CN101348944A - Novel preparation of high bonding ultra-high molecular weight polyethylene fiber - Google Patents
Novel preparation of high bonding ultra-high molecular weight polyethylene fiber Download PDFInfo
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Abstract
The invention discloses a novel method for manufacturing ultra-high molecular weight polyethylene fiber with high adhesive property. The method comprises the following step: (1) during moderately unwrapping the ultra-high molecular weight polyethylene through adopting high shear, an adequate amount of polar polymer containing polar groups such as carboxyl group, carbonyl group, ether group or ester group is added and evenly dispersed in a common solvent along with polyethylene powder, thereby forming a uniform mixed emulsion; (2) the mixed emulsion is fed into a screw extruder in fixed quantity so as to carry out quick swelling and dissolution, thereby forming a transparent and uniform spinning dope; (3) the spinning dope enters a spinning box body after filtration so as to prepare ultra-high molecular weight polyethylene gel fiber which has high evenness and contains the polar polymer; and (4) the gel fiber can be made into the ultra-high molecular weight polyethylene fiber with high adhesive property through the prior post-treatment processes such as extraction and super drawing. The novel method has the advantages that the polar polymer is evenly distributed in the ultra-high molecular weight polyethylene fiber, and does not influence the mechanical property of the fiber while substantially improving the adhesive property of the fiber; moreover, the method has simple process and convenient operation.
Description
Technical field
The present invention relates to a kind of high bonding ultra-high molecular weight polyethylene (hereinafter to be referred as, UHMWPE) the manufacturing new method of fiber belongs to high performance polymer material manufacturing technology field.
Background technology
The UHMWPE fiber is because of having excellent properties such as light weight softness, high-strength and high-modulus, uvioresistant, shock-resistant, seawater corrosion resistance, can be widely used in the multiple fields such as anti-cutting gloves, bulletproof jacket, bulletproof halmet, hawser, and under most situations, need carry out compound use with one or more matrixes such as acrylonitrile-butadiene rubber, polyurethane, epoxy resin.And the surface inertness of polyethylene fiber causes the bonding interface poor-performing between fiber and the matrix, has caused this field worker's great attention.In order to improve the interfacial adhesion strength that UHMWPE fiber and resin matrix are asked, people have proposed a series of surface treatment method, as by surface graft modification, chemical reagent erosion, Cement Composite Treated by Plasma modification, Corona discharge Treatment, photooxidation surface modification treatment etc., make the activation of fiber inactive surfaces layer.
USP4870136 provides a kind of heat of carrying out in spinning process to cause and to finish the surface silicon alkanisation graft reaction of UHMWPE fiber, and carries out crosslinking Treatment, and the adhesive property of fiber is increased, but the ultra-drawing of unfavorable postorder, the mechanical property of fiber is undesirable; In patents such as USP5039549 and USP5755913, CN 03115300.3, propose with under plasma, ozone, corona discharge or the ultraviolet irradiation, will
The monomer of some polar functionalities in the grafting of UHMWPE fiber surface as acrylic acid, propylene phthalein amine, acrylonitrile etc., can improve the surperficial adhesive property of fiber greatly.But this method operation is loaded down with trivial details, and equipment drops into high, and the very difficult grasp of the optimum process condition of handling, and is difficult for realizing industrialization.
(the research of superhigh molecular weight polyethylene fibers bond properties such as Jiang Sheng, fiberglass/composite, 2004 (3): 47) proposed the UHMWPE fiber to be carried out the liquid phase oxidation surface treatment with the chemical reagent of strong oxidizing properties such as chromic acid, potassium permanganate, because this method fiber soaks in the strong oxidizing property environment for a long time, the greater loss that when improving fiber wetness, causes fibrous mechanical property, simultaneously complex operation is strict to equipment, waste liquid seriously polluted.
CN1693544A proposes composite extractant that a kind of utilization contains polar polymer the UHMWPE gel spun fiber of spinning is extracted processing, when keeping the original intensity of fiber to greatest extent, can improve the surperficial adhesive property of fiber, simple to operate and do not need to add any equipment.But this technology is obvious processing effect under the gel spun fiber relaxed state, and in the tensioning extraction process of actual production, and polar polymer is to be difficult to infiltrate in the gel spun fiber and to make its surperficial adhesive property improve DeGrain.
