CN104746165A - Ultra-high molecular weight polyethylene porous fiber and preparation method thereof - Google Patents
Ultra-high molecular weight polyethylene porous fiber and preparation method thereof Download PDFInfo
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- CN104746165A CN104746165A CN201510160662.XA CN201510160662A CN104746165A CN 104746165 A CN104746165 A CN 104746165A CN 201510160662 A CN201510160662 A CN 201510160662A CN 104746165 A CN104746165 A CN 104746165A
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Abstract
The invention provides an ultra-high molecular weight polyethylene porous fiber and a preparation method thereof. The porosity of the ultra-high molecular weight polyethylene porous fiber is 23.60%-58.99%. Compared with the prior art, the ultra-high molecular weight polyethylene porous fiber provided by the invention has a porous structure with super-high specific surface area, and excellent adsorptive property. An experiment result shows that the specific surface area of the ultra-high molecular weight polyethylene porous fiber is 5m<2>/g to 45m<2>/g; and meanwhile, the ultra-high molecular weight polyethylene porous fiber provided by the invention has high-strength and high-modulus mechanical property. The experiment result shows that the tensile strength of the ultra-high molecular weight polyethylene porous fiber provided by the invention is 0.91GPa to 1.67GPa, and the modulus is 7.21-15.3GPa.
Description
Technical field
The present invention relates to polymer adsorbing material technical field, more particularly, relate to a kind of ultra-high molecular weight polyethylene porous fibre and preparation method thereof.
Background technology
Polymer adsorbing material is a kind of novel functional material, has the advantages such as larger aperture and specific area, abundant raw material source, non-oxidizability are strong, regenerating easily, be widely used in the fields such as chemical industry, medical treatment, agricultural, national defence at present because of it.
At field of environment protection, the pollution that the waste water containing a large amount of harmful chemical causes is one of the most serious environmental problem of facing mankind.But traditional sewage treatmentmethod is helpless to the waste water containing trace or traces of harmful compound, the sewage treatmentmethod seeking economical and efficient removes the target that these chemical substances become people's pursuit.Wherein, active carbon has made significant contribution in disposing of sewage, but its lower mechanical strength and higher regeneration expense limit its use.And polymer adsorbing material has the features such as the adjustable of larger specific area, regenerating easily, resin and pore structure, active carbon is substituted gradually in wastewater treatment, and according to the difference of composition in handled waste water, can adsorption selection resin targetedly, acrylonitrile, acrylic acid etc. are grafted on high polymer main chain, generate amidoxim class, acrylamido copolymer, thus effective suction-operated is played to the heavy metal in waste water.
Along with the development of chemical industry; harmful influence kind and quantity also significantly increase; the inflammable and explosive property of a lot of harmful influence, corrosivity and toxic determine the multiple of accident and seriousness, and some can cause, and personnel are acute or slow poisoning is even dead, and very serious to the pollution of ecological environment.Because liquid chemicals leakage accident harmfulness is large, sudden by force, it is high to dispose difficulty, be difficult to take scientific and rational emergency disposal measure immediately according to the character of harmful influence after accident occurs.At present, absorption method is still treat liquid harmful influence leakage accident a kind of method the most conventional, especially more quick effectively for water insoluble harmful influence leakage accident.Therefore, polymer adsorbing material has important development prospect in process harmful influence.
