CN107081008B - Polyolefin film-fibre and preparation method and electret air filtering material prepared therefrom - Google Patents
Polyolefin film-fibre and preparation method and electret air filtering material prepared therefrom Download PDFInfo
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- CN107081008B CN107081008B CN201710222663.1A CN201710222663A CN107081008B CN 107081008 B CN107081008 B CN 107081008B CN 201710222663 A CN201710222663 A CN 201710222663A CN 107081008 B CN107081008 B CN 107081008B
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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
- B01D39/04—Organic material, e.g. cellulose, cotton
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/42—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments
- D01D5/423—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments by fibrillation of films or filaments
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
-
- 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
Abstract
The present invention provides a kind of preparation method of polyolefin film-fibre, comprising the following steps: polyolefin flat filament is successively carried out to sided corona treatment, liquid-phase fluorination processing, fibrillation processing, finally winds, prepares polyolefin film-fibre.Sided corona treatment first is carried out to polyolefin flat filament, liquid-phase fluorination processing is then carried out in fluoride solvent, the rate of fluorination reaction is greatly improved, and form fluorinated layer in homogeneous thickness in polyolefin surfaces, improves the solvent resistance of polyolefin film-fibre.The present invention prepares electret air filtering material as basis material using polyolefin film-fibre, and the filter efficiency of obtained electret air filtering material is high, resistance is small, persistence is long, extends the application field of polyolefine material.
Description
Technical field
The present invention relates to thermoplastic polyolefin fibers fields, and in particular to a kind of film-fibre and preparation method thereof.
Background technique
Polyolefin film-fibre is using plastic film after high power longitudinal stretching, and lateral strength is down to the limit, has
Voluntarily cleave into the intrinsic characteristic of fiber, then a kind of fiber through mechanically or chemically handling.Polyolefin film-fibre
After steam softening, curling, being chopped, it is prepared into non-woven fabrics, has the advantages that efficient low-resistance, is highly suitable to be applied for air filtration
Field.
But polyolefine material such as polyethylene, polypropylene etc. is for the corrosion resistant of the nonpolar solvents such as alkane, aromatic hydrocarbons, gasoline
Corrosion is very poor, is easy to appear swelling set phenomenon, and in some special environment, such as gas station, chemical laboratory, air
In often contain a large amount of volatile solvent, which greatly limits polyolefine material field of air filtration application range and use
Service life.Fluorinated modified polyolefine material can solve the above problems to a certain degree, and existing reported in literature uses strong fluorization agent at present
Fluorine gas carries out gas phase fluorination processing to polyolefin plastics, and the anti-permeability of solvent of polyolefin, still, gas phase fluorination can be improved in this method
Acutely, reaction process is not easy to control, and when the content of fluorine in mixed gas is higher, polyolefin is reacted with fluorine gas to be fired for reaction
Phenomenon is burnt, risk is big；Separately there is reported in literature that fluorine gas is dissolved in solvent appropriate and handles frosting (referred to as solvent
Fluoride process), the reaction of solvent fluoride process is more mild, and still, reaction rate is slower, and conversion ratio is extremely low, is unable to satisfy industrialization and wants
It asks.In addition, there is also influence effectively making for its electret air filtering material because charge stability is not good enough for polypropylene based material
The problem of with service life and filter efficiency.
Summary of the invention
Existing polyolefine material and its electret air filtering material there are aiming at the problem that, the present invention provides a kind of poly-
Alkene film-fibre and preparation method thereof, the film-fibre have good solvent resistance, and this method reacts mild, reaction rate
It is moderate, and prepare electret air filtering material with film-fibre of the invention, can make filtering material reach filter efficiency it is high,
The effect that resistance is small, persistence is long.
A kind of preparation method of polyolefin film-fibre, comprising the following steps:
(1) at least one side of polyolefin flat filament sided corona treatment: is subjected to online sided corona treatment, polyolefin flat filament and electrode bar
Between gap be 1~5mm, processing voltage be 2000~15000V, current strength be 2~10A；
(2) liquid-phase fluorination is handled: the polyolefin flat filament that step (1) obtains is carried out fluorination reaction in fluoride solvent；
(3) fibrillation: the polyolefin flat filament that step (2) is obtained carries out mechanical fibrillation processing, then winds, prepares
Polyolefin film-fibre.
