CN103182342B - Gamma-rays combined with ozone prepares the method for ultrafine PTFE powder - Google Patents
Gamma-rays combined with ozone prepares the method for ultrafine PTFE powder Download PDFInfo
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Abstract
Gamma-rays combined with ozone prepares a method for ultrafine PTFE powder, comprising: the polytetrafluoroethylene (PTFE) raw material of drying is placed in liquid nitrogen chilling; The polytetrafluoroethylene (PTFE) powder that particle diameter is 100-1000 μm is ground into again with pulverizer; Then be put in the container of the automatic production line of Co 60 device; Automatic production line first sprays ozone, and then carrying out irradiation by during Co 60 device, irradiation dose 40-60KGy, exposure time determines according to the radioactivity size of Co 60 device; Polytetrafluoroethylene (PTFE) powder through irradiation is transported to outside radiation chamber by automatic production line; Put into airflow comminution system, fully pulverize and can obtain particle diameter at the superfine powder of polytetrafluoroethylene of 0.2-5 μm.According to method provided by the invention, the degradation rate of polytetrafluoroethylene (PTFE) can be increased, adopt automatic production line also to further increase production efficiency simultaneously.
Description
Technical field
The present invention relates to chemical technology field, particularly a kind of gamma-rays combined with ozone prepares the method for ultrafine PTFE powder.
Background technology
Polytetrafluoroethylene (PTFE) is commonly called as King, is the polymer be polymerized by tetrafluoroethylene monomer, has very strong coherency, is easy to be attached to together, not easily disperses.Ultrafine PTFE powder (micro mist) is low-molecular-weight polytetrafluoroethylene (PTFE), molecular weight is below 10,000, particle diameter is between 0.5-15 μm, ultrafine PTFE powder not only remains the original all premium properties of polytetrafluoroethylene (PTFE), also there is the performance of many uniquenesses: as without self-coagulation, without electrostatic effect, intermiscibility is good, molecular weight is low, good dispersion, self lubricity are high, coefficient of friction reduce, not conglomeration, easily mixes mutually with oily or organic liquid, also can Homogeneous phase mixing etc. with other solia particle.Ultrafine PTFE powder average grain diameter is less than 5 μm, and specific surface is greater than 10m
2/ g, coefficient of friction 0.06 ~ 0.07, lubricity is good, can be dispersed in well in many materials.Can be used as plastics, rubber, ink, coating, anti-stick, the antifriction of lubricant grease, flame-retardant additive, also can make aerosol etc. as dry lubricant.Ultrafine PTFE powder can be made separately kollag and use, also can as the additive of plastics, rubber, coating, ink, lubricating oil, lubricating grease etc.Various typical powder process method and plastics or rubber mix can be adopted, as blended etc.In oil and grease, add ultrafine PTFE powder, can coefficient of friction be reduced, as long as add a few percent, the life-span of lubricating oil can be improved.Its dispersion in organic solvent also can make releasing agent.
Ozone is the allotrope of oxygen, and at normal temperatures, it is a kind of blue gas having off-odor, is insoluble to carbon tetrachloride.Ozone has very strong oxidisability, easily decomposes, and the hydroxyl radical free radical (.OH) produced in decomposable process has extremely strong oxidability.
Prepare the method for ultrafine PTFE powder, determine the structural behaviour of ultrafine PTFE powder, molecular weight and distribution thereof.The preparation method of ultrafine PTFE powder mainly contains two kinds: 1, directly regulate polymerization with tetrafluoroethene, after certain hour, stop polymerisation, product is suitably processed again; 2, with HMW PTFE cracking, then pulverize.The method that cracking reaction prepares ultrafine PTFE powder mainly contains thermal cracking and irradiation to crack.In irradiation to crack process, the cracking of PTFE is subject to the impact of radiation parameter, the difference of the energy source that irradiation dose, irradiation adopt and oxidizing condition, all there is considerable influence to the physical property of ultrafine PTFE powder and chemical property, therefore need to be optimized the equipment and process condition in PTFE irradiation to crack process and strictly to control.
Summary of the invention
For above-mentioned problems of the prior art, a kind of gamma-rays combined with ozone is the object of the present invention is to provide to prepare the method for ultrafine PTFE powder.
