CN103224636B - Method of preparing PTFE micropowder through electron beam combined with ozone and carbon tetrachloride - Google Patents
Method of preparing PTFE micropowder through electron beam combined with ozone and carbon tetrachloride Download PDFInfo
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- CN103224636B CN103224636B CN201310115587.6A CN201310115587A CN103224636B CN 103224636 B CN103224636 B CN 103224636B CN 201310115587 A CN201310115587 A CN 201310115587A CN 103224636 B CN103224636 B CN 103224636B
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Abstract
A method of preparing PTFE micropowder through electron beam combined with ozone and carbon tetrachloride comprises packaging dried polytetrafluoroethylene (PTFE) raw materials with low-temperature-resistant container, rapidly cooling in liquid nitrogen, pulverizing the rapidly cooled PTFE raw materials with a pulverizer, putting the pulverized PTFE raw materials into a cyclic trolley of an electron accelerator, sealing the electron accelerator, opening an air inlet mechanism, introducing the ozone onto surface of the PTFE, opening a spraying apparatus which can spray the carbon tetrachloride to the PTFE raw materials on the cyclic trolley, opening the electron accelerator which generates high-energy electron beams to irradiate the PTFE raw materials, putting the irradiated PTFE into an air-flow crushing system, fully crushing and grading to obtain the PTFE micropowder. According to the invention, the preparation method is simple, and can reduce irradiation time and the irradiation dose, thereby reducing cost.
Description
Technical field
The present invention relates to chemical technology field, particularly a kind of method utilizing electron beam irradiation combined with ozone and tetracol phenixin to prepare PTEE ultrafine powder.
Background technology
Polytetrafluoroethylene (PTFE) ultrafine powder is low-molecular-weight fine powder, and cry again " PTFE wax ", superfine powder of polytetrafluoroethylene median size is less than 5 μm, and specific surface area is greater than 10m
2/ g, frictional coefficient is about 0.06 ~ 0.07, and its oilness is good, can be dispersed in well in many materials.
PTFE product purity 100%, molecular weight is lower than less than 10,000, and particle diameter, the PTFE micro mist series of 0.5 μm, not only remains original premium properties of tetrafluoroethylene, also there is the performance of many uniquenesses, as without self coagulation, without electrostatic effect, intermiscibility is good, molecular weight is low, good dispersity.Self lubricity is high, frictional coefficient reduces obvious etc.
Superfine powder of polytetrafluoroethylene can be made separately solid lubricant and use, also can as the additive of plastics, rubber, coating, ink, lubricating oil, lubricating grease etc.Can by various typical powder process method when itself and plastics or rubber mix, as blended etc., add-on is 5 ~ 20%, adds ptfe micropowder in oil and grease, can reduce frictional coefficient, as long as add percentum, just can improve the life-span of lubricating oil.Its dispersion in organic solvent also can make releasing agent.
The technology of preparing of ultrafine PTFE powder mainly contains telomerization method.Pyrolysis method and radial shake solution, but these methods have certain defect, and the particle prepared as telomerization method is uneven, easily condenses, and pollutes because consumption of organic solvent is large; Thermo-cracking rule complex process, invests high, can produce a large amount of toxic substances in process of production; Current comparative maturity be radial shake solution.
The radiation resistance of polytetrafluoroethylene (PTFE) is poor, degraded is caused by after high-energy radiation, so general electron beam, Co-60 gamma-ray irradiation tetrafluoroethylene raw material, then by superfine powder of polytetrafluoroethylene that irradiated tetrafluoroethylene raw material pulverizing becomes particle diameter less by fluid energy mill.
But, utilize the production cost of electron beam, Co-60 gamma Rays equipment irradiation very high, and high-level safety precaution needs, and further increases production cost.Therefore, market exigence one can produce superfine powder of polytetrafluoroethylene efficiently, the production technology that can effectively reduce costs again.
