CN101824158A - Method for preparing cross-linked polytetrafluoroethylene through electron beam irradiation - Google Patents
Method for preparing cross-linked polytetrafluoroethylene through electron beam irradiation Download PDFInfo
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Abstract
The invention relates to a method for preparing cross-linked polytetrafluoroethylene through electron beam irradiation, which comprises the following steps: 1. arranging a polytetrafluoroethylene sample in an irradiation container; 2. sealing the irradiation container, pumping until the pressure in the irradiation container is 0-1000Pa, and filling an inert gas until the pressure reaches the atmospheric pressure; 3. heating the irradiation container until the temperature in the container rises to 300-400 DEG C, and keeping the temperature constant; 4. arranging the irradiation container under electron beams, irradiating with the irradiation dose rate ranging from 1Gy/s to 1 multiplied by 105Gy/s, so that the irradiation dose reaches 10-3000kGy; and 5. stopping the irradiation, lowering the temperature, filling an inert gas into the irradiation container continuously to blow the sample to the room temperature, and then taking out the sample after being irradiated. The method can fundamentally maintain the mechanical properties of the prepared cross-linked polytetrafluoroethylene material, and has a broad application value in the production of polytetrafluoroethylene-based wear-resistant and radiation-resistant materials.
Description
Technical field
The present invention relates to a kind of method for preparing cross-linked polytetrafluoroethylthrough (PTFE) with the electron beam irradiation method.
Background technology
Polytetrafluoroethylene (PTFE) has excellent properties, have the title of " plastics king ", and it is widely used, and is one of indispensable important materials of modern industry.There are shortcomings such as creep-resistant property, wear resistance, radiation hardness ability in PTFE, and these have limited it and have used under some most advanced and sophisticated condition, and improving these shortcomings simultaneously also is one of important directions of modified ptfe material.The above-mentioned shortcoming of PTFE is attributable to its long chain molecule structure, has the research report to show, if realize the crosslinked of PTFE molecule long-chain, can effectively improve above-mentioned shortcoming.Because the PTFE chemical stability is fabulous, therefore can't realize that it is crosslinked with chemical process.At present, radiation method is unique feasible method of realizing crosslinked PTFE.
The performance of PTFE and its molecular weight are closely related, and have only molecular weight to reach 1,000,000 orders of magnitude and could guarantee that PTFE has mechanical property preferably.With the reduction of PTFE molecular weight, its mechanical property will sharply descend, and the radiation cleavage legal system is equipped with the PTFE ultra-fine powder technology and reduces its molecular weight realization by radiation cleavage.Yet, if PTFE is crosslinked, forming reticulated structure between molecular chain, mechanical property remains unchanged substantially; PTFE molecule segment after crosslinked is difficult to regular arrangement, shows as degree of crystallinity and reduces, and fusing point descends.Therefore, utilize the test of Mechanics Performance Testing and fusing point can characterize PTFE whether crosslinked or cracking takes place.
Be widely used in the preparation industry of crosslinked, the plastic hot shrink-down material of wire cable insulating material now with the high molecular method of energetic ray (electron beam or gamma ray) radiation crosslinking.With cobalt 60 (
60Co) source of radiation is compared, and crosslinking electron beam irradiation PTFE has more industrial application value.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method with the prepared by EB irradiation cross-linked polytetrafluoroethylthrough is provided, prepares crosslinked PTFE material by Electron-beam irradiation technology, and prepare the different crosslinked PTFE material of degree of crosslinking by the control irradiation dose.
In order to solve the problems of the technologies described above, the invention provides a kind of method with the prepared by EB irradiation cross-linked polytetrafluoroethylthrough, comprise the steps:
After making the temperature inside the box rise to 300~400 ℃, step 3, the described irradiation box of heating make temperature keep constant;
Step 4, described irradiation box being placed under the electron beam, is 1~1 * 10 according to the radiation dose rate scope
5Gy/s irradiation makes radiation dose reach 10~3000kGy;
Description of drawings
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Fig. 1 is an electron beam irradiation synoptic diagram of using the method for prepared by EB irradiation cross-linked polytetrafluoroethylthrough of the present invention.
Reference numeral is among the figure:
1, rumbatron; 2, electron beam; 3, irradiation box titanium foil window; 4, irradiation box; 5, irradiation box moving guide rail.
Embodiment
Provide preferred embodiment of the present invention below, and described in detail, enable to understand better function of the present invention, characteristics.
