WO2017197812A1 - Method for preparation and activation of super-hydrophobic electret fiber material for cleaning pm2.5 - Google Patents

Method for preparation and activation of super-hydrophobic electret fiber material for cleaning pm2.5 Download PDF

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Publication number
WO2017197812A1
WO2017197812A1 PCT/CN2016/098632 CN2016098632W WO2017197812A1 WO 2017197812 A1 WO2017197812 A1 WO 2017197812A1 CN 2016098632 W CN2016098632 W CN 2016098632W WO 2017197812 A1 WO2017197812 A1 WO 2017197812A1
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Prior art keywords
cleaning
electret
solution
filter material
voltage
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Ceased
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PCT/CN2016/098632
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French (fr)
Inventor
Lizhi Zhang
Aibing BAO
Rongrong CAI
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South China University of Technology SCUT
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South China University of Technology SCUT
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Application filed by South China University of Technology SCUT filed Critical South China University of Technology SCUT
Priority to US16/300,168 priority Critical patent/US11014028B2/en
Publication of WO2017197812A1 publication Critical patent/WO2017197812A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
    • B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/66—Regeneration of the filtering material or filter elements inside the filter
    • B01D46/70—Regeneration of the filtering material or filter elements inside the filter by acting counter-currently on the filtering surface, e.g. by flushing on the non-cake side of the filter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/66—Regeneration of the filtering material or filter elements inside the filter
    • B01D46/70—Regeneration of the filtering material or filter elements inside the filter by acting counter-currently on the filtering surface, e.g. by flushing on the non-cake side of the filter
    • B01D46/71—Regeneration of the filtering material or filter elements inside the filter by acting counter-currently on the filtering surface, e.g. by flushing on the non-cake side of the filter with pressurised gas, e.g. pulsed air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/66—Regeneration of the filtering material or filter elements inside the filter
    • B01D46/785—Regeneration of the filtering material or filter elements inside the filter by electrical means, e.g. for the generation of electrostatic forces in order to reject particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/0009—After-treatment of articles without altering their shape; Apparatus therefor using liquids, e.g. solvents, swelling agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/0081—After-treatment of articles without altering their shape; Apparatus therefor using an electric field, e.g. for electrostatic charging
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
    • C08J3/093—Halogenated hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J3/095—Oxygen containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
    • C08J3/097—Sulfur containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/203—Solid polymers with solid and/or liquid additives
    • 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
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D01D5/0038—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion the fibre formed by solvent evaporation, i.e. dry electro-spinning
    • 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
    • B01D2239/04—Additives and treatments of the filtering material
    • B01D2239/0414—Surface modifiers, e.g. comprising ion exchange groups
    • B01D2239/0428—Rendering the filter material hydrophobic
    • 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
    • B01D2239/04—Additives and treatments of the filtering material
    • B01D2239/0435—Electret
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2025/00—Use of polymers of vinyl-aromatic compounds or derivatives thereof as moulding material
    • B29K2025/04—Polymers of styrene
    • B29K2025/06—PS, i.e. polystyrene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
    • B29K2027/06—PVC, i.e. polyvinylchloride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
    • B29K2027/12—Use of polyvinylhalogenides or derivatives thereof as moulding material containing fluorine
    • B29K2027/16—PVDF, i.e. polyvinylidene fluoride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29K2033/00—Use of polymers of unsaturated acids or derivatives thereof as moulding material
    • B29K2033/18—Polymers of nitriles
    • B29K2033/20—PAN, i.e. polyacrylonitrile
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29K2069/00—Use of PC, i.e. polycarbonates or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29K2075/00—Use of PU, i.e. polyureas or polyurethanes or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29K2079/00—Use of polymers having nitrogen, with or without oxygen or carbon only, in the main chain, not provided for in groups B29K2061/00 - B29K2077/00, as moulding material
    • B29K2079/08—PI, i.e. polyimides or derivatives thereof
    • B29K2079/085—Thermoplastic polyimides, e.g. polyesterimides, PEI, i.e. polyetherimides, or polyamideimides; Derivatives thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005—Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/002—Agents changing electric characteristics
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
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    • B29K2105/002—Agents changing electric characteristics
    • B29K2105/0023—Agents changing electric characteristics improving electric conduction
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    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
    • B29K2995/0037—Other properties
    • B29K2995/0093—Other properties hydrophobic
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29L2031/14—Filters
    • 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
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
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    • D06M2200/12—Hydrophobic properties
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    • D10B2321/04—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of halogenated hydrocarbons
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Definitions

  • the present invention relates to a method for preparation and activation a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5, and belongs to the field of air cleaning and indoor air quality.
  • High-performance electret filter material for cleaning PM2.5 is not only required to have the characteristics of high efficiency and low resistance, but also required to hold a surface charge for a long time in humid air.
  • the traditional electret filter materials for cleaning PM2.5 are all hydrophilic materials, which are not carried out a surface treatment, so that the surface potential will be decayed and eventually disappear after using a period of time.
  • the traditional electret filter material for cleaning PM2.5 will be significantly dropped in the filtration performance, and the re-production of the filter material will directly lead to the increased production cost.
  • the present invention provides a super-hydrophobic electret for cleaning PM2.5, which not only can make the filter material hold charge in humid air and increase the filtration efficiency, but also can make the filter material cleaned and regenerated via a high-voltage electric field when the filter material reaches saturation in cleaning PM2.5 particle, thus achieving a long-term and high-efficient cleaning of the fiber material for PM2.5.
  • the studies of the electret air-filtering material are mainly focused on the method for preparing the electret of the filter material, which mainly employs two modes of corona discharge and thermal polarization.
  • the electret fibrous filter material having desirable effects can be prepared with the two modes, the disadvantages are obvious, such as unstable electret properties, easy to charge decay, complex device, and high cost.
  • the invention patent CN101905101A disclosed on December 8, 2010 in China describes a method for preparing a meltblown polypropylene electret filter material, which comprises extruding ultra-fine fiber via a high-speed hot air, then corona decharging to prepare electrets, and in turn prepare an electret material.
