WO2023138144A1 - 一种可循环使用驻极体过滤膜及其制备方法、清洗和电荷再生方法 - Google Patents

一种可循环使用驻极体过滤膜及其制备方法、清洗和电荷再生方法 Download PDF

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WO2023138144A1
WO2023138144A1 PCT/CN2022/128473 CN2022128473W WO2023138144A1 WO 2023138144 A1 WO2023138144 A1 WO 2023138144A1 CN 2022128473 W CN2022128473 W CN 2022128473W WO 2023138144 A1 WO2023138144 A1 WO 2023138144A1
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filter membrane
recyclable
electret filter
electret
preparation
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English (en)
French (fr)
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蔡容容
王九思
张立志
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华南理工大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0004—Organic membrane manufacture by agglomeration of particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0081—After-treatment of organic or inorganic membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0081—After-treatment of organic or inorganic membranes
    • B01D67/0095—Drying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
    • B01D71/80—Block polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/04—Hydrophobization
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/39—Electrospinning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/26—Electrical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/38—Hydrophobic membranes

Definitions

  • the invention relates to the technical field of air purification and indoor air quality, in particular to a recyclable electret filter membrane, a preparation method thereof, and a cleaning and charge regeneration method.
  • Porous media particulate filtration technology is considered to be the most effective and health-friendly air purification technology.
  • the porous PM 2.5 filter material must be replaced regularly due to the deposition of particles, the continuous increase of filter resistance and operating energy consumption, and even cause secondary air pollution.
  • the dust removal, regeneration and recycling of filter materials are very important to reduce filter energy consumption and achieve environmental protection.
  • Electret filter material can store static charge for a long time, has an additional electrostatic capture effect, can improve filtration efficiency without increasing filtration resistance, and has been widely used. Due to the inherent charge dissipation, the recycling of electret filter media needs to solve the problems of effective dust removal and charge regeneration at the same time.
  • the domestic invention patent CN105920919A published on September 7, 2016 discloses a method for preparing and activating a superhydrophobic electret filter material for purifying PM 2.5 .
  • the filtered filter material is placed in a high-voltage electric field for reverse purging and corona re-electretization, so as to realize repeated use.
  • the disadvantages of the above technology are: it is difficult to effectively remove the deposited particles by air flow purging; and the activation process uses high-voltage corona electret, which is complicated to operate and may generate ozone.
  • the CN212650438U utility model patent published in China on March 5, 2021 discloses a regeneration device for virus filtering masks.
  • a DC high-voltage electrostatic generator is designed to convert power-frequency AC or DC power into DC high-voltage static electricity, which is used to recharge the electret filter material and assist in killing viruses.
  • the object of the present invention is to provide a recyclable electret filter membrane and its preparation method, cleaning and charge regeneration method.
  • the electrospun fiber membrane with C-F bond on the surface prepared by the present invention can roll away the deposited particles through the rolling of water droplets, and at the same time, triboelectricity occurs between the water droplets and the surface of the filter membrane during the rolling process, so as to realize the dust removal, charge regeneration and recycling of the electret filter membrane.
  • a preparation method for recyclable electret filter membrane comprising the following steps: Dissolve fluorine-containing polymer particles and polyethylene oxide particles in deionized water to prepare a spinning solution, which is then electrospun, calcined, cooled and dried, and corona charged to obtain a recyclable electret filter membrane.
  • the fluoropolymer particles are more than one of polytetrafluoroethylene and perfluoroethylene propylene copolymer;
  • the mass ratio of the fluorine-containing polymer particles to the polyethylene oxide particles is 15:1-25:1;
  • the mass fraction of polyethylene oxide in the spinning solution is 3-7%.
  • the temperature of the calcination is 350-400° C., and the time is 5-10 minutes; the calcination is in an air atmosphere.
  • the charging conditions of the corona charging are: voltage (-10)-(-15) kV, the distance from the needle to the ground plate is 3-5 cm, and the charging time is 5-10 min.
  • the electrospinning conditions are as follows: the spinning voltage is 15-25 kV, the injection speed is 0.06-0.12mm/min, the drum speed is 80-120r/min, and the relative humidity of the environment is 40-60%RH.