The more important thing is, polymer adsorbing material has huge application prospect in extraction URANIUM IN SEAWATER element.Energy crisis is the huge challenge that the current whole world faces, and along with unprecedented soaring to energy demand of the mankind, carbon based energy source is about to exhaust in foreseeable future.Greatly developing nuclear energy is the key point solving mankind's energy crisis, and uranium is most important nuclear fuel.At present, limited land uranium ore also will be petered out in following a century, but in ocean, uranium element total amount but extremely abundant (4,500,000,000 tons); It is the important channel solving uranium ore crisis that URANIUM IN SEAWATER element is extracted in enrichment, therefore holds out broad prospects to its research.But the concentration of URANIUM IN SEAWATER only has 30 to ten/1000000000ths 4/100000000ths, therefore studying one, to have cost-benefit extraction of uranium from seawater method be a huge challenge.At present, absorption method is one of most effective method, and traditional adsorbent is inorganic, metal oxide, because the proportion of inorganic adsorbent is than seawater conference rapid subsidence, therefore need to adopt thermopnore system, adsorbent is placed in thermopnore upper strata, with pump by seawater high input voltage thermopnore lower floor, translate into upper strata again, thus stir the adsorbent of deposition, adsorbent is fully contacted with seawater.But this mode cost is too high, and adsorbent intensity is not high, repeat usage is very low.And utilize radiation induced graft polymer, obtain a kind of polymer adsorbing material, almost, intensity significantly improves for its density and seawater, and the ingenious disturbance by tide or wave does not need extraneous stirring, and material repeat usage is very high.
In addition, high hydroscopic resin in polymer adsorbing material has peculiar water suction, water holding capacity, can the aqueous water of absorptance self heavy hundred times and even thousand times rapidly, the water absorbed under high pressure also not easily overflows, in view of these advantages, hydroscopic high-molecular resin has become a kind of important functional material in recent years, is widely used in the aspects such as medical and health, building, agricultural gardening, fresh-keeping transport, arid area soil solid water.
At present, ultra-high molecular weight polyethylene because of its backbone structure be-(-CH
2-CH
2-)
n-flexible macromolecule polymer, molecule microstructure is extremely regular, gives material high strength, high-modulus and chemically inert excellent properties, with it for superhigh molecular weight polyethylene fibers prepared by raw material is suitable as the host material of polymer adsorbing material very much.But traditional superhigh molecular weight polyethylene fibers specific area is not high, limited sorption capacity.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of ultra-high molecular weight polyethylene porous fibre and preparation method thereof, ultra-high molecular weight polyethylene porous fibre provided by the invention, has the loose structure of superhigh specific surface area, has the mechanical property of high-strength and high-modulus amount simultaneously.
The invention provides a kind of ultra-high molecular weight polyethylene porous fibre, the porosity of described ultra-high molecular weight polyethylene porous fibre is 23.60% ~ 58.99%.
Present invention also offers a kind of preparation method of ultra-high molecular weight polyethylene porous fibre, comprise the following steps:
A) by ultra-high molecular weight polyethylene powder, solvent, antioxidant and mix lubricant, heat, obtain flocculence spinning solution;
B) described flocculence spinning solution is spinned, obtain gel fiber;
C) described gel fiber is carried out successively one-level stretching, fixed length extraction and dry, secondary drawing, obtain ultra-high molecular weight polyethylene porous fibre;
The temperature that described one-level stretches is 20 DEG C ~ 30 DEG C, and strain rate is 0.1s
-1~ 1.2s
-1, draw ratio is 3 ~ 12;
The temperature of described secondary drawing is 100 DEG C ~ 130 DEG C, and strain rate is 0.1s
-1~ 1.5s
-1, draw ratio is 1.5 ~ 6.0.
Preferably, step a) described in the weight average molecular weight of ultra-high molecular weight polyethylene powder be 2.0 × 10
6~ 5.5 × 10
6, molecular weight distribution < 3.0, granularity is 100 order ~ 130 orders.
Preferably, step a) described in solvent comprise in white oil, decahydronaphthalene and kerosene one or more.
Preferably, step a) described in the mass ratio of ultra-high molecular weight polyethylene powder and solvent be (3 ~ 15): (85 ~ 97).
Preferably, step a) described in antioxidant comprise in BHT type antioxidant, Irgafos-168 type antioxidant and composite antioxidant one or more.
Preferably, step a) described in lubricant be aluminum stearate.
Preferably, step a) described in heating temperature be 100 DEG C ~ 125 DEG C, the time is 1h ~ 3h.
Preferably, described step b) be specially:
Described flocculence spinning solution is carried out successively extrude, spinning, spray silk and cooling, obtain gel fiber.
