CN102528998A - Preparation method of ultra high molecular weight polyethylene bulletproof helmet - Google Patents
Preparation method of ultra high molecular weight polyethylene bulletproof helmet Download PDFInfo
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- CN102528998A CN102528998A CN2011104256348A CN201110425634A CN102528998A CN 102528998 A CN102528998 A CN 102528998A CN 2011104256348 A CN2011104256348 A CN 2011104256348A CN 201110425634 A CN201110425634 A CN 201110425634A CN 102528998 A CN102528998 A CN 102528998A
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Abstract
The invention provides a preparation method of an ultra high molecular weight polyethylene bulletproof helmet, which comprises a) providing ultra high molecular weight polyethylene weftless cloth with the areal density of more than 135g/cm2; b) enabling a plurality of layers of the ultra high molecular weight polyethylene weftless cloth to be gradually overlapped in a mould and conducting walkthrough to obtain a walkthrough piece; c) enabling the walkthrough piece to be pre-pressed to obtain a fabricated part; d) pressing the fabricated part for the third time to obtain a molding part; and e) enabling the molding part to be cooled to reach room temperature, and obtaining the ultra high molecular weight polyethylene bulletproof helmet. The bulletproof helmet prepared by the preparation method is light in weight, high in strength and high in modulus, and the preparation method overcomes local stress shortcomings and the like caused by hot pressing molding.
Description
Technical field
The present invention relates to the Antiballistic shaped part preparation field, relate in particular to a kind of preparation method of ultra-high molecular weight polyethylene bulletproof halmet.
Background technology
Superhigh molecular weight polyethylene fibers is also claimed high-strength high-modulus polyethylene (HSHMPE) fiber or elongation chain (ECPE) polyethylene fibre, is meant that relative molecular mass is in (1～7) * 10
6Polyethylene, the ultra high molecular weight polyethylene fiber of after spinning-super drawing, processing.It is the third generation high-performance fiber after carbon fiber, aramid fiber (Kevlar) fiber.
Is a kind of superhigh molecular weight polyethylene fibers composite with said superhigh molecular weight polyethylene fibers through the no latitude cloth that step such as compound obtains; Compare with other fibre reinforced composites; Have light weight, shock-resistant, dielectric properties advantages of higher, change fields such as war and Aero-Space, marine site defence, weaponry in modern times and bringing into play very important effect.Simultaneously, this fiber also has broad application prospects in fields such as automobile, boats and ships, medicine equipment, athletic sports appliances.Therefore, superhigh molecular weight polyethylene fibers is just extremely paid attention to from coming out, and develops very fast.
In order to satisfy the needs of modern medical service, rescue, weaving, national defence, ultra-high molecular weight polyethylene does not have latitude cloth suitability for industrialized production in a large number, multilayer is not had polyethylene board that latitude cloth is compounded to form have excellent properties such as light weight and high impact properties, high tenacity, high strength; Especially be applied to the national defence field; Along with the fast development of weapon science and technology, the power of hot weapons such as modern firearms is increasing, wants to resist the increasing weapon attacking of power; Must increase shellproof thickness; Also increased weight simultaneously, influenced the mobility of wearing shellproof personnel, influence is fought and defence speed.The preparation method of the bulletproof halmet that prior art provides generally is the hot pressing composite algorithm, is mostly a hot pressing.But a hot pressing meeting causes between the no latitude cloth and leaves air, and deaeration can cause fully has pore and bubble in the bulletproof halmet, causes the local stress defective of bulletproof halmet.The intensity and the modulus of bulletproof halmet are reduced.
Summary of the invention
The technical problem that the present invention will solve is to provide the preparation method of the ultra-high molecular weight polyethylene bulletproof halmet of a kind of light weight, high strength, high-modulus.
In order to solve above technical problem, the invention provides a kind of preparation method of ultra-high molecular weight polyethylene bulletproof halmet, it is characterized in that, comprising:
A) provide ultra-high molecular weight polyethylene not have latitude cloth; The surface density of said no latitude cloth is 135g/cm
2More than;
B) the said ultra-high molecular weight polyethylene of several layers is not had the latitude cloth walkthrough under the pressure that in mould, successively superposes again, obtain walkthrough spare;
C) said walkthrough spare is carried out the desire compacting, obtain prefabricated component;
D) said prefabricated component is suppressed for the third time, obtained profiled member;
E) said profiled member is cooled to room temperature, obtains the ultra-high molecular weight polyethylene bulletproof halmet.
Preferably, the ultra-high molecular weight polyethylene in the said step a) does not have latitude cloth and prepares through following method:
The superhigh molecular weight polyethylene fibers of 300～600D is arranged according to same direction, and with the thin polymer film bonding that contains binding agent;
2～4 said films that are bonded with fiber are stacked; Said two fibers that are bonded with in the film of fiber are vertical each other;
The said film that stacks is through compacting, and obtaining surface density is 135g/cm
2Above no latitude cloth.