  • the recyclable electret filter membrane further includes further fluorinated improvement;
  • the fluorinated improved substance is at least one of tridecafluorooctyltriethoxysilane and heptadecafluorodecyltriethoxysilane.
  • the fluorination improvement specifically includes: performing surface fluorination by means of dip coating; the mass fraction of the surface fluorination solution for dip coating is 2-5%.
  • the recyclable electret filter membrane prepared by the above preparation method is an electrospun fiber membrane with C-F bonds on the surface.
  • the recyclable electret filter membrane has a fiber diameter of 1-15 ⁇ m, a gram weight of 50-150g/m 2 , a water contact angle of 140°-160°, an initial surface potential of (-600)-(-950)V, and an initial pressure drop of 60-150Pa; after cleaning and regeneration, the potential is regenerated to (-700)-(-1000)V, and the charge recovery rate is 90-125%.
  • the efficiency is 90%-100%, and the filtration efficiency of PM 2.5 is ⁇ 94%.
  • the above cleaning and charge regeneration method for the recyclable electret filter membrane includes the following steps: washing and triboelectricizing the surface of the recyclable electret filter membrane after holding dust, and then drying to realize charge regeneration and repeated use.
  • the cleaning and charge regeneration method specifically includes: (1) fixing the electret filter membrane after holding dust on a platform with adjustable height and inclination angle;
  • the water droplet rolling cleaning and triboelectrochemical method is as follows: the inclination angle of the recyclable electret filter membrane is 30°-60°; water droplets continuously drop and roll off the surface of the filter membrane, the volume of a single droplet is 10-100 ⁇ L, the drop height is 3-10cm, the drop time interval is 1-10s, and the total drop time is 5-15min; the drying temperature is 40°C-60°C.
  • the present invention has the following advantages and beneficial effects:
  • the present invention adopts the method of water drop rolling contact electrification to realize the charge regeneration of the electret filter membrane, and restores the electrostatic filtration efficiency of the electret filter membrane.
  • the water contact angle on the surface of the electret filter membrane of the present invention can reach 157°.
  • the particles deposited on the filter membrane surface are cleaned by the water drop rolling method, so as to realize dust removal and regeneration, and has good circulation.
  • Fig. 1a is an electron micrograph of the composite filter membrane obtained by blending polytetrafluoroethylene and polyethylene oxide in Example 1.
  • FIG. 1 b is an electron microscope image of the polytetrafluoroethylene filter membrane obtained after calcining in Example 1.
  • Figure 2a is the EDS diagram of the composite filter membrane obtained by blending polytetrafluoroethylene and polyethylene oxide in Example 1.
  • FIG. 2 b is an EDS diagram of the polytetrafluoroethylene filter membrane obtained after calcining in Example 1.
  • Fig. 3 is a schematic diagram of the water droplet rolling cleaning and triboelectrochemical device of the present invention.
  • Fig. 4 is a graph showing changes in surface potential during three dust-holding filtration-cleaning regeneration cycles in Examples 1, 2, 3, and 4.
  • FIG. 3 The schematic diagram of the water drop rolling cleaning and triboelectrochemical device of the present invention is shown in Figure 3.
  • 1 is water pipes. This device uses four water pipes so that water droplets can cover the entire surface of the filter membrane, and the drop height can be adjusted;
  • 2 is water droplets, the volume of water droplets, the time interval of dripping and the total time of dripping can be adjusted;
  • 3 is the electret filter membrane after dust storage, and the inclination angle of the filter membrane can be adjusted;
  • the polytetrafluoroethylene/polyethylene oxide composite filter membrane is prepared by electrospinning by spinning solution, as shown in Figure 1a and Figure 2a;
  • the polytetrafluoroethylene filter membrane was subjected to corona charging, the voltage was -10kV, the distance from the needle to the ground plate was 3cm, and the charging time was 10min to obtain an electret polytetrafluoroethylene filter membrane;
  • the electret polytetrafluoroethylene filter membrane obtained in this example has a fiber diameter of 10 ⁇ m, a water contact angle of 140°, a filter membrane grammage of 71.2 g/m 2 , an initial potential of -740 V, an initial pressure drop of 64 Pa, and an initial filtration efficiency of PM 2.5 of 95.30%.
