CN103170400A - Method for preparing PTFE (polytetrafluoroethene) ultrafine powder by combining ultraviolet rays with ozone and hydrogen peroxide - Google Patents
Method for preparing PTFE (polytetrafluoroethene) ultrafine powder by combining ultraviolet rays with ozone and hydrogen peroxide Download PDFInfo
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- CN103170400A CN103170400A CN2013101166438A CN201310116643A CN103170400A CN 103170400 A CN103170400 A CN 103170400A CN 2013101166438 A CN2013101166438 A CN 2013101166438A CN 201310116643 A CN201310116643 A CN 201310116643A CN 103170400 A CN103170400 A CN 103170400A
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- 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
- C08J3/12—Powdering or granulating
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- 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
- C08J3/28—Treatment by wave energy or particle radiation
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- 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
- C08J2327/00—Characterised 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
- C08J2327/02—Characterised 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
- C08J2327/12—Characterised 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
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
Abstract
The invention relates to a method for preparing PTFE (polytetrafluoroethene) ultrafine powder by combining ultraviolet rays with ozone and hydrogen peroxide. The method is specifically as follows: placing dry PTFE raw material in liquid nitrogen for quenching; further crushing till the particle size is 100-1000 microns by using a crushing machine; then placing into a tray on a platform of an ultraviolet radiation box; charging the ozone into the ultraviolet radiation box; closing the ultraviolet radiation box, and opening a control mechanism of a spraying device to spray the hydrogen peroxide to the PTFE raw material in the tray, wherein the weight ratio of the sprayed hydrogen peroxide to the PTFE raw material in the tray is 3%-8%; using the ultraviolet rays to continuously radiate for 8-12 hours; exhausting waste gas after the end of radiation; taking out and placing into a gas flow crushing system, and fully crushing to get the PTFE ultrafine powder with the particle size of 0.2-5 microns. The method adopting the technical scheme is a production technology which can not only produce the PTFE ultrafine powder with high efficiency, but also effectively reduce cost.
Description
Technical field
The present invention relates to the preparation method of superfine powder of polytetrafluoroethylene, prepare the method for PTFE superfine powder in particular to ultraviolet irradiation combined with ozone and hydrogen peroxide.
Background technology
Polytetrafluoroethylene (PTFE) is commonly called as King, is the polymer that is polymerized by tetrafluoroethylene monomer, and very strong coherency is arranged, and resin is easy to be attached to together, is difficult for disperseing.PTFE superfine powder (micro mist) is low-molecular-weight polytetrafluoroethylene (PTFE), reach the PTFE superfine powder of ultra-fine degree, molecular weight is lower than below 10,000, particle diameter is in the PTFE micro mist series of 0.5-15 μ m, not only keeping original all premium properties of polytetrafluoroethylene (PTFE), the performance that also has 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 reduces, not conglomeration, easily mixed mutually with oil or organic liquid, also can evenly mix obvious etc. with other solia particle.PTFE superfine powder average grain diameter is less than 5 μ m, 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 anti-stick, antifriction, the flame-retardant additive of plastics, rubber, printing ink, coating, lubricant grease, also can make aerosol etc. as dry lubricant.The PTFE superfine powder can be made separately kollag and use, and also can be used as the additive of plastics, rubber, coating, printing ink, lubricating oil, lubricating grease etc.Can as blend etc., add superfine powder of polytetrafluoroethylene in oil and grease with various typical powder process method during with plastics or rubber mix, can reduce coefficient of friction, as long as add a few percent, just can improve the life-span of lubricating oil.Its dispersion in organic solvent also can be made releasing agent.
The method for preparing the PTFE superfine powder has determined structural behaviour, molecular weight and the distribution thereof of PTFE superfine powder.The preparation method of PTFE superfine powder mainly contains two kinds: 1, directly regulate polymerization with TFE, stop polymerisation after certain hour, product is suitably processed again; 2, with HMW PTFE degraded, then pulverize.The method that cracking reaction prepares the PTFE superfine powder mainly contains thermal cracking and irradiation to crack.In the irradiation to crack process, the PTFE degraded is subjected to the impact of radiation parameter, irradiation dose, the energy source that irradiation adopts and the difference of oxidizing condition, physical property and chemical property to the PTFE superfine powder all have considerable influence, therefore need to 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, a kind of method that provides ultraviolet combined with ozone and hydrogen peroxide to prepare the PTFE superfine powder, described method can be produced superfine powder of polytetrafluoroethylene efficiently, can obviously reduce production costs again.