Preferably, step c) described in extraction process extractant used comprise in 103 white oil extractants, n-hexane, gasoline and tetrahydro carbon one or more.
The invention provides a kind of ultra-high molecular weight polyethylene porous fibre, the porosity of described ultra-high molecular weight polyethylene porous fibre is 23.60% ~ 58.99%.Present invention also offers a kind of preparation method of ultra-high molecular weight polyethylene porous fibre, comprise the following steps: a) by ultra-high molecular weight polyethylene powder, solvent, antioxidant and mix lubricant, heat, obtain flocculence spinning solution; B) described flocculence spinning solution is spinned, obtain gel fiber; C) described gel fiber is carried out successively one-level stretching, fixed length extraction and dry, secondary drawing, obtain ultra-high molecular weight polyethylene porous fibre; The temperature that described one-level stretches is 20 DEG C ~ 30 DEG C, and strain rate is 0.1s
-1~ 1.2s
-1, draw ratio is 3 ~ 12; The temperature of described secondary drawing is 100 DEG C ~ 130 DEG C, and strain rate is 0.1s
-1~ 1.5s
-1, draw ratio is 1.5 ~ 6.0.Compared with prior art, ultra-high molecular weight polyethylene porous fibre provided by the invention has the loose structure of superhigh specific surface area, and absorption property is excellent, and experimental result shows, the specific area of ultra-high molecular weight polyethylene porous fibre provided by the invention is 5m
2/ g ~ 45m
2/ g; Simultaneously, ultra-high molecular weight polyethylene porous fibre provided by the invention has the mechanical property of high-strength and high-modulus amount, experimental result shows, the TENSILE STRENGTH of ultra-high molecular weight polyethylene porous fibre provided by the invention is 0.91GPa ~ 1.67GPa, and modulus is 7.21GPa ~ 15.3GPa.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only embodiments of the invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to the accompanying drawing provided.
Fig. 1 is the schematic diagram of gel fiber prepared by the embodiment of the present invention 1;
Fig. 2 is the schematic diagram after the gel fiber winding of the embodiment of the present invention 1 preparation;
The scanning electron microscope (SEM) photograph of the gel fiber cross-section morphology that Fig. 3 provides for the embodiment of the present invention 1;
The scanning electron microscope (SEM) photograph of the ultra-high molecular weight polyethylene porous fibre cross-section morphology that Fig. 4 provides for the embodiment of the present invention 1;
The scanning electron microscope (SEM) photograph of the ultra-high molecular weight polyethylene porous fibre surface topography that Fig. 5 provides for the embodiment of the present invention 1;
Fig. 6 is the product TENSILE STRENGTH variation with temperature curve of the different draw ratio that embodiment 1 and embodiment 6 ~ 16 prepare;
Fig. 7 is the product modulus variation with temperature curve of the different draw ratio that embodiment 1 and embodiment 6 ~ 16 prepare.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, be clearly and completely described technical scheme of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of ultra-high molecular weight polyethylene porous fibre, the porosity of described ultra-high molecular weight polyethylene porous fibre is 23.60% ~ 58.99%.
In the present invention, described ultra-high molecular weight polyethylene porous fibre section has loose structure and applicable specific area, thus while making material have excellent absorption property, maintain structural regularity and the density of ultra-high molecular weight polyethylene, its weight average molecular weight is not less than 2.0 × 10
6and molecular weight distribution is within 3.0, thus material is made to have the mechanical property of high-strength and high-modulus amount.In the present invention, the porosity of described ultra-high molecular weight polyethylene porous fibre is 23.60% ~ 58.99%, is preferably 35% ~ 50%.
