CN1958893A - Polythene cross-linking fibers with shape memory, and preparation method - Google Patents
Polythene cross-linking fibers with shape memory, and preparation method Download PDFInfo
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- CN1958893A CN1958893A CN 200510118386 CN200510118386A CN1958893A CN 1958893 A CN1958893 A CN 1958893A CN 200510118386 CN200510118386 CN 200510118386 CN 200510118386 A CN200510118386 A CN 200510118386A CN 1958893 A CN1958893 A CN 1958893A
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- cross
- polythene
- shape memory
- polyethylene
- linking
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- 239000000835 fiber Substances 0.000 title claims abstract description 73
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 66
- 238000004132 cross linking Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- -1 polyethylene Polymers 0.000 claims abstract description 44
- 239000004698 Polyethylene Substances 0.000 claims abstract description 43
- 230000005855 radiation Effects 0.000 claims abstract description 11
- 229920001903 high density polyethylene Polymers 0.000 claims description 12
- 239000004700 high-density polyethylene Substances 0.000 claims description 12
- 229920001684 low density polyethylene Polymers 0.000 claims description 9
- 239000004702 low-density polyethylene Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 230000002285 radioactive effect Effects 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 5
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 claims description 4
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 4
- 239000003431 cross linking reagent Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 4
- 239000003504 photosensitizing agent Substances 0.000 claims description 4
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012965 benzophenone Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 3
- 239000011259 mixed solution Substances 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 229920010741 Ultra High Molecular Weight Polyethylene (UHMWPE) Polymers 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000006386 memory function Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229920000431 shape-memory polymer Polymers 0.000 description 3
- 230000037303 wrinkles Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012781 shape memory material Substances 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 229920003020 cross-linked polyethylene Polymers 0.000 description 1
- 239000004703 cross-linked polyethylene Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000636 poly(norbornene) polymer Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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Abstract
The present invention relates to a shape memory polyethylene crosslinked fiber and its preparation method. It is characterized by that the restorable deformation temperature of said polyethylene crosslinked fiber is 40-60 deg.C, under the condition of tensioning by 200% the deformation restoration rate of said fiber is 80-99%. Said polyethylene crosslinked fiber is obtained by utilizing polyethylene fiber and making it undergo the process of cross-linking modification treatment under the action of radiation ray.
Description
Technical field
The present invention relates to the modified poly ethylene cross filament, in particular, relate to a kind of polythene cross-linking fibers with shape memory and manufacture method thereof.
Background technology
Shape-memory material is meant that the variation of environment (temperature, illumination, pressure or chemical substance etc.) responds to external world, and adjust accordingly, thereby be returned to the functional material of the state of preestablishing according to these mechanics parameters (shape, position or strain etc.) that change himself.Shape-memory material commonly used has marmem and shape-memory polymer, compare with marmem, shape-memory polymer has light weight, cost is low, shape memory temperature is easy to adjusting, easy coloring, deformation quantity is big, figuration is easy, and is easy to excite characteristics such as its deformation restore funcitons.Present shape-memory polymer mainly is based on polyurethane, polynorbornene, trans 1, the macromolecular material of 4-polyisoprene etc.
The principle of shape memory fiber is, fixedly phase in the fiber (also claiming hard section) has good heat endurance, and but anti-phase (also claiming soft section) has tangible crystalline melt temperature (Tm) or glass transition temperature (Tg) in 10-50 ℃ of temperature range, and Tm or Tg can be set at human body and wear uncomfortable temperature.When environment temperature was lower than Tm or Tg, the motion of polymer segment was frozen, and the densification of strand is arranged and stoped hot transmission, thereby has good warmth retention property when low temperature; When temperature was higher than Tm or Tg, the gap between the macromolecular chain obviously increased, and moisture-penetrable ventilated property significantly improves.In addition, the garment material with suitable memory triggering temperature has performances such as good wrinkle resistance and ABRASION RESISTANCE, after it in use produces fine wrinkle, can make its return to the original form (exempting to press) by elevated temperature.
Polyethylene belongs to typical crystalline polymer, and clearer and more definite fusing point is arranged, and below fusing point, macromolecular chain is subjected to the constraint of lattice energy, and segment is difficult to freely-movable, is in glassy state; In case temperature reaches it more than fusing point, big molecular thermalmotion is broken through the lattice structure constraint, becomes viscous state.This polyethylene does not have SME, but polyethylene is carried out crosslinked after, it then no longer is viscous state when above that polymer is heated to its fusing point, but elastomeric state, can make its distortion this moment by applying external force, cools off under its deformation state, crystallization is appeared again, freezing stress.When polymer is heated to fusing point when above again, watery fusion, stress release, material recovers original form, finishes a memory circulation.Thereby crosslinked polyethylene can be used as the material of preparation shape memory fiber.
