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CN103170400B - The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone and hydrogen peroxide - Google Patents

The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone and hydrogen peroxide Download PDF

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Publication number
CN103170400B
CN103170400B CN201310116643.8A CN201310116643A CN103170400B CN 103170400 B CN103170400 B CN 103170400B CN 201310116643 A CN201310116643 A CN 201310116643A CN 103170400 B CN103170400 B CN 103170400B
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ptfe
polytetrafluoroethylene
hydrogen peroxide
raw material
ultraviolet
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CN103170400A (en
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顾建忠
吴明红
蔡建球
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TAICANG JINKAI SPECIAL CABLE CO Ltd
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TAICANG JINKAI SPECIAL CABLE CO Ltd
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Priority to PCT/CN2013/000797 priority patent/WO2014161113A1/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/12Powdering or granulating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/28Treatment by wave energy or particle radiation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/18Homopolymers or copolymers of tetrafluoroethylene

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

A method for ultrafine PTFE powder prepared by ultraviolet combined with ozone and hydrogen peroxide, is specially: the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen chilling; Being ground into particle diameter with pulverizer is again 100-1000 μm; Then be put in the pallet on the platform of ultraviolet irradiation case; Ozone is poured to described ultraviolet irradiation case; Airtight described ultraviolet irradiation case, and the controlling organization opening spray equipment is to the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide in described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 3%-8%; With ultraviolet continuous irradiation 8-12 hour; Irradiation is complete, combustion gas; Take out and put into airflow comminution system, fully pulverizing and can obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm.Adopt technique scheme, the present invention can produce superfine powder of polytetrafluoroethylene efficiently, the production technology that can effectively reduce costs again.

Description

The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone and hydrogen peroxide
Technical field
The present invention relates to the preparation method of superfine powder of polytetrafluoroethylene, prepare the method for ultrafine PTFE powder in particular to ultraviolet irradiation combined with ozone and hydrogen peroxide.
Background technology
Polytetrafluoroethylene (PTFE) is commonly called as King, is the polymer be polymerized by tetrafluoroethylene monomer, has very strong coherency, and resin is easy to be attached to together, not easily disperses.Ultrafine PTFE powder (micro mist) is low-molecular-weight polytetrafluoroethylene (PTFE), reach the ultrafine PTFE powder of ultra-fine degree, molecular weight is lower than less than 10,000, particle diameter is serial at the PTFE micro mist of 0.5-15 μm, not only remain the original all premium properties of polytetrafluoroethylene (PTFE), also there is the performance of many uniquenesses: as without self-coagulation, without electrostatic effect, intermiscibility is good, molecular weight is low, good dispersion, self lubricity are high, coefficient of friction reduce, not conglomeration, easily mix mutually with oily or organic liquid, with other solia particle also can Homogeneous phase mixing obvious etc.Ultrafine PTFE powder average grain diameter is less than 5 μm, and specific surface is greater than 10m 2/ g, coefficient of friction 0.06 ~ 0.07, lubricity is good, can be dispersed in well in many materials.Can be used as plastics, rubber, ink, coating, anti-stick, the antifriction of lubricant grease, flame-retardant additive, also can make aerosol etc. as dry lubricant.Ultrafine PTFE powder can be made separately kollag and use, also can as the additive of plastics, rubber, coating, ink, lubricating oil, lubricating grease etc.With can by various typical powder process method when plastics or rubber mix, as blended etc., in oil and grease, add superfine powder of polytetrafluoroethylene, coefficient of friction can be reduced, as long as add a few percent, just can improve the life-span of lubricating oil.Its dispersion in organic solvent also can make releasing agent.
Prepare the method for ultrafine PTFE powder, determine the structural behaviour of ultrafine PTFE powder, molecular weight and distribution thereof.The preparation method of ultrafine PTFE powder mainly contains two kinds: 1, directly regulate polymerization with TFE, after certain hour, stop polymerisation, product is suitably processed again; 2, with HMW PTFE degraded, then pulverize.The method that cracking reaction prepares ultrafine PTFE powder mainly contains thermal cracking and irradiation to crack.In irradiation to crack process, PTFE degraded is by the impact of radiation parameter, irradiation dose, the difference of the energy source that irradiation adopts and oxidizing condition, all there is considerable influence to the physical property of ultrafine PTFE powder and chemical property, therefore need be optimized the equipment and process condition in PTFE irradiation to crack process and strictly control.