Preferably, step b) is specially:
B1) said ultra-high molecular weight polyethylene not being had latitude cloth successively is laid in the mould;
B2) the no latitude cloth of said stack is applied the pressure of 5～8MPa, carry out walkthrough and obtain walkthrough spare.
Preferably, step c) is specially:
Under 80～100 ℃, said desire is arranged the pressure that part applies 10～15MPa, carried out pre-embossed 20～30 minutes, obtain prefabricated component.
Preferably, step d) is specially: said prefabricated component is suppressed under 100～120 ℃ for the third time, and the said pressure of compacting for the third time is 20～25MPa, obtains profiled member.
Preferably, comprise that also step e) dyes the said helmet outward.
Preferably, contain 30～200 layers of no latitude cloth in the said prefabricated component.
Preferably, contain 50～100 layers of no latitude cloth in the said prefabricated component.
Preferably, the said press time for the third time is 20～30 minutes.
Preferably, the time of said cooling is 10～20 minutes.
The preparation method of ultra-high molecular weight polyethylene bulletproof halmet provided by the invention provides ultra-high molecular weight polyethylene not have latitude cloth earlier; The surface density of said no latitude cloth requires at 135g/cm
2More than.Then said some said no latitude cloth are successively superposeed, the no latitude cloth after the stack is exerted pressure carry out pre-embossed then, obtain prefabricated component, said prefabricated component is suppressed for the third time, obtain profiled member,, obtain bulletproof halmet said profiled member cooling.Because no latitude cloth provided by the invention is to be 135g/cm with surface density
2More than, so, compare, having under the situation of identical performance with the bullet resistant material of prior art than great, the thickness that bulletproof halmet provided by the invention has gentlier, more approaches uses no latitude cloth still less.In addition, the present invention will not carry out pre-embossed after in the process of preparation bulletproof halmet, will having the stack of latitude cloth earlier, and polyethylene is a kind of thermoplastic polymer, if directly suppress, can deform at the too fast polyethylene fibre that heats up, and fiber and binding agent come off, distortion.And the purpose of carrying out walkthrough, pre-embossed earlier is for polyethylene fibre and the adhesion of binding agent in the no latitude cloth are weakened, but is unlikely to come off, and makes the no latitude cloth attitude that mediates, and eliminates the stress between the no latitude cloth and gets rid of the air between the no latitude cloth.Polyethylene fiber peacekeeping binding agent just can be inter-adhesive.Suppress for the third time after the pre-embossed, the probability that the distortion of polyethylene fibre and displacement take place can be very little again, under the effect of pressure and temperature, bonds each other between the no latitude cloth, finally obtains profiled member.So in the preparation process, adopt pre-embossed can reduce the inner bubble of bulletproof halmet.Pore has improved the intensity and the modulus of bulletproof halmet.
Description of drawings
Fig. 1 is that the present invention prepares the superhigh molecular weight polyethylene fibers schematic flow sheet;
Fig. 2 is an extraction process sketch map of the present invention;
Fig. 3 is a drawing process sketch map of the present invention;
Fig. 4 is that the present invention prepares the mould cross sectional representation that bulletproof halmet is used.
The specific embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiments of the invention are described, but should be appreciated that these just restriction for further specifying feature and advantage of the present invention rather than patent of the present invention being required is described.
The invention provides a kind of preparation method of ultra-high molecular weight polyethylene bulletproof halmet, comprising:
A) provide ultra-high molecular weight polyethylene not have latitude cloth; The surface density of said no latitude cloth is 135g/cm
2More than;
B) the said ultra-high molecular weight polyethylene of several layers is not had the latitude cloth walkthrough under the pressure that in mould, successively superposes again, obtain walkthrough spare;
C) said walkthrough spare is carried out the desire compacting, obtain prefabricated component;
D) said prefabricated component is suppressed for the third time, obtained profiled member;
E) said profiled member is cooled to room temperature, obtains the ultra-high molecular weight polyethylene bulletproof halmet.
In order to solve the technical problem that the present invention proposes, the inventor considers from the material choice to preparation method, need improve, the raw material that at first uses as surface density at 135g/cm
2Above no latitude cloth, and just the dawn number of the polyethylene fibre of needs use will be greatly to need high strength and high-modulus.According to the present invention, preferably use the superhigh molecular weight polyethylene fibers of 360D～600D.Fiber provided by the invention is preparation voluntarily preferably.
Said ultra-high molecular weight polyethylene powder is that weight average molecular weight (Mw) is the linear ultra-high molecular weight polyethylene of (1～7) * 106; Preferably; Said ultra-high molecular weight polyethylene is that weight average molecular weight is the linear ultra-high molecular weight polyethylene of (1.5～4.5) * 106; Preferred, the weight average molecular weight of said ultra-high molecular weight polyethylene is the linear ultra-high molecular weight polyethylenes in (1.8～4.0) * 106.The powder size of said ultra-high molecular weight polyethylene is 40 μ m～200 μ m, and preferred, said ultra-high molecular weight polyethylene powder size is 80 μ m～180 μ m.
