parts of metatitanic acid, the AgNO of 0.6mol/L3Appropriate solution, N methyl pyrrolidones are appropriate, 12 parts of nm boehmite, 13 parts of expanded graphite.The present invention prepares the silicon nanowires containing α quartz, and Static Spinning/electret composite fibre filtering material is prepared by electrostatic spinning technique, with excellent Charge Storage Stability energy, greatly improves the filter efficiency of filter material；Addition Nano Silver is loaded into nano titanium oxide in addition, improves the Durability of antimicrobial effect energy of filtering material, reaches long-term efficient filter effect.
Description
Technical field
The invention belongs to field of air filtration, and in particular to a kind of standby electret PEI-boehmite of electro-spinning
Composite fibre filtering material and preparation method thereof.
Technical background
With going deep into and fast-developing for process of industrialization, the dust granules thing being discharged into air is sharply increased, wherein
PM2.5（Particulate pollutant of the particle diameter less than 2.5 μm）The health of the mankind can be caused serious injury, it is inhaled into meeting after human body
Bronchus is directly entered, triggers the diseases such as asthma, bronchitis, pneumoconiosis and cardiovascular disease, this is to cause China's patients with lung cancer urgency
Acute increased one of the main reasons.Therefore air filter unit becomes study hotspot, the research of its core filtering material and opens
Hair is even more becomes the most important thing.
Traditional melt-blown non-woven electret material is processed by electret, and surface takes electric charge and makes it have filtering effect higher
Rate, but its charge stability is easily affected by environment, and charge decay rate is very fast, filter efficiency declines to a great extent therewith.Additionally, staying
Pole process also increased production cost to a certain extent as a necessary aftertreatment technology.
Electrostatic spinning process needs to apply high pressure, the inorganic electret of excellent performance is added in spinning solution, by quiet
Electrospun, makes fiber and electrodeless electret all take electric charge, and Static Spinning/electret bluk recombination can be greatly enhanced using Electrostatic Absorption
The filter efficiency of tunica fibrosa, and resistance pressure drop is reduced, effective protection can be carried out to PM2.5.
Li little Qi, crystalline substance pair high et al. exist《Electret PEI-silica nano fibrous membrane answering in air filtration
With》Electrostatic spinning technique is used in one text, first with PEI（PEI）It is raw material, the PEI for preparing various concentrations is molten
The electrets such as liquid, addition silica, silicon nitride, barium titanate, the addition of electret makes big quantity space on electrostatic spinning fiber film band
Electric charge, makes its filter efficiency be greatly improved.
The present invention is added to silicon nanowires as inorganic electret in PEI spinning solution, prepares PEI
Composite fibre filtering material, addition Ag-carried nanometer titanium dioxide improves the antimicrobial form of composite fibre filtering material, improves electret
The strainability of filtering material.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of standby electret PEI-boehmite of electro-spinning being combined
Fiber filter material and preparation method thereof.
The standby electret PEI of a kind of electro-spinning-boehmite composite fibre filtering material, by following weight portion
Raw material components：PEI 75-85 parts, silicon monoxide 5-10 parts, Powdered Activated Carbon 8-15 parts, 3- aminopropyl-triethoxy silicon
1-3 parts of alkane coupling agent, glacial acetic acid 0.8-2 parts, appropriate deionized water, metatitanic acid 3-6 parts, the AgNO of 0.6mol/L3Appropriate solution,
Appropriate 1-METHYLPYRROLIDONE, nm boehmite 1-2 parts, expanded graphite 1-3 parts.