Utilize different irradiance methods that polyvinyl resin or polyethylene fiber are handled heat resistance, creep resistance and the surperficial cementability that can improve and improve them, but present all technology all do not relate to the shape memory of polyethylene fiber.
Summary of the invention
The technical problem to be solved in the present invention is, at the above-mentioned deficiency of prior art, provides a kind of modified poly ethylene cross filament, gives polyethylene fiber with shape memory function by modification, has improved heat resistance, creep resistance of polyethylene fiber etc. simultaneously.
Another object of the present invention also is to provide a kind of preparation method of polythene cross-linking fibers with shape memory.
Polythene cross-linking fibers with shape memory provided by the invention is characterized in that, the recoverable deformation temperature of this polythene cross-linking fibers is 40～60 ℃, is stretching below 200%, and the distortion recovery rate of fiber is 80～99%.This polythene cross-linking fibers is by polyethylene fiber is carried out cross-linking modified making under the effect of irradiation ray.
Poly high density polyethylene (HDPE) (HDPE), linear low density of polyethylene (LLDPE), low density polyethylene (LDPE) (LDPE) or the ultra-high molecular weight polyethylene (UHMWPE) of comprising that the present invention uses.Different polyethylene has different molecular chain structures.HDPE is the linear molecule structure, and side chain is few on the strand; More short-chain branch is arranged on the LLDPE strand, do not have long-chain branch substantially, still belong to linear structure; LDPE has the long-chain branch branched structure, also has the part intramolecular transfer to invent a charge against the short-chain branch of formation, and its crystal property, fusing point and mechanical property all are lower than HDPE; UHMWPE is linear linear chain structure, and the weight average relative molecular weight can reach 100-500 ten thousand.
The present invention mainly is at different polyethylene fibers, it is radiation crosslinking modified to utilize various rays and ultraviolet light to carry out, control suitable condition, can not influence on the basis of polyethylene fiber mechanical property substantially, give polyethylene fiber and have shape memory function.
The preparation method of polythene cross-linking fibers with shape memory provided by the invention comprises following steps:
A) polyethylene fiber is placed in the closed container, and container is evacuated to 6.5 * 10
-2Pa;
B) container that will be mounted with polyethylene fiber by automatic circulating system is sent into irradiation system, carries out cross-linking modified under the effect of the irradiation ray that radiation source sends;
C) polyethylene fiber behind irradiation is taken out, place in the vacuum drying chamber and annealed 1 hour down at 80～90 ℃.
Wherein, before step a) is placed into closed container with polyethylene fiber, this polyethylene fiber can also be immersed in certain hour in photosensitizer and the cross-linking agent solution, and then be positioned in the closed container.
The technology characteristics for preparing polythene cross-linking fibers with shape memory by x ray irradiation x provided by the invention also is, polyethylene fiber is positioned in the closed container, is evacuated to 6.5 * 10
-2Pa charges into acetylene gas or high pure nitrogen after perhaps vacuumizing again, is preferably under high vacuum or the complete anaerobic state to carry out; After will filling the polyethylene fiber container and sending into irradiation system, by parameters such as computer monitor irradiation intensities, when with electron accelerator during as radiation source, the control irradiation intensity is at 0.04～1.6J/cm
2Between; When with radioactive source during as radiation source, irradiation dose is 25～250kGy, and when irradiation dose during greater than 100kGy, every irradiation 100kGy took out sample 2-3 minute from irradiation system, prevents that sample temperature is too high and causes disorientation.
Irradiation ray among the present invention can be plasma, ultraviolet ray, electron ray, radioactive source ray or other any suitable irradiation ray.
The beneficial effect of implementing polythene cross-linking fibers with shape memory provided by the invention and preparation method thereof is, utilize irradiation to carry out cross-linking modified to polyethylene fiber, thereby give polyethylene fiber with shape memory function, improved heat resistance, creep resistance of polyethylene fiber etc. simultaneously.
Polyethylene shape memory cross filament provided by the invention has following characteristics:
1. (in the manufacture process) gives fiber required shape when being higher than setting temperature, reduces the temperature to afterwards below the setting temperature, and the gained shape will be remembered;
2. show as elastomer when using below setting temperature and more than the transition temperature;
3. if in use (generally below transition temperature) fiber shape is because of external force change (as wrinkle), more than transition temperature (as laundry and drying temperature) and when setting temperature is following, fiber can return to original shape, Here it is typical shape memory.
4. fiber shows as glassy state at normal temperature (below the transition temperature), and modulus is higher, and elasticity is better than general fibre, but lower than elastomer;
5. heat resistance is better;
6. the raw material of preparation polyethylene shape memory cross filament is different with the raw material of preparation ordinary elasticity fiber, changes proportioning raw materials and composition, can regulate shape-memory properties and transition temperature;
7. shape memory can repeatedly design repeatedly.
