CN101778968B - Thermally stable polyterafluoroethylene fiber and method of making same - Google Patents
Thermally stable polyterafluoroethylene fiber and method of making same Download PDFInfo
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- CN101778968B CN101778968B CN2008800255802A CN200880025580A CN101778968B CN 101778968 B CN101778968 B CN 101778968B CN 2008800255802 A CN2008800255802 A CN 2008800255802A CN 200880025580 A CN200880025580 A CN 200880025580A CN 101778968 B CN101778968 B CN 101778968B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/08—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons
- D01F6/12—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons from polymers of fluorinated hydrocarbons
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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Abstract
A dispersion spun polytetrafluoroethylene fiber exhibiting improved elongation prior to fiber break and increased thermal stability, the fiber prepared by forming a spin mix containing a dispersion of poly(tetrafluoroethylene) particles, forming an intermediate fluoropolymer fiber structure from the spin mix, sintering the intermediate fluoropolymer fiber structure and forming a continuous fluoropolymer filament yarn, drawing the continuous fluoropolymer filament yarn, and thereafter heat setting the continuous fluoropolymer filament yarn.
Description
Technical field
The present invention relates to a kind of heat-staple fluorine-contained polymerisate fibre and preparation method thereof, relate to a kind of polytetrafluoroethylene (PTFE) (" PTFE ") fiber of heat-staple, dispersion spinning especially, it is through preparing said fiber heat setting after stretching.
Background technology
Dispersion spinning or wet method PTFE yarn typically through the preparation of following method: form and contain the water-borne dispersions that gathers (tetrafluoroethylene) particle and the spinning mixture of cellulose ether matrix polymer.Then, said spinning mixture under low relatively pressure (for example, less than 150 pound per square inches), through an aperture, is expressed in the coagulation forming solution that contains sulfuric acid usually, thereby makes matrix polymerization coagulation forming and form the intermediate fiber structure.Said intermediate fiber structure is in case by flush away acid and salt, just through the roller of a series of heating, make said fibre structure drying and the PTFE particles sintering is become continuous PTFE filament yarn.
For productivity ratio that improves the PTFE yarn and the functional character (for example toughness) of improving said yarn; Often through making yarn accelerate the speed on the roller of said yarn a pair of heating in the end than the fast draw roll of rotary speed of the roller of heating through a series of rotary speeies, thus the yarn of stretch dry and sintering.Like this, be stretched on the roller of said yarn a pair of heating in the end or elongate, the speed that the speed that roller is regained because it is stretched is supplied with greater than its heated roller.The amount that said yarn is stretched is called as tensile elongation or draw ratio.For the PTFE yarn of dispersion spinning, typical draw ratio is 6.7～7.4 (being that yarn is stretched to 6.7～7.4 times length greater than its preceding length that stretches).After the stretching, said yarn is wound in bag.
Although stretching PTFE yarn is improved the toughness of said yarn, it also has the influence of not expecting: reduced the heat endurance of said yarn and the percentage elongation before the yarn breakage.Therefore, need a kind of PTFE method of yarn for preparing dispersion spinning, said method can be boosted productivity, and can keep or improve simultaneously the heat endurance of yarn and the percentage elongation before the yarn breakage again.
In dispersion spinning PTFE yarn, keep or improve the stable principal benefits of yarn heat concentrating on the hot gas filtration market.Usually be in or be higher than in 260 degrees centigrade the application owing to be exposed and operate continually at air themperature, be necessary before being delivered for use, the PTFE yarn is heat-treated by the filter medium of PTFE yarn preparation.When this step was accomplished, the standard yarn prepared by the PTFE homopolymers of dispersion spinning shrank 20% or more.Although the contraction PTFE yarn filter medium that obtains performance is good, it needs the user to buy the more PTFE yarn of volume, to remedy the long-pending loss of filter surfaces that is caused owing to shrinking.