  • the triboelectrification of water droplets rolling can regenerate the surface potential of the PTFE filter membrane to above -800V, and the rolling water droplets cleaning can restore the pressure drop to 81Pa, and the filtration efficiency of PM 2.5 remains above 95.1%.
  • the perfluoroethylene propylene copolymer/polyethylene oxide composite filter membrane was prepared by electrospinning with spinning solution;
  • the perfluoroethylene propylene copolymer filter membrane was subjected to corona charging at a voltage of -10kV, the distance from the needle to the ground plate was 3cm, and the charging time was 10min to obtain an electret perfluoroethylene propylene copolymer filter membrane;
  • the electret perfluoroethylene propylene copolymer filter membrane obtained in this example has a fiber diameter of 8 ⁇ m, a water contact angle of 140°, a filter membrane grammage of 90.3 g/m 2 , an initial potential of -900 V, an initial pressure drop of 71 Pa, and an initial filtration efficiency of PM 2.5 of 96.3%.
  • the triboelectrification of water droplets can regenerate the surface potential of the perfluoroethylene propylene copolymer filter membrane to above -850V, and the pressure drop can be restored to 83Pa by water droplet washing, and the filtration efficiency of PM 2.5 remains above 94.2%.
  • silica suspension water (named 1)
  • silica suspension water (named 2)
  • silica suspension water (named 1)
  • silica suspension water (named 2)
  • silica suspension water (named 1)
  • silica suspension water (named 2)
  • silica suspension water (named 1)
  • Dow Corning 184 polydimethylsiloxane mixed with supporting curing agent at a ratio of 10:1)
  • 10g of n-hexane to prepare an adhesive (named 2), take 1ml of No.
  • step (3) The surface fluorinated modified polytetrafluoroethylene filter membrane prepared in step (1) was subjected to corona charging at a voltage of -10kV, the distance from the needle to the ground plate was 3cm, and the charging time was 10min to obtain a surface fluorinated modified polytetrafluoroethylene electret filter membrane;
  • the electret polytetrafluoroethylene surface fluorinated filter membrane obtained in this example has a fiber diameter of 11 ⁇ m, a water contact angle of 157°, a filter membrane grammage of 101.2 g/m 2 , an initial potential of -764 V, an initial pressure drop of 129 Pa, and an initial filtration efficiency of PM 2.5 of 97.2%.
  • water droplet rolling triboelectrification can regenerate the surface potential of the surface fluorinated modified PTFE electret filter membrane to above -701V, water droplet rolling cleaning can restore the pressure drop to 131Pa, and the filtration efficiency of PM 2.5 remains above 96.7%.
  • silica suspension water (named 1)
  • silica suspension water (named 2)
  • silica suspension water named 1
  • Dow Corning 184 polydimethylsiloxane mixed with supporting curing agent at a ratio of 10:1
  • 10g of n-hexane to prepare an adhesive (named 2), take 1ml of No.
  • fluorosilane solution (named 4); soak the prepared perfluoroethylene propylene copolymer fiber filter membrane in solution 3 for 30 minutes, dry at 60°C for 1 hour, repeat three times, then soak the membrane in 4 solution water for 30 minutes, dry at 60°C for 1 hour, repeat three times; finally prepare a surface fluorinated modified perfluoroethylene propylene copolymer electret filter membrane;
  • step (3) The surface fluorinated modified perfluoroethylene propylene copolymer filter membrane prepared in step (1) was subjected to corona charging at a voltage of -10kV, the distance from the needle to the ground plate was 3cm, and the charging time was 10min to obtain a surface fluorinated modified perfluoroethylene propylene copolymer electret filter membrane;
  • the fiber diameter of the fluorinated filter membrane on the surface of the electret perfluoroethylene propylene copolymer obtained in this example is 10 ⁇ m, the water contact angle is 153°, the filter membrane has a grammage of 120.1g/m 2 , an initial potential of -650V, an initial pressure drop of 110Pa, and an initial filtration efficiency of PM 2.5 of 95.1%.