Summary of the invention
The object of the invention is to, provide a kind of method that ultrafine PTFE powder prepared by ultraviolet combined with ozone and hydrogen peroxide, described method can produce superfine powder of polytetrafluoroethylene efficiently, obviously can reduce production cost again.
The method of superfine powder of polytetrafluoroethylene prepared by ultraviolet irradiation polytetrafluoroethylene (PTFE) provided by the present invention, mainly comprises the following steps:
1) the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) pulverized by the polytetrafluoroethylene (PTFE) raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) be put in the pallet on the platform of ultraviolet irradiation case by the polytetrafluoroethylene (PTFE) raw material after described pulverizing, in described pallet, the thickness of polytetrafluoroethylene (PTFE) raw material is 200mm-300mm;
4) pass into ozone to described ultraviolet irradiation case, airtight described ultraviolet irradiation case, in the ozone passed into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%-0.5%;
5) and the controlling organization opening spray equipment to the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide in described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 3%-8%;
6) ultraviolet ray generating apparatus is opened, continuous irradiation 8-12 hour;
7) after irradiation, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas produced in irradiation process is discharged;
8) opening described ultraviolet irradiation case, take out above-mentioned pallet, and the polytetrafluoroethylene (PTFE) after irradiation is put into airflow comminution system, through fully pulverizing, obtaining particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm.
Further, ultraviolet ray generating apparatus is provided with in the casing of described ultraviolet irradiation case, and the casing inner bottom part of ultraviolet irradiation case is a platform, described ultraviolet irradiation case side is provided with chamber door, and on casing, being provided with at least 1 exhaust gear and at least 1 spray equipment, the controlling organization of described spray equipment is positioned at outside chest.
Further, described ultraviolet ray generating apparatus comprises 4 or 5 Non-polarized lamps, and described Non-polarized lamp is 400W, and wavelength is 184.9nm or 253.7nm.
Further, described exhaust gear is air-tight state in irradiation process, is opening after irradiation terminates.
Further, described spray equipment is automatic spraying system, and described automatic spraying system is set to the hydrogen peroxide of the weight ratio set according to the weight automatic spray of polytetrafluoroethylene (PTFE) raw material in pallet.
Further, in pallet described in the hydrogen peroxide of described spray, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 5%.
Further, described airflow comminution system comprises airslide disintegrating mill, described airslide disintegrating mill comprises air current spray nozzle, pulverizing chamber, compressed air spurts into pulverizing chamber by nozzle at high speeds, at the joint place of multiply high pressure draught, through irradiated described polytetrafluoroethylene (PTFE) raw material by impact several times, friction, shearing and pulverizing.
Further, described airflow comminution system also comprises:
Cyclone separator, deduster and air-introduced machine;
Described airslide disintegrating mill also comprises grading room, pulverizing chamber pulverize after polytetrafluoroethylene (PTFE) at air-introduced machine move under influence to grading room, under grading wheel effect, polytetrafluoroethylgranule granule is separated by granule size, the fine grained meeting granularity requirements enters cyclone separator by grading wheel or deduster is collected, and the coarse granule not meeting granularity requirements drops to pulverizing chamber to be continued to pulverize.
Further, the air current spray nozzle of described airslide disintegrating mill is Laval nozzle.
Further, described airslide disintegrating mill has dry filtrating equipment, before described dry filtrating equipment is positioned at nozzle.
The method of ultrafine PTFE powder is prepared according to ultraviolet combined with ozone provided by the invention and hydrogen peroxide, under identical radiation parameter, degradation rate or the reduction exposure time that can increase polytetrafluoroethylene (PTFE) also can reach identical degradation rate, therefore improve production efficiency, ensure to obtain the low molecular superfine powder of polytetrafluoroethylene be of the required size, and manufacture process can strictly control, ensure the quality of production.
