CN116968217A - Preparation method of polyarylate fiber prepreg and bulletproof helmet - Google Patents
Preparation method of polyarylate fiber prepreg and bulletproof helmet Download PDFInfo
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- CN116968217A CN116968217A CN202310840144.7A CN202310840144A CN116968217A CN 116968217 A CN116968217 A CN 116968217A CN 202310840144 A CN202310840144 A CN 202310840144A CN 116968217 A CN116968217 A CN 116968217A
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- polyarylate fiber
- polyarylate
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- 229920001230 polyarylate Polymers 0.000 title claims abstract description 199
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000004744 fabric Substances 0.000 claims abstract description 57
- 238000004513 sizing Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000012745 toughening agent Substances 0.000 claims abstract description 18
- 238000009990 desizing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000002074 melt spinning Methods 0.000 claims abstract description 11
- 238000009941 weaving Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 42
- 229920000642 polymer Polymers 0.000 claims description 9
- 238000010025 steaming Methods 0.000 claims description 9
- 238000009987 spinning Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000002788 crimping Methods 0.000 claims description 6
- 239000003822 epoxy resin Substances 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 claims description 4
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011159 matrix material Substances 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- 238000004026 adhesive bonding Methods 0.000 claims description 3
- 229920001971 elastomer Polymers 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 239000005060 rubber Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000002174 Styrene-butadiene Substances 0.000 claims description 2
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
- XUXNAKZDHHEHPC-UHFFFAOYSA-M sodium bromate Chemical compound [Na+].[O-]Br(=O)=O XUXNAKZDHHEHPC-UHFFFAOYSA-M 0.000 claims description 2
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 2
- 229960002218 sodium chlorite Drugs 0.000 claims description 2
- 239000011115 styrene butadiene Substances 0.000 claims description 2
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 2
- 229920002725 thermoplastic elastomer Polymers 0.000 claims description 2
- 229920001567 vinyl ester resin Polymers 0.000 claims description 2
- -1 acrylic ester Chemical class 0.000 claims 1
- 238000009954 braiding Methods 0.000 abstract 1
- 230000008569 process Effects 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 11
- 230000001681 protective effect Effects 0.000 description 6
- 229920000728 polyester Polymers 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 229920003235 aromatic polyamide Polymers 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000013386 optimize process Methods 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000004974 Thermotropic liquid crystal Substances 0.000 description 1
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000003811 curling process Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229920006240 drawn fiber Polymers 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
- B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
- B29B15/10—Coating or impregnating independently of the moulding or shaping step
- B29B15/12—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
- B29B15/122—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex
- B29B15/125—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex by dipping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B11/00—Making preforms
- B29B11/06—Making preforms by moulding the material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
- B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
- B29B15/10—Coating or impregnating independently of the moulding or shaping step
- B29B15/12—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
- B29B15/14—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length of filaments or wires
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/48—Wearing apparel
- B29L2031/4807—Headwear
- B29L2031/4814—Hats
- B29L2031/4821—Helmets
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a preparation method of polyarylate fiber prepreg and a bulletproof helmet, which comprises the following steps: s1, drying; s2, melt spinning; s3, storing; s4, bundling; s5, hot drawing; s6, sizing treatment; s7, braiding; s8, desizing treatment; s9, heat treatment; s10, preparing a prepreg. According to the invention, the toughening agent is added during melt spinning, and the polyarylate fiber bundles are subjected to sizing treatment, so that the wear resistance, bundling property and weaving property of the polyarylate fiber bundles are improved, and the mechanical property of the polyarylate fiber fabric is improved; the polyarylate fiber prepreg cut into a set shape is stacked layer by layer, a bulletproof helmet blank is paved, and the bulletproof helmet is pressed by adopting a high-temperature high-pressure forming die to obtain the polyarylate fiber bulletproof helmet with high protection performance.
Description
Technical Field
The invention relates to the technical and application fields of polymer materials, in particular to a preparation method of a polyarylate fiber prepreg and a bulletproof helmet.
