CN110193235A - A kind of mineral porous microsphere based nano-fiber and preparation method thereof for air filtration - Google Patents
A kind of mineral porous microsphere based nano-fiber and preparation method thereof for air filtration Download PDFInfo
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- CN110193235A CN110193235A CN201910501023.3A CN201910501023A CN110193235A CN 110193235 A CN110193235 A CN 110193235A CN 201910501023 A CN201910501023 A CN 201910501023A CN 110193235 A CN110193235 A CN 110193235A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/02—Loose filtering material, e.g. loose fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
- B01D2239/0216—Bicomponent or multicomponent fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
- B01D2239/025—Types of fibres, filaments or particles, self-supporting or supported materials comprising nanofibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
- B01D2239/0258—Types of fibres, filaments or particles, self-supporting or supported materials comprising nanoparticles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0631—Electro-spun
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
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- Nonwoven Fabrics (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
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Abstract
The mineral porous microsphere based nano-fiber and preparation method thereof that the invention discloses a kind of for air filtration, mineral porous microsphere is wrapped in the nanofiber, forms fusiform stereochemical structure.On the one hand spun structure prepared by the present invention can intercept large particle by fiber itself, another aspect fusiform node can make the large scale hole between fiber become smaller, to realize effective absorption to fine particle.The load of this function and the spinning fibre structure that is combined as a whole of structure regulating, have that gas permeability is high, filtration pressure difference is small, PM2.5The advantage that capture rate is high and production cost is low.
Description
Technical field
The invention belongs to air filting material technical fields, and in particular to a kind of mineral porous microsphere for air filtration
Based nano-fiber and preparation method thereof.
Background technique
Electrospun fibers have the advantages that porosity height, large specific surface area, fibre diameter are controllable and ingredient is various, right
PM in environment2.5Filtering absorption aspect has good application prospect.But existing spinning fibre structure, that there is also gas permeabilities is low,
Bad mechanical property and PM2.5The problems such as capture rate is low.In PM2.5Filtering absorption aspect, temporarily can not effectively take into account high efficiency filter
It is reduced with pressure drag, the PM for inventing a kind of high-efficient low-resistance need to be explored2.5Electrospun fibers.
In order to solve the short slab of existing electrospun fibers and optimize it to PM2.5Adsorption effect is filtered, is mainly visited in document
Rope electrostatic spinning fertile material, functionalization load, variform fiber composite design its structure and filter absorption property
The relationship of promotion, such as following three examples: (1) molten by the way that low boiling point is added in spinning mother liquor in patent CN103952783A
Agent prepares the beading fibre structure of porous surface by its quick volatilization, improves strainability by specific surface area increase,
But the structure of Integrate porous keeps its mechanical performance poor and solvent volatilization limits its application the serious harm of environment；(2)
By adding magnetic nanoparticle in spinning fibre, realizes and keep the script appearance structure of fiber constant and realize functional structure
It is modified, under the action of external magnetic field, to the magnetic PM in the particular places such as high-speed rail station, subway station and steel mill2.5Particle is realized high
Effect filtering (Kim J, Hong S C, Bae G N, et al.Electrospun magnetic nanoparticle-
decorated nanofiber filter and its applications to high-efficiency air
filtration[J].Environmental Science&Technology,2017:acs.est.7b02884.).But
Need to be aided with external magnetic field, energy consumption is huge.Meanwhile the magnetic nanoparticle of addition is in process of production to the health threat of human body
It is very big；(3) it in Chinese invention patent CN109157915A and CN106237717A, separately designs and prepares variform fiber composite
Continuous multilayer fibrillar meshwork structure and " sandwich " formula solid cavity interlayer structure, propose spinning fibre filter efficiency
It rises, but on the one hand multilayer labyrinth makes it there are filtration pressure differences big, on the other hand the disadvantages such as gas permeability is low have preparation process
The problems such as complicated and at high cost, limits its application in actual production.