Detailed description of the invention
In order to make the object of the invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone provided by the invention and hydrogen peroxide, and its step comprises:
1) quenching: the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) tentatively pulverize: pulverized by the polytetrafluoroethylene (PTFE) raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) be put in the pallet on the platform of ultraviolet irradiation case by the polytetrafluoroethylene (PTFE) raw material after described pulverizing, in described pallet, the thickness of polytetrafluoroethylene (PTFE) raw material is 200mm-300mm;
4) pass into ozone to described ultraviolet irradiation case, airtight described ultraviolet irradiation case, in the ozone passed into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%-0.5%;
5) spray: and the controlling organization opening spray equipment is to the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide in described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 3%-8%;
6) ultraviolet irradiation: open ultraviolet ray generating apparatus, continuous irradiation 8-12 hour;
7) be vented: after irradiation, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas produced in irradiation process is discharged;
8) air-flow crushing: open described ultraviolet irradiation case, take out above-mentioned pallet, and the polytetrafluoroethylene (PTFE) after irradiation is put into airflow comminution system, through fully pulverizing, obtains particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm.
Wherein, described ultraviolet irradiation case is preferably the chest that appearance and size is about 2000 × 10000 × 1000mm, ultraviolet ray generating apparatus is arranged on casing inner top, casing inner bottom part is a platform, ultraviolet irradiation case side is provided with door (can open and place and take out material), has at least 1 exhaust gear at casing top.Wherein, described ultraviolet ray generating apparatus preferably includes 4-5 400W, and wavelength is set as the Non-polarized lamp of 184.9nm or 253.7nm, and described exhaust gear more preferably, can be air-tight state in irradiation process, is opening after irradiation terminates.
Wherein, described airflow comminution system comprises airslide disintegrating mill, described airslide disintegrating mill comprises air current spray nozzle, pulverizing chamber, compressed air spurts into pulverizing chamber by nozzle at high speeds, at the joint place of multiply high pressure draught, through irradiated described polytetrafluoroethylene (PTFE) raw material by impact several times, friction, shearing and pulverizing.
Described airflow comminution system can also comprise cyclone separator, deduster and air-introduced machine.Described airslide disintegrating mill preferably has air current spray nozzle, pulverizing chamber (pulverizing chamber), grading room.Compressed air spurts into pulverizing chamber by nozzle at high speeds, form the high pressure draught that multiply is intersected, at the joint place of multiply high pressure draught, through irradiated polytetrafluoroethylene (PTFE) raw material by impact several times, friction, shear and pulverize, polytetrafluoroethylene (PTFE) after pulverizing moves to grading room with ascending air under air-introduced machine draft effect, under the powerful centrifugal action that the stage turbine of High Rotation Speed produces, according to fineness degree (particle size), polytetrafluoroethylgranule granule is separated, the fine grained meeting granularity requirements (being less than 5 μm) enters deduster by grading wheel and collects, the pulverizing chamber that drops to coarse granule continues to pulverize.The air current spray nozzle of described airslide disintegrating mill is preferably Laval nozzle, for ensureing that crushing effect is better, can also settle filtration drying device (reducing the humidity of particle to be comminuted further) before nozzle.
Embodiment one
The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone provided by the invention and hydrogen peroxide, and its step comprises:
1) quenching: the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) tentatively pulverize: pulverized by the polytetrafluoroethylene (PTFE) raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) be put in the pallet on the platform of ultraviolet irradiation case by the polytetrafluoroethylene (PTFE) raw material after described pulverizing, in described pallet, the thickness of polytetrafluoroethylene (PTFE) raw material is 200mm-300mm;
4) pass into ozone to described ultraviolet irradiation case, airtight described ultraviolet irradiation case, in the ozone passed into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%;
5) spray: and the controlling organization opening spray equipment is to the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide in described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 3%;
6) ultraviolet irradiation: open ultraviolet ray generating apparatus, continuous irradiation 8 hours;
7) be vented: after irradiation, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas produced in irradiation process is discharged;
8) air-flow crushing: open described ultraviolet irradiation case, take out above-mentioned pallet, and the polytetrafluoroethylene (PTFE) after irradiation is put into airflow comminution system, through fully pulverizing, obtains particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm.