  • water droplet rolling triboelectrification can regenerate the surface potential of the surface fluorinated modified perfluoroethylene propylene copolymer electret filter membrane to above -800V, water droplet rolling cleaning can restore the pressure drop to 121Pa, and the filtration efficiency of PM 2.5 remains above 97.7%.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Filtering Materials (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

本发明公开一种可循环使用驻极体过滤膜及其制备方法、清洗和电荷再生方法；本发明通过将含氟聚合物颗粒和聚氧化乙烯颗粒溶解于去离子水中配置成纺丝液，后经静电纺丝，煅烧，冷却干燥，电晕充电得到可循环使用驻极体过滤膜。本发明通过对容尘后的过滤膜表面进行水滴滚落清洗和摩擦电化，再经干燥，实现电荷再生和重复使用。本发明所得过滤膜初始表面电位为（-600）-（-950）V,容尘后经水滴滚动电化可使电位再生至（-700）-（-1000）V, 电荷恢复率为90%-125%，清灰率为90%-100%，对PM 2.5的过滤效率≥ 94%。本发明方法操作简单，循环再生效果稳定，在空气过滤领域具有广阔的应用前景。

Description

一种可循环使用驻极体过滤膜及其制备方法、清洗和电荷再生方法 技术领域
本发明涉及空气净化与室内空气品质技术领域，具体涉及一种可循环使用驻极体过滤膜及其制备方法、清洗和电荷再生方法。
 背景技术
细颗粒物（PM 2.5）污染给人体健康、公共卫生和精密生产制造造成严重危害。多孔介质颗粒物过滤技术被认为是最有效、对健康最有益的空气净化技术。作为空气过滤设备的核心，多孔PM 2.5过滤材料在使用中随着颗粒沉积，过滤阻力和运行能耗不断增大，甚至引起二次空气污染，必须进行定期更换。过滤材料的清灰再生和循环使用对降低过滤能耗和实现环境保护至关重要。
驻极体过滤材料可长期储存静电荷，具有附加静电捕获效应，可在不增大过滤阻力的情况下提升过滤效率，已得到广泛使用。由于固有的电荷耗散，驻极体滤材的循环再生需同时解决有效清灰和电荷再生问题。
国内2016年9月7日公开的CN105920919A发明专利，公开了一种用于净化PM 2.5的超疏水驻极体滤材的制备及活化方法。该方法将过滤后的滤材放置在高压电场中进行反向吹扫和电晕再驻极，实现重复使用。
上述技术不足之处在于：气流吹扫很难有效去除沉积的颗粒；且活化过程采用高压电晕驻极，操作复杂，还可能产生臭氧。
国内2021年3月5日公开的CN212650438U实用新型专利，公开了一种病毒过滤口罩的再生装置，设计了直流高压静电发生器，将工频交流电或直流电转换为直流高压静电，用于使驻极体滤材重新荷电及辅助杀死病毒。
上述技术不足之处在于：每次电荷再生都需采用高压电场进行充电，操作较为麻烦，易产生臭氧；且不能去除已捕获的颗粒物，不适用于一般工业、室内驻极体过滤器的再生。
 技术解决方案
为克服上述现有技术的缺陷和不足，本发明的目的是提供一种可循环使用驻极体过滤膜及其制备方法、清洗和电荷再生方法。本发明所制备的表面含C-F键的静电纺纤维膜可通过水滴滚落带走沉积颗粒，同时水滴在滚落过程中与过滤膜表面发生摩擦电化，以此实现驻极体过滤膜的清灰、电荷再生和循环使用。