Ultra-high molecular weight polyethylene porous fibre provided by the invention adopts the preparation technology be applicable to, remain the loose structure of intermediate product gel fiber, product is made to have the loose structure of superhigh specific surface area, absorption property is excellent, meanwhile, ultra-high molecular weight polyethylene porous fibre provided by the invention adopts weight average molecular weight to be not less than 2.0 × 10
6, molecular weight distribution is within 3.0 and the ultra-high molecular weight polyethylene powder of even particle size distribution is raw material is prepared from, there is the mechanical property of high-strength and high-modulus amount, therefore, be applicable to very much the host material being applied in polymer adsorbing material, pass through functional graft again, on main chain, grafting has the functional group of selective absorption, gives the selective absorption performance of material on high absorption property basis.
Present invention also offers a kind of preparation method of ultra-high molecular weight polyethylene porous fibre, comprise the following steps:
A) by ultra-high molecular weight polyethylene powder, solvent, antioxidant and mix lubricant, heat, obtain flocculence spinning solution;
B) described flocculence spinning solution is spinned, obtain gel fiber;
C) described gel fiber is carried out successively one-level stretching, fixed length extraction and dry, secondary drawing, obtain ultra-high molecular weight polyethylene porous fibre;
The temperature that described one-level stretches is 20 DEG C ~ 30 DEG C, and strain rate is 0.1s
-1~ 1.2s
-1, draw ratio is 3 ~ 12;
The temperature of described secondary drawing is 100 DEG C ~ 130 DEG C, and strain rate is 0.1s
-1~ 1.5s
-1, draw ratio is 1.5 ~ 6.0.
In the present invention, by ultra-high molecular weight polyethylene powder, solvent, antioxidant and mix lubricant, heat, obtain flocculence spinning solution.In the present invention, the weight average molecular weight of described ultra-high molecular weight polyethylene powder is preferably 2.0 × 10
6~ 5.5 × 10
6, be more preferably 4.5 × 10
6; The molecular weight distribution of described ultra-high molecular weight polyethylene powder is narrow as far as possible, is preferably less than 3.0; The granularity of described ultra-high molecular weight polyethylene powder is preferably 100 order ~ 130 orders, is more preferably 120 orders.The source of the present invention to described ultra-high molecular weight polyethylene powder is not particularly limited, and adopts commercial goods well known to those skilled in the art.
In the present invention, described solvent preferably include in white oil, decahydronaphthalene and kerosene one or more, be more preferably white oil.The source of the present invention to described solvent is not particularly limited, and adopts the commercial goods of above-mentioned white oil well known to those skilled in the art, decahydronaphthalene and kerosene.In the present invention, the effect of described solvent is mixed to form weak solution with ultra-high molecular weight polyethylene powder; The mass ratio of described ultra-high molecular weight polyethylene powder and solvent is preferably (3 ~ 15): (85 ~ 97), are more preferably 5:95.
In the present invention, described antioxidant preferably include in BHT type antioxidant, Irgafos-168 type antioxidant and composite antioxidant one or more, be more preferably BHT type antioxidant.The source of the present invention to described antioxidant is not particularly limited, and adopts the commercial goods of above-mentioned BHT type antioxidant well known to those skilled in the art, Irgafos-168 type antioxidant and composite antioxidant.In the present invention, the effect of described antioxidant is the high-temperature oxydation preventing flocculence spinning solution; The mass ratio of described antioxidant and ultra-high molecular weight polyethylene powder is preferably (0.1 ~ 0.8): 100, is more preferably 0.5:100.
In the present invention, described lubricant is preferably aluminum stearate.The source of the present invention to described aluminum stearate is not particularly limited, and object reduces flocculence spinning solution to produce viscous in preparation process.In the present invention, the mass ratio of described lubricant and ultra-high molecular weight polyethylene powder is preferably (0.1 ~ 0.8): 100, is more preferably 0.5:100.