Solvent as the ultra-high molecular weight polyethylene spinning solution is to be the hydrocarbon of liquid under the room temperature; Preferably; Can be hydrogenated naphthalene or alkane series; For example can be selected from one or more solvents as ultra-high molecular weight polyethylene in tetrahydronaphthalene, decahydronaphthalenes, kerosene, mineral oil or the paraffin, preferred, can select molecular weight for use is 40～1000 No. 7 white oils solvents as ultra-high molecular weight polyethylene.
According to the present invention; With said ultra-high molecular weight polyethylene and solvent swelling 20 minutes～60 minutes in temperature is 70 ℃～130 ℃ scope; Preferably, with said ultra-high molecular weight polyethylene and solvent swelling 25 minutes～55 minutes in temperature is 75 ℃～125 ℃ scope.In order to prepare the high super high molecular polyethylene solution of spinning property; The percentage by weight of ultra-high molecular weight polyethylene is 70wt%～97.6wt% in the spinning solution provided by the invention; Preferably; The percentage by weight of ultra-high molecular weight polyethylene is 70wt%～97.6wt% in the spinning solution, and is preferred, and the percentage by weight of ultra-high molecular weight polyethylene is 70wt%～97.6wt% in the spinning solution.
The ultra-high molecular weight polyethylene swelling is prepared after the spinning solution, need further to adopt double screw extruder push dissolving preparation spinning solution spinning solution.Wherein, the feeding mouth temperature of double screw extruder is 90 ℃～120 ℃, 160 ℃～200 ℃ of the temperature of middle extruding dissolving, and outlet temperature is 150 ℃～190 ℃; The time of staying of spinning solution in double screw extruder, preferred, the time of staying of spinning solution in double screw extruder is 3～8 minutes, and be preferred in order to be no more than 10 minutes, and the time of staying of spinning solution in double screw extruder is 4～6 minutes; The rotary speed of double screw extruder is 30～300r/min, and preferred, the rotary speed of double screw extruder is 70～270r/min, and is preferred, and the rotary speed of double screw extruder is 90～200r/min.
After the preparation spinning solution, adopt gel spinning technology to use superhigh molecular weight polyethylene fibers spinning solution provided by the invention to prepare superhigh molecular weight polyethylene fibers.The process conditions of gel spinning are: the aperture of spinneret orifice is 0.6mm～5mm, and preferred, the aperture of spinneret orifice is 0.7mm～2mm; Spinneret orifice draw ratio L/D is 6/1～30/1, and the spinning solution rate of extrusion is 0.5m/min～5m/min, and spinning solution is through 20 ℃～60 ℃ cooling and shaping, and the shower nozzle drafting multiple is no more than 2 times; Preferably, the shower nozzle drafting multiple is no more than 1.8 times.
After the gel fiber moulding, said gel fiber left standstill obtained as-spun fibre in 16 hours～26 hours.
Preparation need extract as-spun fibre behind the as-spun fibre, dry, ultra times hot-stretch.
When as-spun fibre was extracted, the extractant of selecting for use should have good mixing mutually or intermiscibility for solvent, and has low boiling point and high volatility.Used extractant can be volatile lower paraffin hydrocarbon and halogenated hydrocarbons.For example when using paraffin oil, can select for use hexane, heptane, toluene, chloromethanes, solvent wet goods as extractant as solvent, preferred, select for use industrial naptha as extractant, most preferably be solvent naphtha No. 120.As-spun fibre carries out drying to it and makes the extractant volatilization, and then surpass a times hot-stretch through after extracting in 40 ℃～80 ℃ temperature range.
With being dried the extractant of removing on the as-spun fibre after the as-spun fibre extraction, baking temperature can be 40 ℃～90 ℃, and preferred, baking temperature is 50 ℃～70 ℃.Drying is carried out through the mode of dry combustion method, does not have liquid substance in the dry combustion method case, and solvent directly is evaporated to gas.Said dry combustion method operation is preferably through 3 road dry combustion method casees.After the drying, the temperature of carrying out the ultra times hot-stretch in 5 roads is 70 ℃～130 ℃, and is preferred, in 85 ℃～135 ℃ temperature range, surpasses a times hot-stretch.For holding temperature, can preferably in said path, feed the identical saturated steam of temperature.During stretching, make as-spun fibre, in the path, feed protective gas then, can be inert gas or nitrogen through the path, preferred, select for use nitrogen after the heating as protective gas.Drafting machine can be selected hot-rolling drafting machine or cold roller drafting machine for use, and is preferred, selects the hot-rolling drafting machine for use, and the temperature of hot-rolling is preferably 70～90 ℃, can play the effect of preheating to fiber.Among this paper, when fiber being applied stretching, need carry out at a certain temperature; Therefore the pipe, casing, cylinder of both ends open etc. are arranged between drafting machine; Feeding therein needs the gas of temperature then, and the cylinder that fiber passes is promptly instigated in hot path, path among this paper, but is not limited thereto.