Summary of the invention
The complicated, PM for existing electrostatic spinning filter fiber material2.5Capture rate is low, gas permeability is low, filtration pressure difference is big asks
Topic, the purpose of the invention is to provide a kind of for the mineral porous microsphere based nano-fiber of air filtration and its preparation side
Mineral porous microsphere is wrapped in spinning fibre by electrostatic spinning, forms integrated fusiform stereochemical structure by method.This hair
On the one hand the spun structure of bright preparation can intercept large particle by fiber itself, another aspect fusiform node can make
Large scale hole between fiber becomes smaller, to realize effective absorption to fine particle.The load of this function and structure regulating knot
The spinning fibre structure being integrated, has that gas permeability is high, filtration pressure difference is small, PM2.5It is excellent that capture rate is high and production cost is low
Point.
In order to achieve the above technical purposes, the present invention adopts the following technical scheme:
A kind of mineral porous microsphere based nano-fiber for air filtration, mineral porous microsphere are wrapped in the Nanowire
In dimension, fusiform stereochemical structure is formed.
Preferably, the mineral porous microsphere is selected from one of galapectite, sepiolite and attapulgite microballoon, microballoon
Partial size is 2~4 μm.
Mineral porous microsphere of the present invention can be by existing any feasible technology such as spray granulation, chemistry from group
The synthesis such as dress method, recycles natural subsidence-centrifuge separation to control and screen Microsphere Size.
Preferably, in the mineral porous microsphere based nano-fiber, mineral porous microsphere quality accounting is 5~11wt%.
It is furthermore preferred that mineral porous microsphere quality accounting is 7wt% in the mineral porous microsphere based nano-fiber.
Preferably, the nanofiber diameter range is 0.7~0.94 μm.
Preferably, the mineral porous microsphere based nano-fiber specific surface area is 2~4m2/ g, fiber pore volume are 0.007
~0.01cm3/ g, hole average-size are 13~17nm, and surface is hydrophobicity, and static contact angle is 110~125 °.
Preferably, the mineral porous microsphere based nano-fiber is used for the PM of low concentration2.5The filtering of environment is adsorbed, filtering
Adsorption efficiency is 91.34~99.1%, and pressure drag is 111.8~113.4Pa.
The present invention also provides the preparation methods of above-mentioned mineral porous microsphere based nano-fiber, and polycaprolactone (PCL) is molten
Spinning mother liquor is formed in trifluoroethanol；Mineral porous microsphere is added in spinning mother liquor again, before stirring 12~formation spinning for 24 hours
Body is driven, the mineral porous microsphere based nano-fiber with fusiform node is prepared by electrostatic spinning.
Preferably, mass fraction of the polycaprolactone in spinning mother liquor is 10~15wt%, mineral porous microsphere
Mass ratio with polycaprolactone is 5~11:89~95.
Preferably, the electrospinning conditions are as follows: 12~15kV of spinning voltage, stoking rate are 0.003~0.005mm/
Min, syringe needle between roller at a distance from be 15~20cm, the revolving speed of roller is 100~150rpm, ambient humidity 25~30%, ring
30~40 DEG C of border temperature.
Compared with prior art, advantages of the present invention with have the beneficial effect that:
(1) present invention utilizes mineral porous microsphere for the first time, using polycaprolactone (PCL) organic polymer as the support of microballoon
Framework, in three-dimensional space, the filter membrane for form that a step prepares microballoon and spinning fibre is structure as a whole.
(2) simple process of the invention is controllable.It on the one hand, can be porous to mineral by natural subsidence-centrifugal
Microballoon is screened, and the size of spinning node is regulated and controled；On the other hand, further right by controlling the volume of mineral porous microsphere
The node density of spinning fibre and porosity etc. are adjusted, and are accurately controlled to realize to the design of spinning micro nano structure
System.
(3) electrospun fibrous structure is designed using mineral porous microsphere, the equally distributed spinning of preparation
Node can increase the structural strength of fibrous filter membrane, facilitate the service life for increasing fiber.Meanwhile fiber package mineral are porous micro-
The integral structure of ball maintains the good gas permeability of fibrous filter membrane, and practical application has good prospect.
(4) it is being used for PM2.5On the one hand the presence of filtering aspect, mineral porous microsphere can prop up Fiber Laminated network knot
Structure increases interlamellar spacing, so as to expand the volume of fiber and increase dust containing capacity；On the other hand, the spinning that mineral porous microsphere is constituted
Silk node can be realized with fiber itself to PM2.5Large or fine granule form multistage filtering, and have the filterability of efficient stable
Energy.