本发明的目的通过以下技术方案实现：
一种可循环使用驻极体过滤膜的制备方法，包括以下步骤：     将含氟聚合物颗粒和聚氧化乙烯颗粒溶解于去离子水中配置成纺丝液，后经静电纺丝，煅烧，冷却干燥，电晕充电得到可循环使用驻极体过滤膜。
优选的，所述含氟聚合物颗粒为聚四氟乙烯、全氟乙烯丙烯共聚物中的一种以上；
优选的，所述含氟聚合物颗粒与聚氧化乙烯颗粒的质量比为15:1-25:1；
优选的，所述纺丝液中聚氧化乙烯的质量分数为3-7%。
优选的，所述煅烧的温度为350-400℃，时间为5-10min；所述煅烧在空气气氛中。
优选的，所述电晕充电的充电条件为：电压（-10）-（-15）kV, 针到接地板距离为3-5cm，充电时间为5-10min。
优选的，所述静电纺丝的条件为：纺丝电压为15-25 kV,推注速度为0.06-0.12mm/min，滚筒速度为80-120r/min，环境相对湿度为40-60%RH。
优选的，所述的可循环使用驻极体过滤膜还包括进一步氟化改进；所述氟化改进的物质为十三氟辛基三乙氧基硅烷，十七氟癸基三乙氧基硅烷中的一种以上。
进一步优选的，所述氟化改进具体为：采用浸涂的方式进行表面氟化；浸涂的表面氟化溶液的质量分数为2-5%。
上述的制备方法制备的可循环使用驻极体过滤膜，所述可循环使用驻极体过滤膜为表面含C-F键的静电纺丝纤维膜。
优选的，所述可循环使用驻极体过滤膜的纤维直径为1-15µm，克重为50-150g/m 2，水接触角为140°-160°，初始表面电位为（-600）-（-950）V，初始压降为60-150Pa；经清洗再生后，电位再生至（-700）-（-1000）V，电荷恢复率为90-125%，清灰率为90%-100%，对PM 2.5的过滤效率≥94%。
上述的可循环使用驻极体过滤膜的清洗和电荷再生方法，包括如下步骤：对容尘后的可循环使用驻极体过滤膜表面进行水滴滚落清洗和摩擦电化，再经干燥，实现电荷再生和重复使用。
优选的，清洗和电荷再生方法具体为：（1）将容尘后的驻极体过滤膜固定在可调节高度和倾斜角的平台上；
（2）控制过滤膜倾斜角度，单个水滴的体积、滴落高度、滴落时间间隔和滴落总时间，对容尘后的过滤膜进行水滴滚落清洗和摩擦电化；
（3）将清洗后的过滤膜进行干燥。
优选的，所述的水滴滚落清洗和摩擦电化方法为：所述可循环使用驻极体过滤膜的倾斜角度为30°-60°；水滴连续滴落并从过滤膜表面滚落，单个水滴体积为10-100µL，下落高度为3-10cm，滴落时间间隔为1-10s，滴落总时间为5-15min；所述干燥的温度为40℃-60℃。
 有益效果
与现有技术相比，本发明具有如下优点及有益效果：
 （1）本发明首次采用水滴滚动接触电化的方法实现驻极体过滤膜的电荷再生，恢复了驻极体过滤膜的静电过滤效率。表面含C-F键的过滤膜与水滴滚动摩擦，C-F键被破坏并产生电子缺陷结构，使得含氟纤维过滤膜表面LUMO吸引大量外部电子，产生稳定的表面电势。
（2）本发明所述驻极体过滤膜表面水接触角可达157°，利用过滤膜表面的超疏水特性，采用水滴滚动法清洗过滤膜表面沉积的颗粒，实现了清灰再生，并且具有很好的循环性。
 附图说明
图1a是实施例1的聚四氟乙烯和聚氧化乙烯混纺得到的复合过滤膜的电镜图。
图1b是实施例1的煅烧后得到的聚四氟乙烯过滤膜的电镜图。
图2a是实施例1的聚四氟乙烯和聚氧化乙烯混纺得到的复合过滤膜的EDS图。
图2b是实施例1的煅烧后得到的聚四氟乙烯过滤膜的EDS图。
图3是本发明的水滴滚动清洗和摩擦电化装置示意图。
图4是实施例1，2，3，4中三次容尘过滤-清灰再生循环过程中表面电位的变化图。
 本发明的实施方式