In order to realize foregoing invention object, the technical solution used in the present invention is as follows:
Gamma-rays combined with ozone prepares a method for ultrafine PTFE powder, comprises the steps:
(1) the polytetrafluoroethylene (PTFE) raw material liquid nitrogen of drying is carried out quenching; Polytetrafluoroethylene (PTFE) raw meal after quenching is broken into the powder that particle diameter is 100-1000 μm;
(2) polytetrafluoroethylene (PTFE) powder is put into container, the sealing of described container and be positioned at run through 60Coradiation room automatic production line on, be provided with at least 1 releasing device interface in it, 60Coradiation room comprises and is positioned at least 1 60Coradiation device in the middle of radiation chamber, the automatic production line through 60Coradiation device, at least 1 ozone releasing device, radiation divider wall and control room;
(3) polytetrafluoroethylene (PTFE) powder along with open automatic production line at the uniform velocity enter radiation chamber, at polytetrafluoroethylene (PTFE) powder through at least 1 60Coradiation device, described at least 1 ozone releasing device is filled with ozone in the sealing container at polytetrafluoroethylene (PTFE) powder place, and the weight ratio of the ozone be filled with and described polytetrafluoroethylene (PTFE) powder is 0.1%-0.5%;
(4) through described at least 1 60Coradiation device, the gamma ray that at least 1 60Coradiation device produces carries out irradiation to polytetrafluoroethylene (PTFE) powder, and irradiation dose is 40-60KGy;
(5) container be equipped with through the polytetrafluoroethylene (PTFE) powder of irradiation transports radiation chamber by automatic production line;
(6) with airslide disintegrating mill the polytetrafluoroethylene (PTFE) powder through irradiation is pulverized again, classification, fine polytetrafluoroethylpowder powder is dispersed into the superfine powder of polytetrafluoroethylene of average grain diameter less than 5 μm.
Further, described at least 1 ozone releasing device is filled with ozone in the sealing container of polytetrafluoroethylene (PTFE) powder, and the weight ratio of the ozone be filled with and polytetrafluoroethylene (PTFE) powder is 0.3%.
Further, described at least 1 60Coradiation device is single screen cobalt source.
Further, described at least 1 60Coradiation device is double grid plate cobalt source.
Further, step (4) also comprises described automatic production line and is bonded together with the container that polytetrafluoroethylene (PTFE) powder is housed, and the polytetrafluoroethylene (PTFE) powder through irradiation is poured into the charging aperture of the airslide disintegrating mill described in step (5) at the port of export of automatic production line.
Further, described airslide disintegrating mill comprises air current spray nozzle, crushing chamber, and compressed air spurts into crushing chamber by nozzle at high speeds, makes fine polytetrafluoroethylpowder powder particle through irradiation in the joint place impact several times of multiply high pressure draught, friction, shearing and pulverizing.
Further, described airslide disintegrating mill also comprises cyclone separator, deduster and air-introduced machine; Described airslide disintegrating mill comprises graded region, crushing chamber pulverize after polytetrafluoroethylene (PTFE) at air-introduced machine move under influence to graded region, under grading wheel effect, fine polytetrafluoroethylpowder powder particle is separated by granule size, the fine grained meeting granularity requirements enters cyclone separator by grading wheel or deduster is collected, comparatively corase particles in cyclone collection fine particle, small part ultrafine particle is collected by deduster, and the coarse granule not meeting granularity requirements drops to crushing 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, and dry filtrating equipment is positioned at nozzle front.
Further, it is characterized in that, described automatic production line is for can realize auto reversive bucket conveyor or hanging chain induction system.
According to the preparation method of superfine powder of polytetrafluoroethylene provided by the invention, under identical radiation parameter, the degradation rate of polytetrafluoroethylene (PTFE) can be increased, or also can reach identical degradation rate when reducing exposure time, can enhance productivity significantly, save production cost, take into account product quality simultaneously, ensure that the low molecular weight polytetrafluoroethylene average grain diameter obtained is less than 5 μm, and whole manufacture process is strictly controlled.
Detailed description of the invention
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 polytetrafluoroethylene (PTFE) is poor (1000Gy), degraded is caused by after high-energy radiation, the present invention utilizes this characteristic of polytetrafluoroethylene (PTFE) to adopt Co 60 device to carry out radiation degradation process to polytetrafluoroethylene (PTFE), then carries out dispersion treatment with airslide disintegrating mill and can obtain superfine powder of polytetrafluoroethylene material.