Summary of the invention
Technical problem to be solved by this invention provides a kind of manufacture method of high adhesiveness superelevation average molecular weight polyethylene fiber, to remedy the deficiencies in the prior art, satisfies the quantity-produced needs.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of manufacture method of high adhesiveness superelevation average molecular weight polyethylene fiber, comprise the steps: that (1) adopt the high shear appropriateness to separate when twining ultra-high molecular weight polyethylene, add the polar polymer that contains carboxyl, carbonyl, ether or ester group isopolarity group in right amount, itself and polyethylene powders are dispersed in the conventional solvent simultaneously, form the mixed emulsion of homogeneous; (2) mixed emulsion feeds quantitatively that screw extruder carries out quick swelling, dissolving forms spinning solution transparent, homogeneous; (3) spinning solution enters spinning manifold after filtering, makes bar and does the super high molecular weight polyethylene gel fiber that contains polar polymer uniformly; (4) gel spun fiber can make the superhigh molecular weight polyethylene fibers of high adhesiveness through postprocessing working procedures such as the extraction of routine and ultra-drawings.
As optimized technical scheme:
Described poly relative molecular mass is preferably in 200～5,000,000 100～6,000,000;
The described polar polymer that contains ester group, carbonyl, carboxyl, ether, cyano group isopolarity group comprises one or more of polymer such as the polyvinylpyrrolidone of ethylene/vinyl acetate copolymer, polyacrylate, different K values, polyvinylpyrrolidone/vinyl acetate copolymer, polyoxyethylene;
The weight fraction of described polar polymer is preferably 2～8% with respect to 1～10% of the ultra-high molecular weight polyethylene powder;
Described ultra-high molecular weight polyethylene powder separate twine in, can also add function additives such as antioxidant, stabilizing agent, fire retardant as required;
Described ultra-high molecular weight polyethylene is separated and is twined shear rate at 1000～5000s
-1, be preferably in 2000～4000s
-1
The described equipment that twines high-rate of shear of separating can be that one or more combinations such as high speed dispersor, homogenizer, colloid mill are used;
Mixed emulsions such as described ultra-high molecular weight polyethylene, polar polymer realize that quick swelling, dissolving, deaeration can be in the same way or antidromous with double screw extruder, and draw ratio is 1: 30～65;
The time of staying of described mixed emulsion in double screw extruder is 10～60 minutes, is preferably in 20～40 minutes, and temperature of charge is 50～280 ℃, forms spinning solution transparent, homogeneous;
Described blend spinning stoste spinning temperature is 140～280 ℃, is preferably in 200～260 ℃.
The invention has the beneficial effects as follows:
1. adopt the high shear appropriateness to separate when twining ultra-high molecular weight polyethylene, add polar polymer, can make it be scattered in ultra-high molecular weight polyethylene very equably, realize the manufacturing of high adhesiveness UHMWPE fiber, need not add any equipment, technology is simple.
2. ultra-high molecular weight polyethylene and an amount of polar polymer mixed emulsion carry out the quick swelling of high shear, dissolving in double screw extruder, dissolving fully and help reducing the degraded of polymer, when improving the adhesive property of fiber, do not influence the mechanical performance of fiber;
The specific embodiment:
Below in conjunction with the specific embodiment the present invention is done further to elaborate, but the invention is not restricted to this.
Embodiment 0
Ultra-high molecular weight polyethylene (average molecular mass 4,500,000) powder, with the 90# dissolvant white oil be respectively to deliver into separate at 1: 8 to twine in the still at room temperature with weight ratio, under the nitrogen protection, be 2000s in shear rate
-1Effect down cut 10 minutes, obtain homogenous emulsion shape mixed liquor, feeding Φ 25, draw ratio is 36 parallel dual-screw extruding machine, temperature is controlled at 250 ℃, the adjusting screw(rod) rotating speed is 35 rev/mins.Extrudate after filtration, behind the filament spinning component ejection gel fiber, through 35 times of extraction and ultra-drawings, obtain superhigh molecular weight polyethylene fibers.