According to the present invention, total draw ratio of said stretching is 10～13 times, more preferably 11～12 times.Finally obtain the superhigh molecular weight polyethylene fibers that fiber number is 600D.Total draw ratio is that the addition again through the ratio of the speed of every adjacent twice drawing-off obtains.Draw ratio is big more, and fiber is thin more, and modulus and intensity are just low more.
Also comprise at last said fiber is wound into tubular through up-coiler, obtain the product of corresponding specification after the packing.
In order to prepare no latitude cloth, said superhigh molecular weight polyethylene fibers is spread on the thin polymer film that is coated with binding agent in advance with excellent properties.Because the effect of binding agent is that fiber is bonded together and can all or part of parcel fiber; And in bullet resistant material, work to absorb and transmit the bullet energy; Therefore should select to have material that excellent mechanical property and fiber have the good combination ability as adhesive; Can select for use polymer matrix material as adhesive; Preferably, select thermoplastic as adhesive, the thermoplastic that can select for use is polyurethane, polyvinyl polymer, polyacrylic, polyolefin or thermoplastic elastomeric block copolymers.Choosing is more arranged, and said binding agent is selected from polystyrene triblock copolymer (SIS, styrene-isoprene-phenylethene), or Tsing-Hua University's polystyrene triblock copolymer (SIBS, polystyrene-ethene-butylene-styrene).Said binding agent can be the solvent-borne type binding agent, and used solvent can be selected from benzene, toluene, chloroform, carbon tetrachloride, hexane, cyclohexane, chlorination cyclohexane, diethyl ether, methyl-isobutyl ether, ethyl acetate, amyl acetate etc.In binder solution, the weight ratio of binding agent and solvent is 10～40: 90～60, and preferred, the mass ratio of binding agent and solvent is 15～35: 85～65, and is preferred, and the mass ratio of binding agent and solvent is 20～30: 80～70.
Because its main shellproof effect is superhigh molecular weight polyethylene fibers in the no latitude cloth; Therefore suitable binding agent consumption in should unloaded no latitude cloth; In no latitude cloth, the content of binding agent can be 10～30wt%, and the content of preferred binding agent is 14～30wt%; Most preferred, the Han Lang of binding agent is 18～20wt%.
According to the present invention, said thin polymer film be preferably can be good with the binding agent adhesion polyolefin film or polyester film.More preferably polyethylene film, polypropylene film or haloflex film most preferably are polyethylene film.Said polyethylene film is that the number-average molecular weight of said low density polyethylene (LDPE) is preferably 8000～12000 by the low density polyethylene (LDPE) preparation.The mode of coated with adhesive is preferably spraying, manual application, the gluing of upper glue roller machinery.Be parallel to each other between the said superhigh molecular weight polyethylene fibers, spread apart in the same way, the carding operation that can assist through carding machine is more evenly distributed said superhigh molecular weight polyethylene fibers, and single degree of orientation is higher, and surface density is higher.
2～4 blocks of thin polymer films that are bonded with superhigh molecular weight polyethylene fibers are stacked; Filament on the said two adjacent polymeric thing films becomes 0 °/90 ° arrangements, and promptly the filament on two thin polymer films becomes vertical relation so just to make that no latitude cloth tool all can be stressed even at horizontal and vertical both direction mutually.
According to the present invention, can also superhigh molecular weight polyethylene fibers be bonded in the two sides of said thin polymer film according to 0 °/90 ° mode, practiced thrift material, reduced thickness.
At last the said thin polymer film that is bonded with superhigh molecular weight polyethylene fibers is applied the pressure of 5～10MPa under 50～70 ℃, the thin polymer film of long 100m need be suppressed 200～300 seconds, obtained not having latitude cloth.This process is in order to make firm being bonded on the said thin polymer film of said superhigh molecular weight polyethylene fibers, if the too high binding agent of temperature can be crossed the arrangement that influences fiber because of flowability, bubbling or pore phenomenon to occur.The compounding machine that said pressing operation can use those skilled in the art to know carries out; Said compounding machine comprises 2 pressure rollers at least; Filament is spread on the said thin polymer film, thin polymer film is guided in the middle of two pressure rollers through guide wheel, the distance of adjustment pressure roller is a pressure; Under the drive of pressure roller that fiber and thin polymer film is compound, a compression moulding.The temperature of said pressure roller remains between 50～70 ℃, to satisfy binding agent fiber is fixed on the thin polymer film.