  • the invention patent US2015/0107457A1 disclosed on April 23, 2015 in USA describes that a fibrous material is prepared by a centrifugal device, and prepared an electret by corona decharging, and the prepared fibrous electret has the characteristics of high efficiency and low resistance, but the apparatus is too complicated and the cost is high.
  • the electric potential of the electret fibrous filter material is greatly influenced by the environments, for example, in humid air in southern China, such as in the region of Guangdong, the electric potential will be rapidly decayed and disappear, which greatly reduces the efficiency and service life of the filter material.
  • the invention patent CN104289042A disclosed on January 21, 2015 in China describes a method for preparing an electret nanofiber material by electrostatic spinning.
  • the fiber prepared with this method has high filtration effect, but the cleaning and regeneration of the filter material are not mentioned, so that the filter material can not work for a long time.
  • the object of the present invention is to overcome the deficiencies and disadvantages in the prior art and provide a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5.
  • the filter material is prepared by an electrostatic spinning method, comprising the steps of:
  • (1) preparation of polymer solution 0.5-5wt. %of one or more types of inorganic electret nanoparticles are added into a solvent, ultrasonically oscillated for 1-5 hr, then added 5-25wt. %of polymer, stirred on a magnetic stirrer for 6-12 h, and stood for use.
  • electrostatic spinning a non-woven fabric is pasted onto a rotating drum receiver, and adjusted the electrostatic spinning parameters to control the morphology of the electret nanofiber, with process conditions for electrostatic spinning as follows: the electric voltage is 10-30 kV, the receiving distance is 5-25 cm, the injection speed is 1-5mL/h, the temperature is 0-35 °C, and the relative humidity is 0-70%.
  • a low surface energy solution is prepared with methanol or anhydrous ethanol, with a volume ratio of the solute to the solvent in the low surface energy solution of 1: 1000.
  • a low surface energy solution is sprayed with a designed nozzle to carry out surface modification, wherein the nozzle is composed of a sampling barrel, a nitrogen bottle, a gas pipe, a gas control knob, a liquid control knob, and an injection needle; and the spraying time is 1-3 s.
  • the spinning material comprises polyvinylidene fluoride, polyvinyl chloride, polyacrylonitrile, polycarbonate, polyetherimide, polystyrene, polyurethane, and the like.
  • the inorganic electret nanoparticle comprises silicon dioxide, titanium dioxide, barium titanate, silicon nitride, and the like.
  • the low surface energy solution comprises stearic acid solution, hexadecyltrimethoxysilane solution, 1H, 1H, 2H, 2H-perfluorohydrocarbyltriethoxysilane solution, 1H, 1H, 2H, 2H-perfluorohydrocarbyltrichlorosilane solution, and the like.
  • Another object of the present invention is to achieve the cleaning and regeneration of the filter material, so as to achieve the long-term and high-efficiency cleaning of the filter material for PM2.5.
  • the cleaning and regeneration processes comprise the steps as follows:
  • a low surface energy solution is sprayed with a designed nozzle to carry out surface modification, wherein the nozzle is composed of a sampling barrel, a nitrogen bottle, a gas pipe, a gas control knob, a liquid control knob, and an injection needle; and the spraying time is 1-3 s.
  • the super-hydrophobic electret nanofibrous filter material for cleaning PM2.5 described in the present invention is prepared by an electrostatic spinning method, wherein the method is feasible, the operation is simple, the prepared filter material can be widely used in the field of air cleaning, indoor air quality, individual protective mask filter, and high/ultra-high efficiency air filter, and the like.
  • the present invention has the beneficial effects as follows:
  • the preparation of the super-hydrophobic electret nanofiber comprises two stages -electrostatic spinning and spraying a low surface energy liquid, the preparation method is simple, and when cleaning PM2.5 particle, the prepared electret fiber not only has the characteristics of high efficiency and low resistance, but also has the super-hydrophobic effect, and can hold a surface potential for a long time in humid air. Due to the super-hydrophobic effect, the super-hydrophobic electret nanofiber can effectively inhibit the growth of bacteria and microorganisms on the filter material, so as to protect the filter material.
  • the invention also relates to the cleaning and regeneration of the electret fiber, which increases the durability of the electret filter material, so as to achieve the long-term and high-efficient cleaning of the filter material for PM2.5.
  • FIG. 1 is a diagram showing an electrostatic spinning apparatus.
  • a non-woven fabric is pasted onto a rotating drum receiver 2;
  • 1 is the electric motor of the rotating drum receiver;
  • 3 is the injection system of the electrostatic spinning apparatus, which is composed of a syringe and an push injector;
  • 4 is an electrostatic high-voltage supply system. After the high-voltage is applied, the syringe is pushed by the push injector, and a nanofiber is ejected from the syringe, and received on the rotating drum receiver.
  • Figure 2 is a diagram showing a low surface energy solution nozzle.
  • 10 is a high-pressure nitrogen bottle, the nitrogen bottle is opened, the pressure at the gas outlet is controlled via a control valve 9, the gas flow is further controlled via a gas control knob 8, a low surface energy solution is poured into a sampling barrel 5, the low surface energy liquid flow is controlled via a liquid control knob 6, and a liquid is ejected from a nozzle 7 after these controls are finished.
  • FIG 3 is a diagram showing a filter material regeneration apparatus.
  • the filter material 13 is placed in a high-voltage electric field via a clamping tool, and the filter material is carried out a charge regeneration between the positive electrode plate 12 and the negative electrode plate 11, by regulating the high-voltage regulator 14.
  • FIG. 1 is a diagram showing an electrostatic spinning apparatus.
  • a non-woven fabric is pasted onto a rotating drum receiver 2;
  • 1 is the electric motor of the rotating drum receiver;
  • 3 is the injection system of the electrostatic spinning apparatus, which is composed of a syringe and an push injector;
  • 4 is an electrostatic high-voltage supply system. After the high-voltage is applied, the syringe is pushed by the push injector, and a nanofiber is ejected from the syringe, and received on the rotating drum receiver.