In the present invention, by ultra-high molecular weight polyethylene powder, solvent, antioxidant and mix lubricant, heat.The equipment of the present invention to described heating is not particularly limited, and is preferably swelling still; In the present invention, described heating process is preferably carried out under the condition stirred, and object makes ultra-high molecular weight polyethylene powder, solvent, antioxidant and mix lubricant even.In the present invention, the temperature of described heating is preferably 100 DEG C ~ 125 DEG C, is more preferably 120 DEG C; The time of described heating is preferably 1h ~ 3h, is more preferably 2h.In the present invention, the process of described heating is specially:
Ultra-high molecular weight polyethylene powder, solvent, antioxidant and lubricant are mixed under the condition stirred, carry out heating swelling, when solvent swelling state is flocculence, control heating-up temperature, after leaving standstill, removing upper strata excess of solvent, obtains flocculence spinning solution.
After obtaining flocculence spinning solution, described flocculence spinning solution spins by the present invention, obtains gel fiber.Refer to Fig. 1 ~ 3, wherein, Fig. 1 is the schematic diagram of gel fiber prepared by the embodiment of the present invention 1, Fig. 2 is the schematic diagram after the gel fiber winding of the embodiment of the present invention 1 preparation, from Fig. 1 and Fig. 2, intermediate product gel fiber axial length prepared by the embodiment of the present invention 1 is large, makes final products also have the large feature of axial length; The scanning electron microscope (SEM) photograph of the gel fiber cross-section morphology that Fig. 3 provides for the embodiment of the present invention 1, as shown in Figure 3, intermediate product gel fiber section prepared by the embodiment of the present invention 1 has loose structure, and the loose structure for final products with superhigh specific surface area provides basis.
In the present invention, described spinning process is preferably specially:
Described flocculence spinning solution is carried out successively extrude, spinning, spray silk and cooling, obtain gel fiber.
In the present invention, described flocculence spinning solution is extruded.The present invention is not particularly limited the described equipment extruded, and preferably adopts Twin screw extruder; The temperature that described Twin screw extruder carries out extrusion is preferably 190 DEG C ~ 230 DEG C, and screw speed is preferably 200rpm ~ 300rpm.
After completing described extrusion, the polymer after extruding is carried out spinning by the present invention.The equipment of the present invention to described spinning is not particularly limited, and preferably adopts manifold; The process that described manifold carries out spinning is extruded to stretch and extrude by the measuring pump rotating speed and carry-over pinch rolls velocity interpolation controlling manifold and is not stretched.
After completing described spinning process, the polymer after spinning is carried out spray silk and cooling by the present invention.The present invention preferably adopts spinnerets, and the multistrand polymer extruded is entered coolant regions by draw-gear, completes spray silk and cooling, obtains gel fiber.In the present invention, the distance of described spinnerets and cooling-liquid level is preferably 2cm ~ 5cm; The polymer fluid that the process of described spray silk and cooling preferably also comprises spray silk is extruded sprays surfactant, and object is that the multistrand polymer fluid preventing from extruding is again bonding.In the present invention, described surfactant is preferably one or both in lauryl sodium sulfate and neopelex.
After obtaining gel fiber, described gel fiber is carried out one-level stretching, fixed length extraction and dry, secondary drawing by the present invention successively, obtains ultra-high molecular weight polyethylene porous fibre.In the present invention, the temperature that described one-level stretches is 20 DEG C ~ 30 DEG C, is preferably 25 DEG C; The strain rate that described one-level stretches is 0.1s
-1~ 1.2s
-1, be preferably 1.0s
-1; The draw ratio that described one-level stretches is 3 ~ 12, is preferably 10.
After completing the stretching of described one-level, the gel fiber after stretching is carried out fixed length extraction and drying by the present invention.In the present invention, described fixed length extraction process preferably carries out under ultrasound condition, and object is solvent a large amount of in removing gel fiber; Described ultrasonic time is preferably 2min ~ 5min.In the present invention, described fixed length extraction process extractant used preferably include in 103 white oil extractants, n-hexane, gasoline and tetrahydro carbon one or more, be more preferably 103 white oil extractants.In the present invention, the fiber after fixed length being extracted carries out drying.The method of the present invention to described drying is not particularly limited, and object to make extractant volatilize.
