CN105032210B - A kind of polyolefin air-filtering membrane and preparation method thereof - Google Patents
A kind of polyolefin air-filtering membrane and preparation method thereof Download PDFInfo
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Abstract
The present invention prepares polyolefin air-filtering membrane by thermally induced phase separation, and with a thickness of 80 μm~300 μm, porosity is 50%~80%, and air transmission coefficient is 5~200L/ (m2S), filtering PM2.5 effect is especially significant compared with prior art.The present invention also provides thermally induced phase separations to prepare polyolefin air-filtering membrane process, by extrusion, curtain coating, it is two-way the techniques such as draw high, extract, be mass produced with being not only able to high-efficiency and continuous, and can neatly control porosity and pore size.Meanwhile to be far longer than the nano fibrous membrane prepared by the methods of melt-spun, electrostatic spinning by air filtration film strength prepared by biaxial tension.
Description
Technical field
The invention belongs to the preparation field of air filting material, in particular to a kind of polyolefin air-filtering membrane and its preparation
Method.
Background technique
In recent years, China's air pollution is more serious, and people are also higher and higher to the attention rate of air pollution, especially closely
The continuous wide range of haze weather that phase occurs more promotes common people to the worry of air quality.The deterioration of air quality is
The daily biochemistry of people is seriously affected, PM2.5 becomes the project that must be detected daily.
Meanwhile room air be flooded with particulate matter, formaldehyde, total volatile organism (TVOC), bacterium, virus, anaphylactogen,
The various pollutants such as gas with foreign flavor, radioactive source, being put into influences one of maximum five environmental factors to public health.Air is dirty
Dye has become the problem of whole world facing to human health risk, in order to more efficiently purify air, also people one
Environmental clean life living environment, air purifying process have obtained the highest attention of people.
The green living and body in the maintenance mankind such as air filtration articles such as mask, air filter, breathing mask
Critical role is gradually captured in health.Air-filtering membrane, which must have, to be retained the solid hazardous substance in air or sends out therewith
The effects of raw adsorption reaction, can be only achieved purification air, guarantee the purpose of human health.Currently, daily, Medical air in the market
Gas filter membrane, such as mask, air filter, breathing mask etc., majority are prepared using electrospinning process.For example,
CN103480285A discloses a kind of enhancing polysulfone nano-fiber air filter membrane and its electrostatic spinning preparation method,
CN104368245A also discloses a kind of electrostatic spinning air-filtering membrane and preparation method thereof.But electrostatic spinning is prepared into
The air-filtering membrane arrived is easy to damage in use process, and the ability of anti-deformation and heat resistance that are used for a long time are poor.
The present invention pass through the study found that using thermally induced phase separation prepare polyolefin air-filtering membrane, for PM2.5 mistake
It is more significant to filter effect.
Summary of the invention
The purpose of the present invention is to provide a kind of for room air filtration system, can effectively filter the polyene of PM2.5
Hydrocarbon air-filtering membrane and preparation method thereof.
A kind of polyolefin air-filtering membrane, which is characterized in that be prepared using thermally induced phase separation, with a thickness of 80 μm
~300 μm, porosity is 50%~80%, and air transmission coefficient is 5~200L/ (m2·s)。
Both at home and abroad at present without the report for preparing air-filtering membrane using thermally induced phase separation, the present invention uses this side for the first time
Method has simple process, is more suitable for continuously being mass produced, and imitates wherein preparing resulting air-filtering membrane and PM2.5 being filtered
The features such as fruit is more significant, PM2.5 filter efficiency are up to 90% or more, especially currently preferred technical solution filter efficiency
Up to 95%, the significantly larger than filter efficiency of the prior art 80% or so have the unexpected technology of those skilled in the art
Effect.
Above-mentioned technical purpose of the invention is achieved through the following technical solutions:
A, polyolefin powder swelling dissolution: polyolefin resin powder and diluent are thoroughly mixed, wherein polyolefin
The ratio of resin and diluent is 1:1~1:10, under nitrogen protection, is warming up to 80~150 DEG C of heat preservation swellings, it is poly- to obtain swelling
Alkene；
B, it slab: is plasticized the resulting mixture of previous step to form polyolefin melt by extruder, then from die head
It squeezes out, obtains sheet polyolefin casting films, extruder operating temperature is at 100~400 DEG C；
C, one-off drawing: said polyolefins casting films pass through biaxial tension, then at room temperature using extractant to diaphragm
Oil removing and drying are extracted, the stretching ratio of biaxial tension is 3 × 3~12 × 12 times；
D, succeeding stretch and thermal finalization: diaphragm extracted is carried out again in hot-stretch case secondary lateral simple tension and
Thermal finalization processing, lateral simple tension multiplying power are 1~3 times；Heat setting temperature is 5 DEG C~40 DEG C below polyolefin fusing point, heat
Setting time is 3min~20min.Finally obtain the MIcroporous polyolefin film of fibrosis.