Polyolefin flat filament described in step (1) is 0.5~7.0g/min by melt index, and isotacticity is greater than 95% polyene
Hydrocarbon raw material is prepared；It is preferred that the polyolefin flat filament is 2.5~5.0g/min by melt index, isotacticity is 96~98%
Polyolefinic raw materials are prepared.
The polyolefinic raw materials include at least one of polyethylene, polypropylene, may also include polybutene, polypenthylene, second
Alkene and one of butylene or octene copolymer (POE) are a variety of.
Polyolefin flat filament described in further preferred step (1) is linear low density polyethylene to be blended with isotactic polypropylene
The blend of object or isotactic polypropylene and POE squeezed out casting film-forming, cut into narrowband, longitudinal hot-stretch, thermal finalization processing and
At wherein isotactic polypropylene mass content accounts for the 70%~90% of blend total amount.
Polyolefin flat filament described in step (1) with a thickness of 1~100 μm.
The width of polyolefin flat filament described in step (1) is 5~30mm.
The temperature of polyolefin flat filament described in step (1) is 100 DEG C~130 DEG C.
Polyolefin flat filament described in step (1) carries out online sided corona treatment under the traction of deflector roll, and the linear velocity of deflector roll is
90m/min~200m/min.
Sided corona treatment described in step (1) can carry out single or double sided corona treatment to polyolefin flat filament；It is preferred that polyene
Hydrocarbon flat filament carries out two-sided sided corona treatment.
Polyolefin flat filament described in step (2) carries out online liquid-phase fluorination processing, the linear speed of deflector roll under the traction of deflector roll
It spends identical as the linear velocity of sided corona treatment.
Fluoride solvent described in step (2) is totally submerged polyolefin flat filament.
Nitrogen and fluorine gas are continually fed into preferred steps (2) described fluoride solvent, the delivery of fluorine/nitrogen mixed gas is led to
Entering rate is 0.1~5L/min.
The concentration of fluorine gas is 0.2~2mmol/L in fluoride solvent described in step (2).
The volume content of fluorine gas is 1~10%, preferably 3~6% in delivery of fluorine/nitrogen mixed gas described in step (2).
The temperature of fluorination reaction described in step (2) is 20~70 DEG C.
Solvent described in step (2) includes one or more of fluorination butane, fluorination pentane, fluorination hexane, preferably fluorine
Change butane.
The fluorination butane refers to X1-Y1-Y2-X2, X1For CH3、CF3Or CHF2Group；X2For CHF2Or CH2F group, Y1
For CF2、CH2Or CHF group, Y2For CF2、CH2Or CHF group.
The fluorination pentane refers to X1-Y1-Y2-Y3-X2, X1For CF3Or CH2F group；X2For CH3、CF3、CH2F or CHF2
Group；Y1For CF2、CH2Or CHF group, Y2For CF2、CH2Or CHF group, Y3For CF2、CH2Or CHF group.
The fluorination hexane refers to CF3-(CF2)m-Xn-Y(4-m-n)- Z, m are 2 or 3；N is 0 or 1；X is CHF or CH2, Y
For CHF or CH2, Z CH3、CF3Or CHF2。
Fibrillation described in step (3) refers to that polyolefin flat filament after the porcupine roller of fast turn-around punctures cracking, is then formed
Surface has the irregular fiber of many micro fibers.
It is preferred that being pre-processed before the sided corona treatment, the pretreatment, which refers to, is sprayed in pretreatment box using alcohol fluid
Penetrate the surface of impact polyolefin flat filament.
The alcohol includes ethyl alcohol, isopropanol, one or more in n-butanol.
2~10 groups of horizontal spray heads are set in the pretreatment box, the jet velocity of alcohol fluid is 0.5~1.5m/min,
Jet pressure is 100~1000psi.
The pretreatment box exit is equipped with drying unit, can completely remove the liquid on flat bar surface, continuously enter electricity
Dizzy processing unit.
The present invention also provides the polyolefin film-fibres prepared by the above method.
The present invention also provides the electret air filtering materials including said polyolefins film-fibre.