The specific embodiment
Below by specific embodiment the present invention is carried out more detailed description.
Embodiment 1
Get ultra-high molecular weight polyethylene (UHMWPE) fiber and put into closed container, be evacuated down to 6.5 * 10
-2Pa is placed on after the sealing and enters radiation chamber on the conveyer belt automatically, carries out irradiation with gamma-rays as radioactive source, when computer shows that irradiation dose is 50kGy, takes out polyethylene fiber, anneals 1 hour under 80 ℃ in vacuum drying chamber then.
Embodiment 2
Get high density polyethylene (HDPE) (HDPE), linear low density of polyethylene (LLDPE), low density polyethylene (LDPE) (LDPE) or ultra-high molecular weight polyethylene (UHMWPE), with the gamma-rays is the irradiation ray, the accumulation irradiation intensity is 100kGy, and atmosphere is acetylene gas, carries out the cross-linking radiation reaction.Other condition is with embodiment 1.The mechanical property of crosslinked front and back polyethylene fiber sees Table 1.
The mechanical property * 1 of the crosslinked front and back of table 1 polyethylene fiber
| Sample | TENSILE STRENGTH (MPa) | Elongation at break (%) | ||
| Predose | Behind the irradiation | Predose | Behind the irradiation | |
| HDPE | 12.5 | 16.4 | 6.10 | 5.35 |
| LLDPE | 19.4 | 21.9 | 7.05 | 6.08 |
| HDPE | 25.1 | 30.8 | 9.98 | 7.60 |
| UHMWPE | 90800 | 101200 | 3.15 | 2.25 |
* 1The mechanical property of fiber adopts the INSTRON fiber strength tester to measure, and draw speed is 50mm/min, and each sample is surveyed 5 rhizoid bundles, averages.
Embodiment 3
Getting ultra-high molecular weight polyethylene (UHMWPE) under acetylene atmosphere, is the irradiation ray with the plasma, and irradiation intensity is respectively 25,50,100,150,200 and 250kGy, and other condition is with embodiment 1.The gained fiber stretches 150% down at 110 ℃, 40 ℃ of setting down, and then is heated to 60 ℃, and its distortion recovery rate sees Table 2.
The distortion recovery rate of UHMWPE fiber under the different irradiation intensities of table 2
| Irradiation intensity (kGy) | 0 | 25 | 50 | 100 | 150 | 200 | 250 |
| Distortion recovery rate (%) | 0 | 35 | 92 | 99 | 99 | 99 | 99 |
Embodiment 4
Get ultra-high molecular weight polyethylene (UHMWPE) fiber have photosensitizer (benzophenone and derivative thereof, 1.0wt%) and crosslinking agent (acrylate soaked in xylene solution 20wt%) 20 minutes.Soaked fiber is placed in the closed container, is evacuated down to 6.5 * 10
-2Pa feeds high pure nitrogen then, puts into UV-crosslinked reactor, and average irradiation intensity is 0.3J/cm
2Carry out cross-linking modifiedly, after irradiation is finished, take out polyethylene fiber, 90 ℃ of annealing 1 hour down in vacuum drying chamber promptly get and have polythene cross-linking fibers with shape memory.
It is to be noted; the foregoing description only is used for that the invention will be further described; can not be interpreted as limiting the scope of the invention; those skilled in the art can be according to content of the present invention; in the protection domain that does not exceed invention, summary of the invention is made some nonessential and improvement and adjustment others.
Claims (10)
1) a kind of polythene cross-linking fibers with shape memory is characterized in that, the recoverable deformation temperature of this polythene cross-linking fibers is 40～60 ℃, is stretching below 200%, and the distortion recovery rate of fiber is 80～99%.
2) polythene cross-linking fibers with shape memory according to claim 1 is characterized in that, this polythene cross-linking fibers is by polyethylene fiber is carried out cross-linking modified making under the effect of irradiation ray.
3) polythene cross-linking fibers with shape memory according to claim 1 is characterized in that, polyethylene wherein is to be selected from high density polyethylene (HDPE), low density polyethylene (LDPE), linear low density of polyethylene or ultra-high molecular weight polyethylene.
4) a kind of preparation method of polythene cross-linking fibers with shape memory is characterized in that, comprises following processing step:
A) polyethylene fiber is placed in the closed container, and container is evacuated to 6.5 * 10
-2Pa;
B) container that will be mounted with polyethylene fiber by automatic circulating system is sent into irradiation system, carries out cross-linking modified under the effect of the irradiation ray that radiation source sends;
C) polyethylene fiber behind irradiation is taken out, place in the vacuum drying chamber and annealed 1 hour down at 80～90 ℃.
5) preparation method of polythene cross-linking fibers with shape memory according to claim 4, it is characterized in that, wherein also be included in polyethylene fiber is placed into closed container before, to its step of soaking, soak the mixed solution that the solution that adopts is made up of photosensitizer and crosslinking agent.