Comprise the following steps that：
（1）The preparation of Ag-carried nanometer titanium dioxide：
By in metatitanic acid addition deionized water, in 0.4-0.7mol/L, be heated to 105-125 DEG C maintains it to control solution concentration
, there is the white metatitanic acid precipitation of hydrolysis generation in boiling, centrifugal filtration, washing no longer detect SO into precipitating4 2-Ion, leaching
AgNO of the stain in 0.6mol/L3In solution, calcined 1-2 hours at 460-490 DEG C after being dried at 70-90 DEG C, obtain carrying silver
Nano titanium oxide；
（2）The preparation of silicon nanowires：
The small porcelain boat that will be equipped with silicon monoxide powder is placed horizontally in the middle of alumina tube, and the pipe then is placed on into high temperature process furnances
In, vacuumize in 80-100Pa, then temperature is increased to 100-200,800-1100 DEG C and respectively 50-70 points of insulation respectively
Clock, is warmed up to 1300-1400 DEG C and is incubated 3-5 hours afterwards；550-650 DEG C is cooled to the speed of 1-3 DEG C/min and protect afterwards
It is warm 20-40 minutes, while blasting air to furnace chamber with 50sccm, room temperature is naturally cooled to, silicon nanowires is obtained, it is standby；
（3）The preparation of activated carbon supported silicon nanowires：
1. 3- aminopropyl triethoxysilane coupling agents, are added to deionized water, and pH to 4 is adjusted with a small amount of glacial acetic acid,
Stir 20-40 minutes at room temperature, step is added afterwards（1）The silicon nanowires for obtaining is small in 80-100 DEG C of back flow reaction 11-13
When, suction filtration, washing, drying obtain silicon amide nanowire composite；
2. the silicon amide nanowire composite that, will obtain, Powdered Activated Carbon are added to deionized water, with ultrasonic wave 40 DEG C,
Mix 20-40 minute under conditions of 150W, static aging 24 hours at room temperature, cleaned with deionized water and multiple be in efflux
Property, 110-120 DEG C of drying 10-14 hour is to constant weight, then is placed in Muffle furnace 380-420 DEG C and is calcined 3-5 hour, cools down, drying,
Activated carbon supported silicon nanowires is obtained；
（4）The preparation of spinning solution：
1., by step（1）Obtain Ag-carried nanometer titanium dioxide, step（3）Activated carbon supported silicon nanowires is obtained and adds N- methyl
In pyrrolidones, ultrasound 1-3 hours in ultrasonic cleaner is placed on, is set to solution A；
2., take expanded graphite and add deionized water, through sonic oscillation, form the mixed liquor of expanded graphite, add nm boehmite
Ultrasonic disperse 30-50 minutes, obtain well mixed dispersion liquid；
3., at ambient temperature, by PEI and 1-METHYLPYRROLIDONE with 1:The ratio mixing of 3-4, is sealed with sealed membrane
Firmly bottleneck, is placed in oil bath 55-65 DEG C and heats 18-22 hour, is set to solution B, is placed in stirring on magnetic stirring apparatus, is slowly added to
Above-mentioned solution A, continues to stir 3-5 hours, above-mentioned dispersion liquid is continuously added afterwards and continues to stir 5-8 hours, is configured to mobility
Good spinning solution；
（5）Above-mentioned spinning solution is carried out into electrostatic spinning, electrostatic spinning nano fiber electret filtering material is obtained.
Wherein, described electrostatic spinning process parameter is：Voltage is 1-50KV, and syringe needle is 0.1- to template distance is received
2m, spinnerette diameters are 1 μm of -2mm, and spinning speed is 0.1-20mL/h, and the spinning time is 8-10 hours, and environment temperature is 20-
60 DEG C, envionmental humidity is 20-80%.
Compared with prior art, the present invention has advantages below：
（1）The present invention prepares the silicon nanowires containing alpha-quartz, because the volumetric expansion in alpha-quartz forming process is by outer layer
Amorphous silica limitation and alpha-quartz is generated piezo-electric effect, while by the electric charge of generation be stored in outer layer have it is good
In the amorphous silica layer of good electric charge storge quality, so as to show good electret behavior, by electrostatic spinning skill
The step of art one prepares Static Spinning/electret composite fibre filtering material, have that aperture is small, porosity is high when PM2.5 particles are purified,
The advantages of low-drag, and with excellent Charge Storage Stability energy, greatly improve the filter efficiency of filter material.