The electret air filtering material is prepared by following steps:
(1) by said polyolefins film-fibre through boundling, seal wire, steam softening, curling, traction tension force and cutting
Afterwards, chopped film-fibre is prepared；
(2) film-fibre is chopped through two pass shredding, combing, lapping, needle thorn, thermal finalization, electret processing and winding, is prepared
Electret air filtering material.
Beneficial effects of the present invention:
(1) present invention forms fluorinated layer on the surface of polyolefin flat filament by fluorination reaction, therefore film-fibre is resistance to
Solvent borne has significant raising；Electret air filtering material is prepared as substrate by the film-fibre, filter efficiency is high, resistance
Power is small, and persistence is long.
(2) present invention carries out sided corona treatment to polyolefin flat filament, greatly improves the speed of fluorination reaction before fluorination reaction
Rate solves the problems, such as that liquid-phase fluorination rate is too slow in the prior art.
(3) when the gap between polyolefin flat filament and electrode bar is 1~5mm, processing voltage is 2000~15000V, and electric current is strong
When degree is 2~10A, is conducive in subsequent fluorination process, forms fluorinated layer in homogeneous thickness on the surface of polyolefin flat filament, and not
Influence the mechanical performance of film-fibre.
(4) polyolefin flat filament is first pre-processed before corona in the present invention, and sided corona treatment efficiency can be improved and fluorination is anti-
Answer rate.
(5) present invention successively carries out at online sided corona treatment and liquid-phase fluorination in the preparation process of polyolefin film-fibre
Reason controls the time of corona and fluorination treatment by adjusting the linear velocity of deflector roll, improves industrial continuity, also keep away
Exempted from the sided corona treatment effect of polyolefin flat filament because standing time is too long fail the problem of；By the temperature for improving polyolefin flat filament
Degree, can make polyolefin flat filament obtain good corona effects under higher deflector roll linear velocity, solve sided corona treatment time mistake
The problem of growing and damaging fibre structure.
Specific embodiment
Below with reference to embodiment, the present invention and its advantages are described in further detail, but implementation of the invention
Mode is without being limited thereto.
The test method of polyolefin film-fibre:
(1) breaking strength, elongation and initial modulus are referring to " GB/T19975-2005 high-strength chemical-fibre filament draw performance examination
Proved recipe method " standard testing, wherein two collet gauges be 250mm, extension speed be 250mm/min, pre-tension 5cN.
(2) the fibrillation index in " evaluation of Lyocell fiber original fiber degree " of fibrillation index reference Yang Xuhong
Subjective estimate method is measured.
(3) solvent resistance is tested: selected solvent is ethyl alcohol and acetone, and purity is that analysis is pure, and polyolefin film-fibre is put
Enter and taken out after impregnating 72h in above-mentioned solvent, room temperature dries, and tests breaking strength and initial modulus.
The test method of non-woven fabric air filtering material:
(1) filter efficiency: referring in " GB 2626-2006 protective respirator suction-self filtering type against particle respirator "
Section 6.3, standard is tested.
(2) gas-flow resistance: referring to Section 5.4 in " GB 19083-2010 medical protective mask technical requirements " of standard into
Row test, wherein select 0.3 μm of NaCl particle, gas flow 30L/min, test ambient temperature and humidity be respectively 23 DEG C and
30%.
(3) persistence is tested: after measurement is placed 30,90,180 and 360 days respectively, the mistake of electret air filtering material
Filter the situation of change of efficiency and resistance.
Embodiment 1
A. sided corona treatment
By with a thickness of 3 μm, width 20mm, POE (ethylene and butylene copolymer) toughening that temperature is 100 DEG C polypropylene
Flat filament (polyacrylic mass content is 70%) carries out two-sided sided corona treatment, used POE (second online under the traction of deflector roll
Alkene and butylene copolymer) and the melt index of pp material be 0.5g/min, isotacticity is 98%, the linear velocity of deflector roll
For 200m/min, the electrode bar of corona treatment and the gap of flat filament are 3mm, and processing voltage is 5000V, current strength 5A.