Ultraviolet irradiation polytetrafluoroethylene (PTFE) provided by the present invention prepares the method for superfine powder of polytetrafluoroethylene, mainly comprises the following steps:
1) the polytetrafluoroethylene (PTFE) raw material with drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) the polytetrafluoroethylene (PTFE) raw material after described quenching is pulverized with pulverizer, after pulverizing, particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after described pulverizing is put in pallet on the platform of ultraviolet irradiation case, 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 that passes into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%-0.5%;
5) and the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide of the controlling organization of opening spray equipment in the described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 3%-8%;
6) open ultraviolet ray generating apparatus, continuous irradiation 8-12 hour;
7) irradiation complete after, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas that produces in irradiation process is discharged;
8) 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, obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μ m.
Further, be provided with ultraviolet ray generating apparatus 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 one side is provided with chamber door, and be provided with at least 1 exhaust gear and at least 1 spray equipment on casing, 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 finishes.
Further, described spray equipment is automatic spraying system, and described automatic spraying system is set to the hydrogen peroxide according to the weight ratio of the weight automatic spray setting of polytetrafluoroethylene (PTFE) raw material in pallet.
Further, in the described pallet of 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 enters pulverizing chamber by the nozzle high velocity jet, at the joint place of multiply high pressure draught, repeatedly collided, rubbed, sheared and pulverized through irradiated described polytetrafluoroethylene (PTFE) raw material.
Further, described airflow comminution system also comprises:
Cyclone separator, deduster and air-introduced machine;
Described airslide disintegrating mill also comprises grading room, polytetrafluoroethylene (PTFE) after pulverizing chamber is pulverized moves to grading room under the air-introduced machine effect, under the grading wheel effect, polytetrafluoroethylgranule granule is separated by granule size, the fine grained that meets granularity requirements enters cyclone separator by grading wheel or deduster is collected, and the coarse granule that does not meet 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 for preparing the PTFE superfine powder according to ultraviolet combined with ozone provided by the invention and hydrogen peroxide, under identical radiation parameter, can increase the degradation rate of polytetrafluoroethylene (PTFE) or reduce exposure time and also can reach identical degradation rate, therefore improved production efficiency, guarantee the low molecular superfine powder of polytetrafluoroethylene that acquisition is of the required size, and manufacture process can strictly be controlled, and guarantees the quality of production.
The specific embodiment
In order to make the object of the invention, technical scheme and advantage clearer, 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, is not intended to limit the present invention.
Ultraviolet combined with ozone provided by the invention and hydrogen peroxide prepare the method for PTFE superfine powder, 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) the preliminary pulverizing: the polytetrafluoroethylene (PTFE) raw material after described quenching is pulverized with pulverizer, and after pulverizing, particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after described pulverizing is put in pallet on the platform of ultraviolet irradiation case, 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 that passes into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%-0.5%;
5) spray: and the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide of the controlling organization of opening spray equipment in the 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) exhaust: after irradiation is complete, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas that produces 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, obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μ m.
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 the casing inner top, the casing inner bottom part is a platform, ultraviolet irradiation case side is provided with door (can open place and take out material), has at least 1 exhaust gear at the casing top.Wherein, described ultraviolet ray generating apparatus preferably includes 4-5 400W, and wavelength set is 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 finishes.
Wherein, described airflow comminution system comprises airslide disintegrating mill, described airslide disintegrating mill comprises air current spray nozzle, pulverizing chamber, compressed air enters pulverizing chamber by the nozzle high velocity jet, at the joint place of multiply high pressure draught, repeatedly collided, rubbed, sheared and pulverized through irradiated described polytetrafluoroethylene (PTFE) raw material.
Described airflow comminution system can also comprise cyclone separator, deduster and air-introduced machine.Described airslide disintegrating mill be preferably have air current spray nozzle, pulverizing chamber (pulverizing chamber), grading room.compressed air enters pulverizing chamber by the nozzle high velocity jet, form the high pressure draught that multiply is intersected, joint place at the multiply high pressure draught, repeatedly collided through irradiated polytetrafluoroethylene (PTFE) raw material, 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 that meets granularity requirements (less than 5 μ m) 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, and is better for guaranteeing crushing effect, can also be before nozzle placement filter drying device (further reducing to treat the humidity of pulverized particles).
Embodiment one
Ultraviolet combined with ozone provided by the invention and hydrogen peroxide prepare the method for PTFE superfine powder, 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) the preliminary pulverizing: the polytetrafluoroethylene (PTFE) raw material after described quenching is pulverized with pulverizer, and after pulverizing, particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after described pulverizing is put in pallet on the platform of ultraviolet irradiation case, 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 that passes into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%;
5) spray: and the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide of the controlling organization of opening spray equipment in the 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) exhaust: after irradiation is complete, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas that produces 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, obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μ m.