Background
The helmet is used as important individual protective equipment in military operations and field operations, and is used for effectively reducing the impact and injury of bullets, fragments, shock waves and the like on the heads of soldiers. Bulletproof helmets are continuously developed along with the development of material science, and continuously progress towards high protection, light weight and comfort. At present, the main protective material of the bulletproof helmet is high-performance fibers such as para-aramid, ultra-high molecular weight polyethylene, heterocyclic aramid and the like. The polyarylate fiber has mechanical properties such as strength and modulus comparable to those of the aramid fiber, and also has outstanding properties such as wear resistance, chemical resistance, weather resistance, radiation resistance, impact resistance, creep resistance, wet strength retention, and the like, and is being gradually put into the trial production of protective equipment such as bulletproof helmets. The traditional process flow for preparing the bulletproof helmet prepreg by the polyarylate fiber comprises the following steps: the method comprises the steps of slicing, drying, melt spinning, storing, bundling, hot drawing, heat treatment, fabric and prepreg, but the fiber bundles inevitably bear some mechanical stress, such as tension, torsion, shearing force, friction force and the like, in the continuous weaving process of a loom, filaments in the fiber bundles are usually broken along with the continuous action of friction and tension on the yarns, the mechanical property of the fibers is lost under the conditions, and the protective property of the polyarylate fiber fabric is also greatly reduced. Moreover, at present, no polyarylate fiber fabric with high mechanical properties is applied to manufacturing of bulletproof helmets.
Disclosure of Invention
First, the technical problem to be solved
In view of the problems existing in the prior art, the invention provides a preparation method of a polyarylate fiber prepreg, and discloses a preparation optimization process of the polyarylate fiber prepreg, which comprises the following steps: slicing, drying, melt spinning (adding a toughening agent), storing, bundling, hot drawing, sizing, fabric, desizing, heat treatment and prepreg. The optimized process improves the strength and toughness of the polyarylate fiber by adding the toughening agent in the melt spinning process; the wear resistance, bundling property and weaving property of the polyarylate fiber bundles are improved by sizing the polyarylate fiber bundles; after the heat treatment process is put on the fabric for desizing, the loss of the mechanical property of the polyarylate fiber bundles in the weaving process is further compensated, the mechanical property of the polyarylate fiber fabric is improved, and finally the protective property of the polyarylate bulletproof helmet is improved.
In addition, the invention also provides a bulletproof helmet manufactured by the polyarylate fiber prepreg obtained by the preparation method of the polyarylate fiber prepreg.
(II) technical scheme
In order to achieve the above purpose, the main technical scheme adopted by the invention comprises the following steps:
in one aspect, the invention provides a method for preparing a polyarylate fiber prepreg, comprising the following specific steps:
s1, drying a polyarylate fiber slice to obtain a polyarylate fiber dry slice;
s2, carrying out melt spinning on the dried polyarylate fiber slices to obtain nascent polyarylate fibers;
s3, placing the nascent polyarylate fiber in a constant temperature and humidity environment for storage to obtain a finished product polyarylate fiber;
s4, integrating the finished polyarylate fibers into fiber bundles by using a fiber bundle bundling device to obtain the polyarylate fiber bundles;
s5, carrying out hot drawing treatment on the polyarylate fiber bundles to obtain finished polyarylate fiber bundles;
s6, sizing the finished polyarylate fiber bundles to obtain sized polyarylate fiber bundles;
s7, weaving the sized polyarylate fiber bundles to obtain a polyarylate fiber fabric;
s8, desizing the polyarylate fiber fabric to obtain a modified polyarylate fiber fabric;
s9, performing heat treatment on the modified polyarylate fiber fabric to obtain a finished product polyarylate fiber fabric;
and S10, performing gluing or gum dipping treatment on the finished polyarylate fiber fabric to obtain the polyarylate fiber prepreg.
According to the preferred embodiment of the present invention, in step S1, the polyarylate fiber slice is dried by a vacuum drying oven, wherein the temperature in the vacuum drying oven is 120-150 ℃; the water content threshold value is 0 ppm-10 ppm; the molecular weight of the polyarylate fiber slice is 30-40 ten thousand.
