CN100529245C - Method for surface modification of super-high molecular-weight polyethylene fiber surface - Google Patents
Method for surface modification of super-high molecular-weight polyethylene fiber surface Download PDFInfo
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- CN100529245C CN100529245C CNB2007100566866A CN200710056686A CN100529245C CN 100529245 C CN100529245 C CN 100529245C CN B2007100566866 A CNB2007100566866 A CN B2007100566866A CN 200710056686 A CN200710056686 A CN 200710056686A CN 100529245 C CN100529245 C CN 100529245C
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Abstract
The invention relates to an ultrahigh molecular weight polythene fiber surface modifying method, comprising: 1. placing ultrahigh molecular weight polythene fiber in organic iron sulfonate solution to soak for 15-60 min, where the organic iron sulfonate solution is iron trichloride solution with mass concentration of 18-60%, or one of the iron toluenesulfonate solution, ferric tri(dodecanesulfonate), iron 2-acylamido-2-demthyl-1-propanesulfonate, or iron morphine propanesulfonate solution with mass concentration of 5-40%, and the organic iron sulfonate solvent is normal butyl alchohol or water; 2. placing the soaked polythene fiber in vacuum device with vacuum of 650-730mmHg in the proportion of 100-120 ml of intrinsic conducting polymer monomer per kg of fiber to process at 25-85deg.C for 0.5-8 h, and making it, where the intrinsic condcuting polymer monomer is pyrrole or thiophene with purity not lower than 99%. And the method can effectively surface adhesiveness of ultrahigh molecular weight polythene (UHMWPE) fiber and besides, keep the original strength of UHMWPE and the process is simple.
Description
Technical field
The present invention relates to a kind of fiber surface modification technology, be specially a kind of method that is intended to improve the surface modification of super-high molecular-weight polyethylene fiber surface of superhigh molecular weight polyethylene fibers surface adhesive property, international Patent classificating number intends being Int.Cl D01M 15/00 (2006.01).
Background technology
Ultra-high molecular weight polyethylene (UHMWPE) fiber, as novel high-performance fiber, have other high-performance fiber incomparable premium properties, for example, it has very high specific strength and specific modulus, have chemical resistance and weather resisteant, high-energy absorption, lower temperature resistance, electrical insulating property, can see through X-ray and certain water proofing property etc., therefore be widely used in military affairs, space flight navigation engineering, fields such as high-performance light composite and high-grade leisure sports goods (comprise armour plate as protective materials, the bulletproof jacket and the helmet etc.), high-strength rope (comprises hawser, the salvage rope, sailing boat rope and parachute rope etc.), composite (comprises sonar dome, radome, aircraft wing tip structure and large-scale storage tank etc.), sports apparatus (comprises skis, fishing rod and glide plate etc.).But, superhigh molecular weight polyethylene fibers also exists some to treat improved weakness, there is not a stronger interaction force (for example hydrogen bond) as intermolecular, creep properties is bigger than the aramid fiber with rigid molecule structure, strand is linear structure, does not have phenyl ring isopolarity functional group, causes its fusing point lower, processing temperature is less than 130 ℃, and the sensitiveness of serviceability temperature is bigger etc.; Particularly for the UHMWPE fibre reinforced composites, because its molecule does not have chemism, surface energy is lower, being difficult to produce chemical bond between fiber and the resin combines, be difficult for producing stronger interaction force between fiber molecule and molecular resin, cause the cementability of fiber and resin matrix relatively poor, thereby make phenomenons such as the UHMWPE fibre reinforced composites in use easily come unstuck, resin matrix cracking, limited the UHMWPE fiber greatly in the particularly application in lightweight structural material field of composite.Therefore, the UHMWPE fiber is carried out surface modification treatment, the adhesive property that improves itself and resin matrix is an important subject.
At present, improve the method for the interfacial adhesion strength between UHMWPE fiber and resin matrix, can carry out surface modification by methods such as chemical reagent oxidizes, Cement Composite Treated by Plasma, Corona discharge Treatment, photooxidation surface modification treatment or radiation grafting processing, make the activation of UHMWPE fiber inactive surfaces layer, introduce carboxyl, carbonyl or hydroxyl isopolarity group at nonpolar fiber surface and realize.For example:
Chinese patent literature CN1035308A discloses a kind of method of the UHMWPE of raising fiber surface cementability.It adopts the method for the UHMWPE fiber surface being carried out Cement Composite Treated by Plasma.The method can effectively improve wettability and the surperficial adhesive strength of fiber to resin matrix.But this method appointed condition requires high, and the industrialization difficulty is bigger, and deals with improperly fibrous mechanical property is significantly descended.