B. liquid-phase fluorination is handled
The delivery of fluorine/nitrogen mixed gas that content of fluorine is 3% is entered into pipe from the gas of fluorination case liquid bath bottom and is passed through Sheng
There is solvent C F3CF2CHFCH2F and CF3CF2(CHF)2CH320 DEG C of liquid baths in, until the concentration of fluorine gas in a solvent reaches
2mmol/L.The complete flat filament of above-mentioned sided corona treatment enters fluorination case online under the traction of deflector roll and carries out liquid phase fluorination reaction, fluorination
The volume of case is 50L, and the mixed gas of delivery of fluorine/nitrogen is continuously passed through into fluorination case, and the supplement rate of mixed gas is 2L/
Min, while the solvent in liquid bath being exported with 200mL/min rate from the drain pipe of liquid bath bottom, and the benefit in the middle part of liquid bath
Liquid mouth adds solvent.
C. fibrillation
By the flat filament after above-mentioned fluorination treatment through pin density be 75 needles/cm, linear velocity be 260m/min fibrillating roller into
Row mechanical membrane splits fibre, and the angle of needle and film traffic direction is 70 °, and the then thermal finalization at 110 DEG C is made polyolefin film and splits
Fiber.
Comparative example 1-1
It is other to prepare polyolefin film by the material and step of embodiment 1 and split without sided corona treatment in this comparative example
Fiber.
Comparative example 1-2
This comparative example carries out liquid phase fluorination reaction online under the traction of deflector roll, leads without sided corona treatment, flat filament
The linear velocity of roller is 100m/min (extending the fluorination time), and the linear velocity of fibrillating roller is 130m/min, other to press embodiment 1
Material and step prepare polyolefin film-fibre.
Comparative example 1-3
This comparative example is other to prepare polyolefin film by the material and step of embodiment 1 without liquid-phase fluorination processing
Split fiber.
Comparative example 1-4
Both without sided corona treatment in this comparative example, also without liquid-phase fluorination processing, other materials by embodiment 1
Material and step prepare polyolefin film-fibre.
Embodiment 2
Increase pre-treatment step in the present embodiment before fluorination treatment, other materials and step by embodiment 1 prepare poly-
Alkene film-fibre.Pretreatment: polyolefin flat filament is entered in pretreatment box online by deflector roll, 10 groups are arranged in pretreatment box
Horizontal spray head, the vertical range with polyolefin flat filament are 20cm, contain nozzle, nozzle diameter 0.5mm, the work of nozzle in spray head
Make width covering polyolefin flat filament entire width, use jet velocity for 0.5m/min, jet pressure for 100psi ethyl alcohol,
The fluid-mixing (volume ratio=1:1) of isopropanol impacts flat filament, and pretreatment box outlet is equipped with the air-dry machine with heating function, will be flat
The liquid in silk table face is thoroughly blown off, is respectively provided with pipeline and collecting tank below the bottom of pretreatment box and air-dry machine, passes through boiling
Point is different, and heating recovery alcohols drains micro-moisture.
Embodiment 3
Increase pre-treatment step in the present embodiment before fluorination treatment, other materials and step by embodiment 1 prepare poly-
Alkene film-fibre.Pretreatment: polyolefin flat filament is entered in pretreatment box online by deflector roll, 2 groups are arranged in pretreatment box
Horizontal spray head, the vertical range with polyolefin flat filament are 20cm, contain nozzle in spray head, nozzle diameter 10.0mm, nozzle
Working width cover polyolefin flat filament entire width, use jet velocity for 1.5m/min, jet pressure for 1000psi just
Butanol fluid impact flat filament, pretreatment box outlet are equipped with the air-dry machine with heating function, the liquid on flat filament surface are thoroughly blown off,
It is respectively provided with pipeline and collecting tank below the bottom of pretreatment box and air-dry machine, passes through boiling point difference, heating recovery alcohols, row
Walk micro-moisture.
Embodiment 4
A. sided corona treatment
It will be carried out online under the traction of deflector roll with a thickness of 1 μm, width 5mm, the polypropylene flat-filament that temperature is 110 DEG C double
The melt index of face sided corona treatment, used pp material is 2.5g/min, and the linear velocity of isotacticity 96%, deflector roll is
90m/min, the electrode bar of corona treatment and the gap of flat filament are 5mm, and processing voltage is 15000V, current strength 10A.