Summary of the invention
For 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 tetracol phenixin prepare ultrafine PTFE powder method.The present invention utilizes electron beam irradiation and adds ozone and tetracol phenixin to prepare superfine powder of polytetrafluoroethylene, and its preparation method is simple, and can reduce irradiation time and irradiation dose thus reduce cost.In order to realize foregoing invention object, the technical solution used in the present invention is as follows:
Electron beam combined with ozone and tetracol phenixin prepare a method for ultrafine PTFE powder, comprise the steps:
1) the low temperature resistant container package of dried tetrafluoroethylene raw material is placed in liquid nitrogen, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) what sealed by the tetrafluoroethylene raw material after described pulverizing is put on the circular trolley of rumbatron;
4) airtight described rumbatron, and open admission gear, passes into ozone in the annular seal space placing tetrafluoroethylene on described circular trolley, and in the ozone passed into and described pallet, the weight ratio of tetrafluoroethylene raw material is 0.1%-0.5%;
5) open spray equipment, described spray equipment is to the tetrafluoroethylene raw material spray tetracol phenixin on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 3%-8%;
6) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, and irradiation dose is 300-500KGy;
7) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μm.
Further, described rumbatron comprises high-frequency oscillator, and the irradiation window be equipped with high-frequency oscillator, is positioned at the annular seal space below irradiation window, settle the circular trolley of annular seal space, the spray equipment being positioned at annular seal space and at least 1 admission gear be communicated with tightness system.
Further, the energy of described rumbatron is 2Mev, and line is 10MA, and scan uniformity is more than 98%, and sweep length is 1000mm.
Further, in the ozone passed into described in and described pallet, the weight ratio of tetrafluoroethylene raw material is 0.3%.
Further, the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 5%.
Further, described airflow comminution system comprises micronizer mill, described micronizer mill comprises airflow nozzle, crushiing chamber, pressurized air spurts into crushiing chamber by nozzle at high speeds, at the joint place of multiply high pressure draft, through irradiated described tetrafluoroethylene raw material by impact several times, friction, shearing and pulverizing.
Further, described airflow comminution system also comprises:
Cyclonic separator, fly-ash separator and induced draft fan;
Described micronizer mill also comprises grading room, crushiing chamber pulverize after tetrafluoroethylene at induced draft fan move under influence to grading room, under grading wheel effect, polytetrafluoroethylene granule is separated by globule size, the fine particle meeting granularity requirements enters cyclonic separator by grading wheel or fly-ash separator is collected, and the coarse particles not meeting granularity requirements drops to crushiing chamber to be continued to pulverize.
Further, the airflow nozzle of described micronizer mill is laval nozzle.
Further, described micronizer mill has dry filtrating equipment, before described dry filtrating equipment is positioned at nozzle.
The invention has the beneficial effects as follows: the present invention utilizes electron beam irradiation to add ozone and tetracol phenixin obtains superfine powder of polytetrafluoroethylene, by triple synergies of electron beam, ozone and tetracol phenixin, be low molecular superfine powder of polytetrafluoroethylene high molecular tetrafluoroethylene feed degradation, the degradation efficiency of tetrafluoroethylene can be improved by adding ozone and tetracol phenixin, namely reach same tetrafluoroethylene feed degradation rate and can reduce the electron beam irradiation time, thus reduce cost; And preparation technology of the present invention is simple, be easy to control, product performance are stable, practical.
Embodiment
In order to make object of the present 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 radiation resistance of tetrafluoroethylene is poor, degraded is caused by after high-energy radiation, we utilize this characteristic to adopt high-frequency electronic accelerator to carry out radiation degradation process to tetrafluoroethylene exactly, then carry out dispersion treatment with micronizer mill and obtain superfine powder of polytetrafluoroethylene material.