Summary of the invention
The osculant PTFE fibre structure of sintering dispersion spinning can cause PTFE particle fusion and winding in the said structure, thereby forms continuous P TFE filament fiber.Stretching continuous P TFE filament fiber can cause said elongation of fiber, and makes the PTFE molecule carry out molecules align and orientation to a certain extent.This situation causes in fiber, producing internal stress, and said internal stress produces through overcoming winding power.According to prior art; Continuous PTFE filament fiber is after stretching; Be quickly cooled to below the Tg of PTFE (Tg of PTFE is about 320～350 ℃, depends on the molecular weight of said PTFE), with the molecule that freezes on the spot or keeps arranging to resist internal stress and winding power.It is believed that; When this continuous PTFE filament fiber is heated to the Tg that is close to or higher than said PTFE molecule subsequently; For example during hot gas filtration is used; Keep the power of said PTFE molecules align lax and therefore be overcome to a certain extent, cause said filament contraction thus, because said PTFE molecule is in ordered state and orientation than low degree.
The present invention is based on following discovery: the drawing process (drawing scenario) of the PTFE fiber yarn through changing dispersion spinning, can overthrow the understanding of just setting up for a long time---total draw ratio of improving the PTFE yarn can reduce the percentage elongation before the yarn breakage; Can also improve simultaneously the heat endurance (that is, reducing said yarn amount of contraction at elevated temperatures) of said yarn.According to the present invention, after continuous P TFE filament fiber formed through sintering, said fiber was stretched, and under the temperature of the Tg that is higher than said PTFE molecule, made said PTFE molecules align and keep a period of time.It is believed that through under Tg or be higher than under the Tg and keep the fiber that stretches, keep said fibre length simultaneously, make the internal stress of the fibrous inside that produces by stretching lax fully.Further believe, when said continuous P TFE filament fiber is placed in following time of temperature of the Tg that is close to or higher than said PTFE molecule after a while, can less shrinking, because the internal stress of said fiber has been relaxed with winding power in advance.Like this, through stretching,, the PTFE yarn of the dispersion spinning of the preceding percentage elongation of a kind of heat endurance that shows raising and yarn breakage is provided subsequently with the setting of PTFE yarn heat or the thermostabilization that stretch through the PTFE of sintering yarn.
In one aspect of the invention; A kind of method for preparing heat-staple PTFE fiber yarn is provided; It comprises: with heating and make its mode through a series of sintering rolls with 1X rotation/minute running with said yarn sintering; Then so that its mode through a pair of draw roll with 1X rotation/minute running said yarn is cooled off; So that it stretches said yarn with the mode between the heat setting roller of 6X rotation/minute running through said draw roll and a series of, last so that its mode through the heat setting roller in turning round formalizes said yarn heat then.
In another aspect of the present invention; A kind of PTFE fiber of 400 DENIERs is provided, and when under 300 ℃ temperature, handling 30 minutes, said fiber shows and is less than 9% shrinkage factor; Wherein said PTFE fiber is one or more multifilament fibers, and is the fiber of dispersion spinning.
In another aspect of the present invention; A kind of PTFE fiber of 400 DENIERs is provided, and when under 300 ℃ temperature, handling 30 minutes, said fiber shows and is less than 15% shrinkage factor; Wherein said PTFE fiber is one or more multifilament fibers, and is the fiber of dispersion spinning.
In another aspect of the present invention; A kind of PTFE fiber of 1200 DENIERs is provided, and said fiber shows and is less than 5% shrinkage factor when under 300 ℃ temperature, handling 30 minutes; Wherein said PTFE fiber is one or more multifilament fibers, and is the fiber of dispersion spinning.
Brief description
Fig. 1 has illustrated that quantity according to the present invention preparation is the figure of heat endurance of the yarn of 400 DENIERs.
Fig. 2 has illustrated that quantity according to the present invention preparation is the figure of heat endurance of the yarn of 1200 DENIERs.