B. liquid-phase fluorination is handled
The delivery of fluorine/nitrogen mixed gas that content of fluorine is 6% is entered into pipe from the gas of fluorination case liquid bath bottom and is passed through Sheng
There is solvent C F3(CF2)2(CH2)2CF370 DEG C of liquid baths in, until the concentration of fluorine gas in a solvent reaches 2mmol/L.Above-mentioned corona
The flat filament handled enters fluorination case online under the traction of deflector roll and carries out liquid phase fluorination reaction, and the volume for being fluorinated case is 50L, to
The mixed gas of delivery of fluorine/nitrogen is continuously passed through in fluorination case, the supplement rate of mixed gas is 5L/min, while will be in liquid bath
Solvent is exported with 500mL/min rate from the drain pipe of liquid bath bottom, and the fluid infusion in the middle part of liquid bath adds solvent.
C. fibrillation
By the flat filament after above-mentioned fluorination treatment through pin density be 75 needles/cm, linear velocity be 126m/min fibrillating roller into
Row mechanical membrane splits fibre, and the angle of needle and film traffic direction is 75 °, and the then thermal finalization at 120 DEG C is made polyolefin film and splits
Fiber.
Comparative example 4-1
Polypropylene flat-filament with a thickness of 120 μm, width 40mm, other materials by embodiment 4 in this comparative example
Polyolefin film-fibre is prepared with step.
Embodiment 5
A. sided corona treatment
By with a thickness of 100 μm, width 20mm, polyethylene flat filament that temperature is 100 DEG C under the traction of deflector roll online into
The two-sided sided corona treatment of row, used polyethylene raw material are linear low density polyethylene, melt index 5.0g/min, isotactic
Degree is 95.5%, and the linear velocity of deflector roll is 90m/min, and the electrode bar of corona treatment and the gap of flat filament are 1mm, handles voltage
For 2000V, current strength 2A.
B. liquid-phase fluorination is handled
The delivery of fluorine/nitrogen mixed gas that content of fluorine is 10% is entered into pipe from the gas of fluorination case liquid bath bottom and is passed through Sheng
There is solvent (CHF2)CH2CH2CHF2、CH2FCF2CH2CF2CH3And CF3(CF2)3CHFCH345 DEG C of liquid baths in, until fluorine gas is molten
Concentration in agent reaches 0.2mmol/L.The complete flat filament of above-mentioned sided corona treatment enters fluorination case online under the traction of deflector roll to carry out
Liquid phase fluorination reaction, the volume for being fluorinated case is 50L, and the mixed gas of delivery of fluorine/nitrogen, mixed gas are continuously passed through into fluorination case
Supplement rate be 0.1L/min, while by the solvent in liquid bath with 20mL/min rate from the drain pipe of liquid bath bottom export,
And the fluid infusion in the middle part of liquid bath adds solvent.
C. fibrillation
By the flat filament after above-mentioned fluorination treatment through pin density be 30 needles/cm, linear velocity be 135m/min fibrillating roller into
Row mechanical membrane splits fibre, and the angle of needle and film traffic direction is 50 °, and the then thermal finalization at 130 DEG C is made polyolefin film and splits
Fiber.
Comparative example 5-1
When polyolefin carries out sided corona treatment in this comparative example, the electrode bar of corona treatment and the gap of flat filament are
8mm, processing voltage are 1000V, current strength 1A, other to prepare polyolefin film-fibre by the material and step of embodiment 5.
Embodiment 6
A. sided corona treatment
By with a thickness of 30 μm, width 30mm, the poly 1-butene toughening that temperature is 130 DEG C polypropylene flat-filament (polypropylene
Mass content be 90%) carry out single side sided corona treatment, used poly 1-butene and polypropylene online under the traction of deflector roll
The melt index of raw material is 7.0g/min, and isotacticity is 99%, and the linear velocity of deflector roll is 90m/min, corona treatment
The gap of electrode bar and flat filament is 4mm, and processing voltage is 12000V, current strength 5A.