（2）Activated carbon has abundant pore structure and unique chemical functional group, is environmentally friendly superior adsorbent,
The present invention improves load of the activated carbon to silicon nanowires using the silicon nanowires after the activated carbon supported treatment through silane coupler
Amount, both compounding uses improve absorption of the filter material to harmful substance in air.
（3）Surface is carried out using Nano Silver loading nano titanium oxide to be modified, can expand to the utilization scope of light can
See light, the harmful substance such as micronic dust in the air for realizing decomposition filtering material Long-Term Sorption under conditions of visible light catalytic, and
And the microorganism such as bacterium, virus of growth on filtering material is decomposed in both collaborations, improves self-cleaning performance, the antibacterial of filtering material
Enduring quality, reaches long-term efficient filter effect.
（4）The present invention is added boehmite and is fabricated by filtering material using the composite fibre of PEI-boehmite,
The addition of boehmite so that tunica fibrosa surface potential increases, and its filter efficiency is improved significantly, and resistance pressure drop does not become
Change.
Specific embodiment
The standby electret PEI of a kind of electro-spinning-boehmite composite fibre filtering material, by following weight portion
Raw material components：PEI 80, silicon monoxide 8, Powdered Activated Carbon 14,3- aminopropyl triethoxysilanes coupling agent 2, ice second
Acid 1.5, appropriate deionized water, metatitanic acid 6, the AgNO of 0.6mol/L3Appropriate solution, appropriate 1-METHYLPYRROLIDONE, nanometer is vigorous
Nurse stone 2, expanded graphite 2.
Comprise the following steps that：
（1）The preparation of Ag-carried nanometer titanium dioxide：
By in metatitanic acid addition deionized water, in 0.6mol/L, be heated to 115 DEG C makes its maintain boiling, hair to control solution concentration
The raw white metatitanic acid precipitation of hydrolysis generation, centrifugal filtration, washing no longer detect SO into precipitating4 2-Ion, is immersed in
The AgNO of 0.6mol/L3In solution, calcined 1 hour at 480 DEG C after being dried at 80 DEG C, obtain Ag-carried nanometer titanium dioxide；
（2）The preparation of silicon nanowires：
The small porcelain boat that will be equipped with silicon monoxide powder is placed horizontally in the middle of alumina tube, and the pipe then is placed on into high temperature process furnances
In, vacuumize in 90Pa, then temperature is increased to 200,900 DEG C respectively and 60 minutes is incubated respectively, 1350 are warmed up to afterwards
DEG C insulation 4 hours；600 DEG C are cooled to the speed of 2 DEG C/min and be incubated 30 minutes, while blast air with 50sccm arriving afterwards
Furnace chamber, naturally cools to room temperature, obtains silicon nanowires, standby；
（3）The preparation of activated carbon supported silicon nanowires：
1. 3- aminopropyl triethoxysilane coupling agents, are added to deionized water, and pH to 4 is adjusted with a small amount of glacial acetic acid,
Stir 30 minutes at room temperature, step is added afterwards（1）The silicon nanowires for obtaining, in 95 DEG C of back flow reactions 12 hours, suction filtration, washes
Wash, dry, obtain silicon amide nanowire composite；
2. the silicon amide nanowire composite that, will obtain, Powdered Activated Carbon are added to deionized water, with ultrasonic wave 40 DEG C,
Mixed under conditions of 150W 30 minutes, static aging 24 hours at room temperature, cleaned with deionized water repeatedly to efflux in neutrality,
115 DEG C of drying 12 hours are to constant weight, then are placed in Muffle furnace 400 DEG C and are calcined 4 hours, cooling, dry, and activated carbon supported silicon is obtained
Nano wire；
（4）The preparation of spinning solution：
1., by step（1）Obtain Ag-carried nanometer titanium dioxide, step（3）Activated carbon supported silicon nanowires is obtained and adds N- methyl
In pyrrolidones, ultrasound 2 hours in ultrasonic cleaner are placed on, are set to solution A；
2., take expanded graphite and add deionized water, through sonic oscillation, form the mixed liquor of expanded graphite, add nm boehmite
Ultrasonic disperse 40 minutes, obtains well mixed dispersion liquid；
3., at ambient temperature, by PEI and 1-METHYLPYRROLIDONE with 1:4 ratio mixing, uses ParafilmTM
Bottleneck, is placed in oil bath 60 DEG C and heats 20 hours, is set to solution B, is placed on magnetic stirring apparatus and stirs, and is slowly added to above-mentioned solution
A, continues to stir 4 hours, above-mentioned dispersion liquid is continuously added afterwards and continues to stir 7 hours, is configured to the spinning solution of good fluidity；
（5）Above-mentioned spinning solution is carried out into electrostatic spinning, electrostatic spinning nano fiber electret filtering material is obtained.