Preferred forms of the present invention
The present invention relates to a kind of fluorine-contained polymerisate fibre of dispersion spinning, said fiber shows the preceding percentage elongation of improved fibrous fracture and the heat endurance of raising." dispersion spinning " is meant; Said fiber prepares through following method: form insoluble fluoropolymer particles; Like PTFE and the dispersion that is commonly called the polymer of fluorinated olefin polymer, said dispersion is mixed with the solution of soluble matrix polymer with the preparation spinning mixture.Then, through said mixture being expressed into (in said coagulation forming solution, said matrix polymer becomes soluble) in the coagulation forming solution, be osculant fluorine-contained polymerisate fibre structure with this spinning mixture coagulation forming.
A kind of method that is normally used for PTFE and relevant polymer are carried out spinning comprises: with the spinning from the water-borne dispersions of polymer particle and viscose liquid (viscose) of said polymer; Wherein cellulose xanthate is the soluble form of matrix polymer; As for example United States Patent (USP) 3; 655,853; 3,114,672 and 2,772,444 that kind of being instructed.Preferably, compare with those methods that adopt viscose liquid, fluorine-contained polymerisate fibre of the present invention adopts more eco-friendly method preparation.A kind of such method is described in United States Patent (USP) 5,820,984; In 5,762,846 and 5,723,081, said patent mode is by reference incorporated the present invention in full into.Usually; This method has adopted cellulose ether polymer; Like methylcellulose, hydroxyethylcellulose, methylhydroxypropylcellulose, hydroxypropyl methylcellulose, hydroxypropyl cellulose, ethyl cellulose or carboxymethyl cellulose, as soluble matrix polymer, to replace viscose liquid.
In case flush away acid and salt, through heating said fiber and making its sintering roll through a series of operations under the Tg of the PTFE molecule that is higher than said fiber, said osculant fluorine-contained polymerisate fibre structure is sintered and the part drying.The said structure of sintering makes said fluoropolymer particles fusion and twines, and forms continuous fluoropolymer filament fiber.
After the sintering, the continuous fluoropolymer filament fiber that part is dry directly is sent to a series of draw rolls of operation at ambient temperature from said a series of sintering rolls.Consequently, said continuous fluoropolymer filament fiber cools off slightly, preferred about 30 degrees Fahrenheits, but still keep transition state.
After the sintering, said fiber directly is sent to a series of heat setting rollers to rotate greater than the speed of said a series of sintering and draw roll from said a series of draw rolls, said continuous fluoropolymer filament fiber is stretched or elongation.Consequently, said continuous fluoropolymer filament fiber in the end is accelerated between near and first heat setting roller of a draw roll and stretches, and slips over last draw roll, thereby makes tensile fiber.Preferably, said a series of warm-up mill moves under the rotary speed of said a series of draw rolls at about six times.This makes fiber have 6.7～7.4 total drawing ratio.
After the stretching, so that said fiber is through the mode of said a series of heat setting rollers, with said continuous fluoropolymer filament fiber further dry also heat setting or thermostabilization.Said heat setting roller is to be higher than said a series of draw roll, and move under identical with the sintering roll in fact temperature.Consequently, the continuous fluoropolymer filament fiber that is stretched is heated and is keeping a period of time under the temperature of said heat setting roller or near this temperature, makes the internal stress relaxation that in fiber, produces that is caused by stretching.After the heat setting, said continuous fluoropolymer long filament is twined and stores.
Through the embodiment of hereinafter, will make an explanation in further detail to the present invention.In each embodiment, the plain ether PTFE of intermediate fiber fibre structure is according to United States Patent (USP) 5,820,984; 5,762,846 and 5,723,081 described method preparation, and subsequently it is handled.In an example, fibre structure is handled according to prior art, and preparation and to have detected quantity be the PTFE yarn of the every long filament of 400 DENIERs, 6.7 DENIERs, to compare with PTFE yarn of the present invention.In another example, fibre structure is handled according to method of the present invention, and preparation and to have detected quantity be the PTFE yarn of the every long filament of 400 DENIERs, 6.7 DENIERs.In another example, fibre structure is handled according to method of the present invention, and preparation and to have detected quantity be the PTFE yarn of the every long filament of 1200 DENIERs, 6.7 DENIERs.