B. liquid-phase fluorination is handled
The delivery of fluorine/nitrogen mixed gas that content of fluorine is 1% is entered into pipe from the gas of fluorination case liquid bath bottom and is passed through Sheng
There is solvent C F3(CHF)2CF360 DEG C of liquid baths in, until the concentration of fluorine gas in a solvent reaches 1.2mmol/L.At above-mentioned corona
The flat filament managed enters fluorination case online under the traction of deflector roll and carries out liquid phase fluorination reaction, and the volume for being fluorinated case is 50L, to fluorine
Change the mixed gas that delivery of fluorine/nitrogen is continuously passed through in case, the supplement rate of mixed gas is 2.2L/min, while will be in liquid bath
Solvent is exported with 80mL/min rate from the drain pipe of liquid bath bottom, and the fluid infusion in the middle part of liquid bath adds solvent.
C. fibrillation
By the flat filament after above-mentioned fluorination treatment through pin density be 120 needles/cm, linear velocity be 108m/min fibrillating roller into
Row mechanical membrane splits fibre, and the angle of needle and film traffic direction is 85 °, and the then thermal finalization at 130 DEG C is made polyolefin film and splits
Fiber.
Comparative example 6-1
When polyolefin carries out sided corona treatment in this comparative example, the electrode bar of corona treatment and the gap of flat filament are
0.5mm, processing voltage are 20000V, current strength 15A, other to prepare polyolefin film by the material and step of embodiment 6 and split fibre
Dimension.
Prepare electret air filtering material:
Examples 1 to 6, comparative example 1-1,1-2,1-3,1-4,4-1,5-1,6-1 polyolefin film prepared are split into fibre
Dimension is respectively put into deionized water and impregnates 1h, and taking-up is placed on guide frame, the tow on several axis by creel boundling at
200000 D flat and neat silk piece, after tension adjustment frame, then meridian velocity be 55m/min multiple roll seal wire machine travel into
Entering steam pressure is 1.0MPa, in the stainless steel steam chest that temperature is 100 DEG C (vapour source is purified water), then into filling
In box crimping machine, curling owner's back pressure is 0.3MPa, and back pressure 0.2MPa, crimping machine linear velocity is 65m/min, and curling comes out
Tow be equably layered on heat-setting box carrier bar by yarn swaying machine, tow after 120 DEG C of heat-setting box through traction frame into
Enter this formula cutting machine of rom, obtains the chopped film-fibre that length is 38mm.
Chopped film-fibre is abundant by the mass ratio of 95:5 for the 51mm ES fiber of 3D with Japanese Chisso Corporation's fiber number
Mixing, fiber basis weight 150g/m2.Mixture is successively fed into combing through opener, air pressure cotton box after mixing
Machine is combed, and the fibre web come out from carding machine enters cross lapping machine, and pre-needling and the thorn processing of main needle are carried out after lapping, plants needle
Degree is 5000 needles/m, and needling density is 400 thorns/cm2, acupuncture speed 20m/min, punch frequency is 300 thorns/min, and needle thorn is deep
Degree is 10mm, and walk cloth speed is 3.0m/min, and draw ratio 1.2 carries out thermal finalization subsequently into 115 DEG C of oven heats, obtains
Acupuncture nonwoven air filting material.Then acupuncture nonwoven air filting material is handled using Corona charge, electret technique are as follows: stay
Pole tension is 30KV, and output electric current is 1mA, and electret distance is 15mm, and the walk cloth speed by controlling filtering material adjusts electret
Time is 20s, and winding obtains electret non-woven fabric air filtering material, and products obtained therefrom uses 1~6,1-A, 1-B, 1-C, 1- respectively
D, 4-A, 5-A, 6-A are indicated, random to take out portioned product test filter efficiency, resistance and persistence.
The preparation method of polyolefin flat filament is in above-described embodiment and comparative example: after polyolefinic raw materials are blended, leading to
It crosses the processing of extrusion casting technique and is prepared into polyolefin film, then cut into narrowband, handled through the hot-stretch of high power longitudinal direction, thermal finalization
It obtains, specific preparation process can refer to that published application No. is the Chinese patent application files of CN201610466043.8.