The average molecular weight of the polyolefin resin is 1 × 104~1 × 107；It is preferred that 1 × 104~5 × 106；As more excellent
Choosing, the molecular weight of polyolefin are 5 × 105~5 × 106。
The diluent is paraffin oil, solid paraffin, soybean oil, peanut oil, olive oil, phthalic acid ester, adjacent benzene two
The mixture of one or more of formic acid dibutyl ester, dibutyl phthalate and glyceride；Preferably, diluent
For the paraffin oil or solid paraffin of low molecular weight.
The extractant be pentane, hexane, heptane, methylene chloride, carbon tetrachloride, dioxolane, diethyl ether, dioxanes and
The mixture of one or more of methyl ethyl ketone.
The particle size range of the polyolefin powder is 0.01 μm~5 μm.It is preferred that 0.1 μm~2 μm.
The present invention is mass produced with being not only able to high-efficiency and continuous, but also can pass through the ratio of adjusting diluent and resin
Example and the multiplying power stretched twice, neatly control porosity and pore size；Meanwhile the air mistake prepared by biaxial tension
The puncture strength of filter membrane will be far longer than the nano fibrous membrane prepared by the methods of melt-spun, electrostatic spinning.
Polyolefin air-filtering membrane prepared by the present invention, with a thickness of 20 μm~300 μm, porosity is 50%~80%, empty
Vapor permeability is 5~200L/ (m2·s)。
The more evenly microporous barrier of porosity in order to obtain, wherein the ratio of the step a resin and diluent is preferably 1:
3~1:6；In the step c, the stretching ratio of biaxial tension is preferably 5 × 5~10 × 10 times；It is laterally unidirectional draw in step d
Stretching multiplying power is preferably 1.2~2 times.Prepared polyolefin air-filtering membrane, porosity are 60%~75%.
The invention has the following advantages that
(1) the polyolefin air-filtering membrane that thermally induced phase separation is prepared can pass through in production process and adjust dilution
Content, the biaxial tension multiplying power of agent accurately to control the thickness, pore-size distribution and air transmission coefficient of air-filtering membrane, preparation
Air-filtering membrane is especially significant for PM2.5 filter effect, and PM2.5 filter efficiency is up to 90% or more, especially of the invention excellent
The technical solution filter efficiency of choosing is up to 95%, the significantly larger than filter efficiency of the prior art 80% or so, has this field skill
The unexpected technical effect of art personnel.Moreover, the tensile strength of the air-filtering membrane by biaxial tension preparation and puncture are strong
Degree will also be far longer than the nano fibrous membrane prepared by the methods of melt-spun, electrostatic spinning.
(2) thermally induced phase separation preparation method is compared with other prior arts, simple process, and yield is high, is suitble to extensive
Continuous production, efficient production efficiency reduce production cost；And for the present invention using polyolefin, cost of material is cheap,
Final air-filtering membrane cost will substantially reduce.
Detailed description of the invention
7 scanning electron microscope (SEM) photograph of Fig. 1 embodiment
7 graph of pore diameter distribution of Fig. 2 embodiment
7 graph of pore diameter distribution of Fig. 3 comparative example
Specific embodiment
Invention is further described in detail with reference to the accompanying drawings and examples.
Embodiment 1
Preparing polyolefin air-filtering membrane, steps are as follows:
A, polyolefin powder swelling dissolution: polyolefin resin powder and diluent paraffin oil are thoroughly mixed, wherein
The ratio of polyolefin resin and diluent is 1:1, under nitrogen protection, is warming up to 80~150 DEG C of heat preservation swellings, it is poly- to obtain swelling
Alkene；
B, it slab: is plasticized the resulting mixture of previous step to form polyolefin melt by extruder, then from die head
It squeezes out, obtains sheet polyolefin casting films, extruder operating temperature is at 100~400 DEG C；
C, one-off drawing: said polyolefins casting films pass through biaxial tension, then at room temperature using extractant to diaphragm
Oil removing and drying are extracted, the stretching ratio of biaxial tension is 3 × 3 times；
D, succeeding stretch and thermal finalization: diaphragm extracted is carried out again in hot-stretch case secondary lateral simple tension and
Thermal finalization processing, lateral simple tension multiplying power are 1 times；Heat setting temperature is 5 DEG C~40 DEG C below polyolefin fusing point, thermal finalization
Time is 3min~20min.Finally obtain the MIcroporous polyolefin film of fibrosis.