According to a preferred embodiment of the present invention, in step S2, the step of melt spinning the dried slice of the polyarylate fiber to obtain a nascent polyarylate fiber comprises the following specific steps:
s21, adding the polyarylate fiber dry slice and the toughening agent into a double-screw extruder, and melting at 300-370 ℃ to obtain microcrystalline polyarylate; the toughening agent is one or more of ethylene-octene polymer POE, acrylonitrile-butadiene-styrene copolymer ABS, styrene-butadiene thermoplastic elastomer SBS and polyvinyl butyral; the mole content of the toughening agent is 1% -3%;
s22, metering the microcrystalline polyarylate fiber through a metering pump, and feeding the microcrystalline polyarylate fiber into a spinning assembly for spinning to obtain the nascent polyarylate fiber.
Further, the breaking strength of the primary polyarylate fiber is 1GPa, the fiber strength is 8-10 CN/dtex, and the modulus is 370-400 CN/dtex.
Preferably, the toughening agent is preferably an ethylene-octene Polymer (POE), optimally added at 2%.
According to the preferred embodiment of the present invention, the storage conditions in step S3 are: the constant temperature and humidity environment temperature is 21-25 ℃, the humidity is 60-70%, and the storage time is 8-24 h.
According to a preferred embodiment of the present invention, in step S5, the step of performing heat-drawing treatment on the polyarylate fiber bundles to obtain finished polyarylate fiber bundles includes the following specific steps:
s51, drawing the polyarylate fiber bundles by using a steam drawing method to obtain hot drawn polyarylate fiber bundles; the drawing temperature of the steam drawing method is 285-295 ℃, the drawing speed is 45-50 mm/s, and the drawing multiple is 30-35 times.
S52, utilizing a fiber bundle crimping machine to crimp the hot-drawn polyarylate fiber bundles to obtain finished polyarylate fiber bundles; the crimping capacity of the crimping machine is 30-150 multiplied by 10 4 dtex; the bus density of the finished polyarylate fiber bundles is 0.44 to 0.67 multiplied by 10 4 dtex/mm。
Further, in order to impart the chemical fiber with a curling property similar to that of natural fibers, to increase the cohesion between the fibers, it is common to subject the drawn fibers to a curling process in order to improve the textile processability and to improve the fabric's taking property.
According to a preferred embodiment of the present invention, in step S6, the step of performing sizing treatment on the finished polyarylate fiber bundles to obtain modified polyarylate fiber bundles includes the specific steps of:
s61, immersing the finished polyarylate fiber bundles into a sizing agent through a guide roller and a rubber roller to obtain sized polyarylate fiber bundles; the sizing agent is one or more of aqueous polyurethane, aqueous epoxy resin, vinyl ester resin VER matrix and acrylonitrile-butadiene-styrene (ABS) matrix;
and S62, drying the sized polyarylate fiber bundles to obtain modified polyarylate fiber bundles.
Preferably, the sizing agent is an aqueous epoxy resin.
According to a preferred embodiment of the present invention, in step S8, the specific step of desizing the polyarylate fiber fabric includes:
s81, padding the polyarylate fiber fabric into desizing liquid for steaming to obtain desized polyarylate fiber fabric; the oxidant in the desizing liquid is one or more of hydrogen peroxide, sodium chlorite and sodium bromate; the temperature of the steaming is 100-102 ℃, and the steaming time is 10-15 min;
s82, washing the desized polyarylate fiber fabric with water to obtain the modified polyarylate fiber fabric.
According to the preferred embodiment of the present invention, in step S9, the modified polyarylate fiber fabric is heat-treated under a nitrogen flow at 240 to 300 ℃; the heat treatment time is 15-24 hours.
According to a preferred embodiment of the present invention, in step S10, when the final product polyarylate fiber fabric is subjected to glue spreading or dipping treatment, the adhesive used for glue spreading or dipping is one or more of phenolic resin, epoxy resin, polyurethane and acrylate.
On the other hand, the invention also provides a bulletproof helmet manufactured by the polyarylate fiber prepreg obtained by the preparation method.
Further, the prepreg is cut into petal shapes and split impeller shapes, stacked layer by layer, paved into bulletproof helmet blanks, and molded at high temperature and high pressure by adopting a mold to obtain the bulletproof helmet.