Cobalt-60(Co) be one of radio isotope of metallic element cobalt, its half-life is 5.27.It can release energy through β decay becomes nickel-60 up to the high-velocity electrons of 315keV, and can release two bundle gamma rays, its energy is respectively 1.17 and 1.33MeV simultaneously.Gamma-rays, also known as γ particle flux, is the electromagnetic wave that wavelength is shorter than 0.2 dust, has very strong penetration power.
After irradiation-induced degradation, polytetrafluoroethylene (PTFE) becomes low molecule by macromolecule, but low molecular polytetrafluoroethylene (PTFE) is still reunited together, is not dispersed into micromolecular superfine powder.In order to can superfine powder be obtained, must the low molecular polytetrafluoroethylene (PTFE) after irradiation-induced degradation through air-flow crushing and pulverizing.
The airslide disintegrating mill used in the following embodiment of the present invention comprises air current spray nozzle, crushing chamber, compressed air spurts into crushing chamber by nozzle at high speeds, at the joint place of multiply high pressure draught, through irradiated fine polytetrafluoroethylpowder powder particle by impact several times, friction, shearing and pulverizing.Wherein, the air current spray nozzle of airslide disintegrating mill is Laval nozzle, and its front is provided with dry filtrating equipment.Airslide disintegrating mill also comprises cyclone separator, deduster and air-introduced machine.Airslide disintegrating mill also comprises graded region, crushing chamber pulverize after polytetrafluoroethylene (PTFE) at air-introduced machine move under influence to graded region, under the centrifugal action that the stage turbine of High Rotation Speed produces, polytetrafluoroethylgranule granule is pressed granule size and is separated, the fine grained meeting granularity requirements enters cyclone separator by grading wheel or deduster is collected, comparatively corase particles in cyclone collection fine particle, small part ultrafine particle is collected by deduster, and the coarse granule not meeting granularity requirements drops to crushing chamber to be continued to pulverize.
embodiment one
A preparation method for superfine powder of polytetrafluoroethylene, comprises the steps:
(1) the polytetrafluoroethylene (PTFE) raw material liquid nitrogen of drying is carried out cold treatment; Polytetrafluoroethylene (PTFE) raw meal after K cryogenic treatment is broken into the powder that particle diameter is 100-1000 μm;
(2) polytetrafluoroethylene (PTFE) powder is put into container, container be positioned at run through 60Coradiation room bucket conveyor on sealable goods bucket, 60Coradiation room comprises 1 the single screen cobalt source be positioned in the middle of radiation chamber, through the bucket conveyor in single screen cobalt source, be positioned at least 1 ozone releasing device of also contiguous described 60Coradiation device on automatic production line, radiation divider wall and control room;
(3) polytetrafluoroethylene (PTFE) powder at the uniform velocity enters radiation chamber along with the bucket conveyor opened, at least 1 ozone releasing device polytetrafluoroethylene (PTFE) powder through time spray ozone to it, the ozone of spray and the weight ratio of polytetrafluoroethylene (PTFE) powder are 0.5%;
(4) through single screen cobalt source, the gamma ray that single screen cobalt source produces carries out irradiation to polytetrafluoroethylene (PTFE) powder, and irradiation dose is 40KGy, and the speed of bucket conveyor is determined by the radioactivity size in single screen cobalt source, and is controlled by control room;
(5) the goods bucket be equipped with through the polytetrafluoroethylene (PTFE) powder of irradiation transports radiation chamber by bucket conveyor, and the polytetrafluoroethylene (PTFE) powder through irradiation is discharged at air-flow crushing raw material district;
(6) with airslide disintegrating mill the fine polytetrafluoroethylpowder powder through irradiation is pulverized again, classification, fine polytetrafluoroethylpowder powder is dispersed into the superfine powder of polytetrafluoroethylene of average grain diameter below 5 μm.
embodiment two:
A preparation method for superfine powder of polytetrafluoroethylene, comprises the steps:
(1) step (1) is identical with embodiment one;
(2) polytetrafluoroethylene (PTFE) powder is put into container, container be positioned at run through 60Coradiation room bucket conveyor on salable goods bucket (goods bucket is provided with and passes into ozone communicating pipe), 60Coradiation room comprises 2 the single screen cobalt sources be positioned in the middle of radiation chamber, through the bucket conveyor in single screen cobalt source, be positioned at 1 ozone releasing device of also contiguous 60Coradiation device on automatic production line, radiation divider wall and control room;
(3) polytetrafluoroethylene (PTFE) powder at the uniform velocity enters radiation chamber along with the bucket conveyor opened, 2 ozone releasing devices polytetrafluoroethylene (PTFE) powder through time spray ozone to it, the ozone of spray and the weight ratio of polytetrafluoroethylene (PTFE) powder are 0.5%;
(4) after spray ozone, polytetrafluoroethylene (PTFE) powder continues to continue to move with bucket conveyor, through single screen cobalt source, the gamma ray that single screen cobalt source produces carries out irradiation to polytetrafluoroethylene (PTFE) powder, irradiation dose is 60KGy, the speed of bucket conveyor is determined by the radioactivity size in single screen cobalt source, and is controlled by control room;
Step (5) is identical with embodiment one to (6).