Wherein, described electrostatic spinning process parameter is：Voltage is 12KV, and syringe needle is 20cm, spray to template distance is received
Silk a diameter of 0.5mm, spinning speed is 0.6mL/h, and the spinning time is 9 hours, and environment temperature is 25 DEG C, envionmental humidity
It is 55%.
Properties of product test result：
Gas permeability：186.58L/m2S, porosity：>80%, pressure drag：<20Pa, the filter efficiency to 0.006-1 μm of particle can
Up to more than 99.999%.
Claims (3)
1. the standby electret PEI of a kind of electro-spinning-boehmite composite fibre filtering material, it is characterised in that by following
The raw material components of weight portion：PEI 75-85 parts, silicon monoxide 5-10 parts, Powdered Activated Carbon 8-15 parts, 3- aminopropyls three
1-3 parts of Ethoxysilane coupling agent, glacial acetic acid 0.8-2 parts, appropriate deionized water, metatitanic acid 3-6 parts, the AgNO of 0.6mol/L3
Appropriate solution, appropriate 1-METHYLPYRROLIDONE, nm boehmite 1-2 parts, expanded graphite 1-3 parts.
2. a kind of standby electret PEI of electro-spinning according to claims 1-boehmite composite fibre filtering
The preparation method of material, it is characterised in that comprise the following steps that：
（1）The preparation of Ag-carried nanometer titanium dioxide：
By in metatitanic acid addition deionized water, in 0.4-0.7mol/L, be heated to 105-125 DEG C maintains it to control solution concentration
, there is the white metatitanic acid precipitation of hydrolysis generation in boiling, centrifugal filtration, washing no longer detect SO into precipitating4 2-Ion, leaching
AgNO of the stain in 0.6mol/L3In solution, calcined 1-2 hours at 460-490 DEG C after being dried at 70-90 DEG C, obtain carrying silver
Nano titanium oxide；
（2）The preparation of silicon nanowires：
The small porcelain boat that will be equipped with silicon monoxide powder is placed horizontally in the middle of alumina tube, and the pipe then is placed on into high temperature process furnances
In, vacuumize in 80-100Pa, then temperature is increased to 100-200,800-1100 DEG C and respectively 50-70 points of insulation respectively
Clock, is warmed up to 1300-1400 DEG C and is incubated 3-5 hours afterwards；550-650 DEG C is cooled to the speed of 1-3 DEG C/min and protect afterwards
It is warm 20-40 minutes, while blasting air to furnace chamber with 50sccm, room temperature is naturally cooled to, silicon nanowires is obtained, it is standby；
（3）The preparation of activated carbon supported silicon nanowires：
1. 3- aminopropyl triethoxysilane coupling agents, are added to deionized water, and pH to 4 is adjusted with a small amount of glacial acetic acid,
Stir 20-40 minutes at room temperature, step is added afterwards（1）The silicon nanowires for obtaining is small in 80-100 DEG C of back flow reaction 11-13
When, suction filtration, washing, drying obtain silicon amide nanowire composite；
2. the silicon amide nanowire composite that, will obtain, Powdered Activated Carbon are added to deionized water, with ultrasonic wave 40 DEG C,
Mix 20-40 minute under conditions of 150W, static aging 24 hours at room temperature, cleaned with deionized water and multiple be in efflux
Property, 110-120 DEG C of drying 10-14 hour is to constant weight, then is placed in Muffle furnace 380-420 DEG C and is calcined 3-5 hour, cools down, drying,
Activated carbon supported silicon nanowires is obtained；
（4）The preparation of spinning solution：