(III) beneficial effects
The invention provides a preparation method of a polyarylate fiber prepreg, which is mainly improved in the following aspects compared with the traditional process:
(1) The toughening agent is added in the melt spinning process, so that the strength and toughness of the polyarylate fiber are improved;
(2) Sizing the polyarylate fiber bundles to form a layer of coating on the surfaces of the polyarylate fiber bundles, so that the wear resistance, bundling property and weaving property of the polyarylate fiber bundles are improved, the fuzzing phenomenon in the processing process is reduced, and the strength of the material is improved;
(3) The molecular structure of the fibers is changed through hot drawing of the polyarylate fiber bundles, so that the fibers become softer and easier to stretch, and the molecular chains of the fibers are elongated in the drawing process, so that the polyarylate fibers become more slender and tough;
(4) After the heat treatment process is put in the fabric desizing step, the loss of the mechanical property of the polyarylate fiber bundles in the weaving process can be further compensated, and the treatment efficiency can be improved;
(5) The polyarylate fiber prepreg prepared by the invention is applied to the manufacturing of bulletproof helmets, and has high protective performance based on the good mechanical property of the polyarylate fiber fabric.
Drawings
Fig. 1 is a process flow for preparing a polyarylate fiber prepreg.
FIG. 2 is a graph showing the comparison of breaking strength of a polyarylate fiber prepreg prepared with different amounts of toughening agent.
FIG. 3 is a graph showing the elongation at break comparison of the polyarylate fiber prepregs made with different amounts of toughening agent.
FIG. 4 is a comparison of breaking strength of a prepreg of polyarylate fiber prepared at various heat treatment times.
FIG. 5 is a graph showing the elongation at break comparison of a polyarylate fiber prepreg prepared at various heat treatment times.
Fig. 6 is a comparison of break strength of a polyarylate fiber prepreg made with sizing versus no sizing.
FIG. 7 is a graph showing the elongation at break comparison of a polyester fiber prepreg prepared by sizing treatment versus no sizing treatment.
Fig. 8 is a comparison of breaking strength of a polyarylate fiber prepreg made before and after the fabric, respectively, during the heat treatment process.
Fig. 9 is a comparison of elongation at break of a polyarylate fiber prepreg made before and after the fabric, respectively, during the heat treatment process.
Detailed Description
The invention will be better explained by the following detailed description of the embodiments with reference to the drawings.
Experimental example 1
(1) Drying the prepared Thermotropic Liquid Crystal Polyarylate (TLCPAR) slice in a vacuum oven at 140 ℃ to reach a water content of 10ppm, wherein the molecular weight of the TLCPAR slice is 35W;
(2) Adding the dried TLCPAR slice and ethylene-octene Polymer (POE) into a double-screw extruder for melt spinning at 330 ℃, wherein the TLCPAR slice accounts for 99% (molar content), the ethylene-octene Polymer (POE) accounts for 1% (molar content), the screw pressure is 6.5Mpa, and then metering (the rotation speed of a metering pump: 2 rmp) and a spinning component (wherein the spinneret temperature is 320 ℃, the spinneret hole diameter is 0.2mm and the spinneret hole number is 50 f) through a metering pump, spinning and filament collecting (the winding speed is 400 m/min) to obtain the primary polyarylate fiber.
(3) And (3) storing the nascent polyarylate fiber for 24 hours at constant temperature and humidity, controlling the temperature at 24 ℃ and the humidity at 65%, and obtaining the finished polyarylate fiber.
(4) And (3) using a bundling frame of a fiber bundle bundling device to lead out the finished polyarylate fibers from the spinning head, passing through a yarn guide on the bundling frame, integrating the finished polyarylate fibers into flat ribbons, and preparing the finished polyarylate fibers into the polyarylate fiber bundles, wherein the tension on the bundling frame is regulated to be 0.0044cN/dtex.
(5) The polyester fiber bundle after sizing is subjected to common drawing by a steam drawing method, the drawing temperature is 290 ℃, the drawing speed of 50mm/s is used for drawing the polyester fiber bundle to 30 times, and then the drawn polyester fiber bundle is curled, so that the polyester fiber bundle forms the toughness and the curling performance similar to those of natural fibers, the cohesion among the fibers is increased, and the fabric serviceability is improved for improving the textile processing performance.