The present invention utilizes tetrafluoroethylene at high temperature, accept electron beam irradiation in inert atmosphere or the vacuum, obtains crosslinked tetrafluoroethylene.In order to realize the method with the prepared by EB irradiation cross-linked polytetrafluoroethylthrough of the present invention, need have following assembly as shown in Figure 1:
One can divergent bundle 2 rumbatron 1;
One is positioned at the irradiation box 4 of rumbatron 1 lower end, this irradiation box 4 is the highest be heated to temperature arrive 450 ℃ constant, and irradiation box 4 has excellent sealing performance, operation can vacuumize and take a breath;
The upper surface of irradiation box has a titanium foil window 3 that can make electron beam see through, and electron beam passes thus, and is radiated tetrafluoroethylene sample in the casing, sees accompanying drawing 1;
In addition, irradiation box 4 optionally places on the moving guide rail 5, thereby irradiation box 4 can move back and forth, so that irradiation box 4 can be passed electron beam 2 toward ground return, makes electron beam 2 periodically pass titanium foil window 3 with the irradiation sample.
At first the tetrafluoroethylene sample is put on the sample tray of the irradiation box 4 that has titanium foil window 3, the shape of tetrafluoroethylene sample can be lamellar, strip or Powdered, its thickness is decided according to the energy of described electron beam, guarantees that electron beam can penetrate sample.
The described irradiation box of good seal, and to be evacuated to pressure range be 0~1000Pa; Perhaps feed a rare gas element to irradiation box after pressure range is 0~1000Pa being evacuated to, to pressure range be 0~1.5 * 10
5Pa, this rare gas element can be in nitrogen, argon gas or the helium a kind of.
Heat described irradiation box make the temperature inside the box rise to 300~400 ℃ constant, best results when temperature range is 320~370 ℃.
Subsequently, feed the electron beam 2 of an energy region at 0.1~10MeV, irradiation box 4 is moved back and forth according to constant speed on moving guide rail 5 and come and go and pass described electron beam 2, adjust the translational speed of irradiation box 4, making sample is 1~1 * 10 according to radiation dose rate
5Gy/s irradiation continues one section radiated time, makes radiation dose reach 10~3000kGy.
At last, stop irradiation, cooling, not open close inert gas purge sample is opened the tetrafluoroethylene sample through irradiation that irradiation box 4 is taken out gained to room temperature.
Wherein, radiation dose rate is meant once the back and forth radiation dose of interior absorption of sample of time.That is,
The tensile property test: subsequently the tetrafluoroethylene sample is carried out the tensile property test, the tensile property of tetrafluoroethylene carries out according to ISO 527-1/2 experimental standard; After the polytetrafluorethylepowder powder sample made the thick thin slice of 1mm through compressing tablet, sintering, test by above-mentioned standard.
Dsc (DSC) test fusing point: with dsc the tetrafluoroethylene sample is carried out the fusing point test subsequently, adopt N
2As shielding gas, the flow of shielding gas is 40ml/min, and temperature rise rate is 10 ℃/min, and amount of samples is 10mg.
Undertaken by above implementation procedure, irradiation sample is the thick tetrafluoroethylene thin plate of 1mm, beam energy 1.6MeV, the rare gas element that feeds is a 1atm nitrogen, dose rate is 333Gy/s, and radiated time 7.5min, total radiation dose are 150kGy, 330~350 ℃ of radiation temperatures, gained radiation crosslinking tetrafluoroethylene with do not listed in table 1 by radiating tetrafluoroethylene performance.Wherein, do not listed in table 1 and be used for contrast test by radiating tetrafluoroethylene thin plate performance.
Undertaken by above implementation procedure, irradiation sample is the thick tetrafluoroethylene thin plate of 1mm, beam energy 1.6MeV, the rare gas element that feeds is a 1atm nitrogen, dose rate is 333Gy/s, and radiated time 7.5min, total radiation dose are 150kGy, radiation temperature is a room temperature, and gained radiation tetrafluoroethylene performance is listed in table 1.
Undertaken by above implementation procedure, irradiation sample is the thick tetrafluoroethylene thin plate of 1mm, beam energy 1.6MeV, the rare gas element that feeds is a 1atm nitrogen, dose rate is 333Gy/s, and radiated time 7.5min, total radiation dose are 150kGy, radiation temperature is 330~350 ℃, and gained radiation crosslinking tetrafluoroethylene performance is listed in table 1.
Embodiment 4
Undertaken by above implementation procedure, irradiation sample is the thick tetrafluoroethylene thin plate of 1mm, beam energy 1.6MeV, the rare gas element that feeds is a 1atm nitrogen, dose rate is 100Gy/s, and radiated time 3.3min, total radiation dose are 20kGy, radiation temperature is 330~340 ℃, and gained radiation crosslinking tetrafluoroethylene performance is listed in table 1.