After having prepared no latitude cloth, said no latitude cloth is successively overlayed in the mould as shown in Figure 4 of hydraulic press, said mould comprises top die 1 and dip mold 2.Said no latitude cloth is overlayed in the dip mold 2; Arrange, the walkthrough of colding pressing makes no latitude cloth be called preliminary helmet shape; The purpose in this step is in order to make no latitude cloth orientation and circular arc; The no latitude cloth of innermost layer and outermost no latitude cloth changed differing greatly, walkthrough can make the deformation of the no latitude cloth of each layer tentatively finalize the design, make its in precompressed and when suppressing for the third time deformation not too large.Then walkthrough spare is carried out pre-embossed.Polyethylene is a kind of thermoplastic polymer; If directly suppress, can deform at the too fast polyethylene fibre that heats up, fiber and binding agent come off; Distortion and the purpose of advanced pre-embossed is for polyethylene fibre and the adhesion of binding agent in the no latitude cloth are weakened; But be unlikely to come off, make the no latitude cloth attitude that mediates, eliminate the stress between the no latitude cloth and get rid of the air between the no latitude cloth.Polyethylene fiber peacekeeping binding agent just can be inter-adhesive.Suppress for the third time after the pre-embossed, the probability that the distortion of polyethylene fibre and displacement take place can be very little again, under the effect of pressure and temperature, bonds each other between the no latitude cloth, finally obtains profiled member.According to the present invention, the number of plies that the ultra-high molecular weight polyethylene that contains in the said profiled member does not have latitude cloth is 30～200 layers, and what are relevant with surface density and gross mass for the number of plies, and through formula: weight/surface density of every cubic centimetre=number of plies is calculated the needed number of plies.According to the present invention, the said number of plies is more elected 50～100 layers as.The number of plies is more just can defend power to follow strong weapon more.
According to the present invention, said walkthrough is specially: b1) said ultra-high molecular weight polyethylene is not had latitude cloth and successively be laid in the mould;
B2) the no latitude cloth of said stack is applied the pressure of 5～8MPa, carry out walkthrough and obtain walkthrough spare.
Pre-embossed is specially: under 80～100 ℃, said desire is arranged the pressure that part applies 10～15MPa, carried out pre-embossed 20～30 minutes, obtain prefabricated component.
More preferably 85～95 ℃ of the temperature of pre-embossed, pressure is 11～13MPa, squeeze time is preferably 23～27 minutes.In order to obtain the uniform bulletproof halmet of hardness, intensity and modulus, the mould of said pre-embossed is preheating in advance preferably, and the temperature of preheating is 60～70 ℃.Mould is exerted pressure the time, can be gradually pressure be raise, the speed that is preferably the 1MPa per minute is carried out; Until rising to 5～10MPa; After the precompressed, the prefabricated component that obtains has had the basic configuration of bulletproof halmet, but tight not enough; Need further compacting, so the present invention has also carried out compacting for the third time to said prefabricated component.
The process of compacting is specially for the third time: said pre-press is applied the pressure of 20～25MPa under 100～120 ℃, suppress for the third time, obtain profiled member.The purpose of compacting is for the prefabricated component compacting for the third time; Its density is increased; Owing to made polyethylene fibre that fixing orientation and form arranged during pre-embossed, so when suppressing for the third time, temperature is risen to 100～120 ℃; Pressure is risen to 25～30MPa by 5～10MPa rapidly, more preferably 27～28MPa.Kept pressure then 20～30 minutes, pressurize is after 3～5 minutes, and slowly release pressure obtains profiled member.Because the temperature of profiled member is higher; The pliability of polyethylene fibre is higher, all can make it have slight distortion to the touching of bulletproof halmet, so will make its cooling rapidly; The present invention preferably carries out water quench to said profiled member after obtaining profiled member, said profiled member is cooled to room temperature.The time of cooling is preferably 10～20 minutes.
Because cooling water can be reduced to room temperature with the polyethylene fibre under the high temperature upper state rapidly; Make the motion of strand slow down, slight crosslinking curing between the polyethylene molecule can keep the shape invariance of suppressing; Improve the hardness and the modulus of table napkin spare, this process can be referred to as " sulfuration ".
According to the present invention, preparation because what use is superhigh molecular weight polyethylene fibers, so the profiled member of preparation is a white, be commonly called as " openpore ", can be after the cooling with said openpore outer surface painting of coating.
The bulletproof halmet of preparation method's preparation provided by the invention is not superpose according to different machine directions through will there being latitude cloth, forms many structures through many latitudes, and the dimension direction of the no latitude cloth of every adjacent two layers is all inequality.The filament direction of preferred every adjacent two no latitude cloth becomes 0 °/90 ° arrangements.
Below be the embodiment of the invention, specifically set forth the present invention program:
The preparation superhigh molecular weight polyethylene fibers: after the 230kg7 solvent naphtha is preheating to 112 ℃, again the 40000kg ultra-high molecular weight polyethylene is placed on to stir in the swelling still 101 with No. 7 solvent naphthas and carries out preliminary swelling, tentatively swelling time is 20 minutes.After the preliminary swelling, be that second part of No. 7 solvent naphtha 690kg of 98 ℃ are added to and carry out swelling in the swelling still again and obtain spinning solution with temperature again, swelling time is 30 minutes again, and mixing speed is constant, the environment temperature of swelling still is dropped to 98 ℃ swelling the time again.
Obtain uniform spinning solution again after the swelling, spinning solution is sent into sent into double screw extruder 103 again after being cooled to 25 ℃ in the material storage kettle 102 and push dissolving.Wherein, mouthful temperature of sending into of double screw extruder is that 100 ℃, medium temperature are that 185 ℃, outlet temperature are 165 ℃, and the time that in double screw extruder, stops is 5 minutes, and the twin-screw rotary speed is 180rpm.Spinning solution twines, extrudes and process transparent frozen glue solution through separating of twin-screw.