  • Figure 2 is a diagram showing a low surface energy solution nozzle.
  • 10 is a high-pressure nitrogen bottle, the nitrogen bottle is opened, the pressure at the gas outlet is controlled via a control valve 9, the gas flow is further controlled via a gas control knob 8, a low surface energy solution is poured into a sampling barrel 5, the low surface energy liquid flow is controlled via a liquid control knob 6, and a liquid is ejected from a nozzle 7 after these controls are finished.
  • FIG 3 is a diagram showing a filter material regeneration apparatus.
  • the filter material 13 is placed in a high-voltage electric field via a clamping tool, and the filter material is carried out a charge regeneration between the positive electrode plate 12 and the negative electrode plate 11, by regulating the high-voltage regulator 14.
  • a method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5 comprises the steps of:
  • step 1 polyvinyl chloride powders are placed in a vacuum oven at 60°C and dried for 2 h.
  • step 2 10.875g of N, N-dimethylformamide and 10.875g of tetrahydrofuran are accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.25 g of silicon dioxide is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 1 h, the beaker is removed, then 3g dried polyvinyl chloride powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 6 hr, so as to prepare an uniform and stable solution;
  • step 3 the electrostatic apparatus as shown in figure 1 is used to spin, a well-cut non-woven fabric is pasted onto the rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min; the translation speed of the injection device is 60mm/min; the receiving distance is 15cm; the electrostatic high-voltage is 15kV; and the injection speed is 1mL/h
  • step 4 preparation of low surface energy solution: 100 mL of anhydrous ethanol is accurately metered, added 6 drops of 1H, 1H, 2H, 2H-perfluorohydrocarbyltriethoxysilane, and stood for 2 hr.
  • the prepared solution is poured into a spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
  • the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 200-600nm, grams per square meter of 2g/m 2 , a surface electrostatic potential of 3500V, a filtration efficiency for the particle with a diameter of 0.3 ⁇ m of 99.01%, a pressure drop of 18Pa and a hydrophobic angle of 152°.
  • step 6 when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3.
  • a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 10KV, the distance between the positive electrode and the negative electrode is 20 mm, and the processing time is 10s; the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material.
  • ventilation and purging are carried out.
  • the cleaned filter material is sprayed with the apparatus as shown in figure 2, with a spraying time of 3s.
  • the filter material is placed in a high-voltage electric field again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed, likewise, the high-voltage electric voltage is 10kV; the distance between the positive electrode and the negative electrode is 20 mm; the processing time is 10 s, after the regeneration is finished, the cleaning operation is carried out again.
  • a method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5 comprises the steps of:
  • step 1 polyvinylidene fluoride powders are placed in a vacuum oven at 60°C and dried for 2 h.
  • step 2 9g of N, N-dimethylformamide and 9g of butanone are accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.2g of barium titanate is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 2 h, the beaker is removed, then 2g dried polyvinylidene fluoride powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 6 hr, so as to prepare an uniform and stable solution;
  • step 3 the electrostatic apparatus as shown in figure 1 is used to spin, and a well-cut non-woven fabric is pasted onto the rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min; the translation speed of the injection device is 60mm/min; the receiving distance is 12cm; the electrostatic high-voltage is 15kV; and the injection speed is 1mL/h
  • step 4 preparation of low surface energy solution: 100 mL of methanol is accurately metered, added 6 drops of hexadecyltrimethoxy silane, and stood for 2 hr. The prepared solution is poured into a spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
  • step 5 the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 100-500nm, grams per square meter of 2.75g/m 2 , a surface electrostatic potential of 2900V, a filtration efficiency for the particles with a diameter of 0.3 ⁇ m of 99.56%, a pressure drop of 16Pa and a hydrophobic angle of 154°.
  • step 6 when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3. Firstly, a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 12KV, the distance between the positive electrode and the negative electrode is 30mm, and the processing time is 8S, the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material. In order to improve the cleaning effect, at the same time ventilation and purging are carried out. The cleaned filter material is sprayed again with the apparatus as shown in figure 2, with a spraying time of 3s.
  • the filter material is placed in a high voltage electric field again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed, likewise, the high-voltage electric voltage is 12KV, the distance between the positive electrode and the negative electrode is 30mm, the processing time is 8 s; after the regeneration is finished, the cleaning operation is carried out again.
  • a method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5 comprises the steps of:
  • step 1 polyacrylonitrile resin is placed in a vacuum oven at 60°C and dried for 2 h.
  • step 2 26.7g of N, N-dimethylformamide is accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.3g of silicon nitride is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 2 h, the beaker is removed, then 3.3g dried polyacrylonitrile powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 8 hr, so as to prepare an uniform and stable solution;
  • step 3 the electrostatic apparatus as shown in figure 1 is used to spin, a well-cut non-woven fabric is pasted onto a rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min; the translation speed of the injection device is 60mm/min; the receiving distance is 20cm; the electrostatic high-voltage is 20KV; and the injection speed is 1mL/h
  • step 4 preparation of low surface energy solution: 100 mL of methanol is accurately metered, added 6 drops of stearic acid, and stood for 2 hr. The prepared solution is poured into a spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
  • the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 200-600nm, grams per square meter of 3.25g/m 2 , a surface electrostatic potential of 3100V, a filtration efficiency for the particles with a diameter of 0.3 ⁇ m of 99.67%, a pressure drop of 18Pa and a hydrophobic angle of 151°.
  • step 6 when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3. Firstly, a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 18KV, the distance between the positive electrode and the negative electrode is 25mm, and the processing time is 8S; the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material. In order to improve the cleaning effect, at the same time ventilation and purging are carried out. The cleaned filter material is sprayed again with the apparatus as shown in figure 2, with a spraying time of 3s.
  • the filter material is placed in a high-voltage electric field again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed, likewise, the high-voltage electric voltage is 18KV, the distance between the positive electrode and the negative electrode is 25mm, the processing time is 8 s; and after the regeneration is finished, the cleaning operation is carried out again.
  • a method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5 comprises the steps of:
  • step 1 polycarbonate powders are placed in a vacuum oven at 60°C and dried for 2 h.