1., by step（1）Obtain Ag-carried nanometer titanium dioxide, step（3）Activated carbon supported silicon nanowires is obtained and adds N- methyl
In pyrrolidones, ultrasound 1-3 hours in ultrasonic cleaner is placed on, is set to solution A；
2., take expanded graphite and add deionized water, through sonic oscillation, form the mixed liquor of expanded graphite, add nm boehmite
Ultrasonic disperse 30-50 minutes, obtain well mixed dispersion liquid；
3., at ambient temperature, by PEI and 1-METHYLPYRROLIDONE with 1:The ratio mixing of 3-4, is sealed with sealed membrane
Firmly bottleneck, is placed in oil bath 55-65 DEG C and heats 18-22 hour, is set to solution B, is placed in stirring on magnetic stirring apparatus, is slowly added to
Above-mentioned solution A, continues to stir 3-5 hours, above-mentioned dispersion liquid is continuously added afterwards and continues to stir 5-8 hours, is configured to mobility
Good spinning solution；
（5）Above-mentioned spinning solution is carried out into electrostatic spinning, electrostatic spinning nano fiber electret filtering material is obtained.
3. a kind of standby electret PEI of electro-spinning according to claims 2-boehmite composite fibre filtering
The preparation method of material, it is characterised in that described electrostatic spinning process parameter is：Voltage is 1-50KV, syringe needle to reception mould
Plate distance is 0.1-2m, and spinnerette diameters are 1 μm of -2mm, and spinning speed is 0.1-20mL/h, and the spinning time is 8-10 hours, ring
Border temperature is 20-60 DEG C, and envionmental humidity is 20-80%.
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Cited By (4)
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| CN107469466A (en) * | 2017-08-10 | 2017-12-15 | 东华大学 | A kind of compound electret filtering material of micrometer fibers/nanofiber and preparation method thereof |
| CN111850824A (en) * | 2020-07-31 | 2020-10-30 | 云南电网有限责任公司电力科学研究院 | Preparation method of submicron composite film |
| CN111910344A (en) * | 2020-08-14 | 2020-11-10 | 扬州工业职业技术学院 | Preparation method of silver-loaded activated carbon antibacterial fibrous membrane |
| CN114540979A (en) * | 2022-03-04 | 2022-05-27 | 仙桃市鼎业劳保用品有限公司 | Antifouling and antibacterial fabric for protective clothing and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107469466A (en) * | 2017-08-10 | 2017-12-15 | 东华大学 | A kind of compound electret filtering material of micrometer fibers/nanofiber and preparation method thereof |
| CN107469466B (en) * | 2017-08-10 | 2019-11-08 | 东华大学 | A kind of compound electret filtering material of micrometer fibers/nanofiber and preparation method thereof |
| CN111850824A (en) * | 2020-07-31 | 2020-10-30 | 云南电网有限责任公司电力科学研究院 | Preparation method of submicron composite film |
| CN111910344A (en) * | 2020-08-14 | 2020-11-10 | 扬州工业职业技术学院 | Preparation method of silver-loaded activated carbon antibacterial fibrous membrane |
| CN111910344B (en) * | 2020-08-14 | 2021-08-31 | 扬州工业职业技术学院 | Preparation method of silver-loaded activated carbon antibacterial fibrous membrane |
| CN114540979A (en) * | 2022-03-04 | 2022-05-27 | 仙桃市鼎业劳保用品有限公司 | Antifouling and antibacterial fabric for protective clothing and preparation method thereof |
| CN114540979B (en) * | 2022-03-04 | 2023-10-13 | 江西菲力康服装有限公司 | Antifouling and antibacterial fabric for protective clothing and preparation method thereof |
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Application publication date: 20170531 |
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