With frozen glue solution through measuring pump 104, have spinneret 105 (the orifice diameter 0.8mm in 400 holes; Draw ratio L/D is 10/1) extrude with the spray silk speed of 1m/min that to get into temperature be that 25 ℃ the tank 106 that solidifies makes the strand typing, the jet stretch of adopting 107 pairs of gel fibers of jet stretch machine to apply 1.5 times then obtains gel fiber.Gel fiber is put into and is left standstill bucket and 110 left standstill 18 hours.
Referring to Fig. 2; Adopt No. 120 solvent naphthas to carry out five grades extraction the gel fiber after leaving standstill; So-called five grades extraction is to make fiber successively from low to high through first extraction box 201, second extraction box 202, the 3rd extraction box 203, the 4th extraction box 204, the 5th extraction box 205; Wherein the solvent naphtha in the 5th extraction box flows through the 4th extraction box, the 3rd extraction box, second extraction box, first extraction box from high to low successively, and giving of solvent naphtha and gel fiber is in the opposite direction.
Gel fiber is through dry through 55 ℃, 60 ℃, 65 ℃ two-stage successively again after extracting.
Referring to Fig. 3; Dried gel fiber is fed the hot path in the hot path in the hot path of first drafting machine 301, first 302, second drafting machine 303, second 304, the 3rd drafting machine the 305, the 3rd 306, the 4th drafting machine 307 successively, adopt then and receive silk device 308 and receive silk.Wherein, the temperature in the first hot path is that 90 ℃, the temperature in the second hot path are 110 ℃, and the temperature in the 3rd hot path is 125 ℃; First drafting machine, second drafting machine, the 3rd drafting machine, the 4th drafting machine all are five roller drafting machines, in order to reach the object of the invention, do not have concrete restriction for leading refreshing machine the present invention, as long as can satisfy drafting multiple; The roller temperature of first drafting machine is 90 ℃, and the roller temperature of second drafting machine is 110 ℃, and the roller temperature of the 3rd drafting machine is 125 ℃, and the roller temperature of the 4th drafting machine is 15 ℃.Second drafting machine doubly is 3.3 times to leading of applying of as-spun fibre, and the 3rd drafting machine doubly is 3.5 times, the 4th drafting machine to leading of applying of as-spun fibre to leading of applying of as-spun fibre doubly is 3.9 times.Total draw ratio is 10.7 times.
After gel fiber surpasses times hot-stretch through five roads, adopt and receive the superhigh molecular weight polyethylene fibers that silk device receipts silk obtains 360D.
After the 230kg7 solvent naphtha is preheating to 112 ℃, again 40000kg ultra-high molecular weight polyethylene and No. 7 solvent naphthas is placed on to stir in the swelling still 101 and carries out preliminary swelling, preliminary swelling time is 20 minutes.After the preliminary swelling, be that second part of No. 7 solvent naphtha 690kg of 98 ℃ are added to and carry out swelling in the swelling still again and obtain spinning solution with temperature again, swelling time is 30 minutes again, and mixing speed is constant, the environment temperature of swelling still is dropped to 98 ℃ swelling the time again.
Obtain uniform spinning solution again after the swelling, spinning solution is sent into sent into double screw extruder 103 again after being cooled to 25 ℃ in the material storage kettle 102 and push dissolving.Wherein, mouthful temperature of sending into of double screw extruder is that 100 ℃, medium temperature are that 185 ℃, outlet temperature are 165 ℃, and the time that in double screw extruder, stops is 5 minutes, and the twin-screw rotary speed is 180rpm.Spinning solution twines, extrudes and process transparent frozen glue solution through separating of twin-screw.
With frozen glue solution through measuring pump 104, have spinneret 105 (the orifice diameter 0.8mm in 400 holes; Draw ratio L/D is 10/1) extrude with the spray silk speed of 1m/min that to get into temperature be that 25 ℃ the tank 106 that solidifies makes the strand typing, the jet stretch of adopting 107 pairs of gel fibers of jet stretch machine to apply 1.5 times then obtains gel fiber.Gel fiber is put into and is left standstill bucket and 110 left standstill 18 hours.
Referring to Fig. 2; Adopt No. 120 solvent naphthas to carry out five grades extraction the gel fiber after leaving standstill; So-called five grades extraction is to make fiber successively from low to high through first extraction box 201, second extraction box 202, the 3rd extraction box 203, the 4th extraction box 204, the 5th extraction box 205; Wherein the solvent naphtha in the 5th extraction box flows through the 4th extraction box, the 3rd extraction box, second extraction box, first extraction box from high to low successively, and giving of solvent naphtha and gel fiber is in the opposite direction.
Gel fiber is through dry through 55 ℃, 60 ℃, 65 ℃ two-stage successively again after extracting.