Embodiment 1
Ultra-high molecular weight polyethylene (average molecular mass 4,500,000) powder; with the 90# dissolvant white oil be respectively to deliver into separate at 1: 8 to twine in the still at room temperature with weight ratio; add EVA28190 (ethylene-vinyl acetate copolymer simultaneously; vinyl acetate content is 28%; melt index is 190); addition is the 4wt% of polyethylene powders, under the nitrogen protection, is 2000s in shear rate
-1Effect down cut 10 minutes, obtain homogenous emulsion shape mixed liquor, feeding Φ 25, draw ratio is 36 parallel dual-screw extruding machine, temperature is controlled at 250 ℃, the adjusting screw(rod) rotating speed is 35 rev/mins.Extrudate after filtration, behind the filament spinning component ejection gel fiber, through 35 times of extraction and ultra-drawings, obtain high bonding ultra-high molecular weight polyethylene fiber.
Embodiment 2
Ultra-high molecular weight polyethylene (average molecular mass 4,500,000) powder; with the 90# dissolvant white oil be respectively to deliver into separate at 1: 8 to twine in the still at room temperature with weight ratio; add EVA28190 (ethylene-vinyl acetate copolymer simultaneously; vinyl acetate content is 28%; melt index is 190); addition is the 2wt% of polyethylene powders, under the nitrogen protection, is 2000s in shear rate
-1Effect down cut 10 minutes, obtain homogenous emulsion shape mixed liquor, feeding Φ 25, draw ratio is 36 parallel dual-screw extruding machine, temperature is controlled at 250 ℃, the adjusting screw(rod) rotating speed is 35 rev/mins.Extrudate after filtration, behind the filament spinning component ejection gel fiber, through 35 times of extraction and ultra-drawings, obtain high bonding ultra-high molecular weight polyethylene fiber.
Embodiment 3
Ultra-high molecular weight polyethylene (average molecular mass 4,500,000) powder; with the 90# dissolvant white oil be respectively to deliver into separate at 1: 8 to twine in the still at room temperature with weight ratio; add EVA1030 (ethylene-vinyl acetate copolymer simultaneously; vinyl acetate content is 10%; melt index is 30); addition is the 4wt% of polyethylene powders, under the nitrogen protection, is 2000s in shear rate
-1Effect down cut 10 minutes, obtain homogenous emulsion shape mixed liquor, feeding Φ 25, draw ratio is 36 parallel dual-screw extruding machine, temperature is controlled at 250 ℃, the adjusting screw(rod) rotating speed is 35 rev/mins.Extrudate after filtration, behind the filament spinning component ejection gel fiber, through 35 times of extraction and ultra-drawings, obtain high bonding ultra-high molecular weight polyethylene fiber.
Embodiment 4
Ultra-high molecular weight polyethylene (average molecular mass 4,500,000) powder; with the 90# dissolvant white oil be respectively to deliver into separate at 1: 8 to twine in the still at room temperature with weight ratio, add polyacrylate simultaneously, addition is the 4wt% of polyethylene powders; under the nitrogen protection, be 2000s in shear rate
-1Effect down cut 10 minutes, obtain homogenous emulsion shape mixed liquor, feeding Φ 25, draw ratio is 36 parallel dual-screw extruding machine, temperature is controlled at 250 ℃, the adjusting screw(rod) rotating speed is 35 rev/mins.Extrudate after filtration, behind the filament spinning component ejection gel fiber, through 35 times of extraction and ultra-drawings, obtain high bonding ultra-high molecular weight polyethylene fiber.
Embodiment 5
Ultra-high molecular weight polyethylene (average molecular mass 4,500,000) powder; with the 90# dissolvant white oil be respectively to deliver into separate at 1: 8 to twine in the still at room temperature with weight ratio, add polyoxyethylene simultaneously, addition is the 4wt% of polyethylene powders; under the nitrogen protection, be 2000s in shear rate
-1Effect down cut 10 minutes, obtain homogenous emulsion shape mixed liquor, feeding Φ 25, draw ratio is 36 parallel dual-screw extruding machine, temperature is controlled at 250 ℃, the adjusting screw(rod) rotating speed is 35 rev/mins.Extrudate after filtration, behind the filament spinning component ejection gel fiber, through 35 times of extraction and ultra-drawings, obtain high bonding ultra-high molecular weight polyethylene fiber.