(6) Immersing the polyarylate fiber bundles into an aqueous epoxy resin sizing agent through a guide roller and a rubber press roller, after sizing, guiding the polyarylate fiber bundles into a drying roller from the other guide roller, and drying at 180 ℃ and then carrying out filament collection. And (3) forming a coating film on the surface of the polyarylate fiber bundle after sizing.
(7) The polyarylate fiber bundles were woven into a fabric using a spinning machine, and the fabric had a warp and weft density of 65 roots/10 cm.
(8) Padding the fabric into hydrogen peroxide desizing liquid for steaming, keeping the steaming temperature at 100 ℃, and enabling the oxidant to break and degrade slurry macromolecules, so that the fabric is washed out, and washing after steaming for 10 min.
(9) And (3) carrying out heat treatment on the desized polyarylate fiber fabric for 15 hours under the nitrogen flow at the temperature of 280 ℃ to improve the mechanical properties.
(10) And coating phenolic resin adhesive on the surface of the polyarylate fiber fabric after heat treatment, so that the polyarylate fiber fabric fiber is attached with an adhesive film to improve the adhesive force between the fabric and the resin, improve the mechanical property and obtain the polyarylate fiber prepreg after drying.
(11) The mechanical properties of the obtained polyarylate fiber prepreg were tested, and the warp breaking strength was 14kN, the weft breaking strength was 15kN, the warp breaking elongation was 7.5%, and the weft breaking elongation was 5%, as shown in table 1.
The preparation flow of the polyarylate fiber prepreg is shown in fig. 1.
Experimental example 2
The mechanical properties of the obtained polyarylate fiber prepreg were measured by adjusting the content of the toughening agent added in the step (2) of example 1 to 2%, and the other processes were the same as in example 1, and the obtained polyarylate fiber prepreg was 14.8kN in the warp direction, 15.3kN in the weft direction, 8% in the warp direction, and 5.2% in the weft direction, as shown in table 1.
Experimental example 3
The mechanical properties of the obtained polyarylate fiber prepreg were measured by adjusting the content of the toughening agent added in the step (2) of example 1 to 3%, and the other processes were the same as in example 1, wherein the warp breaking strength was 13.8kN, the weft breaking strength was 14.5kN, the warp breaking elongation was 7%, and the weft breaking elongation was 4.5%, as shown in table 1.
Comparative example 1
The comparative example differs from example 1 mainly in that no toughening agent was added in step (2), otherwise the process is the same as in example 1.
The mechanical property detection result of the polyarylate fabric prepreg prepared by the comparative example: the warp breaking strength was 13.5kN, the weft breaking strength was 14kN, the warp breaking elongation was 6.5%, and the weft breaking elongation was 5%, as shown in Table 1.
From the above examples 1 to 3 and comparative example 1, it was found that the mechanical properties of the polyarylate fabric prepreg were effectively improved by adding the toughening agent, and that the mechanical properties of the polyarylate fabric prepreg were best when the toughening agent was added in an amount of 2% (molar content), as shown in fig. 2 and 3.
Experimental example 4
The mechanical properties of the obtained polyarylate fiber prepreg were measured by adjusting the heat treatment time in the step (9) of example 2 to 20 hours, and the same procedure as in example 1, wherein the warp breaking strength was 15.5kN, the weft breaking strength was 16.5kN, the warp breaking elongation was 9%, and the weft breaking elongation was 5.8%, as shown in table 1.
Experimental example 5
The mechanical properties of the obtained polyarylate fiber prepreg were measured by adjusting the heat treatment time in the step (9) of example 2 to 24 hours, and the same procedure as in example 1, wherein the warp breaking strength was 15kN, the weft breaking strength was 15.8kN, the warp breaking elongation was 8.5%, and the weft breaking elongation was 5.6%, as shown in table 1.