Detailed description of the invention
The SEM electron microscope of sample made from Fig. 1 comparative example 1 of the present invention；
The SEM electron microscope of sample made from Fig. 2 embodiment of the present invention 2；
The graph of pore diameter distribution of sample made from Fig. 3 comparative example 1 of the present invention and embodiment 1-3；
The TEM electron microscope of sample made from Fig. 4 embodiment of the present invention 2；
The filter efficiency and pressure drag comparison diagram of sample made from Fig. 5 comparative example 1 of the present invention and embodiment 1-3.
Specific embodiment
The present invention is further elaborated in the following with reference to the drawings and specific embodiments, it is intended that keep technology of the invention special
Property, protocol procedures and innovative point are clearer.Meanwhile it will be understood that this specific embodiment, which is only played, plays explanation to the present invention
Illustration, after other all readings are of the invention, the related amendments or improvement that related technical personnel do on this basis are equally fallen into
In applied protection scope of the invention.
Embodiment 1
(1) polycaprolactone is dissolved in trifluoroethanol, stirs 3h at normal temperature, be made into electrostatic spinning solution.Wherein, gather
The mass fraction of lactone is 15wt%.
(2) HNTs porous microsphere is centrifugally separating to obtain the microballoon having a size of 3 μm or so through natural subsidence-, in mass ratio
HNTs porous microsphere: pla-pcl=5:95 is added into above-mentioned spinning solution, ultrasonic disperse 30min, magnetic agitation 3h, repeatedly
3 times, obtain spinning presoma.Wherein, natural subsidence 2min collects its supernatant, and 8000rpm centrifugation 3min collects its precipitating.
(3) preparation that fusiform node spinning fibre film is carried out using electrospinning device, is denoted as 5-HNTs.Wherein, quiet
Electrospinning process parameter is as follows: spinning voltage 12kV, drum rotation speed 100rpm, and receiving distance is 15cm, and syringe needle size is 19#,
Feed flow rate 0.003mm/min, ambient humidity 25%, 30 DEG C of environment temperature.
The 5-HNTs fusiform node spinning fibre film prepared according to above-mentioned process conditions, is measured its nanofiber
Average diameter be 0.94 μm, the specific surface area of spinning fibre is 2.01m2/ g, fiber pore volume are 0.008419cm3/ g, spinning
The average pore size of fiber is 16.78nm, and spinning fibre film surface is hydrophobicity, and static contact angle is 117 °.
Embodiment 2
(1) polycaprolactone is dissolved in trifluoroethanol, stirs 3h at normal temperature, be made into electrostatic spinning solution.Wherein, gather
The mass fraction of lactone is 15wt%.
(2) HNTs porous microsphere is centrifugally separating to obtain the microballoon having a size of 3 μm or so through natural subsidence-, in mass ratio
HNTs porous microsphere: pla-pcl=7:93 is added into above-mentioned spinning solution, ultrasonic disperse 30min, magnetic agitation 3h, repeatedly
3 times, obtain spinning presoma.Wherein, natural subsidence 3min collects its supernatant, and 8000rpm centrifugation 4min collects its precipitating.
(3) preparation that fusiform node spinning fibre film is carried out using electrospinning device, is denoted as 7-HNTs.Wherein, quiet
Electrospinning process parameter is as follows: spinning voltage 15kV, drum rotation speed 100rpm, and receiving distance is 20cm, and syringe needle size is 19#,
Feed flow rate 0.005mm/min, ambient humidity 30%, 37 DEG C of environment temperature.
The 7-HNTs fusiform node spinning fibre film prepared according to above-mentioned process conditions, is measured its nanofiber
Average diameter be 0.84 μm, the specific surface area of spinning fibre is 3.01m2/ g, fiber pore volume are 0.009837cm3/ g, spinning
The average pore size of fiber is 13.09nm, and spinning fibre film surface is hydrophobicity, and static contact angle is 112 °.
Embodiment 3
(1) polycaprolactone is dissolved in trifluoroethanol, stirs 3h at normal temperature, be made into electrostatic spinning solution.Wherein, gather
The mass fraction of lactone is 15wt%.
