CN103252279A - Method for preparation of ultrafine PTFE powder by combining electron beams with ozone and hydrogen peroxide - Google Patents
Method for preparation of ultrafine PTFE powder by combining electron beams with ozone and hydrogen peroxide Download PDFInfo
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Abstract
The invention relates to a method for preparation of ultrafine PTFE (polytetrafluoroethylene) powder by combining electron beams with ozone and hydrogen peroxide. The method comprises the steps of: packaging a dried PTFE raw material with a low temperature resistant container and putting the container in liquid nitrogen to undergo quenching, and then taking it out; comminuting the quenched PTFE raw material by a comminutor; putting the comminuted PTFE raw material on a cycling trolley of an electron accelerator; closing the electron accelerator, introducing ozone to the surface of the PTFE on the cycling trolley, starting a spraying device, which sprays hydrogen peroxide to the PTFE raw material on the cycling trolley, starting the electron accelerator, irradiating the PTFE raw material, putting the irradiated PTFE into an airflow pulverization system to undergo complete pulverizing and classification, thus obtaining the ultrafine PTFE powder. The preparation method provided in the invention is simple, can reduce the irradiation time and irradiation dose, thereby reducing the cost, and increases the degradation rate of PTFE.
Description
Technical field
The present invention relates to chemical technology field, particularly a kind of method of utilizing electron beam irradiation combined with ozone and hydrogen peroxide to prepare the PTEE superfine powder.
Background technology
The polytetrafluoroethylene (PTFE) superfine powder is low-molecular-weight fine powder, is " PTFE wax " again, and the superfine powder of polytetrafluoroethylene average grain diameter is less than 5 μ m, and specific area is greater than 10m
2/ g, coefficient of friction is about 0.06～0.07, and its lubricity is good, can be dispersed in well in many materials.
PTFE product purity 100%, molecular weight is lower than below 10,000, and particle diameter is not only keeping original premium properties of polytetrafluoroethylene (PTFE) in the PTFE micro mist series of 0.5 μ m, also have many particular performances, as no self-coagulation, no electrostatic effect, intermiscibility is good, molecular weight is low, good dispersion.It is obvious etc. that self lubricity height, coefficient of friction reduce.
Superfine powder of polytetrafluoroethylene can be made kollag separately and use, and also can be used as the additive of plastics, rubber, coating, printing ink, lubricating oil, lubricating grease etc.Can be with various typical powder process method when itself and plastics or rubber mix, as blend etc., addition is 5～20%, adds ptfe micropowder in oil and grease, 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 technology of preparing of PTFE superfine powder mainly contains telomerization method.Pyrolysis method and radial shake solution, but these methods have certain defective, inhomogeneous as the particle of telomerization method preparation, easily cohesion, and owing to consumption of organic solvent pollutes greatly; Thermal cracking rule complex process, investment is high, can produce a large amount of noxious materials in process of production; Comparative maturity is the radial shake solution at present.
The radiation resistance of polytetrafluoroethylene (PTFE) is relatively poor, be subjected to cause degraded behind the high-energy radiation, so general using electron beam, Co-60 gamma-ray irradiation polytetrafluoroethylene (PTFE) raw material are broken into the less superfine powder of polytetrafluoroethylene of particle diameter by fluid energy mill with irradiated polytetrafluoroethylene (PTFE) raw meal then.
But, utilize the production cost of electron beam, Co-60 gamma-rays radiation device irradiation very high, and high-level security protection needs, and has further increased production cost.Therefore, the market exigence is a kind of can produce superfine powder of polytetrafluoroethylene, the production technology that can effectively reduce cost again efficiently.
Summary of the invention
At above-mentioned problems of the prior art, the object of the present invention is to provide a kind of electron beam combined with ozone and hydrogen peroxide to prepare the method for PTFE superfine powder.The present invention utilizes electron beam irradiation and adds ozone and hydrogen peroxide prepares superfine powder of polytetrafluoroethylene, and its preparation method is simple, thereby and can reduce exposure time and irradiation dose has reduced cost.In order to realize the foregoing invention purpose, the technical solution used in the present invention is as follows:
A kind of electron beam combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, comprise the steps:
1) dried polytetrafluoroethylene (PTFE) raw material is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the described chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) on the circulation dolly that is put into electron accelerator with the polytetrafluoroethylene (PTFE) material sealing after the described pulverizing;
4) airtight described electron accelerator, and open admission gear feeds ozone in the annular seal space of the polytetrafluoroethylene (PTFE) of placing on the described circulation dolly, and the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%-0.5% in the ozone that feeds and the described pallet;
5) open spray equipment, described spray equipment sprays hydrogen peroxide to the polytetrafluoroethylene (PTFE) raw material on the described circulation dolly, and the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 3%-8%;
6) unlocking electronic accelerator, electron accelerator produce high-power electron beam the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, and irradiation dose is 300-500KGy;
7) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μ m.