embodiment three:
A preparation method for superfine powder of polytetrafluoroethylene, comprises the steps:
(1) step (1) is identical with embodiment one;
(2) polytetrafluoroethylene (PTFE) powder is put into container, container is positioned at the sealing goods bucket run through in the hanging chain induction system of 60Coradiation room, 60Coradiation room comprises 1 the double grid plate cobalt source be positioned in the middle of radiation chamber, through the hanging chain induction system in double grid plate cobalt source, be positioned at hanging chain induction system and 1 ozone releasing device in contiguous double grid plate cobalt source, radiation divider wall and control room;
(3) polytetrafluoroethylene (PTFE) powder at the uniform velocity enters radiation chamber along with the hanging chain induction system of opening, at least 1 ozone releasing device polytetrafluoroethylene (PTFE) powder through time spray ozone to it, the ozone of spray and the weight ratio of polytetrafluoroethylene (PTFE) powder are 0.1%;
(4) polytetrafluoroethylene (PTFE) powder continues mobile with hanging chain induction system, through double grid plate cobalt source, the gamma ray that double grid plate cobalt source produces carries out irradiation to polytetrafluoroethylene (PTFE) powder, irradiation dose is 50KGy, the speed of hanging chain induction system is determined by the radioactivity size in double grid plate cobalt source, and is controlled by control room;
Step (5) is identical with embodiment one to (6).
embodiment four:
A preparation method for superfine powder of polytetrafluoroethylene, comprises the steps:
(1) step (1) is identical with embodiment one;
(2) polytetrafluoroethylene (PTFE) powder is put into container, container is positioned at the sealing goods bucket run through in the hanging chain induction system of 60Coradiation room, 60Coradiation room comprises 3 the single screen cobalt sources be positioned in the middle of radiation chamber, through the hanging chain induction system in single screen cobalt source, be positioned at 2 ozone releasing devices in also contiguous single screen cobalt source above hanging chain induction system, radiation divider wall and control room;
(3) polytetrafluoroethylene (PTFE) powder at the uniform velocity enters radiation chamber along with the hanging chain induction system of opening, 2 ozone releasing devices polytetrafluoroethylene (PTFE) powder through time spray ozone to it, the ozone of spray and the weight ratio of polytetrafluoroethylene (PTFE) powder are 0.3%;
(4) polytetrafluoroethylene (PTFE) powder is along with hanging chain induction system continuation movement, through single screen cobalt source, the gamma ray that single screen cobalt source produces carries out irradiation to polytetrafluoroethylene (PTFE) powder, irradiation dose is 60KGy, the speed of hanging chain induction system is determined by the radioactivity size in single screen cobalt source, and is controlled by control room;
Step (5) is identical with embodiment one to (6).
embodiment five:
A preparation method for superfine powder of polytetrafluoroethylene, comprises the steps:
(1) step (1) is identical with embodiment one;
(2) polytetrafluoroethylene (PTFE) powder is put into container, container is positioned at the salable goods bucket run through in the hanging chain induction system of 60Coradiation room, 60Coradiation room comprises 2 the double grid plate cobalt sources be positioned in the middle of radiation chamber, through the hanging chain induction system in double grid plate cobalt source, be positioned at automatic production line and 3 ozone releasing devices in contiguous double grid plate cobalt source, radiation divider wall and control room;
(3) polytetrafluoroethylene (PTFE) powder along with open hanging chain induction system at the uniform velocity enter radiation chamber, ozone releasing device polytetrafluoroethylene (PTFE) powder through time spray ozone to it, the ozone of spray and the weight ratio of polytetrafluoroethylene (PTFE) powder are 0.5%;
(4) polytetrafluoroethylene (PTFE) powder continues to move ahead along with hanging chain induction system, through double grid plate cobalt source, the gamma ray that double grid plate cobalt source produces carries out irradiation to polytetrafluoroethylene (PTFE) powder, irradiation dose is 60KGy, the speed of hanging chain induction system is determined by the radioactivity size in double grid plate cobalt source, and is controlled by control room;
Step (5) is identical with embodiment one to (6).