As is clear from comparison of the performance test results of examples 2, 4 and 5, the heat treatment time has a certain effect on the mechanical properties of the polyarylate fiber prepreg, and the mechanical properties are best when heat treated for 20 hours, as shown in FIGS. 4 and 5. The sufficient heat treatment can promote the solid phase polycondensation reaction between the fibers and between the fiber bundles, increase the viscosity and improve the mechanical property.
Comparative example 2
This comparative example differs from example 4 mainly in that the sizing treatment of the polyarylate fiber bundles of step (6) and the desizing treatment of step (8) were not performed, and the other processes were the same as in example 4.
The polyarylate fiber prepreg obtained by this comparative example 2 had a warp breaking strength of 14.5kN, a weft breaking strength of 15kN, a warp breaking elongation of 8%, and a weft breaking elongation of 5.3%, as shown in table 1, fig. 6 and fig. 7. As shown. Therefore, the sizing treatment can form a layer of coating on the surface of the polyarylate fiber bundle, so that the phenomena of fuzzing and breakage in the processing process are reduced, the weapon protection effect of the processing performance is improved, and the strength of the material is improved.
Comparative example 3
The difference between this comparative example and example 4 is mainly that after step (9) is adjusted to step (5), the other processes are the same as those of example 4.
The polyarylate fiber prepreg obtained by this comparative example 3 had a warp breaking strength of 13kN, a weft breaking strength of 14kN, a warp breaking elongation of 8%, and a weft breaking elongation of 4.5%, as shown in table 1, fig. 8, and fig. 9. The experimental result shows that after the heat treatment process is put on the fabric, the solid phase polycondensation reaction between the fibers and between the fiber bundles can be promoted to increase the viscosity, the mechanical property is improved, and the loss of the mechanical property of the polyarylate fiber bundles in the weaving process is compensated.
TABLE 1 mechanical Properties of polyarylate fiber prepregs
To further compare the conventional preparation method of the polyarylate fiber prepreg with the preparation method of the present invention, the mechanical properties of the polyarylate fiber prepreg obtained in example 4 (representing the preparation method of the present invention) and the polyarylate fiber prepreg obtained in comparative example 3 (representing the conventional preparation method) were tested for yarns detached from the fabric in the warp and weft directions, and the test results are shown in table 2.
TABLE 2 mechanical Properties of polyarylate yarns
As is clear from the above examples, the mechanical properties of the prepared polyarylate fiber prepreg fabric are best under the process conditions of sizing and desizing treatment processes and heat treatment for 20 hours, which means that the optimized process can obviously improve the mechanical properties of the polyarylate fiber prepreg, and the mechanical properties of the polyarylate fiber prepreg can be effectively improved after the heat treatment is carried out on the fabric, as shown in fig. 2 to 9.
It should be noted that the above embodiments can be freely combined as needed. The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method of preparing a polyarylate fiber prepreg comprising:
s1, drying a polyarylate fiber slice to obtain a polyarylate fiber dry slice;
s2, carrying out melt spinning on the dried polyarylate fiber slices to obtain nascent polyarylate fibers;
s3, placing the nascent polyarylate fiber in a constant temperature and humidity environment for storage to obtain a finished product polyarylate fiber;
s4, integrating the finished polyarylate fibers into fiber bundles by using a fiber bundle bundling device to obtain the polyarylate fiber bundles;
s5, carrying out hot drawing treatment on the polyarylate fiber bundles to obtain finished polyarylate fiber bundles;
s6, sizing the finished polyarylate fiber bundles to obtain sized polyarylate fiber bundles;
s7, weaving the sized polyarylate fiber bundles to obtain a polyarylate fiber fabric;
s8, desizing the polyarylate fiber fabric to obtain a modified polyarylate fiber fabric;
s9, performing heat treatment on the modified polyarylate fiber fabric to obtain a finished product polyarylate fiber fabric;
and S10, performing gluing or gum dipping treatment on the finished polyarylate fiber fabric to obtain the polyarylate fiber prepreg.
2. The method of preparing a polyarylate fiber prepreg according to claim 1, wherein the drying the polyarylate fiber chips comprises: the polyarylate fiber slices are dried by a vacuum drying box, and the temperature in the vacuum drying box is 120-150 ℃; the water content threshold value is 0 ppm-10 ppm; the molecular weight of the polyarylate fiber slice is 30-40 ten thousand.