  • step 2 27g of dichloromethane is accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.3g of titanium dioxide is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 3 h, the beaker is removed, then 3g dried polycarbonate powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 6 hr, so as to prepare an uniform and stable solution;
  • step 3 the electrostatic apparatus as shown in figure 1 is used to spin, a well-cut non-woven fabric is pasted onto a rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min; the translation speed of the injection device is 60mm/min; the receiving distance is 18cm; the electrostatic high-voltage is 18KV; and the injection speed is 1mL/h
  • step 4 preparation of low surface energy solution: 100 mL of anhydrous ethanol is accurately metered, added 6 drops of 1H, 1H, 2H, 2H-perfluorohydrocarbyltrichlorosilane, and stood for 2 hr.
  • the prepared solution is poured into the spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
  • step 5 the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 100-400nm, grams per square meter of 1.8g/m 2 , a surface electrostatic potential of 2500V, a filtration efficiency for the particles with a diameter of 0.3 ⁇ m of 99.46%, a pressure drop of 14Pa and a hydrophobic angle of 156°.
  • step 6 when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3.
  • a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 15KV, the distance between the positive electrode and the negative electrode is 40mm, and the processing time is 10S; the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material.
  • ventilation and purging are carried out.
  • the cleaned filter material is sprayed again with the apparatus as shown in figure 2, with a spraying time of 3s.
  • the filter material is placed in a high voltage electric field again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed, likewise, the high-voltage electric voltage is 15KV, the distance between the positive electrode and the negative electrode is 40mm, the processing time is 8 s; and after the regeneration is finished, the cleaning operation is carried out again.
  • a method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5 comprises the steps of:
  • step 1 polyetherimide powders are placed in a vacuum oven at 60°C and dried for 2 h.
  • step 2 10g of N, N-N, N-dimethylformamide and 10g of methyl pyrrolidone are accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.25g of silicon dioxide is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 3 h, the beaker is removed, then 5g dried polyetherimide powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 6 hr, so as to prepare an uniform and stable solution;
  • step 3 the electrostatic apparatus as shown in figure 1 is used to spin, a well-cut non-woven fabric is pasted onto a rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min; the translation speed of the injection device is 60mm/min; the receiving distance is 15cm; the electrostatic high-voltage is 20KV; and the injection speed is 1mL/h
  • step 4 preparation of low surface energy solution: 100 mL of anhydrous ethanol is accurately metered, added 6 drops of 1H, 1H, 2H, 2H-perfluorohydrocarbyltrichlorosilane, and stood for 2 hr.
  • the prepared solution is poured into the spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
  • step 5 the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 300-800nm, grams per square meter of 3.65g/m 2 , a surface electrostatic potential of 3000V, a filtration efficiency for the particles with a diameter of 0.3 ⁇ m of 99.23%, a pressure drop of 16Pa and a hydrophobic angle of 153°.
  • step 6 when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3. Firstly, a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 15KV, the distance between the positive electrode and the negative electrode is 15mm, and the processing time is 20S; the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material. In order to improve the cleaning effect, at the same time ventilation and purging are carried out. The cleaned filter material is sprayed again with the apparatus as shown in figure 2, with a spraying time of 3s.
  • the filter material is placed in a high voltage electric field again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed, likewise, the high-voltage electric voltage is 15KV, the distance between the positive electrode and the negative electrode is 15mm, and the processing time is 20 s; and after the regeneration is finished, the cleaning operation is carried out again.

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Abstract

Disclosed is a method for preparation and activation of a super hydrophobic electret nanofibrous filter material for cleaning PM2.5, comprising the steps as follows: (1)dissolving polymer powders and resin into a corresponding solvent so as to prepare a polymer solution, then stirring on a magnetic stirrer and standing for use; (2) in order to reinforce the electrostatic effect of the fiber, before preparing the polymer solution, adding in organic electret nanoparticles into the solvent, then oscillating with an ultrasonic oscillator; (3) in order to reinforce the super hydrophobic effect of the filter, spraying a low surface energy solution on the prepared nanofiber with a designed nozzle to carry out modification.

Description

Method for preparation and activation of super-hydrophobic electret fiber material for cleaning PM2.5 Field of the invention
The present invention relates to a method for preparation and activation a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5, and belongs to the field of air cleaning and indoor air quality.
Background of the invention
High-performance electret filter material for cleaning PM2.5 is not only required to have the characteristics of high efficiency and low resistance, but also required to hold a surface charge for a long time in humid air. The traditional electret filter materials for cleaning PM2.5 are all hydrophilic materials, which are not carried out a surface treatment, so that the surface potential will be decayed and eventually disappear after using a period of time. In addition, after the surface potential is decayed, the traditional electret filter material for cleaning PM2.5 will be significantly dropped in the filtration performance, and the re-production of the filter material will directly lead to the increased production cost. Accordingly, the present invention provides a super-hydrophobic electret for cleaning PM2.5, which not only can make the filter material hold charge in humid air and increase the filtration efficiency, but also can make the filter material cleaned and regenerated via a high-voltage electric field when the filter material reaches saturation in cleaning PM2.5 particle, thus achieving a long-term and high-efficient cleaning of the fiber material for PM2.5.
At present, the studies of the electret air-filtering material are mainly focused on the method for preparing the electret of the filter material, which mainly employs two modes of corona discharge and thermal polarization. Although the electret fibrous filter material having desirable effects can be prepared with the two modes, the disadvantages are obvious, such as unstable electret properties, easy to charge decay, complex device, and high cost. The invention patent CN101905101A disclosed on December 8, 2010 in China describes a method for preparing a meltblown polypropylene electret filter material, which comprises extruding ultra-fine fiber via a high-speed hot air, then corona decharging to prepare electrets, and in turn prepare an electret material. Although the prepared electret has a high efficiency, the resistance is high and the potential decay is fast. The invention patent US2015/0107457A1 disclosed on April 23, 2015 in USA, describes that a fibrous material is prepared by a centrifugal device, and prepared an electret by corona decharging, and the prepared fibrous electret has the characteristics of high efficiency and low resistance, but the apparatus is too complicated and the cost is high. The electric potential of the electret fibrous filter material is greatly influenced by the environments, for example, in humid air in southern China, such as in the region of Guangdong, the electric potential will be rapidly decayed and disappear, which greatly reduces the efficiency and service life of the filter material. The invention patent CN104289042A disclosed on January 21, 2015 in China, describes a method for preparing an electret nanofiber material by electrostatic spinning. The fiber prepared with this method has high filtration effect, but the cleaning and regeneration of the filter material are not mentioned, so that the filter material can not work for a long time.