Embodiment 2
Preparing polyolefin air-filtering membrane, steps are as follows:
A, polyolefin powder swelling dissolution: polyolefin resin powder and diluent olive oil are thoroughly mixed, wherein
The ratio of polyolefin resin and diluent is 1:10, under nitrogen protection, is warming up to 80~150 DEG C of heat preservation swellings, is swollen
Polyolefin；
B, it slab: is plasticized the resulting mixture of previous step to form polyolefin melt by extruder, then from die head
It squeezes out, obtains sheet polyolefin casting films, extruder operating temperature is at 100~400 DEG C；
C, one-off drawing: said polyolefins casting films pass through biaxial tension, then at room temperature using extractant to diaphragm
Oil removing and drying are extracted, the stretching ratio of biaxial tension is 12 × 12 times；
D, succeeding stretch and thermal finalization: diaphragm extracted is carried out again in hot-stretch case secondary lateral simple tension and
Thermal finalization processing, lateral simple tension multiplying power are 3 times；Heat setting temperature is 5 DEG C~40 DEG C below polyolefin fusing point, thermal finalization
Time is 3min~20min.Finally obtain the MIcroporous polyolefin film of fibrosis.
Embodiment 3
Preparing polyolefin air-filtering membrane, steps are as follows:
A, polyolefin powder swelling dissolution: polyolefin resin powder and diluent phthalic acid ester are sufficiently stirred mixed
It closes, wherein the ratio of polyolefin resin and diluent is 1:3, under nitrogen protection, is warming up to 80~150 DEG C of heat preservation swellings, obtains
To swelling polyolefin；
B, it slab: is plasticized the resulting mixture of previous step to form polyolefin melt by extruder, then from die head
It squeezes out, obtains sheet polyolefin casting films, extruder operating temperature is at 100~400 DEG C；
C, one-off drawing: said polyolefins casting films pass through biaxial tension, then at room temperature using extractant to diaphragm
Oil removing and drying are extracted, the stretching ratio of biaxial tension is 5 × 5 times；
D, succeeding stretch and thermal finalization: diaphragm extracted is carried out again in hot-stretch case secondary lateral simple tension and
Thermal finalization processing, lateral simple tension multiplying power are 1.2 times；For heat setting temperature 5 DEG C~40 DEG C below polyolefin fusing point, heat is fixed
The type time is 3min~20min.Finally obtain the MIcroporous polyolefin film of fibrosis.
Embodiment 4
Preparing polyolefin air-filtering membrane, steps are as follows:
A, polyolefin powder swelling dissolution: polyolefin resin powder and diluent phthalic acid ester are sufficiently stirred mixed
It closes, wherein the ratio of polyolefin resin and diluent is 1:6, under nitrogen protection, is warming up to 80~150 DEG C of heat preservation swellings, obtains
To swelling polyolefin；
B, it slab: is plasticized the resulting mixture of previous step to form polyolefin melt by extruder, then from die head
It squeezes out, obtains sheet polyolefin casting films, extruder operating temperature is at 100~400 DEG C；
C, one-off drawing: said polyolefins casting films pass through biaxial tension, then at room temperature using extractant to diaphragm
Oil removing and drying are extracted, the stretching ratio of biaxial tension is 10 × 10 times；
D, succeeding stretch and thermal finalization: diaphragm extracted is carried out again in hot-stretch case secondary lateral simple tension and
Thermal finalization processing, lateral simple tension multiplying power are 2 times；Heat setting temperature is 5 DEG C~40 DEG C below polyolefin fusing point, thermal finalization
Time is 3min~20min.Finally obtain the MIcroporous polyolefin film of fibrosis.
Comparative example 1
Using a kind of electrostatic spinning air-filtering membrane and preparation method thereof disclosed in CN104368245A, polyolefin sky is prepared
Gas filter membrane.