(2) HNTs porous microsphere is centrifugally separating to obtain the microballoon having a size of 3 μm or so through natural subsidence-, in mass ratio
HNTs porous microsphere: pla-pcl=9:91 is added into above-mentioned spinning solution, ultrasonic disperse 30min, magnetic agitation 3h, repeatedly
3 times, obtain spinning presoma.Wherein, natural subsidence 2min collects its supernatant, and 8000rpm centrifugation 3min collects its precipitating.
(3) preparation that fusiform node spinning fibre film is carried out using electrospinning device, is denoted as 9-HNTs.Wherein, quiet
Electrospinning process parameter is as follows: spinning voltage 15kV, drum rotation speed 100rpm, and receiving distance is 20cm, and syringe needle size is 19#,
Feed flow rate 0.005mm/min, ambient humidity 30%, 37 DEG C of environment temperature.
The 9-HNTs fusiform node spinning fibre film prepared according to above-mentioned process conditions, is measured its nanofiber
Average diameter be 0.89 μm, the specific surface area of spinning fibre is 2.15m2/ g, fiber pore volume are 0.00767cm3/ g, spinning
The average pore size of fiber is 14.259nm, and spinning fibre film surface is hydrophobicity, and static contact angle is 121 °.
Comparative example 1
(1) polycaprolactone (PCL) is dissolved in trifluoroethanol, stirs 3h at normal temperature, is made into electrostatic spinning solution.Its
In, the mass fraction of pla-pcl is 15wt%.
(2) preparation of pure PCL spinning fibre film is carried out using electrospinning device.Wherein, electrostatic spinning process parameter is such as
Under: spinning voltage 12kV, drum rotation speed 100rpm, receiving distance is 15cm, and syringe needle size is 20#, feed flow rate 0.003mm/
Min, ambient humidity 25%, 30 DEG C of environment temperature.
The pure PCL spinning fibre film prepared according to above-mentioned process conditions, through measuring the average diameter of its nanofiber
It is 0.71 μm, the specific surface area of spinning fibre is 1.68m2/ g, fiber pore volume are 0.005586cm3/ g, spinning fibre are averaged
Aperture is 13.32nm, and spinning fibre film surface is hydrophobicity, and static contact angle is 128 °.
Embodiment 4
Sample made from embodiment 1-3 and comparative example 1 is applied to the PM of low concentration2.5The filtering of environment is adsorbed, described low dense
The PM of degree2.5Environment refers to PM2.5Environment of the performance figure (AQI) between 300-350.
In PM2.5Under the experimental situation that performance figure is 330.4, sample mistake made from testing example 3-5 and comparative example 1
Filter preceding and filtered PM2.5Mass concentration, meanwhile, test the pressure difference of its filtering front and back tunica fibrosa.
The filtering adsorption efficiency of the HNTs porous microsphere base spinning fibre film is 91.34~99.1%, and pressure drag is
111.8~113.4Pa.
The filtering adsorption efficiency of the pure PCL spinning fibre film is 88.86%, pressure drag 114Pa.
Fig. 1 and Fig. 2 is the SEM electron microscope of pure PCL and 7-HNTs fusiform node tunica fibrosa respectively.Analysis obtains, pure PCL
Aperture size between spinning membrane fiber is larger, and in 7-HNTs fusiform node spinning film, interfibrous aperture size is obvious
It reduces, this is because node is evenly distributed on spinning fibre, caused by the compactness for increasing spinning film.
Fig. 3 is the graph of pore diameter distribution of spinning fibre film.The pore-size distribution it is found that pure PCL tunica fibrosa itself is analyzed from figure
Wider range, aperture mean value are 13.32nm.After adding HNTs microballoon preparation fusiform node, the small hole number of tunica fibrosa increases
More, pore-size distribution region becomes to concentrate, and concentrates on being less than at the mean value of pure PCL fiber aperture.This is because the spindle in fiber
The presence of shape node, can be become smaller with the big hole between fill fiber, pore-size so that tunica fibrosa small hole number
Increase, pore-size distribution is also concentrated to the direction that becomes smaller.This is consistent with the result observed in SEM figure, illustrates that micro nano structure designs
The fusiform fibre structure of preparation has the smaller more uniform advantage of aperture size, is conducive to PM2.5The filtering of particle with block
It cuts.