Undertaken by above implementation procedure, irradiation sample is the thick tetrafluoroethylene thin plate of 1mm, beam energy 1.6MeV, the rare gas element that feeds is the 1atm argon gas, dose rate is 1000Gy/s, and radiated time 16.7min, total radiation dose are 1000kGy, 330~360 ℃ of radiation temperatures, gained radiation crosslinking tetrafluoroethylene performance is listed in table 1.
Embodiment 6
Undertaken by above implementation procedure, irradiation sample is the thick tetrafluoroethylene thin plate of 1mm, beam energy 1.6MeV, being evacuated to pressure is 500~1000Pa, dose rate is 333Gy/s, and radiated time 10min, total radiation dose are 200kGy, 320~360 ℃ of radiation temperatures, gained radiation crosslinking tetrafluoroethylene performance is listed in table 1.
Embodiment 7
Undertaken by above implementation procedure; irradiation sample is polytetrafluorethylepowder powder (400 order); the sample apparent thickness is 0.3mm; beam energy 1.6MeV; the rare gas element that feeds is the 1atm nitrogen protection; dose rate is 667Gy/s; radiated time 12.5min, total radiation dose are 500kGy, 320~350 ℃ of radiation temperatures; gained radiation crosslinking polytetrafluorethylepowder powder; with its pulverizing, depress to 1mm thickness sheet at 30MPa pressure more earlier, made thin slice in 0.5 hour at 400 ℃ of sintering temperatures again; the measurement that stretches the results are shown in result's contrast of table 1.
The polytetrafluorethylepowder powder of irradiation (400 order) does not depress to 1mm thickness sheet in 30MPa pressure, makes thin slice in 0.5 hour at 400 ℃ of following sintering again, is used for the tensile property test, the results are shown in result's contrast of table 1.
Table 1
Claims (8)
1. one kind prepares the method for cross-linked polytetrafluoroethylthrough with the electron beam irradiation method, it is characterized in that, comprises the steps:
Step 1, at first the tetrafluoroethylene sample is put into an irradiation box;
Step 2, the described irradiation box of good seal, and to be evacuated to pressure range be 0~1000Pa;
After making the temperature inside the box rise to 300~400 ℃, step 3, the described irradiation box of heating make temperature keep constant;
Step 4, described irradiation box being placed under the electron beam, is 1~1 * 10 according to the radiation dose rate scope
5Gy/s irradiation makes radiation dose reach 10~3000kGy;
Step 5, stop irradiation, the described sample behind the irradiation is taken out in cooling, and constantly feed the described sample of an inert gas purge to room temperature in described irradiation box then.
2. method according to claim 1 is characterized in that, described step 2 also comprises: being evacuated to pressure range is to import a rare gas element to irradiation box behind 0~1000Pa, to pressure range be 0~1.5 * 10
5Pa, the described rare gas element of step 2 can be the same or different with the described rare gas element of step 5.
3. method according to claim 1 and 2 is characterized in that, the temperature range of described step 3 is 320 ℃~370 ℃.
4. method according to claim 1 and 2 is characterized in that, described irradiation box upper surface has a titanium foil window that can make electron beam pass.
5. method according to claim 1 and 2 is characterized in that, being shaped as of described tetrafluoroethylene sample is lamellar, strip or Powdered.
6. method according to claim 1 and 2 is characterized in that, described tetrafluoroethylene sample is the thick thin plate of 1mm, and described beam energy is 1.6MeV.
7. method according to claim 1 and 2 is characterized in that, described rare gas element is nitrogen, argon gas.
8. method according to claim 1 and 2 is characterized in that irradiation box is located on the moving guide rail, and constant speed moves back and forth, and makes the described sample of the periodic irradiation of described electron beam.