Only if hereinafter has explanation in addition, in each example, measured the draw ratio of PTFE yarn, percentage elongation, toughness and shrinkage factor before the fracture.All shrinkage factor data all are to be under the tensioning state, are placed into the mean value of handling 6 samples of 30 minutes in the standard ovens.All extension test data all are the mean value from the 5 strands of yarn breakages of each in 4 different bobbins.All stretchings are all carried out on the standard tension analyzer.Percentage elongation before the fracture is measured as the fracture strength on instron tensile strength tester.
About TENSILE STRENGTH and the preceding percentage elongation of fracture, more specifically be pars fibrosa to be stretched, and adopt instron tensile strength tester that fiber is applied power.In whole drawing process, measure the amount of the power on the fiber that is applied to.TENSILE STRENGTH is definite divided by DENIER through whole ft lbfs.Elongation before the fibrous fracture is exactly said percentage elongation.For example, 6 inches long fibers are stretched and test.When fracture, the length of fiber is 7.2 inches.Like this, the amount of stretching is 1.2 inches.Should be worth divided by 6 inches of initial lengths, having obtained the percentage elongation before the fracture is 0.20 or 20% (percentage elongation during fracture).
Control yarn---the yarn of the every long filament of 400 DENIERs, 6.7 DENIERs prepares with the standard tensile method
By density is that every cubic centimetre spinning mixture of 1.275 grams prepares osculant PTFE fibre structure.Then, as follows said fibre structure is handled: through making its roller, be heated to the temperature of the about twice of Tg that is higher than said PTFE molecule through a series of heating.Directly through a series of draw rolls, said draw roll moves at ambient temperature with the continuous P TFE filament fiber that obtains, and to rotate greater than the about six times speed of the roller of said heating.
The character of the preparation condition of PTFE control yarn and target finished product yarn is described below.
| The spinning mixing ratio | 1.275g/cc |
| Draw ratio-single step | 6.7 |
| The target percentage elongation | 22％ |
| The toughness that typically obtains | 1.8g/d |
| Aim colour " L " | 15.00 |
| Shrinkage factor under 177dC | 7.58％ |
| Shrinkage factor under 230dC | 5.33％ |
| Shrinkage factor under 260dC | 13.67％ |
| Shrinkage factor under 300dC | 21.25％ |
Embodiment 1---the yarn of the every long filament of 400 DENIERs, 6.7 DENIERs, and with the drawing process preparation that changes
Following parameter is regulated, and to confirm their influences to toughness and heat endurance: tensile elongation or total drawing ratio, the step that yarn stretches in the sintering process increases annealing or heat setting step after stretching, and the spinning hybrid density.Said test is on the yarn of the every long filament of 400 DENIERs, 6.7 DENIERs, to carry out.
Tested six set conditions, the result is positive.Find: can overthrow the association of just setting up for a long time---improve total the stretching and can reduce percentage elongation and improve toughness, simultaneously yarn amount of contraction has at high temperature been reduced～35%.The continuity of the drawing process of said change is good surprisingly, thereby has obtained the productivity ratio higher than expection.In all cases, improve total stretching, the better continuity of total drawing ratio that has produced than in the standard tensile zone, has improved by two stages or stretching in advance.
Said test comprises 2 different spinning mixing ratios.They are that every cubic centimetre of 1.275 gram and 1.291 restrain every cubic centimetre.Be considered to standard spinning mixing ratio 1.275 restrain every cubic centimetre, and commercial use on
yarn in the scope of confirming.All are labeled as the test condition of " 1 " and all under this spinning mixing ratio, carry out.1.291 restrain every cubic centimetre and be considered to the spinning mixing ratio of " being rich in PTFE "; Not in the scope of confirming, commerce is used on
yarn at present.All are labeled as the test condition of " 2 " and all under this spinning mixing ratio, carry out.