Said flow pulverizer comprises screw feeder, air current spray nozzle, pulverizing chamber, grading room, air-introduced machine, and the air current spray nozzle of airslide disintegrating mill is Laval nozzle.Airslide disintegrating mill also has dry filtrating equipment, before being positioned at nozzle.Airslide disintegrating mill put into by the polytetrafluoroethylene (PTFE) that irradiation is good, pulverizing chamber is entered by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to pulverizing chamber high velocity jet, accelerate in supersonic jet through irradiated fine polytetrafluoroethylpowder powder particle, and in the repeated stock of nozzle intersection, collision, reach pulverizing.Pulverized material enters grading room with ascending air, due to grading rotor High Rotation Speed, particle had both been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that air-flow viscous effect produces, the centrifugal force be subject to when particle is greater than centripetal force, namely the corase particles more than classification footpath returns pulverizing chamber and continues impact comminution, fine particle below classification footpath enters cyclone separator with air-flow, deduster is collected, comparatively corase particles in cyclone collection fine particle, small part ultrafine particle is collected by deduster, large about 10%-20%, gas is discharged by air-introduced machine.
Embodiment two
The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone provided by the invention and hydrogen peroxide, and its step comprises:
1) quenching: the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) tentatively pulverize: pulverized by the polytetrafluoroethylene (PTFE) raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) be put in the pallet on the platform of ultraviolet irradiation case by the polytetrafluoroethylene (PTFE) raw material after described pulverizing, in described pallet, the thickness of polytetrafluoroethylene (PTFE) raw material is 200mm-300mm;
4) pass into ozone to described ultraviolet irradiation case, airtight described ultraviolet irradiation case, in the ozone passed into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.5%;
5) spray: and the controlling organization opening spray equipment is to the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide in described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 8%;
6) ultraviolet irradiation: open ultraviolet ray generating apparatus, continuous irradiation 10 hours;
7) be vented: after irradiation, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas produced in irradiation process is discharged;
8) air-flow crushing: open described ultraviolet irradiation case, take out above-mentioned pallet, and the polytetrafluoroethylene (PTFE) after irradiation is put into airflow comminution system, through fully pulverizing, obtains particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm.
Said flow pulverizer comprises screw feeder, air current spray nozzle, pulverizing chamber, grading room, air-introduced machine, and the air current spray nozzle of airslide disintegrating mill is Laval nozzle.Airslide disintegrating mill also has dry filtrating equipment, before being positioned at nozzle.Airslide disintegrating mill put into by the polytetrafluoroethylene (PTFE) that irradiation is good, pulverizing chamber is entered by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to pulverizing chamber high velocity jet, accelerate in supersonic jet through irradiated fine polytetrafluoroethylpowder powder particle, and in the repeated stock of nozzle intersection, collision, reach pulverizing.Pulverized material enters grading room with ascending air, due to grading rotor High Rotation Speed, particle had both been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that air-flow viscous effect produces, the centrifugal force be subject to when particle is greater than centripetal force, namely the corase particles more than classification footpath returns pulverizing chamber and continues impact comminution, fine particle below classification footpath enters cyclone separator with air-flow, deduster is collected, comparatively corase particles in cyclone collection fine particle, small part ultrafine particle is collected by deduster, large about 10%-20%, gas is discharged by air-introduced machine.
Embodiment three
The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone provided by the invention and hydrogen peroxide, and its step comprises:
1) quenching: the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) tentatively pulverize: pulverized by the polytetrafluoroethylene (PTFE) raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) be put in the pallet on the platform of ultraviolet irradiation case by the polytetrafluoroethylene (PTFE) raw material after described pulverizing, in described pallet, the thickness of polytetrafluoroethylene (PTFE) raw material is 200mm-300mm;
4) pass into ozone to described ultraviolet irradiation case, airtight described ultraviolet irradiation case, in the ozone passed into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.3%;
5) spray: and the controlling organization opening spray equipment is to the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide in described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 5%;
6) ultraviolet irradiation: open ultraviolet ray generating apparatus, continuous irradiation 12 hours;
7) be vented: after irradiation, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas produced in irradiation process is discharged;
8) air-flow crushing: open described ultraviolet irradiation case, take out above-mentioned pallet, and the polytetrafluoroethylene (PTFE) after irradiation is put into airflow comminution system, through fully pulverizing, obtains particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm.