Further, described electron accelerator comprises high-frequency generator, with the irradiation window that high-frequency generator is equipped with, is positioned at the annular seal space of irradiation window below, settle the circulation dolly of annular seal space, at least 1 admission gear that the position is positioned at the spray equipment of annular seal space and is communicated with sealing device.
Further, the energy of described electron accelerator is 2Mev, and line is 10MA, and scan uniformity is more than 98%, and sweep length is 1000mm.
Further, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.3% in the ozone of described feeding and the described pallet.
Further, the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 5%.
Further, described airflow comminution system comprises airslide disintegrating mill, described airslide disintegrating mill comprises air current spray nozzle, pulverizing chamber, compressed air is gone into pulverizing chamber by the nozzle high velocity jet, at the joint place of multiply high pressure draught, collided repeatedly, 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 the dry filter device, before described dry filter device is positioned at nozzle.
The invention has the beneficial effects as follows: the present invention utilizes electron beam irradiation to add ozone and hydrogen peroxide obtains superfine powder of polytetrafluoroethylene, triple synergies by electron beam, ozone and hydrogen peroxide, high molecular polytetrafluoroethylene (PTFE) raw material is degraded to low molecular superfine powder of polytetrafluoroethylene, can improve the degradation efficiency of polytetrafluoroethylene (PTFE) by adding ozone and hydrogen peroxide, namely reach same polytetrafluoroethylene (PTFE) raw material degradation rate and can reduce the electron beam irradiation time, thereby reduced cost; And preparation technology of the present invention is simple, be easy to control, properties of product are stable, practical.
The specific embodiment
In order to make purpose of the present 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 explaining the present invention, and be not used in restriction the present invention.
The radiation resistance of polytetrafluoroethylene (PTFE) is relatively poor, be subjected to cause degraded behind the high-energy radiation, we utilize this characteristic to adopt the high-frequency electronic accelerator that polytetrafluoroethylene (PTFE) is carried out radiation degradation exactly and handle, and carry out dispersion treatment with airslide disintegrating mill again and obtain the superfine powder of polytetrafluoroethylene material.
High frequency high voltage electron accelerator is a kind of device that can produce the high current electron ray.It is with 50Hz power frequency low-voltage electric energy, become the 100KHz high-frequency electrical energy with high-frequency generator, give by diode by the high-frequency coupling mode again and become the power supply of voltage multiplying rectifier current parallel with the space capacitance group, obtain high high direct voltage after the series connection, accelerate electronics with it, just can obtain needed high current high energy electron ray.The energy of the electron accelerator that we adopt is 2Mev, and line is 10mA, and scan uniformity is more than 98%, and sweep length 1000mm, polytetrafluoroethylene (PTFE) raw material are placed on the circulation dolly below the electron accelerator irradiation window and carry out irradiation.Wherein, the plate that is used for the electron beam irradiation of placement material is of a size of 1000mm * 1000mm * 12mm, and it is 0.012m that material fills with the back volume
3, crab traversing speed 10m/ branch, electron beam line 10mA, the dosage that takes a round are 10KGy, 300KGy is exactly 30 circles, by that analogy.
In order to increase the degradation rate of polytetrafluoroethylene (PTFE), in irradiation process, we adopt the way of adding ozone and hydrogen peroxide to reduce irradiation dose, thereby saved cost, ozone has extremely strong oxidability, it is the oxidant that occurring in nature is only second to fluorine, hydrogen peroxide nebulizes by special spray equipment and is sprayed on the surface of polytetrafluoroethylene (PTFE) raw material, because hydrogen peroxide produces hydroxyl radical free radical (.OH) in irradiation process, hydroxyl radical free radical (.OH) is a kind of important active oxygen, is to lose an electronics by hydroxyl (OH-) to form from molecular formula.Hydroxyl radical free radical has extremely strong electronic capability oxidability just, oxidizing potential 2.8V, it is the oxidant that occurring in nature is only second to fluorine, triple synergistic oxidation reactions by electron beam, ozone and hydrogen peroxide are degraded to low molecular superfine powder of polytetrafluoroethylene to high molecular polytetrafluoroethylene (PTFE) raw material.