下面结合实施例及附图对发明作进一步详细的描述，但本发明的实施方式不限于此。
本发明的水滴滚动清洗和摩擦电化装置示意图如图3。1为水管道，本装置采用四根水管道使得水滴可以覆盖整个过滤膜表面，滴落高度可调节；2为水滴，水滴的体积，滴落时间间隔及滴落总时间可调节；3为容尘后的驻极体过滤膜，过滤膜的倾斜角度可调节；4为容尘后过滤膜表面的灰尘颗粒，水滴滚动可带走颗粒实现清灰再生。
实施例 1
（1）用天平准确称取9g聚四氟乙烯，0.2g聚氧化乙烯和8.7g去离子水置于50mL烧杯中，然后加入搅拌子，在磁力搅拌器上搅拌36h，配置成均匀稳定的纺丝液；
（2）设置好纺丝参数，参数为纺丝电压为18 kV,推注速度为0.06mm/min，滚筒速度为120r/min，环境相对湿度为60%RH。利用纺丝液进行静电纺丝制备得到聚四氟乙烯/聚氧化乙烯复合过滤膜，如图1a、图2a所示；
（3）将制备的复合过滤膜在室温下干燥4h，然后在390℃温度下煅烧10min得到聚四氟乙烯过滤膜，如图1b、图2b所示；煅烧前由于聚氧化乙烯的存在使得氧元素质量分数为4.64%，煅烧后聚氧化乙烯被去除，故过滤膜中不再含有氧元素。
（4）将聚四氟乙烯过滤膜进行电晕充电，电压为-10kV，针到接地板距离为3cm，充电时间为10min，得到驻极体聚四氟乙烯过滤膜；
（5）对驻极体聚四氟乙烯过滤膜进行容尘过滤，时间为120 min，容尘颗粒为氯化钠，容尘量为1.6 g/m 2；
（6）采用水滴滚动清洗和滚动摩擦电化装置对容尘后的聚四氟乙烯过滤膜进行清洗和电荷再生，如图3所示，共有四股水流同时滴落到过滤膜表面，过滤膜倾斜角为60°，单个水滴体积为10µL，水滴滴落高度为3cm，水滴滴落时间间隔为1s，滴落总时间为5min，之后将聚四氟乙烯过滤膜在60℃下干燥1h。
（7）重复步骤（5）,（6）进行三次循环实验。
本实施例所得驻极体聚四氟乙烯过滤膜纤维直径为10µm，水接触角为140°，过滤膜克重为71.2g/m 2，初始电位为-740V，初始压降为64Pa，对PM 2.5的初始过滤效率为95.30% 。如图4所示，水滴滚落摩擦电化可使聚四氟乙烯过滤膜表面电位再生至-800V以上，水滴滚落清洗可使压降恢复至81Pa，对PM 2.5的过滤效率保持在95.1%以上。
实施例 2
（1）用天平准确称取10.8g全氟乙烯丙烯共聚物，0.2g聚氧化乙烯和2g去离子水置于50mL烧杯中，然后加入搅拌子，在磁力搅拌器上搅拌36h，配置成均匀稳定的纺丝液；
（2）设置好纺丝参数，参数为纺丝电压为21 kV,推注速度为0.06mm/min，滚筒速度为80r/min，环境相对湿度为60%RH。利用纺织液进行静电纺丝制备得到全氟乙烯丙烯共聚物/聚氧化乙烯复合过滤膜；
（3）将制备的复合过滤膜在室温下干燥4h，然后在300℃温度下煅烧10min得到全氟乙烯丙烯共聚物过滤膜。
（4）将全氟乙烯丙烯共聚物过滤膜进行电晕充电，电压为-10kV，针到接地板距离为3cm，充电时间为10min，得到驻极体全氟乙烯丙烯共聚物过滤膜；
（5）对驻极体全氟乙烯丙烯共聚物过滤膜进行容尘过滤，时间为120 min，容尘颗粒为氯化钠，容尘量为1.7 g/m 2；
（6）采用水滴滚动清洗和滚动摩擦电化装置对容尘后的全氟乙烯丙烯共聚物过滤膜进行清洗和电荷再生，如图3所示，共有四股水流同时滴落到过滤膜表面，过滤膜倾斜角为45°，单个水滴体积为50µL，水滴滴落高度为3cm，水滴滴落时间间隔为3s，滴落总时间为5min，之后将全氟乙烯丙烯共聚物过滤膜在60℃下干燥1h。