High frequency high voltage electron accelerator is a kind of device that can produce high current electron rays.It is by 50Hz power frequency low-voltage electric energy, 100KHz high-frequency electrical energy is become with high-frequency oscillator, voltage multiplying rectifier current parallel is become to power by diode with space capacitor bank by high-frequency coupling mode again, high high direct voltage is obtained after series connection, accelerate electronics with it, just can obtain required high current high energy electron ray.The energy of the rumbatron that we adopt is 2Mev, and line is 10mA, scan uniformity more than 98%, sweep length 1000mm, and tetrafluoroethylene raw material is placed on the circular trolley below electron accelerator irradiation window and carries out irradiation.Wherein, the plate for the electron beam irradiation placing material is of a size of 1000mm × 1000mm × 12mm, and it is 0.012m that material fills with rear volume
3, crab traversing speed 10m/ divides, electron beam line 10mA, and the dosage that takes a round is 10KGy, 300KGy is exactly 30 circles, by that analogy.In order to increase the degradation rate of tetrafluoroethylene, in irradiation process, we adopt the way of adding ozone and tetracol phenixin to reduce irradiation dose, thus saved cost, pass into the way of ozone at ptfe surface to reduce irradiation dose, ozone has extremely strong oxidation capacity, is the oxygenant that occurring in nature is only second to fluorine, being reacted by the dual synergistic oxidation of electron beam and ozone, is low molecular superfine powder of polytetrafluoroethylene high molecular tetrafluoroethylene feed degradation.That is reach same tetrafluoroethylene feed degradation rate and can reduce the electron beam irradiation time, reach minimizing irradiation time, we also utilize the feature that tetracol phenixin is easily degraded under electron beam effect simultaneously, tetrafluoroethylene is easily degraded to negative ion under electron beam effect, negative ion after degraded is unstable, ozonize, and ozone is strong oxidizer, be conducive to macromolecular compound to be degraded to micromolecular compound, thus be conducive to the degradation efficiency improving tetrafluoroethylene.
The invention provides a kind of method that electron beam combined with ozone and tetracol phenixin prepare ultrafine PTFE powder, comprise the steps:
1) the low temperature resistant container package of dried tetrafluoroethylene raw material is placed in liquid nitrogen, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) what sealed by the tetrafluoroethylene raw material after described pulverizing is put on the circular trolley of rumbatron;
4) airtight described rumbatron, and open admission gear, passes into ozone in the annular seal space placing tetrafluoroethylene on described circular trolley, and in the ozone passed into and described pallet, the weight ratio of tetrafluoroethylene raw material is 0.1%-0.5%;
5) open spray equipment, described spray equipment is to the tetrafluoroethylene raw material spray tetracol phenixin on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 3%-8%;
6) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, and irradiation dose is 300-500KGy;
7) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μm.
Wherein, described rumbatron comprises high-frequency oscillator, the irradiation window be equipped with high-frequency oscillator, be positioned at the annular seal space below irradiation window, settle the circular trolley of annular seal space, the spray equipment being positioned at annular seal space and at least 1 admission gear be communicated with tightness system, the energy of described rumbatron is 2Mev, line is 10MA, and scan uniformity is more than 98%, and sweep length is 1000mm.
Wherein, described airflow comminution system comprises micronizer mill, described micronizer mill comprises airflow nozzle, crushiing chamber, pressurized air spurts into crushiing chamber by nozzle at high speeds, at the joint place of multiply high pressure draft, through irradiated described tetrafluoroethylene raw material by impact several times, friction, shearing and pulverizing.Described airflow comminution system also comprises: cyclonic separator, fly-ash separator and induced draft fan;
Described micronizer mill also comprises grading room, crushiing chamber pulverize after tetrafluoroethylene at induced draft fan move under influence to grading room, under grading wheel effect, polytetrafluoroethylene granule is separated by globule size, the fine particle meeting granularity requirements enters cyclonic separator by grading wheel or fly-ash separator is collected, and the coarse particles not meeting granularity requirements drops to crushiing chamber to be continued to pulverize.The airflow nozzle of described micronizer mill is laval nozzle.Described micronizer mill has dry filtrating equipment, before described dry filtrating equipment is positioned at nozzle.