The invention provides the method that a kind of electron beam combined with ozone and hydrogen peroxide prepare the PTFE superfine powder, comprise the steps:
1) dried polytetrafluoroethylene (PTFE) raw material is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the described chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) on the circulation dolly that is put into electron accelerator with the polytetrafluoroethylene (PTFE) material sealing after the described pulverizing;
4) airtight described electron accelerator, and open admission gear feeds ozone in the annular seal space of the placement polytetrafluoroethylene (PTFE) on the described circulation dolly, and the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%-0.5% in the ozone that feeds and the described pallet;
5) open spray equipment, described spray equipment sprays hydrogen peroxide to the polytetrafluoroethylene (PTFE) raw material on the described circulation dolly, and the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 3%-8%;
6) unlocking electronic accelerator, electron accelerator produce high-power electron beam the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, and irradiation dose is 300-500KGy;
7) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μ m.
Wherein, described electron accelerator comprises high-frequency generator, with the irradiation window that high-frequency generator is equipped with, is positioned at the annular seal space of irradiation window below, settle the circulation dolly of annular seal space, at least 1 admission gear that is positioned at the spray equipment of annular seal space and is communicated with sealing device., the energy of described electron accelerator is 2Mev, and line is 10MA, and scan uniformity is more than 98%, and sweep length is 1000mm.
Wherein, described airflow comminution system comprises airslide disintegrating mill, described airslide disintegrating mill comprises air current spray nozzle, pulverizing chamber, compressed air is gone into pulverizing chamber by the nozzle high velocity jet, at the joint place of multiply high pressure draught, collided repeatedly, rubbed, sheared and pulverized through irradiated described polytetrafluoroethylene (PTFE) raw material.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.The air current spray nozzle of described airslide disintegrating mill is Laval nozzle.Described airslide disintegrating mill has the dry filter device, before described dry filter device is positioned at nozzle.
Embodiment one
A kind of electron beam combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, comprise the steps:
1) dried polytetrafluoroethylene (PTFE) raw material is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the described chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after the described pulverizing is put in the annular seal space on the circulation dolly of electron accelerator;
4) airtight described electron accelerator, and open admission gear feeds ozone on the ptfe surface on the described circulation dolly, and the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.3% in the ozone that feeds and the described pallet;
5) unlocking electronic accelerator, electron accelerator produce high-power electron beam and the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, every 0.012m
3The irradiation dose of polytetrafluoroethylene (PTFE) powder (preferably fill with plate, the thickness of the polytetrafluoroethylene (PTFE) of containing is 12mm) is 400KGy, and umber of exposures is 4 times, each 5 minutes;
6) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 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 the dry filter device, be positioned at nozzle before.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 speed Laval 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, because classification rotor high-speed rotation, particle both had been subjected to the centrifugal force of classification rotor, be subjected to the centripetal force that the air-flow viscous effect produces again, the centrifugal force that is subjected to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in the 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
A kind of electron beam combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, comprise the steps:
1) the polytetrafluoroethylene (PTFE) raw material with drying is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after the described pulverizing is placed in the annular seal space on the circulation dolly of electron accelerator;
4) open spray equipment, described spray equipment sprays hydrogen peroxide to the polytetrafluoroethylene (PTFE) raw material on the described circulation dolly, and the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 5%;
5) unlocking electronic accelerator, electron accelerator produce high-power electron beam and the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, every 0.012m
3The irradiation dose of polytetrafluoroethylene (PTFE) powder (preferably fill with plate, the thickness of the polytetrafluoroethylene (PTFE) of containing is 12mm) is 400KGy, and umber of exposures is 4 times, each 5 minutes;
6) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 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 the dry filter device, be positioned at nozzle before.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 speed Laval 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, because classification rotor high-speed rotation, particle both had been subjected to the centrifugal force of classification rotor, be subjected to the centripetal force that the air-flow viscous effect produces again, the centrifugal force that is subjected to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in the 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
A kind of electron beam combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, comprise the steps:
1) dried polytetrafluoroethylene (PTFE) raw material is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the described chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after the described pulverizing is put in the annular seal space on the circulation dolly of electron accelerator;
4) airtight described electron accelerator, and open admission gear feeds ozone on the ptfe surface on the described circulation dolly, and the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.3% in the ozone that feeds and the described pallet;