Test is under 3 kinds of different drawing process, to carry out, and has obtained 6 sample groups.Drawing process is designated as A, B and C, has obtained test condition 1A, 1B, 1C, 2A, 2B and 2C." A " sample is represented the standard tensile method, but has total stretching of raising." B " sample is represented to be divided into for 2 steps with always stretching, and for example between one group of roller, stretches, and heat setting on second group of roller is then carried out stretching the second time subsequently.This method does not have advantage." C " sample is represented drawing process of the present invention.
| Condition | Test 1A | Test 1B | Test 1C |
| The spinning mixing ratio | 1.275g/cc | 1.275g/cc | 1.275g/cc |
| Phase I stretches | 0.0 | 4.0 | 7.4 |
| Second stage stretches | 7.4 | 1.85 | 0 |
| The total stretching | 7.40 | 7.40 | 7.40 |
| The percentage elongation that obtains | 14.13％ | 15.70％ | 33.51％ |
| The toughness that obtains | 1.8g/d | 1.53g/d | 1.12g/d |
| The color that obtains | 17.2 | 15.9 | 15.5 |
| Shrinkage factor under 177dC | 7.17％ | 5.92％ | 1.67％ |
| Shrinkage factor under 230dC | 5.50％ | 8.58％ | 5.08％ |
| Shrinkage factor under 260dC | 13.25％ | 13.25％ | 3.58％ |
| Shrinkage factor under 300dC | 22.33％ | 20.67％ | 8.50％ |
| The average line shaft size | 0.47lbs | 1.6lbs | 0.89lbs |
| PTFE percentage in the final yarns | 96.865 | 94.516 | 95.555 |
| Condition | Test 2A | Test 2B | Test 2C |
| The spinning mixing ratio | 1.291g/cc | 1.291g/cc | 1.291g/cc |
| Phase I stretches | 0.0 | 4.0 | 7.4 |
| Second stage stretches | 6.8 | 1.85 | 0 |
| The total stretching | 6.80 | 7.40 | 7.40 |
| The percentage elongation that obtains | 14.36％ | 16.18％ | 20.74％ |
| The toughness that obtains | 1.84g/d | 1.76g/d | 1.81g/d |
| The color that obtains | 14.4 | 16.2 | 20.7 |
| Shrinkage factor under 177dC | 6.25％ | 7.00％ | 2.50％ |
| Shrinkage factor under 230dC | 7.25％ | 9.17％ | 4.83％ |
| Shrinkage factor under 260dC | 11.25％ | 14.00％ | 8.17％ |
| Shrinkage factor under 300dC | 17.17％ | 22.75％ | 14.75％ |
| The average line shaft size | 1.05lbs | 1.25lbs | 0.06lbs |
| PTFE percentage in the final yarns | 96.137 | 95.574 | 95.221 |
Shown in said data, when in standard tensile condition stretched when increasing, as was expected has reduced for percentage elongation.But in the drawing process that changes, this association is overthrown, and shows unexpected result." B " test shows, the percentage elongation that under two kinds of drawing process, improves, and the percentage elongation result under " C " condition enlarges markedly.
Toughness does not receive positive influences in any of said spinning mixed method.Although toughness still keeps impregnable relatively state under the condition of 1.291g/cc, under the 1.275g/cc of standard condition, because drawing process departs from standard conditions, significant loss of strength has appearred.
The heat endurance of " C " sample has all obtained significant raising under the condition of test 1 and 2.The figure of the shrinkage factor that obtains is characterized among Fig. 1 provides.
Test 2---before twining, to carry out the mode of draw stage and heat setting in advance, prepare the yarn of the every long filament of 1200 DENIERs, 6.7 DENIERs
This is second test being carried out, its objective is the yarn for the DIMENSIONAL STABILITY that obtains at high temperature to have raising.This test has prepared the fiber of 420 pounds the every long filament of 1200 DENIERs, 6.7 DENIERs, and the toughness of said fiber reduces slightly, and the DENIER uniformity improves, and the DIMENSIONAL STABILITY under the high temperature significantly improves.