6) preparation method of polythene cross-linking fibers with shape memory according to claim 5, it is characterized in that, photosensitizer wherein is that weight percentage is 1.0% benzophenone and derivative solution thereof, and crosslinking agent wherein is that weight percentage is 20% acrylate solution.
7) preparation method of polythene cross-linking fibers with shape memory according to claim 4 is characterized in that, wherein can also be included in the step a) container vacuumized after, in container, charge into the step of acetylene gas or high pure nitrogen.
8) preparation method of polythene cross-linking fibers with shape memory according to claim 4 is characterized in that, radiation source wherein is electron accelerator or radioactive source.
9) preparation method of polythene cross-linking fibers with shape memory according to claim 4 is characterized in that, irradiation ray wherein is plasma, ultraviolet ray, electron ray or radioactive source ray.
10) preparation method of polythene cross-linking fibers with shape memory according to claim 4 is characterized in that, wherein when adopting radioactive source as radiation source, irradiation intensity is 0.04～1.6J/cm
2When adopting electron accelerator as radiation source, irradiation intensity is 25～250kGy.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510118386 CN1958893A (en) | 2005-10-31 | 2005-10-31 | Polythene cross-linking fibers with shape memory, and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510118386 CN1958893A (en) | 2005-10-31 | 2005-10-31 | Polythene cross-linking fibers with shape memory, and preparation method |
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| CN1958893A true CN1958893A (en) | 2007-05-09 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102356191A (en) * | 2009-03-18 | 2012-02-15 | 鲍姆胡特挤出有限责任公司 | Polyethylene fiber, its use and process for its manufacture |
| CN102400375A (en) * | 2010-09-14 | 2012-04-04 | 公安部第一研究所 | Method for producing modified ultrahigh molecular weight polyethylene fiber by using mutual radiation grafting technology |
| CN102517672A (en) * | 2011-11-09 | 2012-06-27 | 武汉纺织大学 | Preparation method for high-modulus and high-tensile-resilience special fiber |
| CN101768868B (en) * | 2010-01-04 | 2013-02-20 | 广东省均安牛仔服装研究院 | Resin styling liquid and denim crumpling process method |
| CN105399966A (en) * | 2015-12-29 | 2016-03-16 | 哈尔滨工业大学 | Preparation of shape-memory polymer and application of shape-memory polymer to 4D printing |
| CN114437381A (en) * | 2022-02-21 | 2022-05-06 | 中国科学院上海应用物理研究所 | Modified crosslinked polyethylene, preparation method and application thereof, and formed polyethylene |
| CN114990714A (en) * | 2022-06-07 | 2022-09-02 | 五邑大学 | Ultra-high molecular weight polyethylene fiber with reversible shape memory effect and preparation method thereof |
-
2005
- 2005-10-31 CN CN 200510118386 patent/CN1958893A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102356191A (en) * | 2009-03-18 | 2012-02-15 | 鲍姆胡特挤出有限责任公司 | Polyethylene fiber, its use and process for its manufacture |
| CN101768868B (en) * | 2010-01-04 | 2013-02-20 | 广东省均安牛仔服装研究院 | Resin styling liquid and denim crumpling process method |
| CN102400375A (en) * | 2010-09-14 | 2012-04-04 | 公安部第一研究所 | Method for producing modified ultrahigh molecular weight polyethylene fiber by using mutual radiation grafting technology |
| CN102517672A (en) * | 2011-11-09 | 2012-06-27 | 武汉纺织大学 | Preparation method for high-modulus and high-tensile-resilience special fiber |
| CN102517672B (en) * | 2011-11-09 | 2013-07-03 | 武汉纺织大学 | Preparation method for high-modulus and high-tensile-resilience special fiber |
| CN105399966A (en) * | 2015-12-29 | 2016-03-16 | 哈尔滨工业大学 | Preparation of shape-memory polymer and application of shape-memory polymer to 4D printing |
| CN114437381A (en) * | 2022-02-21 | 2022-05-06 | 中国科学院上海应用物理研究所 | Modified crosslinked polyethylene, preparation method and application thereof, and formed polyethylene |
| CN114437381B (en) * | 2022-02-21 | 2024-04-26 | 中国科学院上海应用物理研究所 | Modified crosslinked polyethylene, preparation method and application thereof, and formed polyethylene |
| CN114990714A (en) * | 2022-06-07 | 2022-09-02 | 五邑大学 | Ultra-high molecular weight polyethylene fiber with reversible shape memory effect and preparation method thereof |
| CN114990714B (en) * | 2022-06-07 | 2023-08-25 | 五邑大学 | Ultrahigh molecular weight polyethylene fiber with reversible shape memory effect and preparation method thereof |
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