American documentation literature USP4870136 discloses a kind of method that improves the fiber surface adhesive property.The method is earlier with a certain proportion of UHMWPE powder, radical initiator, silane compound and diluent melting mixing in the screw rod machine, carry out the plasticising melt spinning, cause the silanization graft reaction of finishing UHMWPE by heat in the spinning stage, fiber with spinning carries out hot-stretch in the medium of extractant and crosslinking agent then, finishes cross-linking reaction again in boiling water.The adhesive property of this method gained fiber surface improves, but because it has added a large amount of initators and graft compound and has stretched after graft reaction is finished again in the UHMWPE fiber spinning dope, thereby cause the tensile fiber multiple lower, the mechanical property of gained UHMWPE fiber is also relatively poor.
Silverstein M.S. etc. are at " the superhigh molecular weight polyethylene fibers surface property of acid etch and the relation between the caking property " " Relationship between surface properties andadhesion for etched ultra high molecular weight polyethylenefibers " (Composites Science and Technology, 1993,48 (1-4), introduced surface modifying method in article 151-157) with chromic acid agent treated UHMWPE fiber, discovery is after chromic acid is handled, and the surperficial adhesive property of UHMWPE fiber has improved 6 times.But this method makes fiber surface be subjected to corrosion, and is bigger to the fibre strength influence.
American documentation literature USP5039549 and USP5755913 disclosed method are under plasma, ozone, corona discharge or ultraviolet irradiation, surface modifying method with some polar functionalities monomers (as acrylic acid, acrylamide, acrylonitrile etc.) in the grafting of UHMWPE fiber surface, can improve the surperficial adhesive property of UHMWPE fiber greatly, but this method operation is loaded down with trivial details, and the optimum process condition that grafting is handled is difficult to grasp, and industrial prospect is remote.
American documentation literature USP6172163 also discloses a kind of method that improves the fiber surface adhesive property.The method is to utilize poly high crystalline energy, adopts the method for pure physics, the unformed area of fiber surface is dissolved after crystallization and form one deck " molecular brush " again at fiber surface.After UHMWPE fiber of Chu Liing and the resin compounded, the fiber adhesive property is greatly improved in this way.But the same operation of this method is loaded down with trivial details, the process conditions harshness, and deal with the remarkable decline that also can cause the UHMWPE fibrous mechanical property improperly.
Chinese patent literature CN1693544A discloses a kind of method of the UHMWPE of raising fiber surface cementability.The method is that polar polymer is dissolved in the conventional extractant of UHMWPE gel spun fiber, make composite extractant, the UHMWPE gel spun fiber is extracted in composite extractant, back operation such as drawn is handled and is made the UHMWPE fiber that adhesive property improves a lot then again.Though this method can keep original intensity of UHMWPE fiber preferably, it is limited that the fiber adhesive strength improves degree, do not reach desirable and practical target.
Summary of the invention
At the deficiencies in the prior art, the technical problem to be solved in the present invention is the method for a kind of surface modification of super-high molecular-weight polyethylene fiber surface of design, it can improve the surperficial adhesive property of superhigh molecular weight polyethylene fibers effectively, keep the original intensity of UHMWPE fiber simultaneously, and it is simple to have technology, does not pollute, and appointed condition is not had specific (special) requirements, cost is lower, is convenient to the characteristics of industrial applications.
The technical scheme that the present invention solve the technical problem is: design a kind of method of surface modification of super-high molecular-weight polyethylene fiber surface, its technology is as follows:
1. superhigh molecular weight polyethylene fibers is placed the organic sulfonic acid iron salt solutions to soak 15-60 minute; Described organic sulfonic acid iron salt solutions is a kind of in toluenesulfonic acid iron, DBSA iron, 2-acrylamide-2-methyl isophthalic acid-propane sulfonic acid iron or the 4-morphine propane sulfonic acid ferrous solution, and mass concentration is 5-40%; The solvent of described organic sulfonic acid molysite is n-butanol or water;
2. the superhigh molecular weight polyethylene fibers that will soak is put into the vacuum plant that vacuum is 650-730mmHg according to the ratio of per kilogram fiber 100-120 milliliter intrinsic conducting polymer monomer, temperature is 25-85 ℃, handle after 0.5-8 hour, promptly make the bigger superhigh molecular weight polyethylene fibers of surperficial adhesive property; Described intrinsic conducting polymer monomer is a kind of in pyrroles or the thiophene, and the purity of pyrroles or thiophene liquid is not less than 99%.