embodiment one
Electron beam combined with ozone and tetracol phenixin prepare a method for ultrafine PTFE powder, comprise the steps:
1) the low temperature resistant container package of dried tetrafluoroethylene raw material is placed in liquid nitrogen, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) the tetrafluoroethylene raw material after described pulverizing is put in the annular seal space on the circular trolley of rumbatron;
4) airtight described rumbatron, and open admission gear, passes into ozone on the ptfe surface on described circular trolley, and in the ozone passed into and described pallet, the weight ratio of tetrafluoroethylene raw material is 0.3%;
5) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, every 0.012m
3tetrafluoroethylene powder (preferably fill with plate, contain tetrafluoroethylene thickness be 12mm) irradiation dose be 400KGy, umber of exposures is 4 times, each 5 minutes;
6) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μm.
Said flow pulverizer comprises screw feeder, airflow nozzle, crushiing chamber, grading room, induced draft fan, and the airflow nozzle of micronizer mill is laval nozzle.Micronizer mill also has dry filtrating equipment, before being positioned at nozzle.Micronizer mill put into by the tetrafluoroethylene that irradiation is good, crushiing chamber is entered by screw feeder, pressurized air passes through the supersonic nozzle of peculiar set-up to crushiing 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 upstream, due to grading rotor high speed rotating, 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 coarse particle more than classification footpath returns crushiing chamber and continues impact grinding, fine particle below classification footpath enters cyclonic separator with air-flow, fly-ash separator is collected, comparatively coarse particle in cyclone collection fine particle, small part ultrafine particle is collected by fly-ash separator, large about 10%-20%, gas is discharged by induced draft fan.
embodiment two
Electron beam combined with ozone and tetracol phenixin prepare a method for ultrafine PTFE powder, comprise the steps:
1) the tetrafluoroethylene raw material of drying is placed in liquid nitrogen with low temperature resistant container package, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after quenching, after pulverizing, particle diameter is 100-1000 μm;
3) the tetrafluoroethylene raw material after described pulverizing is placed in the annular seal space on the circular trolley of rumbatron;
4) open spray equipment, described spray equipment is to the tetrafluoroethylene raw material spray tetracol phenixin on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 5%;
5) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, every 0.012m
3tetrafluoroethylene powder (preferably fill with plate, contain tetrafluoroethylene thickness be 12mm) irradiation dose be 400KGy, umber of exposures is 4 times, each 5 minutes;
6) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μm.
Said flow pulverizer comprises screw feeder, airflow nozzle, crushiing chamber, grading room, induced draft fan, and the airflow nozzle of micronizer mill is laval nozzle.Micronizer mill also has dry filtrating equipment, before being positioned at nozzle.Micronizer mill put into by the tetrafluoroethylene that irradiation is good, crushiing chamber is entered by screw feeder, pressurized air passes through the supersonic nozzle of peculiar set-up to crushiing 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 upstream, due to grading rotor high speed rotating, 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 coarse particle more than classification footpath returns crushiing chamber and continues impact grinding, fine particle below classification footpath enters cyclonic separator with air-flow, fly-ash separator is collected, comparatively coarse particle in cyclone collection fine particle, small part ultrafine particle is collected by fly-ash separator, large about 10%-20%, gas is discharged by induced draft fan.
embodiment three
Electron beam combined with ozone and tetracol phenixin prepare a method for ultrafine PTFE powder, comprise the steps:
1) the low temperature resistant container package of dried tetrafluoroethylene raw material is placed in liquid nitrogen, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) the tetrafluoroethylene raw material after described pulverizing is put in the annular seal space on the circular trolley of rumbatron;
4) airtight described rumbatron, and open admission gear, passes into ozone on the ptfe surface on described circular trolley, and in the ozone passed into and described pallet, the weight ratio of tetrafluoroethylene raw material is 0.3%;
5) open spray equipment, described spray equipment is to the tetrafluoroethylene raw material spray tetracol phenixin on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 5%;
6) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, every 0.012m
3tetrafluoroethylene powder (preferably fill with plate, contain tetrafluoroethylene thickness be 12mm) irradiation dose be 300KGy, umber of exposures is 3 times, each 3 minutes;
7) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μm.