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 (8)
1. gamma-rays combined with ozone prepares a method for ultrafine PTFE powder, it is characterized in that, comprises the steps:
(1) the polytetrafluoroethylene (PTFE) raw material liquid nitrogen of drying is carried out quenching; Polytetrafluoroethylene (PTFE) raw meal after quenching is broken into the powder that particle diameter is 100-1000 μm;
(2) polytetrafluoroethylene (PTFE) powder is put into container, the sealing of described container and be positioned at run through 60Coradiation room automatic production line on, at least 1 releasing device interface is provided with in it, 60Coradiation room comprises and is positioned at least 1 60Coradiation device in the middle of radiation chamber, the automatic production line through 60Coradiation device, at least 1 ozone releasing device, radiation divider wall and control room, and wherein said automatic production line is for can realize auto reversive bucket conveyor or hanging chain induction system;
(3) polytetrafluoroethylene (PTFE) powder along with open automatic production line at the uniform velocity enter radiation chamber, at polytetrafluoroethylene (PTFE) powder through at least 1 60Coradiation device, described at least 1 ozone releasing device is filled with ozone in the sealing container at polytetrafluoroethylene (PTFE) powder place, and the weight ratio of the ozone be filled with and described polytetrafluoroethylene (PTFE) powder is 0.1%-0.5%;
(4) through described at least 1 60Coradiation device, the gamma ray that at least 1 60Coradiation device produces carries out irradiation to polytetrafluoroethylene (PTFE) powder, and irradiation dose is 40-60KGy;
(5) container be equipped with through the polytetrafluoroethylene (PTFE) powder of irradiation transports radiation chamber by automatic production line, described automatic production line is bonded together with the container that polytetrafluoroethylene (PTFE) powder is housed, and the polytetrafluoroethylene (PTFE) powder through irradiation is poured into the charging aperture of airslide disintegrating mill at the port of export of automatic production line;
(6) with airslide disintegrating mill the polytetrafluoroethylene (PTFE) powder through irradiation is pulverized again, classification, fine polytetrafluoroethylpowder powder is dispersed into the superfine powder of polytetrafluoroethylene of average grain diameter less than 5 μm.
2. the method for claim 1, is characterized in that, described at least 1 ozone releasing device is filled with ozone in the sealing container of polytetrafluoroethylene (PTFE) powder, and the weight ratio of the ozone be filled with and polytetrafluoroethylene (PTFE) powder is 0.3%.
3. the method for claim 1, is characterized in that, described at least 1 60Coradiation device is single screen cobalt source.
4. the method for claim 1, is characterized in that, described at least 1 60Coradiation device is double grid plate cobalt source.
5. the method for claim 1, it is characterized in that, described airslide disintegrating mill comprises air current spray nozzle, crushing chamber, compressed air spurts into crushing chamber by nozzle at high speeds, makes fine polytetrafluoroethylpowder powder particle through irradiation in the joint place impact several times of multiply high pressure draught, friction, shearing and pulverizing.
6. method as claimed in claim 5, is characterized in that: described airslide disintegrating mill also comprises cyclone separator, deduster and air-introduced machine; Described airslide disintegrating mill comprises graded region, crushing chamber pulverize after polytetrafluoroethylene (PTFE) at air-introduced machine move under influence to graded region, under grading wheel effect, fine polytetrafluoroethylpowder powder particle is separated by granule size, the fine grained meeting granularity requirements enters cyclone separator by grading wheel or deduster is collected, and the coarse granule not meeting granularity requirements drops to crushing chamber to be continued to pulverize.
7. method as claimed in claim 6, it is characterized in that, the air current spray nozzle of described airslide disintegrating mill is Laval nozzle.
8. method as described in claim 7, it is characterized in that, described airslide disintegrating mill has dry filtrating equipment, and dry filtrating equipment is positioned at nozzle front.
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| CN107236063B (en) * | 2017-06-14 | 2018-01-23 | 广州华大生物科技有限公司 | A kind of preparation method of low molecular weight polytetrafluoroethylene |
| US11028239B2 (en) * | 2018-02-07 | 2021-06-08 | Daikin Industries, Ltd. | Manufacturing method for low molecular weight polytetrafluoroethylene, and powder |
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