Compared with prior art, advantage of the present invention is that superhigh molecular weight polyethylene fibers surface adhesive property improves significantly, whole surface modification treatment process can not damaged the mechanical property of fiber simultaneously, and technology is simple, do not have to pollute and (do not handle the etching technics of the required complexity of superhigh molecular weight polyethylene fibers method as there being the chromic acid liquid phase, do not produce the complex process technology of the back three wastes etc.) yet, be easy to control course of reaction (as the process conditions harshness of method of plasma processing to the generation plasma, be difficult for controlling etc.), production equipment less demanding (as not needing the necessary anti-strong acid corrosive nature of chromic acid liquid phase processing method production equipment etc.), intrinsic conducting polymer monomer consumption particularly of the present invention is few, and (liquid phase method is handled monomer consumption 1kg fiber and is needed the 2000ml intrinsic conducting polymer approximately, be about 20 times of the present invention), with low cost, be easy to industrialization promotion and use.
The specific embodiment
The present invention is further elaborated below in conjunction with specific embodiment.
The technical scheme that the present invention solve the technical problem is: design a kind of method of surface modification of super-high molecular-weight polyethylene fiber surface, its technology is as follows:
1. superhigh molecular weight polyethylene fibers is placed liquor ferri trichloridi or organic sulfonic acid molysite (Fe (III)) solution to soak 15-60 minute; Described liquor ferri trichloridi mass concentration is 18-60%; The organic sulfonic acid iron salt solutions is a kind of in p-methyl benzenesulfonic acid iron, DBSA iron, 2-acrylamide-2-methyl isophthalic acid-propane sulfonic acid iron or the 4-morphine propane sulfonic acid ferrous solution, and mass concentration is 5-40%; The solvent of described organic sulfonic acid molysite is n-butanol or water;
2. the superhigh molecular weight polyethylene fibers that will soak is put into the vacuum plant that vacuum is 650-730mmHg according to the ratio of per kilogram fiber 100-120 milliliter intrinsic conducting polymer monomer, temperature is 25-85 ℃, handle after 0.5-8 hour, promptly can be made into the superhigh molecular weight polyethylene fibers that surperficial adhesive property improves or improves; Described intrinsic conducting polymer monomer is a kind of in pyrroles or the thiophene, and the purity of pyrroles or thiophene liquid is not less than 99%.
The further feature of the inventive method is that the liquor ferri trichloridi mass concentration is 30-50%.
The intrinsic conduction material surface of prior art applies can adopt electrochemical method and vapour deposition simultaneous oxidation and polymerization.Though electrochemical method is widely used and need not oxidant, but also there is fatal weakness, be that its electrode must be a conductor, and polyethylene is not a conductor, can't adopt electrochemical method, therefore the present invention has selected CVD method for use, but has designed unique technological process, can realize preferably that the top layer of polyethylene insulation body applies.The oxidant organic sulfonic acid iron salt solutions that the inventive method adopts is with low cost, and oxidisability is strong, is swift in response the production efficiency height with the intrinsic conduction material.In addition, the Fe of embodiment (III) sulfonate can be avoided causing the not thorough problem of reaction because of the molysite crystallization.The inventive method is compared with chemical liquid phase oxidation and plasma method, and production process is simple, and is less demanding to equipment, can not cause damage to fiber itself, and its surperficial adhesion strength is improved a lot.
The present invention does not address part and is applicable to prior art.
Provide specific embodiments of the invention below, but embodiment does not limit the present invention.
Embodiment 1
It is that 20% liquor ferri trichloridi soaked 60 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% pyrroles's liquid, under 25 ℃ of temperature, vacuum 730mmHg, handled 0.5 hour, and can make the superhigh molecular weight polyethylene fibers that surperficial adhesive property improves or improves.
Embodiment 2
It is that 30% liquor ferri trichloridi soaked 30 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% pyrroles's liquid, under 55 ℃ of temperature, vacuum 730mmHg, handled 0.5 hour, and can make the superhigh molecular weight polyethylene fibers that surperficial adhesive property improves or improves.