本实施例所得驻极体全氟乙烯丙烯共聚物过滤膜纤维直径为8µm，水接触角为140°，滤膜克重为90.3g/m 2，初始电位为-900V，初始压降为71Pa，对PM 2.5的初始过滤效率为96.3% 。如图4所示，水滴滚落摩擦电化可使全氟乙烯丙烯共聚物过滤膜表面电位再生至-850V以上，水滴滚落清洗可使压降恢复至83Pa，对PM 2.5的过滤效率保持在94.2%以上。
实施例 3
（1）按照实施例1中步骤（1）-（3）制备聚四氟乙烯纤维过滤膜；
（2）将0.1g二氧化硅纳米颗粒与30ml正己烷混合制备二氧化硅悬浮水（命名为①），将1g道康宁184聚二甲基硅氧烷（与配套固化剂以10：1混合）与10g正己烷混合制备胶粘剂（命名为②），取1ml②号溶水加入至①号溶水得到新溶水（命名为③），将 0.5g十七氟癸基三乙氧基硅烷，24.375g正己烷与0.125g醋酸混合得到氟硅烷溶液（命名为④）；将制备的聚四氟乙烯纤维过滤膜浸泡在③号溶液中30分钟，60℃干燥1小时，重复三次，再将膜浸泡在④号溶水中30分钟，60℃干燥1小时，重复三次；最终制备出表面氟化改性的聚四氟乙烯驻极体过滤膜；
（3）将步骤（1）制备的表面氟化改性的聚四氟乙烯过滤膜进行电晕充电，电压为-10kV，针到接地板距离3cm，充电时间为10min，得到表面氟化改性的聚四氟乙烯驻极体过滤膜；
（4）对表面氟化改性的聚四氟乙烯驻极体过滤膜进行容尘过滤，时间为120 min，容尘颗粒为氯化钠，容尘量为1.6 g/m 2；
（5）采用水滴滚动清洗和滚动摩擦电化装置对容尘后的表面氟化改性的聚四氟乙烯驻极体过滤膜进行清洗和电荷再生，如图3所示，共有四股水流同时滴落到过滤膜表面，过滤膜倾斜角为45°，单个水滴体积为100µL，水滴滴落高度为5cm，水滴滴落时间间隔为2s，滴落总时间为10min，之后将表面氟化改性的聚四氟乙烯驻极体过滤膜在60℃下干燥1h；
（6）重复步骤（4）,（5）进行循环实验，共进行三次循环。
本实施例所得驻极体聚四氟乙烯表面氟化过滤膜纤维直径为11µm，水接触角为157°，过滤膜克重为101.2g/m 2，初始电位为-764V，初始压降为129Pa，对PM 2.5的初始过滤效率为97.2% 。如图4所示，水滴滚落摩擦电化可使表面氟化改性的聚四氟乙烯驻极体过滤膜表面电位再生至-701V以上，水滴滚落清洗可使压降恢复至131Pa，对PM 2.5的过滤效率保持在96.7%以上。
实施例 4
（1）按照实施例1中步骤（1）-（3）制备全氟乙烯丙烯共聚物纤维过滤膜；
（2）将0.1g二氧化硅纳米颗粒与30ml正己烷混合制备二氧化硅悬浮水（命名为①），将1g道康宁184聚二甲基硅氧烷（与配套固化剂以10：1混合）与10g正己烷混合制备胶粘剂（命名为②），取1ml②号溶水加入至①号溶水得到新溶水（命名为③），将 0.7g十三氟辛基三乙氧基硅烷，21.155g正己烷与0.145g醋酸混合得到氟硅烷溶液（命名为④）；将制备的全氟乙烯丙烯共聚物纤维过滤膜浸泡在③号溶液中30分钟，60℃干燥1小时，重复三次，再将膜浸泡在④号溶水中30分钟，60℃干燥1小时，重复三次；最终制备出表面氟化改性的全氟乙烯丙烯共聚物驻极体过滤膜；
（3）将步骤（1）制备的表面氟化改性的全氟乙烯丙烯共聚物过滤膜进行电晕充电，电压为-10kV，针到接地板距离3cm，充电时间为10min，得到表面氟化改性的全氟乙烯丙烯共聚物驻极体过滤膜；
（4）对表面氟化改性的聚四氟乙烯驻极体过滤膜进行容尘过滤，时间为120 min，容尘颗粒为氯化钠，容尘量为1.6 g/m 2；
（5）采用水滴滚动清洗和滚动摩擦电化装置对容尘后的表面氟化改性的全氟乙烯丙烯共聚物驻极体过滤膜进行清洗和电荷再生，如图3所示，共有四股水流同时滴落到过滤膜表面，过滤膜倾斜角为30°，单个水滴体积为100µL，水滴滴落高度为10cm，水滴滴落时间间隔为10s，滴落总时间为15min，之后将表面氟化改性的全氟乙烯丙烯共聚物驻极体过滤膜在60℃下干燥1h；