Said flow pulverizer comprises screw feeder, airflow nozzle, crushiing chamber, grading room, induced draft fan, and the airflow nozzle of micronizer mill is laval nozzle.Micronizer mill also has dry filtrating equipment, before being positioned at nozzle.Micronizer mill put into by the tetrafluoroethylene that irradiation is good, crushiing chamber is entered by screw feeder, pressurized air passes through the supersonic nozzle of peculiar set-up to crushiing 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 upstream, due to grading rotor high speed rotating, 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 coarse particle more than classification footpath returns crushiing chamber and continues impact grinding, fine particle below classification footpath enters cyclonic separator with air-flow, fly-ash separator is collected, comparatively coarse particle in cyclone collection fine particle, small part ultrafine particle is collected by fly-ash separator, large about 10%-20%, gas is discharged by induced draft fan.
embodiment four
Electron beam combined with ozone and tetracol phenixin prepare a method for ultrafine PTFE powder, comprise the steps:
1) the low temperature resistant container package of dried tetrafluoroethylene raw material is placed in liquid nitrogen, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) the tetrafluoroethylene raw material after described pulverizing is put in the annular seal space on the circular trolley of rumbatron;
4) airtight described rumbatron, and open admission gear, passes into ozone on the ptfe surface on described circular trolley, and in the ozone passed into and described pallet, the weight ratio of tetrafluoroethylene raw material is 0.1%;
5) open spray equipment, described spray equipment is to the tetrafluoroethylene raw material spray tetracol phenixin on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 3%;
6) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, every 0.012m
3tetrafluoroethylene powder (preferably fill with plate, contain tetrafluoroethylene thickness be 12mm) irradiation dose be 500KGy, umber of exposures is 3 times, each 4 minutes;
7) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μm.
Said flow pulverizer comprises screw feeder, airflow nozzle, crushiing chamber, grading room, induced draft fan, and the airflow nozzle of micronizer mill is laval nozzle.Micronizer mill also has dry filtrating equipment, before being positioned at nozzle.Micronizer mill put into by the tetrafluoroethylene that irradiation is good, crushiing chamber is entered by screw feeder, pressurized air passes through the supersonic nozzle of peculiar set-up to crushiing 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 upstream, due to grading rotor high speed rotating, 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 coarse particle more than classification footpath returns crushiing chamber and continues impact grinding, fine particle below classification footpath enters cyclonic separator with air-flow, fly-ash separator is collected, comparatively coarse particle in cyclone collection fine particle, small part ultrafine particle is collected by fly-ash separator, large about 10%-20%, gas is discharged by induced draft fan.
embodiment five
Electron beam combined with ozone and tetracol phenixin prepare a method for ultrafine PTFE powder, comprise the steps:
1) the low temperature resistant container package of dried tetrafluoroethylene raw material is placed in liquid nitrogen, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) the tetrafluoroethylene raw material after described pulverizing is put in the annular seal space on the circular trolley of rumbatron;
4) airtight described rumbatron, and open admission gear, passes into ozone on the ptfe surface on described circular trolley, and in the ozone passed into and described pallet, the weight ratio of tetrafluoroethylene raw material is 0.5%;
5) open spray equipment, described spray equipment is to the tetrafluoroethylene raw material spray tetracol phenixin on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 8%;
6) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, every 0.012m
3tetrafluoroethylene powder (preferably fill with plate, contain tetrafluoroethylene thickness be 12mm) irradiation dose be 300KGy, umber of exposures is 2 times, each 3 minutes;
7) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μm.