3. The method of preparing a polyarylate fiber prepreg according to claim 1, wherein the melt spinning the dried slices of the polyarylate fiber to obtain a nascent polyarylate fiber comprises:
s21, adding the polyarylate fiber dry slice and the toughening agent into a double-screw extruder, and melting at 300-370 ℃ to obtain microcrystalline polyarylate; the toughening agent is one or more of ethylene-octene polymer POE, acrylonitrile-butadiene-styrene copolymer ABS, styrene-butadiene thermoplastic elastomer SBS and polyvinyl butyral; the mole content of the toughening agent is 1% -3%;
s22, metering the microcrystalline polyarylate fiber through a metering pump, and feeding the microcrystalline polyarylate fiber into a spinning assembly for spinning to obtain the nascent polyarylate fiber.
4. The method of preparing a polyarylate fiber prepreg according to claim 1, wherein said placing said nascent polyarylate fiber in a constant temperature and humidity environment comprises: the constant temperature and humidity environment temperature is 21-25 ℃, the humidity is 60-70%, and the storage time is 8-24 h.
5. The method for preparing a polyarylate fiber prepreg according to claim 1, wherein the step of subjecting the polyarylate fiber bundles to a heat drawing treatment to obtain finished polyarylate fiber bundles comprises:
s51, drawing the polyarylate fiber bundles by using a steam drawing method to obtain hot drawn polyarylate fiber bundles; the drafting temperature of the steam drafting method is 285-295 ℃, the drafting speed is 45-50 mm/s, and the drafting multiple is 30-35 times;
s52, utilizing a fiber bundle crimping machine to crimp the hot-drawn polyarylate fiber bundles to obtain finished polyarylate fiber bundles; the crimping capacity of the crimping machine is 30-150 multiplied by 10 4 dtex; the bus density of the finished polyarylate fiber bundles is 0.44 to 0.67 multiplied by 10 4 dtex/mm。
6. The method of preparing a polyarylate fiber prepreg according to claim 1, wherein the sizing the finished polyarylate fiber bundles to obtain sized polyarylate fiber bundles comprises:
s61, immersing the finished polyarylate fiber bundles into a sizing agent through a guide roller and a rubber roller to obtain immersed polyarylate fiber bundles; the sizing agent is one or more of aqueous polyurethane, aqueous epoxy resin, vinyl ester resin VER matrix and acrylonitrile-butadiene-styrene (ABS) matrix;
and S62, drying the pulp-soaked polyarylate fiber bundles to obtain the pulp-soaked polyarylate fiber bundles.
7. The method for preparing a polyarylate fiber prepreg according to claim 1, wherein the desizing the polyarylate fiber fabric to obtain a modified polyarylate fiber fabric comprises:
s81, padding the polyarylate fiber fabric into desizing liquid for steaming to obtain desized polyarylate fiber fabric; the oxidant in the desizing liquid is one or more of hydrogen peroxide, sodium chlorite and sodium bromate; the temperature of the steaming is 100-102 ℃, and the steaming time is 10-15 min;
s82, washing the desized polyarylate fiber fabric with water to obtain the modified polyarylate fiber fabric.
8. The method for preparing a polyarylate fiber prepreg according to claim 1, wherein the heat treating the modified polyarylate fiber fabric to obtain a finished polyarylate fiber fabric comprises: carrying out heat treatment on the modified polyarylate fiber fabric under the nitrogen flow at 240-300 ℃; the heat treatment time is 15-24 hours.
9. The method of preparing a polyarylate fiber prepreg according to claim 1, wherein the subjecting the finished polyarylate fiber fabric to a gumming or dipping treatment comprises: the adhesive used in the gluing or gumming treatment is one or more of phenolic resin, epoxy resin, polyurethane and acrylic ester.
10. A bulletproof helmet of the polyarylate fiber prepreg, characterized in that the bulletproof helmet is manufactured using the polyarylate fiber prepreg obtained by the method for manufacturing the polyarylate fiber prepreg according to any one of claims 1 to 9.
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