5) open spray equipment, described spray equipment sprays hydrogen peroxide to the polytetrafluoroethylene (PTFE) raw material on the described circulation dolly, and the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 5%;
6) unlocking electronic accelerator, electron accelerator produce high-power electron beam and the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, every 0.012m
3The irradiation dose of polytetrafluoroethylene (PTFE) powder (preferably fill with plate, the thickness of the polytetrafluoroethylene (PTFE) of containing is 12mm) is 300KGy, and umber of exposures is 3 times, each 3 minutes;
7) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 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 the dry filter device, be positioned at nozzle before.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 speed Laval 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, because classification rotor high-speed rotation, particle both had been subjected to the centrifugal force of classification rotor, be subjected to the centripetal force that the air-flow viscous effect produces again, the centrifugal force that is subjected to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in the 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
A kind of electron beam combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, comprise the steps:
1) dried polytetrafluoroethylene (PTFE) raw material is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the described chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after the described pulverizing is put in the annular seal space on the circulation dolly of electron accelerator;
4) airtight described electron accelerator, and open admission gear feeds ozone on the ptfe surface on the described circulation dolly, and the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1% in the ozone that feeds and the described pallet;
5) open spray equipment, described spray equipment sprays hydrogen peroxide to the polytetrafluoroethylene (PTFE) raw material on the described circulation dolly, and the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 3%;
6) unlocking electronic accelerator, electron accelerator produce high-power electron beam and the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, every 0.012m
3The irradiation dose of polytetrafluoroethylene (PTFE) powder (preferably fill with plate, the thickness of the polytetrafluoroethylene (PTFE) of containing is 12mm) is 500KGy, and umber of exposures is 3 times, each 4 minutes;
7) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 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 the dry filter device, be positioned at nozzle before.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 speed Laval 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, because classification rotor high-speed rotation, particle both had been subjected to the centrifugal force of classification rotor, be subjected to the centripetal force that the air-flow viscous effect produces again, the centrifugal force that is subjected to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in the 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 five
A kind of electron beam combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, comprise the steps:
1) dried polytetrafluoroethylene (PTFE) raw material is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the described chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after the described pulverizing is put in the annular seal space on the circulation dolly of electron accelerator;
4) airtight described electron accelerator, and open admission gear feeds ozone on the ptfe surface on the described circulation dolly, and the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.5% in the ozone that feeds and the described pallet;
5) open spray equipment, described spray equipment sprays hydrogen peroxide to the polytetrafluoroethylene (PTFE) raw material on the described circulation dolly, and the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 8%;
6) unlocking electronic accelerator, electron accelerator produce high-power electron beam and the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, every 0.012m
3The irradiation dose of polytetrafluoroethylene (PTFE) powder (preferably fill with plate, the thickness of the polytetrafluoroethylene (PTFE) of containing is 12mm) is 300KGy, and umber of exposures is 2 times, each 3 minutes;
7) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 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 the dry filter device, be positioned at nozzle before.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 speed Laval 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, because classification rotor high-speed rotation, particle both had been subjected to the centrifugal force of classification rotor, be subjected to the centripetal force that the air-flow viscous effect produces again, the centrifugal force that is subjected to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in the 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 six
A kind of electron beam combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, comprise the steps:
1) dried polytetrafluoroethylene (PTFE) raw material is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the described chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after the described pulverizing is put in the annular seal space on the circulation dolly of electron accelerator;
4) airtight described electron accelerator, and open admission gear feeds ozone on the ptfe surface on the described circulation dolly, and the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1% in the ozone that feeds and the described pallet;
5) open spray equipment, described spray equipment sprays hydrogen peroxide to the polytetrafluoroethylene (PTFE) raw material on the described circulation dolly, and the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 8%;
6) unlocking electronic accelerator, electron accelerator produce high-power electron beam and the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, every 0.012m
3The irradiation dose of polytetrafluoroethylene (PTFE) powder (preferably fill with plate, the thickness of the polytetrafluoroethylene (PTFE) of containing is 12mm) is 400KGy, and umber of exposures is 3 times, each 3 minutes;
7) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 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 the dry filter device, be positioned at nozzle before.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 speed Laval 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, because classification rotor high-speed rotation, particle both had been subjected to the centrifugal force of classification rotor, be subjected to the centripetal force that the air-flow viscous effect produces again, the centrifugal force that is subjected to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in the 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 seven
A kind of electron beam combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, comprise the steps:
1) dried polytetrafluoroethylene (PTFE) raw material is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the described chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after the described pulverizing is put in the annular seal space on the circulation dolly of electron accelerator;
4) airtight described electron accelerator, and open admission gear feeds ozone on the ptfe surface on the described circulation dolly, and the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.5% in the ozone that feeds and the described pallet;
5) open spray equipment, described spray equipment sprays hydrogen peroxide to the polytetrafluoroethylene (PTFE) raw material on the described circulation dolly, and the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 3%;
6) unlocking electronic accelerator, electron accelerator produce high-power electron beam and the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, every 0.012m
3The irradiation dose of polytetrafluoroethylene (PTFE) powder (preferably fill with plate, the thickness of the polytetrafluoroethylene (PTFE) of containing is 12mm) is 400KGy, and umber of exposures is 3 times, each 3 minutes;
7) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 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 the dry filter device, be positioned at nozzle before.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 speed Laval 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, because classification rotor high-speed rotation, particle both had been subjected to the centrifugal force of classification rotor, be subjected to the centripetal force that the air-flow viscous effect produces again, the centrifugal force that is subjected to when particle is greater than centripetal force, be that the above corase particles in classification footpath returns pulverizing chamber continuation impact comminution, the following fine particle in classification footpath enters cyclone separator, deduster collection with air-flow, cyclone separator collect in the 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 embodiment has only expressed embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. an electron beam combined with ozone and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, comprise the steps:
1) dried polytetrafluoroethylene (PTFE) raw material is placed in the liquid nitrogen with low temperature resistant container package, takes out behind the chilling;
2) the polytetrafluoroethylene (PTFE) raw material after the described chilling processing is pulverized with pulverizer, pulverizing the back particle diameter is 100-1000 μ m;
3) the polytetrafluoroethylene (PTFE) raw material after the described pulverizing is put on the circulation dolly of electron accelerator of sealing;
4) airtight described electron accelerator, and open admission gear feeds ozone in the annular seal space of the polytetrafluoroethylene (PTFE) of placing on the described circulation dolly, and the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.1%-0.5% in the ozone that feeds and the described pallet;
5) open spray equipment, described spray equipment sprays hydrogen peroxide to the polytetrafluoroethylene (PTFE) raw material on the described circulation dolly, and the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 3%-8%;
6) unlocking electronic accelerator, electron accelerator produce high-power electron beam the polytetrafluoroethylene (PTFE) raw material are carried out irradiation, and irradiation dose is 300-500KGy;
7) polytetrafluoroethylene (PTFE) behind the irradiation is put into airflow comminution system, through pulverizing fully and classification, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μ m.
2. electron beam combined with ozone according to claim 1 and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, described electron accelerator comprises that the higher-order of oscillation swings device, the irradiation window that is equipped with high-frequency generator, be positioned at the annular seal space of irradiation window below, settle the circulation dolly of annular seal space, at least 1 admission gear that is positioned at the spray equipment of annular seal space and is communicated with sealing device.
3. electron beam combined with ozone according to claim 2 and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, the energy of described electron accelerator is 2Mev, and line is 10MA, and scan uniformity is more than 98%, and sweep length is 1000mm.
4. electron beam combined with ozone according to claim 1 and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, the weight ratio of polytetrafluoroethylene (PTFE) raw material is 0.3% in the ozone of described feeding and the described pallet.
5. electron beam combined with ozone according to claim 1 and hydrogen peroxide prepare the method for PTFE superfine powder, it is characterized in that, the weight ratio of the polytetrafluoroethylene (PTFE) raw material on the hydrogen peroxide of described spray and the described circulation dolly is 5%.
6. electron beam 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 is gone into pulverizing chamber by the nozzle high velocity jet, at the joint place of multiply high pressure draught, collided repeatedly, rubbed, sheared and pulverized through irradiated described polytetrafluoroethylene (PTFE) raw material.
7. electron beam combined with ozone according to claim 6 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.
8. electron beam combined with ozone according to claim 7 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.
9. prepare the method for PTFE superfine powder according to the described electron beam combined with ozone of arbitrary claim among the claim 1-8 and hydrogen peroxide, it is characterized in that described airslide disintegrating mill has the dry filter device, before described dry filter device is positioned at nozzle.
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