Embodiment 5
Electrostatic spinning air-filtering membrane and thermotropic phase air-filtering membrane, test result comparison, as shown in table 1
Table 1
Embodiment 6
Polyolefin air-filtering membrane step is prepared using embodiment 4, wherein the ratio of step a resin and diluent is stated, institute
The stretching ratio and step d transverse direction simple tension multiplying power of step c biaxial tension are stated, as shown in table 2.
Table 2
| Serial number | Step a resin and diluent | Step c biaxial tension multiplying power | Step d transverse direction simple tension multiplying power |
| 1 | 1:1 | 3×3 | 1 |
| 2 | 1:3 | 5×5 | 1.2 |
| 3 | 1:5 | 7×7 | 1.5 |
| 4 | 1:6 | 10×10 | 2 |
| 5 | 1:10 | 12×12 | 3 |
Wherein, test result is as shown in table 3.
Table 3
| Serial number | PM2.5 filter efficiency | MD tensile strength (MPa) | TD tensile strength (MPa) |
| 1 | 99.00% | 350 | 310 |
| 2 | 98.00% | 250 | 290 |
| 3 | 97.00% | 250 | 210 |
| 4 | 95.00% | 180 | 120 |
| 5 | 90.00% | 80 | 60 |
Above-mentioned MD is Machine Direction, i.e. longitudinal tensile strength；TD is Transverse Direction,
That is transverse tensile strength.The more evenly microporous barrier of porosity in order to obtain, when the ratio of the step a resin and diluent is preferred
In 1:3~1:6；In the step c, the stretching ratio of biaxial tension is preferably 5 × 5~10 × 10 times；It is lateral list in step d
It is preferably 1.2~2 times to stretching ratio, prepared polyolefin air-filtering membrane, porosity is 60%~75%.As it can be seen that
Optimization technique parameter has PM2.5 filter efficiency height, the marked improvements such as tensile strength.
Embodiment 7
Mixing is mixed according to the ratio of 1:4 in polyethylene resin powder and paraffin oil, 10h is swollen at 90 DEG C, obtains
Mixture after to swelling；Mixture is cooled to sheet material by squeezing out curtain coating, chilling roller, carries out one-off drawing, and one-off drawing is
Biaxial tension, draft temperature are 110 DEG C, and stretching ratio is 9 × 9 times；Film after one-off drawing carries out extraction oil removing in heptane,
Tunica albuginea after obtaining oil removing；For above-mentioned tunica albuginea using cross directional stretch, stretching ratio is 1.5 times, and draft temperature is 120 DEG C；Finally
The thermal finalization at 130 DEG C, setting time 3min, obtains finished product.Its pore-size distribution and scanning electron microscope are as depicted in figs. 1 and 2.
Comparative example 7
Using a kind of electrostatic spinning air-filtering membrane and preparation method thereof disclosed in CN104368245A, polyolefin sky is prepared
Gas filter membrane.Its pore-size distribution is as shown in Figure 3.
Embodiment 8
Mixing is mixed according to the ratio of 1:2.5 in polyethylene resin powder and paraffin oil, is swollen 10h at 90 DEG C,
Mixture after being swollen；Mixture is cooled to sheet material by squeezing out curtain coating, chilling roller, carries out one-off drawing, one-off drawing
For biaxial tension, draft temperature is 110 DEG C, and stretching ratio is 9 × 9 times；Film after one-off drawing carries out extraction in heptane and removes
Oil, the tunica albuginea after obtaining oil removing；For above-mentioned tunica albuginea using cross directional stretch, stretching ratio is 1.5 times, and draft temperature is 120 DEG C；Most
The thermal finalization at 130 DEG C afterwards, setting time 3min, obtains finished product.
Embodiment 9
Mixing is mixed according to the ratio of 1:4 in polyethylene resin powder and paraffin oil, 10h is swollen at 90 DEG C, obtains
Mixture after to swelling；Mixture is cooled to sheet material by squeezing out curtain coating, chilling roller, carries out one-off drawing, and one-off drawing is
Biaxial tension, draft temperature are 110 DEG C, and stretching ratio is 6 × 6 times；Film after one-off drawing carries out extraction oil removing in heptane,
Tunica albuginea after obtaining oil removing；For above-mentioned tunica albuginea using cross directional stretch, stretching ratio is 1.5 times, and draft temperature is 120 DEG C；Finally
The thermal finalization at 130 DEG C, setting time 3min, obtains finished product.