In test process, the spinning hybrid density is remained on the output quantity of every cubic centimetre of 59.5 or 1.29 gram.Yarn stretches with the ratio of 6.2X.Because the unaccountable density fluctuation (upset) that continues nearly 6 hours spinning mixture, test has obtained the dispersion productive rate (dispersion yield) less than 50%.The average line shaft size is 1.3 pounds.
Prepared bobbin in test process: standard 1200 DENIERs competitions (campaign) generally produce the yarn that the average line shaft size is 5 pounds a 12000-15000 pound.
Tensile property:
The tensile property of 1200 DENIERs
| W00843 | Test result | Target | |
| Toughness | 1.57 | 1.25 | Minimum 1.5 |
| Standard deviation | 0.08 | 0.11 | |
| Percentage elongation | 28.54 | 57.76 | 32 |
| Standard deviation | 3.41 | 16.59 |
Yarn shrinkage factor is at high temperature measured as follows: the yarn to 200 millimeters long is measured, put it into pre-heated, calibration, in the air oven 30 minutes, measure then.Confirm shrinking percentage then.Figure to result and test setting characterizes as shown in Figure 4.
Those skilled in the art will know, and can within the scope of above-mentioned explanation, carry out various changes.This change that is within those skilled in the art's the limit of power has also constituted a part of the present invention, and is included in the claim of hereinafter.
Essence of the present invention has been described, desired claim is following:
Claims (25)
1. polytetrafluoroethylene fibre, when it in the time of 30 minutes, shows the shrinkage factor less than 9% through 300 ℃ Temperature Treatment, wherein said polytetrafluoroethylene fibre is one or more multifilament fibers and dispersion spinning fiber,
Said polytetrafluoroethylene fibre prepares according to the method that comprises the steps: the said polytetrafluoroethylene fibre of sintering, and said polytetrafluoroethylene fibre and the said polytetrafluoroethylene fibre of heat setting afterwards afterwards stretch;
The temperature of sintering roll is higher than the Tg of the polytetrafluoroethylene (PTFE) molecule of said fiber during sintering;
The heat setting roller is under temperature that is higher than draw roll when stretching and the temperature identical with the sintering roll temperature, to move during heat setting.
2. polytetrafluoroethylene fibre as claimed in claim 1, wherein when through 260 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 4%.
3. polytetrafluoroethylene fibre as claimed in claim 1, wherein when through 230 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 5.5%.
4. polytetrafluoroethylene fibre as claimed in claim 1, wherein when through 177 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 2%.
5. polytetrafluoroethylene fibre as claimed in claim 1 before the polytetrafluoroethylene fibre fracture, shows the percentage elongation greater than 30%.
6. polytetrafluoroethylene fibre as claimed in claim 2, wherein when through 230 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 5.5%; And when through 177 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 2%.
7. polytetrafluoroethylene fibre as claimed in claim 1, wherein said fiber are within the scope of 385 DENIERs～412 DENIERs.
8. polytetrafluoroethylene fibre as claimed in claim 1, wherein said method are that said polytetrafluoroethylene fibre provides 7.4 total drawing ratio.
9. polytetrafluoroethylene fibre, when it in the time of 30 minutes, shows the shrinkage factor less than 15% through 300 ℃ Temperature Treatment, wherein said polytetrafluoroethylene fibre is one or more multifilament fibers and dispersion spinning fiber,
Said polytetrafluoroethylene fibre prepares according to the method that comprises the steps: the said polytetrafluoroethylene fibre of sintering, and said polytetrafluoroethylene fibre and the said polytetrafluoroethylene fibre of heat setting afterwards afterwards stretch;
The temperature of sintering roll is higher than the Tg of the polytetrafluoroethylene (PTFE) molecule of said fiber during sintering;
The heat setting roller is under temperature that is higher than draw roll when stretching and the temperature identical with the sintering roll temperature, to move during heat setting.
10. polytetrafluoroethylene fibre as claimed in claim 9, wherein when its through 260 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 9%.
11. polytetrafluoroethylene fibre as claimed in claim 9, wherein when through 230 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 5%.