The 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.The polytetrafluoroethylene (PTFE) that irradiation is good is put into airslide disintegrating mill, enter pulverizing chamber by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to the 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 the grading rotor High Rotation Speed, particle both had been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that the air-flow viscous effect produces, the centrifugal force that is subject to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns to pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in fine particle than corase particles, the small part ultrafine particle is collected by deduster, about 10%-20%, gas is discharged by air-introduced machine greatly.
Embodiment two
Ultraviolet combined with ozone provided by the invention and hydrogen peroxide prepare the method for PTFE superfine powder, 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) the preliminary pulverizing: the polytetrafluoroethylene (PTFE) raw material after described quenching is pulverized with pulverizer, and after pulverizing, particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after described pulverizing is put in pallet on the platform of ultraviolet irradiation case, 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 that passes into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.5%;
5) spray: and the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide of the controlling organization of opening spray equipment in the 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) exhaust: after irradiation is complete, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas that produces 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, obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μ m.
The 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.The polytetrafluoroethylene (PTFE) that irradiation is good is put into airslide disintegrating mill, enter pulverizing chamber by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to the 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 the grading rotor High Rotation Speed, particle both had been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that the air-flow viscous effect produces, the centrifugal force that is subject to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns to pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in fine particle than corase particles, the small part ultrafine particle is collected by deduster, about 10%-20%, gas is discharged by air-introduced machine greatly.
Embodiment three
Ultraviolet combined with ozone provided by the invention and hydrogen peroxide prepare the method for PTFE superfine powder, 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) the preliminary pulverizing: the polytetrafluoroethylene (PTFE) raw material after described quenching is pulverized with pulverizer, and after pulverizing, particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after described pulverizing is put in pallet on the platform of ultraviolet irradiation case, 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 that passes into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.3%;
5) spray: and the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide of the controlling organization of opening spray equipment in the 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) exhaust: after irradiation is complete, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas that produces 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, obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μ m.
The 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.The polytetrafluoroethylene (PTFE) that irradiation is good is put into airslide disintegrating mill, enter pulverizing chamber by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to the 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 the grading rotor High Rotation Speed, particle both had been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that the air-flow viscous effect produces, the centrifugal force that is subject to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns to pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in fine particle than corase particles, the small part ultrafine particle is collected by deduster, about 10%-20%, gas is discharged by air-introduced machine greatly.
Embodiment four
Ultraviolet combined with ozone provided by the invention and hydrogen peroxide prepare the method for PTFE superfine powder, 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) the preliminary pulverizing: the polytetrafluoroethylene (PTFE) raw material after described quenching is pulverized with pulverizer, and after pulverizing, particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after described pulverizing is put in pallet on the platform of ultraviolet irradiation case, 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 that passes into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.3%;
5) spray: and the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide of the controlling organization of opening spray equipment in the 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) exhaust: after irradiation is complete, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas that produces 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, obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μ m.
The 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.The polytetrafluoroethylene (PTFE) that irradiation is good is put into airslide disintegrating mill, enter pulverizing chamber by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to the 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 the grading rotor High Rotation Speed, particle both had been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that the air-flow viscous effect produces, the centrifugal force that is subject to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns to pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in fine particle than corase particles, the small part ultrafine particle is collected by deduster, about 10%-20%, gas is discharged by air-introduced machine greatly.
Adopt Non-polarized lamp because electrodeless startup is fast in the present embodiment, and the pressure drop loss can avoid starting the time, service life is longer, can reach the service life of 5-6, makes the cost of this method lower.
Embodiment five
Ultraviolet combined with ozone provided by the invention and hydrogen peroxide prepare the method for PTFE superfine powder, 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) the preliminary pulverizing: the polytetrafluoroethylene (PTFE) raw material after described quenching is pulverized with pulverizer, and after pulverizing, particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after described pulverizing is put in pallet on the platform of ultraviolet irradiation case, 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 that passes into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%;
5) spray: and the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide of the controlling organization of opening spray equipment in the 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) exhaust: after irradiation is complete, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas that produces 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, obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μ m.
The 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.The polytetrafluoroethylene (PTFE) that irradiation is good is put into airslide disintegrating mill, enter pulverizing chamber by screw feeder, compressed air passes through the supersonic nozzle of particular arrangement to the 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 the grading rotor High Rotation Speed, particle both had been subject to the centrifugal force of grading rotor, be subject to again the centripetal force that the air-flow viscous effect produces, the centrifugal force that is subject to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns to pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in fine particle than corase particles, the small part ultrafine particle is collected by deduster, about 10%-20%, gas is discharged by air-introduced machine greatly.