After completing the extraction of described fixed length and dry run, the porous fibre obtained is carried out secondary drawing by the present invention.In the present invention, the temperature of described secondary drawing is 100 DEG C ~ 130 DEG C, is preferably 110 DEG C ~ 120 DEG C; The strain rate of described secondary drawing is 0.1s
-1~ 1.5s
-1, be preferably 1.0s
-1; The draw ratio of described secondary drawing is 1.5 ~ 6.0, is preferably 3 ~ 5.The present invention, by restrained stretching condition, selects the draft temperature, strain rate and the draw ratio that are applicable to, achieves while controlling product reservation gel fiber loose structure, ensures that product has higher TENSILE STRENGTH and modulus.
The invention provides a kind of ultra-high molecular weight polyethylene porous fibre, the porosity of described ultra-high molecular weight polyethylene porous fibre is 23.60% ~ 58.99%.Present invention also offers a kind of preparation method of ultra-high molecular weight polyethylene porous fibre, comprise the following steps: a) by ultra-high molecular weight polyethylene powder, solvent, antioxidant and mix lubricant, heat, obtain flocculence spinning solution; B) described flocculence spinning solution is spinned, obtain gel fiber; C) described gel fiber is carried out successively one-level stretching, fixed length extraction and dry, secondary drawing, obtain ultra-high molecular weight polyethylene porous fibre; The temperature that described one-level stretches is 20 DEG C ~ 30 DEG C, and strain rate is 0.1s
-1~ 1.2s
-1, draw ratio is 3 ~ 12; The temperature of described secondary drawing is 100 DEG C ~ 130 DEG C, and strain rate is 0.1s
-1~ 1.5s
-1, draw ratio is 1.5 ~ 6.0.Compared with prior art, ultra-high molecular weight polyethylene porous fibre provided by the invention has the loose structure of superhigh specific surface area, and absorption property is excellent, and experimental result shows, the specific area of ultra-high molecular weight polyethylene porous fibre provided by the invention is 5m
2/ g ~ 45m
2/ g; Simultaneously, ultra-high molecular weight polyethylene porous fibre provided by the invention has the mechanical property of high-strength and high-modulus amount, experimental result shows, the TENSILE STRENGTH of ultra-high molecular weight polyethylene porous fibre provided by the invention is 0.91GPa ~ 1.67GPa, and modulus is 7.21GPa ~ 15.3GPa.
In order to further illustrate the present invention, be described in detail below by following examples.Following examples of the present invention ultra-high molecular weight polyethylene powder used is provided by Tecona; White oil used is provided by Shangyu city Zheng Yuan oil product Chemical Co., Ltd.; BHT type antioxidant used is provided by Aladdin reagent Co., Ltd; Stearic acid aluminium used is provided by Aladdin reagent Co., Ltd; Lauryl sodium sulfate used is provided by Aladdin reagent Co., Ltd; 103 white oil extractants used are provided by Shanghai Xi Le Chemical Co., Ltd..
Embodiment 1
(1) be 4.5 × 10 by 0.395kg weight average molecular weight
6molecular weight distribution is within 3.0, granularity is that 120 object ultra-high molecular weight polyethylene powder, 7.5kg white oil, 1.97gBHT type antioxidant and 1.97g aluminum stearate mix, thermal agitation 2h is added under 120 DEG C of conditions in swelling still, heating solvent swelling state to polymer composition is flocculence, controls heating-up temperature, after leaving standstill, the unnecessary white oil in removing upper strata, obtains flocculence spinning solution;
(2) by flocculence spinning solution through double screw extruder 200 DEG C, screw speed extrudes under being 250rpm condition, again through manifold spinning, extruded by spinnerets, obtain multistrand polymer and pass through draw-gear, coolant regions is entered after sprinkling lauryl sodium sulfate, cool, obtain gel fiber.
(3) by gel fiber 25 DEG C, draw ratio is 10, strain rate is 1.0s
-1condition under carry out one-level stretching, then adopt 103 white oil extractants to extract 4min under ultrasound condition, dry, finally 120 DEG C, draw ratio is 3, strain rate is 1.0s
-1condition under carry out secondary drawing, obtain ultra-high molecular weight polyethylene porous fibre.