12. polytetrafluoroethylene fibre as claimed in claim 9, wherein when through 177 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 3%.
13. polytetrafluoroethylene fibre as claimed in claim 10, wherein when through 230 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 5%; And when through 177 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 3%.
14. polytetrafluoroethylene fibre as claimed in claim 9, wherein said method are said polytetrafluoroethylene fibre 7.4 total drawing ratio is provided.
15. polytetrafluoroethylene fibre as claimed in claim 9, wherein said method have obtained greater than the percentage elongation before 20% the said polytetrafluoroethylene fibre fracture.
16. polytetrafluoroethylene fibre as claimed in claim 9 is by the mixture preparation of the spinning mixture density with every cubic centimetre of 1.275 gram.
17. polytetrafluoroethylene fibre as claimed in claim 9, wherein said fiber are within the scope of 385 DENIERs～412 DENIERs.
18. polytetrafluoroethylene fibre, when it in the time of 30 minutes, shows the shrinkage factor less than 5% through 300 ℃ Temperature Treatment, wherein said polytetrafluoroethylene (PTFE) is one or more multifilament fibers and dispersion spinning fiber,
Described polytetrafluoroethylene fibre prepares according to the method that comprises the steps: the said polytetrafluoroethylene fibre of sintering, and said polytetrafluoroethylene fibre and the said polytetrafluoroethylene fibre of heat setting afterwards afterwards stretch;
The temperature of sintering roll is higher than the Tg of the polytetrafluoroethylene (PTFE) molecule of said fiber during sintering;
The heat setting roller is under temperature that is higher than draw roll when stretching and the temperature identical with the sintering roll temperature, to move during heat setting.
19. polytetrafluoroethylene fibre as claimed in claim 18, wherein when its through 260 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 4.5%.
20. polytetrafluoroethylene fibre as claimed in claim 18, wherein when through 230 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 3%.
21. polytetrafluoroethylene fibre as claimed in claim 18, wherein when through 177 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 2%.
22. polytetrafluoroethylene fibre as claimed in claim 19, wherein when through 230 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 3%; And when through 177 ℃ Temperature Treatment in the time of 30 minutes, said fiber shows the shrinkage factor less than 2%.
23. polytetrafluoroethylene fibre as claimed in claim 18, wherein said fiber are within the scope of 600 DENIERs～1350 DENIERs.
24. polytetrafluoroethylene fibre as claimed in claim 18, wherein before said polytetrafluoroethylene fibre fracture, said fiber shows the percentage elongation greater than 40%.
25. polytetrafluoroethylene fibre as claimed in claim 18 can provide 6.7 or the method preparation of higher total drawing ratio for said polytetrafluoroethylene fibre through a kind of.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US76324207A | 2007-06-14 | 2007-06-14 | |
| US11/763,242 | 2007-06-14 | ||
| US11/763,249 | 2007-06-14 | ||
| US11/763,249 US7498079B1 (en) | 2007-06-13 | 2007-06-14 | Thermally stable polytetrafluoroethylene fiber and method of making same |
| PCT/US2008/066854 WO2008157307A1 (en) | 2007-06-14 | 2008-06-13 | Thermally stable polyterafluoroethylene fiber and method of making same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101778968A CN101778968A (en) | 2010-07-14 |
| CN101778968B true CN101778968B (en) | 2012-09-05 |
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| CN2008800255802A Active CN101778968B (en) | 2007-06-14 | 2008-06-13 | Thermally stable polyterafluoroethylene fiber and method of making same |
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| Country | Link |