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CN102806132A (en) * | 2011-06-02 | 2012-12-05 | 浙江中科辐射高分子材料研发中心 | Preparation method for PE (polyethylene)/PTFE (polytetrafluoroethylene) mixed micronization wax for UV (ultraviolet) photocuring printing ink |
CN103172880A (en) * | 2013-04-03 | 2013-06-26 | 太仓金凯特种线缆有限公司 | Method for preparing PTFE (Polytetrafluoroethylene) superfine powder by gamma ray |
CN103183835A (en) * | 2013-04-03 | 2013-07-03 | 太仓金凯特种线缆有限公司 | Method for preparing PTFE (polytetrafluoroethylene) ultrafine powder by combining gamma rays, ozone and hydrogen peroxide |
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CN103193997A (en) * | 2013-04-03 | 2013-07-10 | 太仓金凯特种线缆有限公司 | Method for preparing PTFE (Polytetrafluoroethylene) ultrafine powder in manner of combining ultraviolet rays with ozone and carbon tetrachloride |
CN103191819A (en) * | 2013-04-03 | 2013-07-10 | 太仓金凯特种线缆有限公司 | Method for preparing PTFT (Polytetrafluoroethylene) ultrafine powder by electron beam combined ozone |
CN103252279A (en) * | 2013-04-03 | 2013-08-21 | 太仓金凯特种线缆有限公司 | Method for preparation of ultrafine PTFE powder by combining electron beams with ozone and hydrogen peroxide |
CN103252278A (en) * | 2013-04-03 | 2013-08-21 | 太仓金凯特种线缆有限公司 | Method for preparation of ultrafine PTFE powder by electron beams |
CN103252277A (en) * | 2013-04-03 | 2013-08-21 | 太仓金凯特种线缆有限公司 | Method for preparation of ultrafine PTFE powder by combining electron beams with hydrogen peroxide and carbon tetrachloride |
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RU2669841C1 (en) * | 2017-08-09 | 2018-10-16 | Сергей Витальевич Слесаренко | Method of obtaining polymer materials |
CN111117724A (en) * | 2019-12-23 | 2020-05-08 | 上海零慕纳米材料科技有限公司 | Preparation method of modified PTFE (Polytetrafluoroethylene) ultrafine powder, modified PTFE ultrafine powder and nano energy-saving antiwear agent |
CN112768151A (en) * | 2020-12-31 | 2021-05-07 | 中国人民解放军96901部队23分队 | Preparation method of irradiation-resistant cross-linked polytetrafluoroethylene film for low-noise cable |
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CN103172880A (en) * | 2013-04-03 | 2013-06-26 | 太仓金凯特种线缆有限公司 | Method for preparing PTFE (Polytetrafluoroethylene) superfine powder by gamma ray |
CN103183835A (en) * | 2013-04-03 | 2013-07-03 | 太仓金凯特种线缆有限公司 | Method for preparing PTFE (polytetrafluoroethylene) ultrafine powder by combining gamma rays, ozone and hydrogen peroxide |
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CN103252279A (en) * | 2013-04-03 | 2013-08-21 | 太仓金凯特种线缆有限公司 | Method for preparation of ultrafine PTFE powder by combining electron beams with ozone and hydrogen peroxide |
CN103252278A (en) * | 2013-04-03 | 2013-08-21 | 太仓金凯特种线缆有限公司 | Method for preparation of ultrafine PTFE powder by electron beams |
CN103252277A (en) * | 2013-04-03 | 2013-08-21 | 太仓金凯特种线缆有限公司 | Method for preparation of ultrafine PTFE powder by combining electron beams with hydrogen peroxide and carbon tetrachloride |
CN103172880B (en) * | 2013-04-03 | 2015-02-04 | 太仓金凯特种线缆有限公司 | Method for preparing PTFE (Polytetrafluoroethylene) superfine powder by gamma ray |
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CN103252277B (en) * | 2013-04-03 | 2015-11-04 | 太仓金凯特种线缆有限公司 | Electron beam prepares the method for ultrafine PTFE powder in conjunction with hydrogen peroxide and carbon tetrachloride |
CN103252278B (en) * | 2013-04-03 | 2015-11-04 | 太仓金凯特种线缆有限公司 | A kind of method utilizing electron beam to prepare ultrafine PTFE powder |
CN103191819B (en) * | 2013-04-03 | 2015-11-18 | 太仓金凯特种线缆有限公司 | Electron beam combined with ozone prepares the method for ultrafine PTFE powder |
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RU2669841C1 (en) * | 2017-08-09 | 2018-10-16 | Сергей Витальевич Слесаренко | Method of obtaining polymer materials |
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CN111117724A (en) * | 2019-12-23 | 2020-05-08 | 上海零慕纳米材料科技有限公司 | Preparation method of modified PTFE (Polytetrafluoroethylene) ultrafine powder, modified PTFE ultrafine powder and nano energy-saving antiwear agent |
CN112768151A (en) * | 2020-12-31 | 2021-05-07 | 中国人民解放军96901部队23分队 | Preparation method of irradiation-resistant cross-linked polytetrafluoroethylene film for low-noise cable |
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