The performance parameter of 1 polyolefin film-fibre of table
The solvent resistance of 2 polyolefin film-fibre of table is tested
The strainability persistence of 3 electret air filtering material of table is tested
As can be seen from Table 1, polyolefin flat filament is after sided corona treatment, liquid-phase fluorination processing, the fracture of obtained film-fibre
Intensity, elongation, initial modulus and fibrillation index do not occur significant change, illustrate appropriate sided corona treatment and liquid-phase fluorination
Processing will not influence the mechanical performance of polyolefin film-fibre.But when the current strength of sided corona treatment is big greater than 10A, voltage
When gap between 15000V and polyolefin flat filament and electrode bar is less than 1mm, i.e., when sided corona treatment is excessive, such as comparative example
6-1, the mechanical performance of film-fibre have certain decline, this is because under the action of high voltage electric field, the structure of polyolefin flat filament
It is destroyed, flat filament wildness becomes coarse, and the mechanical performance of film-fibre is caused to decline.
As can be seen from Table 2, polyolefin flat filament successively passes through sided corona treatment, liquid-phase fluorination processing, fibrillation processing, is prepared into
Film-fibre still maintains higher breaking strength and initial modulus after ethyl alcohol or acetone soak, this illustrates at corona
Reason and liquid-phase fluorination processing improve the solvent resistance of film-fibre, this is because sided corona treatment accelerates the progress of polyolefin flat filament
The reaction rate of liquid-phase fluorination, the surface of polyolefin flat filament form fluorinated layer in homogeneous thickness, improve the resistance to of film-fibre
Solvent borne.But when polyolefin flat filament only carries out sided corona treatment or liquid-phase fluorination and handles, such as comparative example 1-1,1-2 and
There is sharp fall in the solvent resistance of 1-3, film-fibre, this is because the reactivity of polyolefin flat filament is extremely low, with dissolution
The reaction rate of fluorine gas in a solvent is very low, it is difficult to which in the uniform fluorinated layer of the Surface Creation of flat filament, and polyolefin is a kind of
Non-polar material, it is very poor to the corrosion resistance of alcohols, ketone equal solvent；In the case where corona free processing, even if extending fluorination
Time, the solvent resistance such as comparative example 1-2, film-fibre are still very poor.In the processing of both corona frees, also fluoride-free is handled
Under the conditions of, the solvent resistance of film-fibre is equally very poor.But when the intensity deficiency of sided corona treatment, such as comparative example 5-
1, i.e., the gap that the current strength of sided corona treatment is less than 2A, voltage is less than between 2000V and polyolefin flat filament and electrode bar is greater than
When 5mm or when the intensity of sided corona treatment is excessively high, such as comparative example 6-1, i.e., when the current strength of sided corona treatment be greater than 10A,
When voltage is greater than the gap between 15000V and polyolefin flat filament and electrode bar less than 1mm, polyolefin flat filament is being carried out at corona
After reason, liquid-phase fluorination processing, the solvent resistance of film-fibre is lower, this is because the electric current of sided corona treatment, voltage strength are too low
When, the surface-active of polyolefin flat filament can not be improved, to subsequent liquid phase fluorination reaction without facilitation；When sided corona treatment is excessive
When, the internal structure of polyolefin flat filament is destroyed, the solvent resistance decline of film-fibre.
As can be seen from Table 3, when polyolefin flat filament is with a thickness of 5~100 μm, when width is 5~30mm, polyolefin flat filament warp
After sided corona treatment, fluorination treatment, it is prepared into electret air filtering material, filter efficiency with higher and lower filtration resistance excessively
Power is placed after a period of time (30 days~360 days), and the filter efficiency of filtering material, filtration resistance variation are little, this illustrates corona
The service life and persistence of filtering material are improved with fluorination treatment, the reason is that polyolefin flat filament is in sided corona treatment, liquid phase fluorine
After change processing, stable fluorinated layer in homogeneous thickness, fluorinated layer and fluorinated layer and polyene are formd on the surface of polyolefin flat filament
Layer gap between hydrocarbon flat filament can steadily store charge, after being prepared into electret air filtering material, the filtering of filtering material
Efficiency and persistence increase, filtration resistance reduces.When polyolefin flat filament is without sided corona treatment, such as comparative example 1-1 and 1-2,
The filter efficiency and persistence of the electret air filtering material of preparation decline, this is because polyolefin is in liquid phase fluorination reaction
When, fluorination rates are slower, and the fluorinated layer on surface is relatively thin and uneven, even if extend fluorination the time, be also unable to reach at corona
Same effect is managed, such as comparative example 1-2.