Said flow pulverizer comprises screw feeder, airflow nozzle, crushiing chamber, grading room, induced draft fan, and the airflow nozzle of micronizer mill is laval nozzle.Micronizer mill also has dry filtrating equipment, before being positioned at nozzle.Micronizer mill put into by the tetrafluoroethylene that irradiation is good, crushiing chamber is entered by screw feeder, pressurized air passes through the supersonic nozzle of peculiar set-up to crushiing 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 upstream, due to grading rotor high speed rotating, 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 coarse particle more than classification footpath returns crushiing chamber and continues impact grinding, fine particle below classification footpath enters cyclonic separator with air-flow, fly-ash separator is collected, comparatively coarse particle in cyclone collection fine particle, small part ultrafine particle is collected by fly-ash separator, large about 10%-20%, gas is discharged by induced draft fan.
embodiment six
Electron beam combined with ozone and tetracol phenixin prepare a method for ultrafine PTFE powder, comprise the steps:
1) the low temperature resistant container package of dried tetrafluoroethylene raw material is placed in liquid nitrogen, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) the tetrafluoroethylene raw material after described pulverizing is put in the annular seal space on the circular trolley of rumbatron;
4) airtight described rumbatron, and open admission gear, passes into ozone on the ptfe surface on described circular trolley, and in the ozone passed into and described pallet, the weight ratio of tetrafluoroethylene raw material is 0.1%;
5) open spray equipment, described spray equipment is to the tetrafluoroethylene raw material spray tetracol phenixin on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 8%;
6) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, every 0.012m
3tetrafluoroethylene powder (preferably fill with plate, contain tetrafluoroethylene thickness be 12mm) irradiation dose be 400KGy, umber of exposures is 3 times, each 3 minutes;
7) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μm.
Said flow pulverizer comprises screw feeder, airflow nozzle, crushiing chamber, grading room, induced draft fan, and the airflow nozzle of micronizer mill is laval nozzle.Micronizer mill also has dry filtrating equipment, before being positioned at nozzle.Micronizer mill put into by the tetrafluoroethylene that irradiation is good, crushiing chamber is entered by screw feeder, pressurized air passes through the supersonic nozzle of peculiar set-up to crushiing 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 upstream, due to grading rotor high speed rotating, 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 coarse particle more than classification footpath returns crushiing chamber and continues impact grinding, fine particle below classification footpath enters cyclonic separator with air-flow, fly-ash separator is collected, comparatively coarse particle in cyclone collection fine particle, small part ultrafine particle is collected by fly-ash separator, large about 10%-20%, gas is discharged by induced draft fan.
embodiment seven
Electron beam combined with ozone and tetracol phenixin prepare a method for ultrafine PTFE powder, comprise the steps:
1) the low temperature resistant container package of dried tetrafluoroethylene raw material is placed in liquid nitrogen, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) the tetrafluoroethylene raw material after described pulverizing is put in the annular seal space on the circular trolley of rumbatron;
4) airtight described rumbatron, and open admission gear, passes into ozone on the ptfe surface on described circular trolley, and in the ozone passed into and described pallet, the weight ratio of tetrafluoroethylene raw material is 0.5%;
5) open spray equipment, described spray equipment is to the tetrafluoroethylene raw material spray tetracol phenixin on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 3%;
6) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, every 0.012m
3tetrafluoroethylene powder (preferably fill with plate, contain tetrafluoroethylene thickness be 12mm) irradiation dose be 400KGy, umber of exposures is 3 times, each 3 minutes;
7) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtain the superfine powder of polytetrafluoroethylene of particle diameter below 5 μm.
Said flow pulverizer comprises screw feeder, airflow nozzle, crushiing chamber, grading room, induced draft fan, and the airflow nozzle of micronizer mill is laval nozzle.Micronizer mill also has dry filtrating equipment, before being positioned at nozzle.Micronizer mill put into by the tetrafluoroethylene that irradiation is good, crushiing chamber is entered by screw feeder, pressurized air passes through the supersonic nozzle of peculiar set-up to crushiing 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 upstream, due to grading rotor high speed rotating, 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 coarse particle more than classification footpath returns crushiing chamber and continues impact grinding, fine particle below classification footpath enters cyclonic separator with air-flow, fly-ash separator is collected, comparatively coarse particle in cyclone collection fine particle, small part ultrafine particle is collected by fly-ash separator, large about 10%-20%, gas is discharged by induced draft fan.