Said flow pulverizer comprises screw feeder, air current spray nozzle, pulverizing chamber, grading room, air-introduced machine, and the air current spray nozzle of airslide disintegrating mill is Laval nozzle.Airslide disintegrating mill also has dry filtrating equipment, before being positioned at nozzle.Airslide disintegrating mill put into by the polytetrafluoroethylene (PTFE) that irradiation is good, pulverizing chamber is entered by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to pulverizing chamber high velocity jet, accelerate in supersonic jet through irradiated fine polytetrafluoroethylpowder powder particle, and in the repeated stock of nozzle intersection, collision, reach pulverizing.Pulverized material enters grading room with ascending air, due to grading rotor High Rotation Speed, particle had both been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that air-flow viscous effect produces, the centrifugal force be subject to when particle is greater than centripetal force, namely the corase particles more than classification footpath returns pulverizing chamber and continues impact comminution, fine particle below classification footpath enters cyclone separator with air-flow, deduster is collected, comparatively corase particles in cyclone collection fine particle, small part ultrafine particle is collected by deduster, large about 10%-20%, gas is discharged by air-introduced machine.
Embodiment four
The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone provided by the invention and hydrogen peroxide, and its step comprises:
1) quenching: the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) tentatively pulverize: pulverized by the polytetrafluoroethylene (PTFE) raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) be put in the pallet on the platform of ultraviolet irradiation case by the polytetrafluoroethylene (PTFE) raw material after described pulverizing, in described pallet, the thickness of polytetrafluoroethylene (PTFE) raw material is 200mm-300mm;
4) pass into ozone to described ultraviolet irradiation case, airtight described ultraviolet irradiation case, in the ozone passed into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.3%;
5) spray: and the controlling organization opening spray equipment is to the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide in described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 5%;
6) ultraviolet irradiation: open ultraviolet ray generating apparatus, continuous irradiation 12 hours;
7) be vented: after irradiation, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas produced in irradiation process is discharged;
8) air-flow crushing: open described ultraviolet irradiation case, take out above-mentioned pallet, and the polytetrafluoroethylene (PTFE) after irradiation is put into airflow comminution system, through fully pulverizing, obtains particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm.
Said flow pulverizer comprises screw feeder, air current spray nozzle, pulverizing chamber, grading room, air-introduced machine, and the air current spray nozzle of airslide disintegrating mill is Laval nozzle.Airslide disintegrating mill also has dry filtrating equipment, before being positioned at nozzle.Airslide disintegrating mill put into by the polytetrafluoroethylene (PTFE) that irradiation is good, pulverizing chamber is entered by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to pulverizing chamber high velocity jet, accelerate in supersonic jet through irradiated fine polytetrafluoroethylpowder powder particle, and in the repeated stock of nozzle intersection, collision, reach pulverizing.Pulverized material enters grading room with ascending air, due to grading rotor High Rotation Speed, particle had both been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that air-flow viscous effect produces, the centrifugal force be subject to when particle is greater than centripetal force, namely the corase particles more than classification footpath returns pulverizing chamber and continues impact comminution, fine particle below classification footpath enters cyclone separator with air-flow, deduster is collected, comparatively corase particles in cyclone collection fine particle, small part ultrafine particle is collected by deduster, large about 10%-20%, gas is discharged by air-introduced machine.
Adopt in the present embodiment Non-polarized lamp due to electrodeless startup fast, and can avoid pressure drop loss when starting, service life is longer, can reach the service life of 5-6, makes the cost of this method lower.
Embodiment five
The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone provided by the invention and hydrogen peroxide, and its step comprises:
1) quenching: the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) tentatively pulverize: pulverized by the polytetrafluoroethylene (PTFE) raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) be put in the pallet on the platform of ultraviolet irradiation case by the polytetrafluoroethylene (PTFE) raw material after described pulverizing, in described pallet, the thickness of polytetrafluoroethylene (PTFE) raw material is 200mm-300mm;
4) pass into ozone to described ultraviolet irradiation case, airtight described ultraviolet irradiation case, in the ozone passed into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%;
5) spray: and the controlling organization opening spray equipment is to the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide in described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 3%;
6) ultraviolet irradiation: open ultraviolet ray generating apparatus, continuous irradiation 10 hours;
7) be vented: after irradiation, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas produced in irradiation process is discharged;
8) air-flow crushing: open described ultraviolet irradiation case, take out above-mentioned pallet, and the polytetrafluoroethylene (PTFE) after irradiation is put into airflow comminution system, through fully pulverizing, obtains particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm.