Content of the invention
The object of the present invention is to overcome the deficiencies and disadvantages in the prior art and provide a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5. The filter material is prepared by an electrostatic spinning method, comprising the steps of:
(1) preparation of polymer solution: 0.5-5wt. ％of one or more types of inorganic electret nanoparticles are added into a solvent, ultrasonically oscillated for 1-5 hr, then added 5-25wt. ％of polymer, stirred on a magnetic stirrer for 6-12 h, and stood for use.
(2) electrostatic spinning: a non-woven fabric is pasted onto a rotating drum receiver, and adjusted the electrostatic spinning parameters to control the morphology of the electret nanofiber, with process conditions for electrostatic spinning as follows: the electric voltage is 10-30 kV, the receiving distance is 5-25 cm, the injection speed is 1-5mL/h, the temperature is 0-35 ℃, and the relative humidity is 0-70％.
(3) preparation of low surface energy solution: a low surface energy solution is prepared with methanol or anhydrous ethanol, with a volume ratio of the solute to the solvent in the low surface energy solution of 1: 1000.
(4) spraying: a low surface energy solution is sprayed with a designed nozzle to carry out surface modification, wherein the nozzle is composed of a sampling barrel, a nitrogen bottle, a gas pipe, a gas control knob, a liquid control knob, and an injection needle； and the spraying time is 1-3 s.
The spinning material comprises polyvinylidene fluoride, polyvinyl chloride, polyacrylonitrile, polycarbonate, polyetherimide, polystyrene, polyurethane, and the like.
The inorganic electret nanoparticle comprises silicon dioxide, titanium dioxide, barium titanate, silicon nitride, and the like.
The low surface energy solution comprises stearic acid solution, hexadecyltrimethoxysilane solution, 1H, 1H, 2H, 2H-perfluorohydrocarbyltriethoxysilane solution, 1H, 1H, 2H, 2H-perfluorohydrocarbyltrichlorosilane solution, and the like.
Another object of the present invention is to achieve the cleaning and regeneration of the filter material, so as to achieve the long-term and high-efficiency cleaning of the filter material for PM2.5. The cleaning and regeneration processes comprise the steps as follows:
(1) cleaning: when the filter material reaches saturation in cleaning PM2.5 particle, the filter material is removed, then placed in a high-voltage electric field as a barrier medium, applied a high-voltage having the same charge as that of the particle, and achieved the cleaning effect due to the repulsive interaction with the particle charge； and in order to improve the cleaning effect, at the same time carried out purging, wherein during the cleaning process, the high voltage is 5-15 kV； the electrode type is plate； the area is equivalent to the area of the fiber material, the distance between the positive electrode and the negative electrode is 10-50 mm； and the processing time is not less than 5 s.
(2) spraying: a low surface energy solution is sprayed with a designed nozzle to carry out surface modification, wherein the nozzle is composed of a sampling barrel, a nitrogen bottle, a gas pipe, a gas control knob, a liquid control knob, and an injection needle； and the spraying time is 1-3 s.
(3) regeneration: the sprayed filter material is placed in a high-voltage electric field as a barrier medium again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed to carry out a high-voltage charged processing, so that the filter material  is recharged to carry out a cleaning operation, wherein during the regeneration process, the high-voltage is 5-15 kV and the processing time is not less than 5 s.
The super-hydrophobic electret nanofibrous filter material for cleaning PM2.5 described in the present invention is prepared by an electrostatic spinning method, wherein the method is feasible, the operation is simple, the prepared filter material can be widely used in the field of air cleaning, indoor air quality, individual protective mask filter, and high/ultra-high efficiency air filter, and the like.
As compared with the prior art, the present invention has the beneficial effects as follows:
(1) the preparation of the super-hydrophobic electret nanofiber comprises two stages -electrostatic spinning and spraying a low surface energy liquid, the preparation method is simple, and when cleaning PM2.5 particle, the prepared electret fiber not only has the characteristics of high efficiency and low resistance, but also has the super-hydrophobic effect, and can hold a surface potential for a long time in humid air. Due to the super-hydrophobic effect, the super-hydrophobic electret nanofiber can effectively inhibit the growth of bacteria and microorganisms on the filter material, so as to protect the filter material.
(2) The invention also relates to the cleaning and regeneration of the electret fiber, which increases the durability of the electret filter material, so as to achieve the long-term and high-efficient cleaning of the filter material for PM2.5.
Description of the drawings
Figure 1 is a diagram showing an electrostatic spinning apparatus. A non-woven fabric is pasted onto a rotating drum receiver 2； 1 is the electric motor of the rotating drum receiver； 3 is the injection system of the electrostatic spinning apparatus, which is composed of a syringe and an push injector； and 4 is an electrostatic high-voltage supply system. After the high-voltage is applied, the syringe is pushed by the push injector, and a nanofiber is ejected from the syringe, and received on the rotating drum receiver.
Figure 2 is a diagram showing a low surface energy solution nozzle. 10 is a high-pressure nitrogen bottle, the nitrogen bottle is opened, the pressure at the gas outlet is controlled via a control valve 9, the gas flow is further controlled via a gas control knob 8, a low surface energy solution is poured into a sampling barrel 5, the low surface energy liquid flow is controlled via a liquid control knob 6, and a liquid is ejected from a nozzle 7 after these controls are finished.