But when the thickness of polyolefin flat filament is greater than 100 μm, and width is greater than 30mm, such as comparative example 4-1, polyene
For hydrocarbon flat filament even across sided corona treatment, liquid-phase fluorination processing, mechanical performance, the solvent resistance of prepared film-fibre are poor,
Filter efficiency, the persistence of obtained electret air filtering material are also poor, this is because with flat filament thickness and width
Increase, the fibrillation networking and continuity in fibrillation process are poor, obtained film-fibre and air filting material
Uniformity and stability are poor.
Polyolefin is successively preprocessed, after sided corona treatment, fluorination treatment, and such as embodiment 2 and embodiment 3, prepared is poly-
Mechanical performance, the solvent resistance of alkene film-fibre are optimal, and the filter efficiency of electret air filtering material is high, persistence is good,
This is because sided corona treatment efficiency and fluorination reaction rate can be improved in pretreatment.
Claims (10)
1. a kind of preparation method of polyolefin film-fibre, which comprises the following steps:
(1) sided corona treatment: at least one side of polyolefin flat filament is subjected to online sided corona treatment, between polyolefin flat filament and electrode bar
Gap is 1~5mm, and processing voltage is 2000~15000V, and current strength is 2~10A；
(2) liquid-phase fluorination is handled: the polyolefin flat filament that step (1) obtains is carried out fluorination reaction in fluoride solvent；
(3) fibrillation: the polyolefin flat filament that step (2) is obtained carries out mechanical fibrillation processing, then winds, prepares polyene
Hydrocarbon film-fibre；
The polyolefin flat filament with a thickness of 1~100 μm.
2. a kind of preparation method of polyolefin film-fibre according to claim 1, which is characterized in that the polyolefin is flat
Silk is 0.5~7.0g/min by melt index, and polyolefinic raw materials of the isotacticity greater than 95% are prepared.
3. a kind of preparation method of polyolefin film-fibre according to claim 2, which is characterized in that the polyolefin is flat
The width of silk is 5~30mm.
4. a kind of preparation method of polyolefin film-fibre according to claim 1, which is characterized in that the fluoride solvent
In be continually fed into the mixed gas of delivery of fluorine/nitrogen.
5. a kind of preparation method of polyolefin film-fibre according to claim 4, which is characterized in that the fluoride solvent
Middle concentration of fluorine is 0.2~2mmol/L.
6. a kind of preparation method of polyolefin film-fibre according to claim 4, which is characterized in that the fluorine gas/nitrogen
The volume content of fluorine gas is 1~10% in the mixed gas of gas.
7. a kind of preparation method of polyolefin film-fibre according to claim 1, which is characterized in that the fluoride solvent
Including fluorination butane, fluorination pentane, fluorination one of hexane or a variety of.
8. a kind of preparation method of polyolefin film-fibre according to claim 1, which is characterized in that the polyolefin is flat
Silk is pre-processed before the sided corona treatment, and the pretreatment refers to the table using alcohol fluid injection impact polyolefin flat filament
Face.
9. the polyolefin film-fibre of any one of claim 1~8 the method preparation.
10. electret air filtering material, which is characterized in that the polyene comprising the method preparation of any one of claim 1~8
Hydrocarbon film-fibre.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6432175B1 (en) * | 1998-07-02 | 2002-08-13 | 3M Innovative Properties Company | Fluorinated electret |
| US6802315B2 (en) * | 2001-03-21 | 2004-10-12 | Hollingsorth & Vose Company | Vapor deposition treated electret filter media |
| CN103801155B (en) * | 2007-07-26 | 2016-09-28 | 3M创新有限公司 | Highly charged and the nanometer fiber net of charge stable |
| CN101805984A (en) * | 2009-11-25 | 2010-08-18 | 瓮福（集团）有限责任公司 | Method for improving uvioresistant performance of polypropylene flat-filament |
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Denomination of invention: Polyolefin split-film fiber as well as preparation method and electret air filtration material prepared by polyolefin split-film fiber Effective date of registration: 20200310 Granted publication date: 20190531 Pledgee: Shenzhen hi tech investment small loan Co., Ltd Pledgor: SHENZHEN SELEN SCIENCE & TECHNOLOGY Co.,Ltd. Registration number: Y2020980000562 |
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