Referring to Fig. 3; Dried gel fiber is fed the hot path in the hot path in the hot path of first drafting machine 301, first 302, second drafting machine 303, second 304, the 3rd drafting machine the 305, the 3rd 306, the 4th drafting machine 307 successively, adopt then and receive silk device 308 and receive silk.Wherein, the temperature in the first hot path is that 90 ℃, the temperature in the second hot path are 110 ℃, and the temperature in the 3rd hot path is 125 ℃; First drafting machine, second drafting machine, the 3rd drafting machine, the 4th drafting machine all are five roller drafting machines, in order to reach the object of the invention, do not have concrete restriction for leading refreshing machine the present invention, as long as can satisfy drafting multiple; The roller temperature of first drafting machine is 90 ℃, and the roller temperature of second drafting machine is 110 ℃, and the roller temperature of the 3rd drafting machine is 125 ℃, and the roller temperature of the 4th drafting machine is 15 ℃.Second drafting machine doubly is 1.3 times to leading of applying of as-spun fibre, and the 3rd drafting machine doubly is 2.5 times, the 4th drafting machine to leading of applying of as-spun fibre to leading of applying of as-spun fibre doubly is 3.9 times.Total draw ratio is 8.7 times.
Embodiment 3
Use the superhigh molecular weight polyethylene fibers of embodiment 1 preparation, said fiber is sprawled being coated with on the low-density polyethylene film of polystyrene triblock copolymer.With 2 blocks of said thin polymer films that are bonded with fiber under the effect of guide wheel through two pressure rollers that rotate, the temperature of pressure roller is 60 ℃, the 8MPa that exerts pressure, obtaining fabric width is the no latitude cloth of 1.6m.Because what use is the filament of 600D, so the surface density of said no latitude cloth is 160g/cm
2
Getting 30 layers of above-mentioned bilayer does not have latitude cloth mutual superposition in mould, and walkthrough under 5MPa overflows the air between the lamination, obtains walkthrough spare.The pressure that said walkthrough spare is applied 12MPa under 85 ℃ carries out pre-embossed, after keep-uping pressure 25 minutes temperature is risen to 120 ℃, and pressure rises to 30MPa; Constant temperature pressurize 25 minutes; Obtain profiled member, with cooling water said profiled member is cooled to room temperature at last, cut into 0.3m
2Specification obtain bulletproof halmet, said bulletproof halmet weight is 1.35kg.Adopt America NI J0101.04 side monomer testing standard that this bulletproof halmet is carried out the ballistic performance test, the result shows it can resist 9.6g, and speed is 847m/ 7.62 millimeters bore all-metals coating bullets of second.
Embodiment 4
Use the superhigh molecular weight polyethylene fibers of embodiment 1 preparation, said fiber is sprawled being coated with on the low-density polyethylene film of binding agent.With 2 blocks of said thin polymer films that are bonded with fiber under the effect of guide wheel through two pressure rollers that rotate, the 9.2MPa that exerts pressure obtains fabric width and is the no latitude cloth of 1.2m because what use is the filament of 600D, so the surface density of said no latitude cloth is 160g/cm
2
Getting 100 layers of above-mentioned bilayer does not have latitude cloth mutual superposition in mould, and walkthrough under 8MPa overflows the air between the lamination, obtains walkthrough spare.The pressure that under 80 ℃, applies 11MPa carries out pre-embossed, and the air between the lamination is overflowed, and after keep-uping pressure 25 minutes temperature is risen to 125 ℃; Pressure rises to 25MPa, and constant temperature pressurize 25 minutes obtains profiled member; With cooling water said profiled member is cooled to room temperature at last, cuts into 0.5m
2Specification obtain bulletproof halmet, said bulletproof halmet weight is 1.30kg.Adopt America NI J0101.04 side monomer testing standard that this bulletproof halmet is carried out the ballistic performance test, the result shows it can resist 10.8g, and speed is that 7.62 millimeters bore all-metals of 869 meter per seconds coat bullet.
Embodiment 5
Use the superhigh molecular weight polyethylene fibers of embodiment 1 preparation, said fiber is sprawled being coated with on the low-density polyethylene film of binding agent.With 2 blocks of said thin polymer films that are bonded with fiber under the effect of guide wheel through two pressure rollers that rotate, the 9.2MPa that exerts pressure obtains fabric width and is the no latitude cloth of 1.2m because what use is the filament of 600D, so the surface density of said no latitude cloth is 160g/cm
2
Getting 200 layers of above-mentioned bilayer does not have latitude cloth mutual superposition in mould, and walkthrough under 5MPa overflows the air between the lamination, obtains walkthrough spare.The pressure that under 80 ℃, applies 10MPa carries out pre-embossed, and the air between the lamination is overflowed, and after keep-uping pressure 25 minutes temperature is risen to 140 ℃; Pressure rises to 30MPa, and constant temperature pressurize 30 minutes obtains profiled member; With cooling water said profiled member is cooled to room temperature at last, cuts into 0.5m
2Specification obtain bulletproof halmet, said bulletproof halmet weight is 1.32kg.Adopt America NI J0101.04 side monomer testing standard that this bulletproof halmet is carried out the ballistic performance test, the result shows it can resist 10.8g, and speed is that 7.62 millimeters bore all-metals of 869 meter per seconds coat bullet.