Figure 3 is a diagram showing a filter material regeneration apparatus. The filter material 13 is placed in a high-voltage electric field via a clamping tool, and the filter material is carried out a charge regeneration between the positive electrode plate 12 and the negative electrode plate 11, by regulating the high-voltage regulator 14.
Detailed description of the invention
The method for preparation and activation of the super-hydrophobic electret nanofibrous filter material for cleaning PM2.5 is described in detail below in combination with the drawings.
Figure 1 is a diagram showing an electrostatic spinning apparatus. A non-woven fabric is pasted onto a rotating drum receiver 2； 1 is the electric motor of the rotating drum receiver； 3 is the injection system of the electrostatic spinning apparatus, which is composed of a syringe and an push injector； and 4 is an electrostatic high-voltage supply system. After the high-voltage is  applied, the syringe is pushed by the push injector, and a nanofiber is ejected from the syringe, and received on the rotating drum receiver.
Figure 2 is a diagram showing a low surface energy solution nozzle. 10 is a high-pressure nitrogen bottle, the nitrogen bottle is opened, the pressure at the gas outlet is controlled via a control valve 9, the gas flow is further controlled via a gas control knob 8, a low surface energy solution is poured into a sampling barrel 5, the low surface energy liquid flow is controlled via a liquid control knob 6, and a liquid is ejected from a nozzle 7 after these controls are finished.
Figure 3 is a diagram showing a filter material regeneration apparatus. The filter material 13 is placed in a high-voltage electric field via a clamping tool, and the filter material is carried out a charge regeneration between the positive electrode plate 12 and the negative electrode plate 11, by regulating the high-voltage regulator 14.
Example 1
A method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5, comprises the steps of:
step 1: polyvinyl chloride powders are placed in a vacuum oven at 60℃ and dried for 2 h.
step 2: 10.875g of N, N-dimethylformamide and 10.875g of tetrahydrofuran are accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.25 g of silicon dioxide is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 1 h, the beaker is removed, then 3g dried polyvinyl chloride powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 6 hr, so as to prepare an uniform and stable solution；
step 3: the electrostatic apparatus as shown in figure 1 is used to spin, a well-cut non-woven fabric is pasted onto the rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min； the translation speed of the injection device is 60mm/min； the receiving distance is 15cm； the electrostatic high-voltage is 15kV； and the injection speed is 1mL/h
step 4: preparation of low surface energy solution: 100 mL of anhydrous ethanol is accurately metered, added 6 drops of 1H, 1H, 2H, 2H-perfluorohydrocarbyltriethoxysilane, and stood for 2 hr. The prepared solution is poured into a spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
step 5: the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 200-600nm, grams per square meter of 2g/m2, a surface electrostatic potential of 3500V, a filtration efficiency for the particle with a diameter of 0.3μm of 99.01％, a pressure drop of 18Pa and a hydrophobic angle of 152°.
step 6: when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3. Firstly, a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 10KV, the distance between the positive electrode and the negative electrode is 20 mm, and the processing time is 10s； the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material. In order to improve the cleaning effect, at the same time ventilation and purging are carried out. The cleaned filter material is sprayed with the apparatus as shown in figure 2, with a spraying time of 3s. After the spraying is finished, the filter material is placed in a high-voltage electric field again, and the positive electrode and the negative electrode in the high-voltage  electric field are reversed, likewise, the high-voltage electric voltage is 10kV； the distance between the positive electrode and the negative electrode is 20 mm； the processing time is 10 s, after the regeneration is finished, the cleaning operation is carried out again.
Example 2
A method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5, comprises the steps of:
step 1: polyvinylidene fluoride powders are placed in a vacuum oven at 60℃ and dried for 2 h.
step 2: 9g of N, N-dimethylformamide and 9g of butanone are accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.2g of barium titanate is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 2 h, the beaker is removed, then 2g dried polyvinylidene fluoride powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 6 hr, so as to prepare an uniform and stable solution；
step 3: the electrostatic apparatus as shown in figure 1 is used to spin, and a well-cut non-woven fabric is pasted onto the rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min； the translation speed of the injection device is 60mm/min； the receiving distance is 12cm； the electrostatic high-voltage is 15kV； and the injection speed is 1mL/h
step 4: preparation of low surface energy solution: 100 mL of methanol is accurately metered, added 6 drops of hexadecyltrimethoxy silane, and stood for 2 hr. The prepared solution is poured into a spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
step 5: the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 100-500nm, grams per square meter of 2.75g/m2, a surface electrostatic potential of 2900V, a filtration efficiency for the particles with a diameter of 0.3μm of 99.56％, a pressure drop of 16Pa and a hydrophobic angle of 154°.
step 6: when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3. Firstly, a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 12KV, the distance between the positive electrode and the negative electrode is 30mm, and the processing time is 8S, the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material. In order to improve the cleaning effect, at the same time ventilation and purging are carried out. The cleaned filter material is sprayed again with the apparatus as shown in figure 2, with a spraying time of 3s. After the spraying is finished, the filter material is placed in a high voltage electric field again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed, likewise, the high-voltage electric voltage is 12KV, the distance between the positive electrode and the negative electrode is 30mm, the processing time is 8 s； after the regeneration is finished, the cleaning operation is carried out again.
Example 3
A method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5, comprises the steps of:
step 1: polyacrylonitrile resin is placed in a vacuum oven at 60℃ and dried for 2 h. 
step 2: 26.7g of N, N-dimethylformamide is accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.3g of silicon nitride is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 2 h, the beaker is removed, then 3.3g dried polyacrylonitrile powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 8 hr, so as to prepare an uniform and stable solution；
step 3: the electrostatic apparatus as shown in figure 1 is used to spin, a well-cut non-woven fabric is pasted onto a rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min； the translation speed of the injection device is 60mm/min； the receiving distance is 20cm； the electrostatic high-voltage is 20KV； and the injection speed is 1mL/h
step 4: preparation of low surface energy solution: 100 mL of methanol is accurately metered, added 6 drops of stearic acid, and stood for 2 hr. The prepared solution is poured into a spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
step 5: the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 200-600nm, grams per square meter of 3.25g/m2, a surface electrostatic potential of 3100V, a filtration efficiency for the particles with a diameter of 0.3μm of 99.67％, a pressure drop of 18Pa and a hydrophobic angle of 151°.
step 6: when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3. Firstly, a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 18KV, the distance between the positive electrode and the negative electrode is 25mm, and the processing time is 8S； the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material. In order to improve the cleaning effect, at the same time ventilation and purging are carried out. The cleaned filter material is sprayed again with the apparatus as shown in figure 2, with a spraying time of 3s. After the spraying is finished, the filter material is placed in a high-voltage electric field again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed, likewise, the high-voltage electric voltage is 18KV, the distance between the positive electrode and the negative electrode is 25mm, the processing time is 8 s； and after the regeneration is finished, the cleaning operation is carried out again.