Embodiment 3
It is that 30% liquor ferri trichloridi soaked 30 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% pyrroles's liquid, under 55 ℃ of temperature, vacuum 700mmHg, handled 0.5 hour, and can make the superhigh molecular weight polyethylene fibers that surperficial adhesive property improves or improves.
Embodiment 4
It is that 60% liquor ferri trichloridi soaked 15 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% pyrroles's liquid, under 85 ℃ of temperature, vacuum 730mmHg, handled 1 hour, can make described superhigh molecular weight polyethylene fibers.
Embodiment 5
It is that 60% liquor ferri trichloridi soaked 15 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% pyrroles's liquid, under 85 ℃ of temperature, vacuum 650mmHg, handled 2 hours, can make described superhigh molecular weight polyethylene fibers.
Embodiment 6
It is that 50% liquor ferri trichloridi soaked 40 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% pyrroles's liquid, under 55 ℃ of temperature, vacuum 730mmHg, handled 1 hour, can make described superhigh molecular weight polyethylene fibers.
Embodiment 7
It is that 18% liquor ferri trichloridi soaked 60 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% pyrroles's liquid, under 85 ℃ of temperature, vacuum 730mmHg, handled 1 hour, can make described superhigh molecular weight polyethylene fibers.
Embodiment 8
It is that 60% liquor ferri trichloridi soaked 30 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% thiophene liquid, under 85 ℃ of temperature, vacuum 730mmHg, handled 4 hours, can make described superhigh molecular weight polyethylene fibers.
Embodiment 9
It is that 60% liquor ferri trichloridi soaked 30 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% thiophene liquid, under 25 ℃ of temperature, vacuum 650mmHg, handled 8 hours, can make described superhigh molecular weight polyethylene fibers.
Embodiment 10
It is that 5% p-methyl benzenesulfonic acid molten iron solution soaked 60 minutes that the UHMWPE fiber is placed mass concentration, take out to dry or directly place then and fill the vacuum plant that purity is 99% thiophene liquid, under 85 ℃ of temperature, vacuum 730mmHg, handled 1 hour, and can make described superhigh molecular weight polyethylene fibers.
Embodiment 11
It is that 5% p-methyl benzenesulfonic acid molten iron solution soaked 60 minutes that the UHMWPE fiber is placed mass concentration, take out to dry or directly place then and fill the vacuum plant that purity is 99% thiophene liquid, under 45 ℃ of temperature, vacuum 650mmHg, handled 2 hours, and can make described superhigh molecular weight polyethylene fibers.
Embodiment 12
It is that 20% p-methyl benzenesulfonic acid molten iron solution soaked 30 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% thiophene liquid, under 55 ℃ of temperature, vacuum 730mmHg, handled 2 hours, and can make described superhigh molecular weight polyethylene fibers.
Embodiment 13
It is that 20% p-methyl benzenesulfonic acid molten iron solution soaked 30 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% thiophene liquid, under 35 ℃ of temperature, vacuum 700mmHg, handled 6 hours, and can make described superhigh molecular weight polyethylene fibers.
Embodiment 14
It is that 40% p-methyl benzenesulfonic acid ferrous solution soaked 15 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% thiophene liquid, under 25 ℃ of temperature, vacuum 730mmHg, handled 2 hours, and can make described superhigh molecular weight polyethylene fibers.
Embodiment 15
It is that 40% DBSA ferrous solution soaked 60 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% pyrroles's liquid, under 85 ℃ of temperature, vacuum 650mmHg, handled 1 hour, and can make described superhigh molecular weight polyethylene fibers.
Embodiment 16
It is that 10% DBSA ferrous solution soaked 30 minutes that the UHMWPE fiber is placed mass concentration, take out then and place and fill the vacuum plant that purity is 99% pyrroles's liquid, under 85 ℃, vacuum 730mmHg, handled 2 hours, and can make described superhigh molecular weight polyethylene fibers.
The UHMWPE fiber of the present invention after to embodiment gained surface modification carried out the adhesive strength performance test.Experimental technique is as follows:
UHMWPE fiber with gained is fixed on the square frame earlier, after epoxy resin (trade mark is 618), diluent (trade mark is 711) and curing agent (trade mark is the amine 105 that contracts) mixed by 2: 2: 1, get resin beads and carefully drip on described UHMWPE fiber, require resin beads diameter on the UHMWPE fiber between 100-600um; Solidify after 48 hours, accurately measure the embedding degree of depth L (mm) of resin beads, method with the droplet experiment, adopt LLY-6 type tensometer to measure the adhesive property of UHMWPE fiber and resin, anchor clamps 10mm, decrease speed is 10mm/min, calculates the peak shear strength (MPa) of UHMWPE fiber by (1) formula:
τ
max＝F
max/πdL (1)
In the formula, F
MaxFor the fiber maximum is extracted brute force (N); D is fibre diameter (mm); L is the embedding degree of depth (mm) of resin beads.