|---|---|
| EP (1) | EP2167710B1 (en) |
| CN (1) | CN101778968B (en) |
| AT (1) | ATE542933T1 (en) |
| WO (1) | WO2008157307A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102493007B (en) * | 2011-11-15 | 2014-01-29 | 厦门柏润氟材料科技有限公司 | Microwave sintering and drafting device for pasty polytetrafluoroethylene extruded fibers |
| WO2013159020A1 (en) * | 2012-04-19 | 2013-10-24 | Toray Fluorofibers (America), Inc. | Dispersion spun fluoropolymer fiber prepared from non-melt-processible polytetrafluoroethylene and perfluoroalkoxy |
| US9422642B2 (en) * | 2013-07-29 | 2016-08-23 | Toray Fluorofibers (America), Inc. | Wear polytetrafluoroethylene (PTFE) fiber and method of making same |
| EP2942426B1 (en) * | 2014-05-05 | 2019-04-17 | Filmop International s.r.l. | Poy yarn |
| EP3670716A1 (en) * | 2018-12-17 | 2020-06-24 | Evonik Operations GmbH | Oriented fluoropolymers |
| CN110158166A (en) * | 2019-04-03 | 2019-08-23 | 苏州耐德新材料科技有限公司 | A kind of preparation process of chlor-alkali amberplex polytetrafluoroethylene (PTFE) monofilament |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4064214A (en) * | 1975-09-22 | 1977-12-20 | E. I. Du Pont De Nemours And Company | Process for making polytetrafluoroethylene yarn |
| EP0352749A2 (en) * | 1988-07-25 | 1990-01-31 | Asahi Kasei Kogyo Kabushiki Kaisha | A filament comprising a tetrafluoroethylene polymer and a process for producing the same |
| CN1152948A (en) * | 1994-06-30 | 1997-06-25 | 大金工业株式会社 | Bulky long fibre and split yarn of polytetrafluoroethylene, method of mfg. the same, cotton like material mfg. method using the fiber and yarn, and dust collecting filter cloth |
| US5807633A (en) * | 1994-10-04 | 1998-09-15 | Daikin Industries, Ltd. | Polytetrafluoroethylene composite fiber, cotton-like materials obtained therefrom and processes for production thereof |
| US5820984A (en) * | 1996-12-20 | 1998-10-13 | E. I. Du Pont De Nemours And Company | Dispersion spinning process for poly(tetrafluoroethylene) and related polymers |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5723081A (en) * | 1996-12-20 | 1998-03-03 | E. I. Du Pont De Nemours And Company | Dispersion spinning process for polytetrafluoroethylene and related polymers |
| AU2002237116A1 (en) * | 2002-03-07 | 2003-09-16 | Manegro Administracao E Participacoes Ltda. | Expanded ptfe fiber |
-
2008
- 2008-06-13 CN CN2008800255802A patent/CN101778968B/en active Active
- 2008-06-13 EP EP08780812A patent/EP2167710B1/en active Active
- 2008-06-13 AT AT08780812T patent/ATE542933T1/en active
- 2008-06-13 WO PCT/US2008/066854 patent/WO2008157307A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4064214A (en) * | 1975-09-22 | 1977-12-20 | E. I. Du Pont De Nemours And Company | Process for making polytetrafluoroethylene yarn |
| EP0352749A2 (en) * | 1988-07-25 | 1990-01-31 | Asahi Kasei Kogyo Kabushiki Kaisha | A filament comprising a tetrafluoroethylene polymer and a process for producing the same |
| CN1152948A (en) * | 1994-06-30 | 1997-06-25 | 大金工业株式会社 | Bulky long fibre and split yarn of polytetrafluoroethylene, method of mfg. the same, cotton like material mfg. method using the fiber and yarn, and dust collecting filter cloth |
| US5807633A (en) * | 1994-10-04 | 1998-09-15 | Daikin Industries, Ltd. | Polytetrafluoroethylene composite fiber, cotton-like materials obtained therefrom and processes for production thereof |
| US5820984A (en) * | 1996-12-20 | 1998-10-13 | E. I. Du Pont De Nemours And Company | Dispersion spinning process for poly(tetrafluoroethylene) and related polymers |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2167710B1 (en) | 2012-01-25 |
| EP2167710A4 (en) | 2011-01-05 |
| CN101778968A (en) | 2010-07-14 |
| ATE542933T1 (en) | 2012-02-15 |
| EP2167710A1 (en) | 2010-03-31 |
| WO2008157307A1 (en) | 2008-12-24 |
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