Example 4
A method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5, comprises the steps of:
step 1: polycarbonate powders are placed in a vacuum oven at 60℃ and dried for 2 h.
step 2: 27g of dichloromethane is accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.3g of titanium dioxide is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 3 h, the beaker is removed, then 3g dried polycarbonate powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 6 hr, so as to prepare an uniform and stable solution；
step 3: the electrostatic apparatus as shown in figure 1 is used to spin, a well-cut non-woven fabric is pasted onto a rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min； the translation speed of the injection  device is 60mm/min； the receiving distance is 18cm； the electrostatic high-voltage is 18KV； and the injection speed is 1mL/h
step 4: preparation of low surface energy solution: 100 mL of anhydrous ethanol is accurately metered, added 6 drops of 1H, 1H, 2H, 2H-perfluorohydrocarbyltrichlorosilane, and stood for 2 hr. The prepared solution is poured into the spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
step 5: the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 100-400nm, grams per square meter of 1.8g/m2, a surface electrostatic potential of 2500V, a filtration efficiency for the particles with a diameter of 0.3μm of 99.46％, a pressure drop of 14Pa and a hydrophobic angle of 156°.
step 6: when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3. Firstly, a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 15KV, the distance between the positive electrode and the negative electrode is 40mm, and the processing time is 10S； the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material. In order to improve the cleaning effect, at the same time ventilation and purging are carried out. The cleaned filter material is sprayed again with the apparatus as shown in figure 2, with a spraying time of 3s. After the spraying is finished, the filter material is placed in a high voltage electric field again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed, likewise, the high-voltage electric voltage is 15KV, the distance between the positive electrode and the negative electrode is 40mm, the processing time is 8 s； and after the regeneration is finished, the cleaning operation is carried out again.
Example 5
A method for preparation and activation of a super-hydrophobic electret nanofibrous filter material for cleaning PM2.5, comprises the steps of:
step 1: polyetherimide powders are placed in a vacuum oven at 60℃ and dried for 2 h.
step 2: 10g of N, N-N, N-dimethylformamide and 10g of methyl pyrrolidone are accurately weighed with an electronic balance, and placed in a 50mL beaker, then 0.25g of silicon dioxide is weighed, and placed in the solution, oscillated with an ultrasonic oscillator for 3 h, the beaker is removed, then 5g dried polyetherimide powders are accurately weighed with an electronic balance, and placed in the beaker, the beaker is placed on a magnetic stirrer and stirred for 6 hr, so as to prepare an uniform and stable solution；
step 3: the electrostatic apparatus as shown in figure 1 is used to spin, a well-cut non-woven fabric is pasted onto a rotating drum, and the electrostatic spinning parameters are adjusted as follows: the receiving speed of the rotating drum is 25r/min； the translation speed of the injection device is 60mm/min； the receiving distance is 15cm； the electrostatic high-voltage is 20KV； and the injection speed is 1mL/h
step 4: preparation of low surface energy solution: 100 mL of anhydrous ethanol is accurately metered, added 6 drops of 1H, 1H, 2H, 2H-perfluorohydrocarbyltrichlorosilane, and stood for 2 hr. The prepared solution is poured into the spraying device as shown in figure 2, then the surface of the electret fiber is modified with the low surface energy solution, and the spraying time is 3s.
step 5: the nanofiber layer in the prepared super-hydrophobic electret material for cleaning PM2.5 has a diameter of 300-800nm, grams per square meter of 3.65g/m2, a surface electrostatic  potential of 3000V, a filtration efficiency for the particles with a diameter of 0.3μm of 99.23％, a pressure drop of 16Pa and a hydrophobic angle of 153°.
step 6: when the super-hydrophobic electret material reaches saturation in cleaning PM2.5 particle, the electret filter material is removed, and cleaned and regenerated in the high-voltage electric field as shown in figure 3. Firstly, a high-voltage having the same charge as that of the particle is applied, wherein the electric potential is 15KV, the distance between the positive electrode and the negative electrode is 15mm, and the processing time is 20S； the particle will be shed from the filter material due to the repulsive effect, thus achieving the cleaning of the filter material. In order to improve the cleaning effect, at the same time ventilation and purging are carried out. The cleaned filter material is sprayed again with the apparatus as shown in figure 2, with a spraying time of 3s. After the spraying is finished, the filter material is placed in a high voltage electric field again, and the positive electrode and the negative electrode in the high-voltage electric field are reversed, likewise, the high-voltage electric voltage is 15KV, the distance between the positive electrode and the negative electrode is 15mm, and the processing time is 20 s； and after the regeneration is finished, the cleaning operation is carried out again.

Claims (10)

  1. A method for preparation and activation of a super-hydrophobic electret nanofibrous material for high-efficient cleaning PM2.5, characterized by comprising the steps as follows: the fibrous material is prepared by an electrostatic spinning method, wherein the spinning material comprises polyvinylidene fluoride, polyvinyl chloride, polyacrylonitrile, polycarbonate, polyetherimide, polystyrene, polyurethane and the like； and in order to reinforce the electrostatic effect of the nanofiber layer, inorganic electret nanoparticles are added into the spinning solution, wherein the inorganic electret nanoparticle comprises silicon dioxide, titanium dioxide, barium titanate, silicon nitride and the like； then the prepared nanofiber is modified with a low surface energy solution which is sprayed from a designed nozzle, wherein the low surface energy solution comprises stearic acid solution, hexadecyltrimethoxysilane solution, 1H, 1H, 2H, 2H-perfluorohydrocarbyltriethoxysilane solution, 1H, 1H, 2H, 2H-perfluorohydrocarbyltrichlorosilane solution, and the like.