（6）重复步骤（4）,（5）进行循环实验，共进行三次循环。
本实施例所得驻极体全氟乙烯丙烯共聚物表面氟化过滤膜纤维直径为10µm，水接触角为153°，过滤膜克重为120.1g/m 2，初始电位为-650V，初始压降为110Pa，对PM 2.5的初始过滤效率为95.1% 。如图4所示，水滴滚落摩擦电化可使表面氟化改性的全氟乙烯丙烯共聚物驻极体过滤膜表面电位再生至-800V以上，水滴滚落清洗可使压降恢复至121Pa，对PM 2.5的过滤效率保持在97.7%以上。
以上实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

  1. 一种可循环使用驻极体过滤膜的制备方法，其特征在于，包括以下步骤：     将含氟聚合物颗粒和聚氧化乙烯颗粒溶解于去离子水中配置成纺丝液，后经静电纺丝，煅烧，冷却干燥，电晕充电得到可循环使用驻极体过滤膜。
  2. 根据权利要求1所述的可循环使用驻极体过滤膜的制备方法，其特征在于，所述含氟聚合物颗粒为聚四氟乙烯、全氟乙烯丙烯共聚物中的一种以上；所述含氟聚合物颗粒与聚氧化乙烯颗粒的质量比为15:1-25:1；所述纺丝液中聚氧化乙烯的质量分数为3-7%。
  3. 根据权利要求1所述的可循环使用驻极体过滤膜的制备方法，其特征在于，所述煅烧的温度为350-400℃，时间为5-10min；
    所述电晕充电的充电条件为：电压（-10）-（-15）kV, 针到接地板距离为3-5cm，充电时间为5-10min。
  4. 根据权利要求1所述的可循环使用驻极体过滤膜的制备方法，其特征在于，所述静电纺丝的条件为：纺丝电压为15-25 kV,推注速度为0.06-0.12mm/min，滚筒速度为80-120r/min，环境相对湿度为40-60%RH。
  5. 根据权利要求1所述的可循环使用驻极体过滤膜的制备方法，其特征在于，所述的可循环使用驻极体过滤膜还包括进一步氟化改进；所述氟化改进的物质为十三氟辛基三乙氧基硅烷，十七氟癸基三乙氧基硅烷中的一种以上。
  6. 根据权利要求5所述的可循环使用驻极体过滤膜的制备方法，其特征在于，所述氟化改进具体为：采用浸涂的方式进行表面氟化；浸涂的表面氟化溶液的质量分数为2-5%。
  7. 权利要求1-6任一项所述的制备方法制备的可循环使用驻极体过滤膜，其特征在于，所述可循环使用驻极体过滤膜为表面含C-F键的静电纺丝纤维膜。
  8. 根据权利要求7所述的可循环使用驻极体过滤膜，其特征在于，所述可循环使用驻极体过滤膜的纤维直径为1-15µm，克重为50-150g/m 2，水接触角为140°-160°，初始表面电位为（-600）-（-950）V，初始压降为60-150Pa；经清洗再生后，电荷恢复率为90-125%，清灰率为90%-100%，对PM 2.5的过滤效率≥94%。
  9. 权利要求7所述的可循环使用驻极体过滤膜的清洗和电荷再生方法，其特征在于，包括如下步骤：对容尘后的可循环使用驻极体过滤膜表面进行水滴滚落清洗和摩擦电化，再经干燥，实现电荷再生和重复使用。
  10. 权利要求9所述的可循环使用驻极体过滤膜的清洗和电荷再生方法，其特征在于，所述的水滴滚落清洗和摩擦电化方法为：所述可循环使用驻极体过滤膜的倾斜角度为30°-60°；水滴连续滴落并从过滤膜表面滚落，单个水滴体积为10-100µL，下落高度为3-10cm，滴落时间间隔为1-10s，滴落总时间为5-15min；所述干燥的温度为40℃-60℃。
     
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