UHMWPE fiber experimental result after the described surface modification of embodiment is listed in table 1.Wherein, embodiment is numbered 0 the comparative example that is, does not promptly have the UHMWPE fiber of modification.By table 1 measured data as can be seen, through the UHMWPE of the inventive method modification fiber, average shear intensity is up to 10.89 (MPa), and with conventional or do not have the UHMWPE fiber of modification to compare, its shear strength has improved 1.18-2.21 doubly, and effect is fairly obvious.
The surperficial adhesive strength list position (MPa) of table 1 UHMWPE fiber
| The embodiment numbering | 0 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
| Shear strength | 3.67 | 10.69 | 11.79 | 11.03 | 10.28 | 9.56 | 11.23 | 10.51 | 8.00 |
| The embodiment numbering | 9 | 10 | 11 | 12 | 13 | 14 | 15 | 16 | |
| Shear strength | 7.89 | 10.73 | 10.81 | 10.27 | 10.31 | 10.01 | 10.93 | 11.49 |
Claims (1)
1. the method for a surface modification of super-high molecular-weight polyethylene fiber surface, its technology is as follows:
(1). place the organic sulfonic acid iron salt solutions to soak 15-60 minute superhigh molecular weight polyethylene fibers; Described organic sulfonic acid iron salt solutions is a kind of in toluenesulfonic acid iron, DBSA iron, 2-acrylamide-2-methyl isophthalic acid-propane sulfonic acid iron or the 4-morphine propane sulfonic acid ferrous solution, and mass concentration is 5-40%; The solvent of described organic sulfonic acid molysite is n-butanol or water;
(2). the superhigh molecular weight polyethylene fibers that will soak is put into the vacuum plant that vacuum is 650-730mmHg according to the ratio of per kilogram fiber 100-120 milliliter intrinsic conducting polymer monomer, temperature is 25-85 ℃, handle after 0.5-8 hour, promptly make the bigger superhigh molecular weight polyethylene fibers of surperficial adhesive property; Described intrinsic conducting polymer monomer is a kind of in pyrroles or the thiophene, and the purity of pyrroles or thiophene liquid is not less than 99%.
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| CN102154832B (en) * | 2010-12-31 | 2013-08-07 | 泉州红瑞兴纺织有限公司 | Fabric coating finishing agent with electromagnetic shielding function and preparation method thereof |
| CN102250370B (en) * | 2011-06-14 | 2012-10-17 | 中国科学院宁波材料技术与工程研究所 | Method for modifying surface of high molecular weight polyethylene powder through interfacial polycondensation |
| CN102493168B (en) * | 2011-12-22 | 2014-07-30 | 北京服装学院 | Method for improving creep resistant performance of ultra-high molecular weight polyethylene fiber |
| US9181430B2 (en) * | 2013-02-28 | 2015-11-10 | Sabic Global Technologies B.V. | Wear and friction properties of engineering thermoplastics with ultra-high molecular weight polyethylene |
| CN104328652A (en) * | 2014-10-04 | 2015-02-04 | 上海工程技术大学 | Method for improving hydrophilicity of polyethylene non-woven fabric |
| CN105544180A (en) * | 2015-12-22 | 2016-05-04 | 中国航空工业集团公司济南特种结构研究所 | A coating-treatment surface modification method for ultrahigh molecular weight polyethylene fibers |
| CN106367967A (en) * | 2016-08-29 | 2017-02-01 | 北京普诺泰新材料科技有限公司 | Treating agent for improving interface bonding strength of UHMWPE and treating method of treating agent |
| CN113718527A (en) * | 2021-09-22 | 2021-11-30 | 湖南中泰特种装备有限责任公司 | High-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber and preparation method thereof |
| CN114164662A (en) * | 2022-01-07 | 2022-03-11 | 湖南中泰特种装备有限责任公司 | Method for manufacturing conductive ultrahigh molecular weight polyethylene fiber |
| CN115383849B (en) * | 2022-08-31 | 2023-03-28 | 福建省格绿木业有限公司 | Lateral light-transmitting wood decorative plate and preparation method thereof |
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