  2. A method for preparation and activation of a super-hydrophobic electret nanofibrous material for high-efficient cleaning PM2.5, characterized by comprising a method for cleaning and the regeneration of the filter material, wherein a cleaning and regeneration apparatus comprises filter material, positive plate electrode, negative plate electrode, high-voltage generator, power supply, and nozzle.
  3. The method of claim1, wherein the electrostatic spinning method comprises the steps as follows:
    (1) preparation of polymer solution: 0.5-5wt. ％ of one or more types of the inorganic electret nanoparticles are added into a solvent and ultrasonically oscillated for 1-5 hr, then added 5-25wt. ％ of polymer, then stirred on a magnetic stirrer for 6-12 hr, and stood for use,
    (2) electrostatic spinning: a non-woven fabric is pasted on a rotating drum receiver, adjusted the electrostatic spinning parameters to control the morphology of the electret nanofiber, wherein the process conditions for electrostatic spinning are as follows: the electric voltage is 10-30kV, the receiving distance is 5-25cm, the injection speed is 1-5mL/h, the temperature is 0-35℃, and the relative humidity is 0-70％.
  4. The method of claim 1, wherein the method for super-hydrophobization of the electret nanofiber layer comprises the steps as follows:
    (1) preparation of low surface energy solution: a low surface energy solution is prepared with methanol or anhydrous ethanol, wherein the volume fraction of the solute to the solvent in the low surface energy solution is 1: 1000,
    (2) spraying: the low surface energy solution is sprayed with a designed nozzle to carry out surface modification, wherein the nozzle is composed of a sampling barrel, a nitrogen bottle, a gas pipe, a gas control knob, a liquid control knob, and an injection needle, and the spraying time is 1-3 s.
  5. The method of claim 2, wherein the method for cleaning and regeneration of the fiber material comprises the steps as follows:
    (1) cleaning: when the fiber material reaches saturation in cleaning PM2.5 particles, the fiber material is removed and placed in a high-voltage electric field as a barrier medium, applied a  high-voltage having the same charge as that of the particle, and at the same time carrying out purging, thus due to the repulsive interaction with the particle charge, obtaining the cleaning effect, and the particulates being taken away with the purging gas； wherein during the cleaning process, the high-voltage is 5-15kV, the electrode type is plate； the area is equivalent to the area of the fiber material, the distance between the positive electrode and the negative electrode is10-50mm； and the processing time is not less than 5 s,
    (2) spraying: a low surface energy solution is sprayed with a designed nozzle to carry out surface modification, wherein the nozzle is composed of a sampling barrel, a nitrogen bottle, a gas pipe, a gas control knob, a liquid control knob, and an injection needle； and the spraying time is 1-3 s,
    (3) regeneration: the sprayed filter material is placed in a high-voltage electric field as a barrier medium again, the positive electrode and the negative electrode in the high-voltage electric field are reversed to carry out a high-voltage charged processing, so that the filter material is recharged and carried out a cleaning operation, wherein during the regeneration process, the high-voltage is 5-15kV and the processing time is not less than 5s.
  6. The method of claim 1, wherein the solute and the solvent in the polymer solution respectively comprise:
    polyvinylidene fluoride: N, N-dimethylformamide and butanone in a mass ratio of 1: 1
    polyvinyl chloride: N, N-dimethylformamide and tetrahydrofuran in a mass ratio of 1: 1；
    polyacrylonitrile: N, N-dimethylformamide；
    polycarbonate: dichloromethane；
    polyetherimide: N, N-dimethylformamide and methyl pyrrolidone in a mass ratio of 1: 1；
    polystyrene: N, N-dimethylformamide and tetrahydrofuran in a mass ratio of 3: 1； and
    polyurethane: butanone.
  7. The method of claim 1, wherein the polymer solution comprises one or more types of inorganic electret nanoparticles, the inorganic electret nanoparticle comprises silicon dioxide, titanium dioxide, barium titanate, and silicon nitride, and the specification of the inorganic electret nanoparticle respectively comprises:
    silicon dioxide: 99.5％, 15nm；
    titanium dioxide: 99.8％, 40nm；
    barium titanate: 99.9％, <100nm；
    silicon nitride : 95％, 85nm.
  8. The method of claim 1, wherein the solute and the solvent in the low surface energy solution respectively comprise:
    stearic acid: anhydrous ethanol；
    hexadecyltrimethoxysilane: methanol；
    1H, 1H, 2H, 2H-perfluorohydrocarbyltriethoxysilane: anhydrous ethanol；
    1H, 1H, 2H, 2H-perfluorohydrocarbyltrichlorosilane: anhydrous ethanol.
  9. The method of claim 1, wherein the filter material has a two-layer structure of non-woven fabric and super-hydrophobic electret nanofiber, the grams per square meter of the non-woven  fabric is 100-350 g/m2, the thickness is 1-10mm, and the filtration efficiency of the blank non-woven fabric for small particle having a particle diameter of 0.3 μm is 13.47％.
  10. The method of claim 1, wherein the filter material has a two-layer structure of non-woven fabric and super-hydrophobic electret nanofiber, the nanofiber layer has a nanofiber diameter between 100 nm and 900 nm, a grams per square meter of 0.01-5g/m2, a porosity of ≥85％， a surface potential of 1000V-4000V, a hydrophobic angle of more than 150°, a filtration efficiency for the particle having a particle diameter range of 0.3-10μm of up to 99％, and a pressure drop of less than 20 Pa.
PCT/CN2016/098632 2016-05-17 2016-09-10 Method for preparation and activation of super-hydrophobic electret fiber material for cleaning pm2.5 Ceased WO2017197812A1 (en)

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