Embodiment 1 to 5 is more as shown in table 1 with the mechanical property and the adhesive property of the embodiment 0 prepared superhigh molecular weight polyethylene fibers that does not add polar polymer.
Table 1 the present invention makes the mechanical property and the adhesive strength of superhigh molecular weight polyethylene fibers
| The embodiment numbering | Fracture strength CN/dtex | Young's modulus CN/dtex | Breaking elongation CN/dtex | Pull-out strength CN/dtex |
| 0 | 35.25 | 972 | 4.07 | 10.23 |
| 1 | 31.31 | 939 | 4.42 | 26.73 |
| 2 | 33.63 | 953 | 4.26 | 20.54 |
| 3 | 31.09 | 926 | 4.19 | 21.59 |
| 4 | 30.95 | 896 | 4.91 | 29.06 |
| 5 | 33.73 | 977 | 4.15 | 18.77 |
Wherein, the assay method of UHMWPE fiber adhesion strength is as follows: the UHMWPE fiber is passed the capsule that has aperture, about the about 7mm of capsule height, with epoxy resin and curing agent with 4: 1 mixed evenly after, inject capsule.After solidifying 48h, accurately measure the embedding degree of depth L (mm) of fiber in capsule, adopt the method for extracting experiment to measure the adhesive property of fiber and epoxy resin with DXLL-20000 type tensometer.Folder is apart from being 200mm, and decrease speed is 50mm/min, is calculated as follows the pull-out strength of fiber: pull-out strength=test intensity * 7/L.
Claims (10)
1. a high bonding ultra-high molecular weight polyethylene fiber is made new method, it is characterized in that: adopt the high shear appropriateness to separate when twining ultra-high molecular weight polyethylene, add the polar polymer that contains carboxyl, carbonyl, ether or ester group isopolarity group in right amount, itself and polyethylene powders are dispersed in the conventional solvent simultaneously, form the mixed emulsion of homogeneous; Mixed emulsion quantitatively feeds screw extruder to carry out quick swelling, dissolving, deaeration and forms spinning solution transparent, homogeneous; Spinning solution enters spinning manifold after filtering, makes bar and does the super high molecular weight polyethylene gel fiber that contains polar polymer uniformly; Gel spun fiber can make the superhigh molecular weight polyethylene fibers of high adhesiveness through postprocessing working procedures such as the extraction of routine and ultra-drawings.
2. a kind of high bonding ultra-high molecular weight polyethylene fiber manufacture method according to claim 1 is characterized in that: described poly relative molecular mass is preferably in 200-500 ten thousand at 100-600 ten thousand.
3. a kind of high bonding ultra-high molecular weight polyethylene fiber manufacture method according to claim 1 is characterized in that: the described polar polymer that contains ester group, carbonyl, carboxyl, ether, cyano group isopolarity group comprises one or more of polymer such as the polyvinylpyrrolidone of ethylene/vinyl acetate copolymer, polyacrylate, different K values, polyvinylpyrrolidone/vinyl acetate copolymer, polyoxyethylene.
4. according to claim 1,3 described a kind of high bonding ultra-high molecular weight polyethylene fiber manufacture methods, it is characterized in that: the weight fraction of described polar polymer is preferably 2-8%. with respect to the 1-10% of ultra-high molecular weight polyethylene powder
5. according to the described a kind of high bonding ultra-high molecular weight polyethylene fiber manufacture method of claim 1 to 4, it is characterized in that: described ultra-high molecular weight polyethylene powder separate twine in, can also add function additives such as antioxidant, stabilizing agent, fire retardant as required.
6. a kind of high bonding ultra-high molecular weight polyethylene fiber manufacture method according to claim 1 is characterized in that: described ultra-high molecular weight polyethylene is separated and is twined shear rate at 1000-5000s
-1, be preferably in 2000-4000s
-1.
7. according to claim 1,4 described a kind of high bonding ultra-high molecular weight polyethylene fiber manufacture methods, it is characterized in that: the described equipment that twines high-rate of shear of separating can be that one or more combinations such as high speed dispersor, homogenizer, colloid mill are used.
8. a kind of high bonding ultra-high molecular weight polyethylene fiber manufacture method according to claim 1, it is characterized in that: mixed emulsions such as described ultra-high molecular weight polyethylene, polar polymer realize that quick swelling, dissolving, deaeration can be in the same way or antidromous with double screw extruder, and draw ratio is 1: 30-65.