Said flow pulverizer comprises screw feeder, air current spray nozzle, pulverizing chamber, grading room, air-introduced machine, and the air current spray nozzle of airslide disintegrating mill is Laval nozzle.Airslide disintegrating mill also has dry filtrating equipment, before being positioned at nozzle.Airslide disintegrating mill put into by the polytetrafluoroethylene (PTFE) that irradiation is good, pulverizing chamber is entered by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to pulverizing chamber high velocity jet, accelerate in supersonic jet through irradiated fine polytetrafluoroethylpowder powder particle, and in the repeated stock of nozzle intersection, collision, reach pulverizing.Pulverized material enters grading room with ascending air, due to grading rotor High Rotation Speed, particle had both been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that air-flow viscous effect produces, the centrifugal force be subject to when particle is greater than centripetal force, namely the corase particles more than classification footpath returns pulverizing chamber and continues impact comminution, fine particle below classification footpath enters cyclone separator with air-flow, deduster is collected, comparatively corase particles in cyclone collection fine particle, small part ultrafine particle is collected by deduster, large about 10%-20%, gas is discharged by air-introduced machine.
The foregoing is only preferred embodiment of the present invention, be not used for limiting practical range of the present invention; If do not depart from the spirit and scope of the present invention, the present invention is modified or equivalent to replace, in the middle of the protection domain that all should be encompassed in the claims in the present invention.

Claims (8)

1. a method for ultrafine PTFE powder prepared by ultraviolet combined with ozone and hydrogen peroxide, it is characterized in that, comprises following steps:
1) the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) pulverized by the polytetrafluoroethylene (PTFE) raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) be put in the pallet on the platform of ultraviolet irradiation case by the polytetrafluoroethylene (PTFE) raw material after described pulverizing, in described pallet, the thickness of polytetrafluoroethylene (PTFE) raw material is 200mm-300mm;
4) pass into ozone to described ultraviolet irradiation case, airtight described ultraviolet irradiation case, in the ozone passed into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%-0.5%;
5) and the controlling organization opening spray equipment to the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide in described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 3%-8%;
6) ultraviolet ray generating apparatus is opened, continuous irradiation 8-12 hour;
7) after irradiation, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas produced in irradiation process is discharged;
8) opening described ultraviolet irradiation case, take out above-mentioned pallet, and the polytetrafluoroethylene (PTFE) after irradiation is put into airflow comminution system, through fully pulverizing, obtaining particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm;
Ultraviolet ray generating apparatus is provided with in the casing of described ultraviolet irradiation case, and the casing inner bottom part of ultraviolet irradiation case is a platform, described ultraviolet irradiation case side is provided with chamber door, and on casing, being provided with at least 1 exhaust gear and at least 1 spray equipment, the controlling organization of described spray equipment is positioned at outside described ultraviolet irradiation case.
2. the method for ultrafine PTFE powder prepared by ultraviolet combined with ozone according to claim 1 and hydrogen peroxide, it is characterized in that, described ultraviolet ray generating apparatus comprises 4 or 5 Non-polarized lamps, and described Non-polarized lamp is 400W, and wavelength is 184.9nm or 253.7nm.
3. the method for ultrafine PTFE powder prepared by ultraviolet combined with ozone according to claim 1 and hydrogen peroxide, it is characterized in that, described exhaust gear is air-tight state in irradiation process, is opening after irradiation terminates.
4. the method for ultrafine PTFE powder prepared by ultraviolet combined with ozone according to claim 1 and hydrogen peroxide, it is characterized in that, described spray equipment is automatic spraying system, and described automatic spraying system is set to the hydrogen peroxide of the weight ratio set according to the weight automatic spray of polytetrafluoroethylene (PTFE) raw material in pallet.
5. the method for ultrafine PTFE powder prepared by ultraviolet combined with ozone according to claim 1 and hydrogen peroxide, it is characterized in that, described airflow comminution system comprises airslide disintegrating mill, described airslide disintegrating mill comprises air current spray nozzle, pulverizing chamber, compressed air spurts into pulverizing chamber by nozzle at high speeds, at the joint place of multiply high pressure draught, through irradiated described polytetrafluoroethylene (PTFE) raw material by impact several times, friction, shearing and pulverizing.