ESEM sign is carried out to the ultra-high molecular weight polyethylene porous fibre that embodiment 1 provides.Refer to Fig. 4 and Fig. 5, wherein, the scanning electron microscope (SEM) photograph of the ultra-high molecular weight polyethylene porous fibre cross-section morphology that Fig. 4 provides for the embodiment of the present invention 1, as shown in Figure 4, the ultra-high molecular weight polyethylene porous fibre section that the embodiment of the present invention 1 provides has loose structure, substantially increase the specific area of fiber, thus make material have excellent absorption property.The scanning electron microscope (SEM) photograph of the ultra-high molecular weight polyethylene porous fibre surface topography that Fig. 5 provides for the embodiment of the present invention 1, as shown in Figure 5, the ultra-high molecular weight polyethylene porous fibrous structure that the embodiment of the present invention 1 provides is regular, and density is high, thus makes material have the mechanical property of high-strength and high-modulus amount.
Carry out porosity test to the ultra-high molecular weight polyethylene porous fibre that the embodiment of the present invention 1 prepares, porosity measurement experimental technique is: first weigh fiber dry weight m
1appropriate xylene solvent is poured in conical flask, and fiber is immersed in xylene solvent, then vacuumize and make solvent fully enter fiber hole, now there is a large amount of bubble to overflow from solvent, to solvent, no longer include bubble spilling illustrate that intrastitial hole is filled by solvent completely, then take out fiber rapidly, with the residual solvent on the filter paper being moistened with xylene solvent adsorbing fiber surface gently, then weigh fibre weight m rapidly
2.Fiber porosity can be obtained according to formula (I).Wherein ρ
xand ρ
pbe respectively xylene solvent and poly density.
Experimental result shows, the porosity that the ultra-high molecular weight polyethylene porous fibre that the embodiment of the present invention 1 prepares breaks is 58.99%, and specific area is 45m
2/ g.
Embodiment 2
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment ultra-high molecular weight polyethylene powder weight average molecular weight used is 2.0 × 10
6.
The porosity of the ultra-high molecular weight polyethylene porous fibre that the embodiment of the present invention 2 prepares is 25%, and specific area is 5m
2/ g.
Embodiment 3
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment ultra-high molecular weight polyethylene powder weight average molecular weight used is 5.5 × 10
6.
The porosity of the ultra-high molecular weight polyethylene porous fibre that the embodiment of the present invention 3 prepares is 55%.
Embodiment 4
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the granularity of the ultra-high molecular weight polyethylene powder that the present embodiment is used is 100 orders.
The porosity of the ultra-high molecular weight polyethylene porous fibre that the embodiment of the present invention 4 prepares is 30%.
Embodiment 5
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the granularity of the ultra-high molecular weight polyethylene powder that the present embodiment is used is 130 orders.
The porosity of the ultra-high molecular weight polyethylene porous fibre that the embodiment of the present invention 5 prepares is 50%.
Embodiment 6
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 100 DEG C, draw ratio is 1.5, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 7
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 110 DEG C, draw ratio is 1.5, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 8
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 120 DEG C, draw ratio is 1.5, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 9
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 130 DEG C, draw ratio is 1.5, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 10
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 100 DEG C, draw ratio is 3.0, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 11
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 110 DEG C, draw ratio is 3.0, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 12
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 130 DEG C, draw ratio is 3.0, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 13
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 100 DEG C, draw ratio is 6.0, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 14
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 110 DEG C, draw ratio is 6.0, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 15
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 120 DEG C, draw ratio is 6.0, strain rate is 1.0s
-1condition under carry out secondary drawing.
Embodiment 16
The present invention prepares ultra-high molecular weight polyethylene porous fibre according to the technical scheme described in embodiment 1, and difference is, the present embodiment 130 DEG C, draw ratio is 6.0, strain rate is 1.0s
-1condition under carry out secondary drawing.