Fig. 4 is the TEM transmission electron microscope picture of 7-HNTs fusiform node tunica fibrosa, it can be observed that spinning polymer PCL will
HNTs microballoon is uniformly wrapped in its fiber, illustrates that it constructs the integrated spindle-shaped structure of fiber package microballoon.In this way
Structure can increase the mechanical property of fibrous filter membrane, facilitate the service life for increasing fiber.
Fig. 5 is spinning fibre film PM2.5Filter efficiency and pressure drag graph of relation.As shown in Figure 5, pure PCL, 5-
HNTs, 7-HNTs and 9-HNTs spinning fibre film filter efficiency are respectively 88.86,91.34,99.1 and 93%, and its pressure difference hinders
Power is respectively 114,113.4,112.5 and 111.8Pa.Analysis is it is found that fusiform node tunica fibrosa prepared by addition HNTs microballoon
To PM2.5Strainability be obviously improved.Meanwhile the purer PCL spinning film of pressure drag has reduction by a small margin, illustrates it
It maintains and suitably improves the permeability of tunica fibrosa.
Conclusions explanation carries out micro nano structure design using mineral porous microsphere, can construct integrated fusiform
Node fibre structure.This structure, can be in the case where maintaining even appropriate reduction filtration pressure difference resistance, significantly compared with fibrillar structure
It is promoted to PM2.5The filter effect of particle, helps to solve current spinning fibre to cannot be considered in terms of the difficulty of high efficiency filter and gas permeability
Topic.
Claims (10)
1. a kind of mineral porous microsphere based nano-fiber for air filtration, it is characterised in that: mineral porous microsphere is wrapped in
In the nanofiber, fusiform stereochemical structure is formed.
2. the mineral porous microsphere based nano-fiber according to claim 1 for air filtration, it is characterised in that: described
Mineral porous microsphere be selected from one of galapectite, sepiolite and attapulgite microballoon, microspherulite diameter is 2~4 μm.
3. the mineral porous microsphere based nano-fiber according to claim 1 for air filtration, it is characterised in that: described
In mineral porous microsphere based nano-fiber, mineral porous microsphere quality accounting is 5~11wt%.
4. porous microsphere based nano-fiber according to claim 3, it is characterised in that: the mineral porous microsphere base nanometer
In fiber, mineral porous microsphere quality accounting is 7wt%.
5. the mineral porous microsphere based nano-fiber according to claim 1 for air filtration, it is characterised in that: described
Nanofiber diameter range is 0.7~0.94 μm.
6. the mineral porous microsphere based nano-fiber according to claim 1 for air filtration, it is characterised in that: described
Mineral porous microsphere based nano-fiber specific surface area is 2~4m2/ g, fiber pore volume are 0.007~0.01cm3/ g, Kong Pingjun ruler
Very little is 13~17nm, and surface is hydrophobicity, and static contact angle is 110~125 °.
7. the mineral porous microsphere based nano-fiber according to claim 1 for air filtration, it is characterised in that: described
Mineral porous microsphere based nano-fiber is used for the PM of low concentration2.5The filtering of environment is adsorbed, and filtering adsorption efficiency is 91.34~
99.1%, pressure drag is 111.8~113.4Pa.
8. the preparation method of the described in any item mineral porous microsphere based nano-fibers for air filtration of claim 1-7,
It is characterized by: polycaprolactone is dissolved in formation spinning mother liquor in trifluoroethanol；Spinning mother liquor is added in mineral porous microsphere again
In, the mineral porous microsphere with fusiform node is prepared by electrostatic spinning in stirring 12~form spinning presoma for 24 hours
Based nano-fiber.
9. the preparation method of the mineral porous microsphere based nano-fiber according to any one of claims 8 for air filtration, feature exist
In: mass fraction of the polycaprolactone in spinning mother liquor be 10~15wt%, mineral porous microsphere and polycaprolactone
Mass ratio is 5~11:89~95.
10. the preparation method of the mineral porous microsphere based nano-fiber according to any one of claims 8 for air filtration, feature exist
In: the electrospinning conditions are as follows: 12~15kV of spinning voltage, stoking rate are 0.003~0.005mm/min, syringe needle and rolling
Distance between cylinder is 15~20cm, and the revolving speed of roller is 100~150rpm, ambient humidity 25~30%, environment temperature 30~40
℃。
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