6. the method for ultrafine PTFE powder prepared by ultraviolet combined with ozone according to claim 5 and hydrogen peroxide, it is characterized in that, described airflow comminution system also comprises:
Cyclone separator, deduster and air-introduced machine;
Described airslide disintegrating mill also comprises grading room, pulverizing chamber pulverize after polytetrafluoroethylene (PTFE) at air-introduced machine move under influence to grading room, under grading wheel effect, polytetrafluoroethylgranule granule is separated by granule size, the fine grained meeting granularity requirements enters cyclone separator by grading wheel or deduster is collected, and the coarse granule not meeting granularity requirements drops to pulverizing chamber to be continued to pulverize.
7. the method for ultrafine PTFE powder prepared by ultraviolet combined with ozone according to claim 6 and hydrogen peroxide, it is characterized in that, the air current spray nozzle of described airslide disintegrating mill is Laval nozzle.
8. the method for ultrafine PTFE powder prepared by ultraviolet combined with ozone according to claim 5 and hydrogen peroxide, it is characterized in that, described airslide disintegrating mill has dry filtrating equipment, before described dry filtrating equipment is positioned at nozzle.
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CN103170400B (en) * 2013-04-03 2016-02-24 太仓金凯特种线缆有限公司 The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone and hydrogen peroxide
CN110341070A (en) * 2019-07-09 2019-10-18 太仓金凯特新材料科技有限公司 A kind of method of ultraviolet light Strong oxdiative atmosphere preparation ultrafine PTFE powder
CN112206905A (en) * 2020-09-07 2021-01-12 杭州电子科技大学 Method and device for ultramicro treatment of bioactive substances

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0214880A1 (en) * 1985-07-18 1987-03-18 Commissariat A L'energie Atomique Process for the production of graft copolymers of polyvinylidene fluoride, and membranes thereof obtained by this process
US5100689A (en) * 1987-04-10 1992-03-31 University Of Florida Surface modified surgical instruments, devices, implants, contact lenses and the like
CN1100988A (en) * 1993-09-29 1995-04-05 段大可 Technology for processing polytetrafluoroethylene regenerated powder and original powder and fine powder
CN1487020A (en) * 2003-07-17 2004-04-07 上海交通大学 Aramid fiber/polyimide composite material and preparation method thereof
CN1646610A (en) * 2002-04-23 2005-07-27 劳雷尔产品有限公司 Method of treating fluoropolymer particles and the products thereof
CN102672968A (en) * 2012-05-07 2012-09-19 四川久远科技股份有限公司 Method for manufacturing ultrafine powder from polytetrafluoroethylene through irradiation cracking

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3766031A (en) * 1972-04-10 1973-10-16 Garlock Inc Process for non-destructive radiation degradation of polytetrafluoroethylene
JP3317452B2 (en) * 1992-10-05 2002-08-26 株式会社レイテック Modified polytetrafluoroethylene and method for producing the same
CN101638487B (en) * 2009-09-04 2011-10-26 赵德耀 Polytetrafluoroethylene nanoscale powder material and preparation method thereof
CN101979429B (en) * 2010-10-14 2012-08-29 中国科学院宁波材料技术与工程研究所 Surface modification method for polytetrafluoroethylene product
CN102924854B (en) * 2012-11-05 2015-01-14 歌山建设集团有限公司 Teflon composite material and preparation method thereof
CN103170400B (en) * 2013-04-03 2016-02-24 太仓金凯特种线缆有限公司 The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone and hydrogen peroxide

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0214880A1 (en) * 1985-07-18 1987-03-18 Commissariat A L'energie Atomique Process for the production of graft copolymers of polyvinylidene fluoride, and membranes thereof obtained by this process
US5100689A (en) * 1987-04-10 1992-03-31 University Of Florida Surface modified surgical instruments, devices, implants, contact lenses and the like
CN1100988A (en) * 1993-09-29 1995-04-05 段大可 Technology for processing polytetrafluoroethylene regenerated powder and original powder and fine powder
CN1646610A (en) * 2002-04-23 2005-07-27 劳雷尔产品有限公司 Method of treating fluoropolymer particles and the products thereof
CN1487020A (en) * 2003-07-17 2004-04-07 上海交通大学 Aramid fiber/polyimide composite material and preparation method thereof
CN102672968A (en) * 2012-05-07 2012-09-19 四川久远科技股份有限公司 Method for manufacturing ultrafine powder from polytetrafluoroethylene through irradiation cracking

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