The above is only preferred embodiment of the present invention, is not to limit practical range of the present invention; If do not break away from the spirit and scope of the present invention, the present invention is modified or is equal to replacement, all should be encompassed in the middle of the protection domain of claim of the present invention.
Claims (10)
1. a ultraviolet combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, comprise following steps:
1) the polytetrafluoroethylene (PTFE) raw material with drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) the polytetrafluoroethylene (PTFE) raw material after described quenching is pulverized with pulverizer, after pulverizing, particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after described pulverizing is put in pallet on the platform of ultraviolet irradiation case, 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 that passes into and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%-0.5%;
5) and the polytetrafluoroethylene (PTFE) raw material spray hydrogen peroxide of the controlling organization of opening spray equipment in the described pallet, in the hydrogen peroxide of described spray and described pallet, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 3%-8%;
6) open ultraviolet ray generating apparatus, continuous irradiation 8-12 hour;
7) irradiation complete after, open the exhaust gear of above-mentioned ultraviolet irradiation case, the waste gas that produces in irradiation process is discharged;
8) 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, obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μ m.
2. ultraviolet combined with ozone according to claim 1 and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, be provided with ultraviolet ray generating apparatus 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 one side is provided with chamber door, and be provided with at least 1 exhaust gear and at least 1 spray equipment on casing, the controlling organization of described spray equipment is positioned at outside chest.
3. ultraviolet combined with ozone according to claim 2 and hydrogen peroxide prepare the method for PTFE superfine powder, 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.
4. ultraviolet combined with ozone according to claim 2 and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, described exhaust gear is air-tight state in irradiation process, are opening after irradiation finishes.
5. ultraviolet combined with ozone according to claim 1 and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, described spray equipment is automatic spraying system, and described automatic spraying system is set to the hydrogen peroxide according to the weight ratio of the weight automatic spray setting of polytetrafluoroethylene (PTFE) raw material in pallet.
6. ultraviolet combined with ozone according to claim 5 and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, in the described pallet of the hydrogen peroxide of described spray, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 5%.
7. ultraviolet combined with ozone according to claim 1 and hydrogen peroxide prepare the method for PTFE superfine powder, 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 enters pulverizing chamber by the nozzle high velocity jet, at the joint place of multiply high pressure draught, repeatedly collided, rubbed, sheared and pulverized through irradiated described polytetrafluoroethylene (PTFE) raw material.
8. ultraviolet combined with ozone according to claim 7 and hydrogen peroxide prepare the method for PTFE superfine powder, 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, polytetrafluoroethylene (PTFE) after pulverizing chamber is pulverized moves to grading room under the air-introduced machine effect, under the grading wheel effect, polytetrafluoroethylgranule granule is separated by granule size, the fine grained that meets granularity requirements enters cyclone separator by grading wheel or deduster is collected, and the coarse granule that does not meet granularity requirements drops to pulverizing chamber to be continued to pulverize.
9. ultraviolet combined with ozone according to claim 8 and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, the air current spray nozzle of described airslide disintegrating mill is Laval nozzle.
10. the described ultraviolet combined with ozone of arbitrary claim and hydrogen peroxide prepare the method for PTFE superfine powder according to claim 1-9, 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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| CN201310116643.8A CN103170400B (en) | 2013-04-03 | 2013-04-03 | The method of ultrafine PTFE powder prepared by ultraviolet combined with ozone and hydrogen peroxide |
| PCT/CN2013/000797 WO2014161113A1 (en) | 2013-04-03 | 2013-06-28 | Method for preparing ptfe superfine powder by combining ultraviolet rays with ozone and hydrogen peroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014161113A1 (en) * | 2013-04-03 | 2014-10-09 | 太仓金凯特种线缆有限公司 | Method for preparing ptfe superfine powder by combining ultraviolet rays 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 |
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| 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)
| 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 | Composite aramid fiber/polyimide material and its prepn |
| 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)
| 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 |
-
2013
- 2013-04-03 CN CN201310116643.8A patent/CN103170400B/en active Active
- 2013-06-28 WO PCT/CN2013/000797 patent/WO2014161113A1/en active Application Filing
Patent Citations (6)
| 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 | Composite aramid fiber/polyimide material and its prepn |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014161113A1 (en) * | 2013-04-03 | 2014-10-09 | 太仓金凯特种线缆有限公司 | Method for preparing ptfe superfine powder by combining ultraviolet rays 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 |
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| CN103170400B (en) | 2016-02-24 |
| WO2014161113A1 (en) | 2014-10-09 |
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