The above embodiment only have expressed embodiments of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It 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 (7)
1. electron beam combined with ozone and tetracol phenixin prepare a method for ultrafine PTFE powder, it is characterized in that, comprise the steps:
1) the low temperature resistant container package of dried tetrafluoroethylene raw material is placed in liquid nitrogen, takes out after chilling;
2) pulverized by the tetrafluoroethylene raw material pulverizer after described quenching, after pulverizing, particle diameter is 100-1000 μm;
3) what sealed by the tetrafluoroethylene raw material after described pulverizing is put on the circular trolley of rumbatron;
4) airtight described rumbatron, and open admission gear, passes into ozone in the annular seal space placing tetrafluoroethylene on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the ozone passed into and described circular trolley is 0.1%-0.5%;
5) open spray equipment, described spray equipment is to the tetrafluoroethylene raw material spray tetracol phenixin on described circular trolley, and the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 3%-8%;
6) unlocking electronic accelerator, rumbatron produces high-power electron beam and carries out irradiation to tetrafluoroethylene raw material, and irradiation dose is 300-500KGy;
7) tetrafluoroethylene after irradiation is put into airflow comminution system, through pulverizing and classification fully, obtains the superfine powder of polytetrafluoroethylene of particle diameter at below 5um,
Wherein, the energy of described rumbatron is 2Mev, and line is 10MA, and scan uniformity is more than 98%, and sweep length is 1000mm;
Described rumbatron comprises high-frequency oscillator, and the irradiation window be equipped with high-frequency oscillator, is positioned at the annular seal space below irradiation window, settles the circular trolley of annular seal space, the spray equipment being positioned at annular seal space and at least 1 admission gear be communicated with tightness system.
2. electron beam combined with ozone according to claim 1 and tetracol phenixin prepare the method for ultrafine PTFE powder, it is characterized in that, described in the weight ratio of tetrafluoroethylene raw material on the ozone that passes into and described circular trolley be 0.3%.
3. electron beam combined with ozone according to claim 1 and tetracol phenixin prepare the method for ultrafine PTFE powder, it is characterized in that, the weight ratio of the tetrafluoroethylene raw material on the tetracol phenixin of described spray and described circular trolley is 5%.
4. electron beam combined with ozone according to claim 1 and tetracol phenixin prepare the method for ultrafine PTFE powder, it is characterized in that, described airflow comminution system comprises micronizer mill, described micronizer mill comprises airflow nozzle, crushiing chamber, pressurized air spurts into crushiing chamber by nozzle at high speeds, at the joint place of multiply high pressure draft, through irradiated described tetrafluoroethylene raw material by impact several times, friction, shearing and pulverizing.
5. electron beam combined with ozone according to claim 4 and tetracol phenixin prepare the method for ultrafine PTFE powder, it is characterized in that, described airflow comminution system also comprises:
Cyclonic separator, fly-ash separator and induced draft fan;
Described micronizer mill also comprises grading room, crushiing chamber pulverize after tetrafluoroethylene at induced draft fan move under influence to grading room, under grading wheel effect, polytetrafluoroethylene granule is separated by globule size, the fine particle meeting granularity requirements enters cyclonic separator by grading wheel or fly-ash separator is collected, and the coarse particles not meeting granularity requirements drops to crushiing chamber to be continued to pulverize.
6. electron beam combined with ozone according to claim 5 and tetracol phenixin prepare the method for ultrafine PTFE powder, it is characterized in that, the airflow nozzle of described micronizer mill is laval nozzle.
7. the electron beam combined with ozone according to claim arbitrary in claim 1-6 and tetracol phenixin prepare the method for ultrafine PTFE powder, it is characterized in that, described micronizer mill has dry filtrating equipment, before described dry filtrating equipment is positioned at nozzle.
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