It is to be carried out to ultra-high molecular weight polyethylene of the present invention/thermotropic phase liquid crystal composite micro porous film and preparation method thereof above
It illustrates, is used to help understand the present invention, but embodiment of the present invention are not limited by the above embodiments, it is any without departing from this
Made changes, modifications, substitutions, combinations, simplifications under inventive principle, should be equivalent substitute mode, are included in the present invention
Protection scope within.
Claims (2)
1. a kind of polyolefin air filtration membrane preparation method, which is characterized in that
A, polyolefin powder swelling dissolution: polyolefin resin powder and diluent are thoroughly mixed, and under nitrogen protection, are risen
Temperature to 80~150 DEG C of heat preservations are swollen, and obtain swelling polyolefin；
B, slab: being plasticized the resulting mixture of previous step to form polyolefin melt by extruder, then squeezes out from die head,
By being cast chilling roller cooling treatment, sheet polyolefin casting films are obtained, extruder operating temperature is at 100~400 DEG C；
C, one-off drawing: said polyolefins casting films pass through biaxial tension, then at room temperature using extractant to diaphragm oil removing
And it is dry；
D, diaphragm extracted succeeding stretch and thermal finalization: is carried out to secondary lateral simple tension and Re Ding again in hot-stretch case
Type processing；For heat setting temperature 5 DEG C~40 DEG C below polyolefin fusing point, heat-setting time is 3min~20min,
The ratio of the step a resin and diluent is in 1:4~1:6；In the step c, the stretching ratio of biaxial tension is 9 ×
9~10 × 10 times；Lateral simple tension multiplying power is 1.2~2 times in step d,
The average molecular weight of the polyolefin resin is 1 × 104~1 × 107,
The diluent is paraffin oil, solid paraffin, soybean oil, peanut oil, olive oil, phthalic acid ester, phthalic acid
The mixture of one or more of dibutyl ester, dibutyl phthalate and glyceride,
The extractant is pentane, hexane, heptane, methylene chloride, carbon tetrachloride, dioxolane, diethyl ether, dioxanes and methyl
The mixture of one or more of ethyl ketone,
The particle size range of the polyolefin powder is 0.01 μm~5 μm,
Film PM2.5 filter efficiency is 95~98%.
2. a kind of polyolefin air-filtering membrane of claim 1 the method preparation, which is characterized in that prepared polyolefin is empty
For gas filter membrane with a thickness of 80 μm~300 μm, porosity is 65%~80%, and air transmission coefficient is 5~50L/ (m2·s)。
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| CN106985482B (en) * | 2017-02-17 | 2020-02-14 | 武汉纺织大学 | Composite film on surface of nanofiber and preparation method thereof |
| CN106891557B (en) * | 2017-03-15 | 2019-06-07 | 中国科学技术大学 | A kind of polyolefine micro/nano-fibre film and preparation method thereof |
| CN113845708A (en) * | 2020-06-28 | 2021-12-28 | 河北金力新能源科技股份有限公司 | Comfortable PE breathable film with high protective property and preparation method thereof |
| US20220134293A1 (en) * | 2020-10-30 | 2022-05-05 | Entegris, Inc. | Low metal content polyolefin filter membrane |
| CN113276384A (en) * | 2021-04-28 | 2021-08-20 | 河北金力新能源科技股份有限公司 | Fresh air exchange membrane and preparation method and application thereof |
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| CN102015080A (en) * | 2008-02-22 | 2011-04-13 | 立达赛路达克有限公司 | Polyethylene membrane and method of its production |
| CN103921449A (en) * | 2014-04-23 | 2014-07-16 | 深圳市星源材质科技股份有限公司 | Ultrathin high-strength polyolefin microporous film and preparation method thereof |
| CN104258636A (en) * | 2014-05-19 | 2015-01-07 | 中材科技股份有限公司 | An air purification and filtration material and a preparing method thereof |
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| CN102015080A (en) * | 2008-02-22 | 2011-04-13 | 立达赛路达克有限公司 | Polyethylene membrane and method of its production |
| CN103921449A (en) * | 2014-04-23 | 2014-07-16 | 深圳市星源材质科技股份有限公司 | Ultrathin high-strength polyolefin microporous film and preparation method thereof |
| CN104258636A (en) * | 2014-05-19 | 2015-01-07 | 中材科技股份有限公司 | An air purification and filtration material and a preparing method thereof |
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