Comparative example 1
The superhigh molecular weight polyethylene fibers of getting 400D prepares superhigh molecular weight polyethylene fibers according to the method for embodiment 1; Method with embodiment 3 prepares no latitude cloth then; Prepare bulletproof halmet with 30 layers of said no latitude cloth; Adopt America NI J0101.04 side monomer testing standard that this bulletproof halmet is carried out the ballistic performance test; The result shows a 9.6g, and speed is that 7.62 millimeters bore all-metals of 847m/ second coat the bulletproof halmet that bullets can puncture comparative example 1 preparation, and intensity and modulus are lower than the bulletproof halmet that said embodiment 3 prepares.
More than the preparation method of a kind of ultra-high molecular weight polyethylene bulletproof halmet provided by the invention has been carried out detailed introduction; Having used concrete example among this paper sets forth principle of the present invention and embodiment; The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (10)
1. the preparation method of a ultra-high molecular weight polyethylene bulletproof halmet is characterized in that, comprising:
A) provide ultra-high molecular weight polyethylene not have latitude cloth; The surface density of said no latitude cloth is 135g/cm
2More than;
B) the said ultra-high molecular weight polyethylene of several layers is not had the latitude cloth walkthrough under the pressure that in mould, successively superposes again, obtain walkthrough spare;
C) said walkthrough spare is carried out the desire compacting, obtain prefabricated component;
D) said prefabricated component is suppressed for the third time, obtained profiled member;
E) said profiled member is cooled to room temperature, obtains the ultra-high molecular weight polyethylene bulletproof halmet.
2. preparation method according to claim 1 is characterized in that, the ultra-high molecular weight polyethylene in the said step a) does not have latitude cloth and prepares through following method:
The superhigh molecular weight polyethylene fibers of 300～600D is arranged according to same direction, and with the thin polymer film bonding that contains binding agent;
2～4 said films that are bonded with fiber are stacked; Said two fibers that are bonded with in the film of fiber are vertical each other;
The said film that stacks is through compacting, and obtaining surface density is 135g/cm
2Above no latitude cloth.
3. preparation method according to claim 1 is characterized in that step b) is specially:
B1) said ultra-high molecular weight polyethylene not being had latitude cloth successively is laid in the mould;
B2) the no latitude cloth of said stack is applied the pressure of 5～8MPa, carry out walkthrough and obtain walkthrough spare.
4. preparation method according to claim 1 is characterized in that step c) is specially:
Under 80～100 ℃, said desire is arranged the pressure that part applies 10～15MPa, carried out pre-embossed 20～30 minutes, obtain prefabricated component.
5. preparation method according to claim 1 is characterized in that step d) is specially: said prefabricated component is suppressed under 100～120 ℃ for the third time, and the said pressure of compacting for the third time is 20～25MPa, obtains profiled member.
6. preparation method according to claim 1 is characterized in that, comprises that also step e) dyes the said helmet outward.
7. preparation method according to claim 1 is characterized in that, contains 30～200 layers of no latitude cloth in the said prefabricated component.
8. preparation method according to claim 7 is characterized in that, contains 50～100 layers of no latitude cloth in the said prefabricated component.
9. preparation method according to claim 1 is characterized in that, the said press time for the third time is 20～30 minutes.
10. preparation method according to claim 1 is characterized in that, the time of said cooling is 10～20 minutes.
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| CN103407168A (en) * | 2013-06-28 | 2013-11-27 | 句容市百事特复合材料有限公司 | Composite material with special reinforced fiber morphology |
| CN105216192A (en) * | 2015-09-07 | 2016-01-06 | 上海斯瑞科技有限公司 | A kind of bulletproof halmet and preparation method thereof |
| EP3012103A4 (en) * | 2013-06-20 | 2016-12-21 | Zhengzhou Zhongyuan Defense Mat Co Ltd | Non-weft cloth, manufacturing method therefor, and non-weft cloth product |
| EP3012101A4 (en) * | 2013-06-20 | 2016-12-21 | Zhengzhou Zhongyuan Defense Mat Co Ltd | Uni-directional cloth, laid fabric and preparation method thereof, and laid fabric product |
| CN107289816A (en) * | 2016-08-16 | 2017-10-24 | 包头北方嘉瑞防务科技有限公司 | A kind of bulletproof halmet and preparation method thereof |
| CN111113945A (en) * | 2019-12-17 | 2020-05-08 | 湖南中泰特种装备有限责任公司 | Method for manufacturing PE helmet |
| CN113390295A (en) * | 2021-06-02 | 2021-09-14 | 中国科学院力学研究所 | Bulletproof helmet |
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| EP3012103A4 (en) * | 2013-06-20 | 2016-12-21 | Zhengzhou Zhongyuan Defense Mat Co Ltd | Non-weft cloth, manufacturing method therefor, and non-weft cloth product |
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Application publication date: 20120704 |