TENSILE STRENGTH and modulus test are carried out to the ultra-high molecular weight polyethylene porous fibre that above-described embodiment 1 and embodiment 6 ~ 16 prepare, method of testing is: be fixed on the fixture of tensile test device by mass of fibers two ends, tensile fiber initial length is 4mm, draw speed is 50 μm/min, and Uniform Tension fiber is until fibrous fracture.Experimental result as shown in figs. 6-7.Wherein, Fig. 6 is the product TENSILE STRENGTH variation with temperature curve of the different draw ratio that embodiment 1 and embodiment 6 ~ 16 prepare, wherein, A to be secondary drawing multiple be 1.5 product, B to be secondary drawing multiple be 3.0 product, C to be secondary drawing multiple be 6.0 product.Fig. 7 is the product modulus variation with temperature curve of the different draw ratio that embodiment 1 and embodiment 6 ~ 16 prepare, wherein, A to be secondary drawing multiple be 1.5 product, B to be secondary drawing multiple be 3.0 product, C to be secondary drawing multiple be 6.0 product.From Fig. 6 ~ 7, the invention provides the mechanical property that ultra-high molecular weight polyethylene porous fibre has high-strength and high-modulus amount.
The above-mentioned explanation of the disclosed embodiments, enables professional and technical personnel in the field realize or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a ultra-high molecular weight polyethylene porous fibre, is characterized in that, the porosity of described ultra-high molecular weight polyethylene porous fibre is 23.60% ~ 58.99%.
2. a preparation method for ultra-high molecular weight polyethylene porous fibre, is characterized in that, comprises the following steps:
A) by ultra-high molecular weight polyethylene powder, solvent, antioxidant and mix lubricant, heat, obtain flocculence spinning solution;
B) described flocculence spinning solution is spinned, obtain gel fiber;
C) described gel fiber is carried out successively one-level stretching, fixed length extraction and dry, secondary drawing, obtain ultra-high molecular weight polyethylene porous fibre;
The temperature that described one-level stretches is 20 DEG C ~ 30 DEG C, and strain rate is 0.1s
-1~ 1.2s
-1, draw ratio is 3 ~ 12;
The temperature of described secondary drawing is 100 DEG C ~ 130 DEG C, and strain rate is 0.1s
-1~ 1.5s
-1, draw ratio is 1.5 ~ 6.0.
3. preparation method according to claim 2, is characterized in that, step a) described in the weight average molecular weight of ultra-high molecular weight polyethylene powder be 2.0 × 10
6~ 5.5 × 10
6, molecular weight distribution < 3.0, granularity is 100 order ~ 130 orders.
4. preparation method according to claim 2, is characterized in that, step a) described in solvent comprise in white oil, decahydronaphthalene and kerosene one or more.
5. preparation method according to claim 2, is characterized in that, step a) described in the mass ratio of ultra-high molecular weight polyethylene powder and solvent be (3 ~ 15): (85 ~ 97).
6. preparation method according to claim 2, is characterized in that, step a) described in antioxidant comprise in BHT type antioxidant, Irgafos-168 type antioxidant and composite antioxidant one or more.
7. preparation method according to claim 2, is characterized in that, step a) described in lubricant be aluminum stearate.
8. preparation method according to claim 2, is characterized in that, step a) described in heating temperature be 100 DEG C ~ 125 DEG C, the time is 1h ~ 3h.
9. preparation method according to claim 2, is characterized in that, described step b) be specially:
Described flocculence spinning solution is carried out successively extrude, spinning, spray silk and cooling, obtain gel fiber.
10. preparation method according to claim 2, is characterized in that, step c) described in extraction process extractant used comprise in 103 white oil extractants, n-hexane, gasoline and tetrahydro carbon one or more.
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| CN105413664A (en) * | 2016-01-15 | 2016-03-23 | 中国科学技术大学 | Modified UHMW (Ultra High Molecular Weight) polyethylene fiber, and preparation method and application thereof |
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