9. according to the superhigh molecular weight polyethylene fibers manufacture method of claim 1,8 described a kind of high adhesiveness, it is characterized in that: the time of staying of described mixed emulsion in double screw extruder is 10-60 minute, be preferably in 20-40 minute, temperature of charge is 50-280 ℃, forms spinning solution transparent, homogeneous;
10. a kind of high bonding ultra-high molecular weight polyethylene fiber manufacture method according to claim 1 is characterized in that: described blend spinning stoste spinning temperature is 140-280 ℃, is preferably in 200-260 ℃.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100438317A CN101348944A (en) | 2007-07-16 | 2007-07-16 | Novel preparation of high bonding ultra-high molecular weight polyethylene fiber |
| DE602007008600T DE602007008600D1 (en) | 2006-11-08 | 2007-10-09 | METHOD FOR PRODUCING FIBERS FROM POLYETHYLENE WITH ULTRA-HIGH MOLECULAR WEIGHT |
| EP07816520A EP2080824B1 (en) | 2006-11-08 | 2007-10-09 | A process for producing fiber of ultra high molecular weight polyethylene |
| AT07816520T ATE478178T1 (en) | 2006-11-08 | 2007-10-09 | METHOD FOR PRODUCING ULTRA HIGH MOLECULAR WEIGHT POLYETHYLENE FIBERS |
| PCT/CN2007/002906 WO2008055405A1 (en) | 2006-11-08 | 2007-10-09 | A process for producing fiber of ultra high molecular weight polyethylene |
| US12/299,205 US20100233480A1 (en) | 2006-11-08 | 2007-10-09 | Process for producing fiber of ultra high molecular weight polyethylene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100438317A CN101348944A (en) | 2007-07-16 | 2007-07-16 | Novel preparation of high bonding ultra-high molecular weight polyethylene fiber |
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| CN101348944A true CN101348944A (en) | 2009-01-21 |
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| CNA2007100438317A Pending CN101348944A (en) | 2006-11-08 | 2007-07-16 | Novel preparation of high bonding ultra-high molecular weight polyethylene fiber |
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| CN103215681A (en) * | 2013-03-27 | 2013-07-24 | 金云良 | Method for using mobility and bipolarity functional group additive in preparation of modified ultra-high molecular weight polyethylene fibers |
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| CN109161978A (en) * | 2018-09-03 | 2019-01-08 | 中国科学院宁波材料技术与工程研究所 | A kind of high bonding, the preparation method of high-strength ultra high molecular weight polyethylene fiber and products thereof |
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- 2007-07-16 CN CNA2007100438317A patent/CN101348944A/en active Pending
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| CN104868188B (en) * | 2015-04-05 | 2017-08-25 | 铜仁学院 | A kind of useless film process reuse technology on lithium battery diaphragm production line |
| CN104868188A (en) * | 2015-04-05 | 2015-08-26 | 铜仁学院 | Technology for treating and recycling waste diaphragms in lithium battery diaphragm production line |
| CN104821382A (en) * | 2015-04-13 | 2015-08-05 | 铜仁学院 | Method for improving surface activity of polyethylene lithium battery diaphragm |
| CN106149068A (en) * | 2016-08-31 | 2016-11-23 | 华南理工大学 | A kind of superhigh molecular weight polyethylene fibers flat filament and preparation method thereof |
| CN106835321A (en) * | 2016-12-26 | 2017-06-13 | 山东非金属材料研究所 | Polar polymer modified ultra-high molecular weight polyethylene fiber and preparation method thereof |
| CN109161978A (en) * | 2018-09-03 | 2019-01-08 | 中国科学院宁波材料技术与工程研究所 | A kind of high bonding, the preparation method of high-strength ultra high molecular weight polyethylene fiber and products thereof |
| CN109161978B (en) * | 2018-09-03 | 2021-06-11 | 中国科学院宁波材料技术与工程研究所 | Preparation method of high-bonding, high-strength and ultrahigh molecular weight polyethylene fiber and product thereof |
| CN110541207A (en) * | 2019-09-06 | 2019-12-06 | 南京工业大学 | Method for modifying surface of ultra-high molecular weight polyethylene fiber |
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