CN117050511A - Low-temperature-resistant nylon composite material - Google Patents
Low-temperature-resistant nylon composite material Download PDFInfo
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- CN117050511A CN117050511A CN202311093655.3A CN202311093655A CN117050511A CN 117050511 A CN117050511 A CN 117050511A CN 202311093655 A CN202311093655 A CN 202311093655A CN 117050511 A CN117050511 A CN 117050511A
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- 239000004677 Nylon Substances 0.000 title claims abstract description 66
- 229920001778 nylon Polymers 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 43
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 21
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 21
- 239000012764 mineral filler Substances 0.000 claims abstract description 21
- 239000012745 toughening agent Substances 0.000 claims abstract description 21
- 229920013636 polyphenyl ether polymer Polymers 0.000 claims abstract description 19
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 58
- 239000004917 carbon fiber Substances 0.000 claims description 58
- 239000000203 mixture Substances 0.000 claims description 54
- 238000006243 chemical reaction Methods 0.000 claims description 39
- 238000001035 drying Methods 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000000605 extraction Methods 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- 150000001721 carbon Chemical class 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 9
- 239000003365 glass fiber Substances 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 238000011010 flushing procedure Methods 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 8
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 8
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 8
- 239000003208 petroleum Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000004804 winding Methods 0.000 claims description 8
- 229920001971 elastomer Polymers 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000005060 rubber Substances 0.000 claims description 4
- -1 salt compound Chemical class 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 claims description 3
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims description 3
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 3
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- 229920001897 terpolymer Polymers 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 2
- 229920000459 Nitrile rubber Polymers 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010881 fly ash Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- OCWMFVJKFWXKNZ-UHFFFAOYSA-L lead(2+);oxygen(2-);sulfate Chemical compound [O-2].[O-2].[O-2].[Pb+2].[Pb+2].[Pb+2].[Pb+2].[O-]S([O-])(=O)=O OCWMFVJKFWXKNZ-UHFFFAOYSA-L 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002857 polybutadiene Polymers 0.000 claims description 2
- 229920001021 polysulfide Polymers 0.000 claims description 2
- 239000005077 polysulfide Substances 0.000 claims description 2
- 150000008117 polysulfides Polymers 0.000 claims description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 2
- 239000010456 wollastonite Substances 0.000 claims description 2
- 229910052882 wollastonite Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 16
- 239000000835 fiber Substances 0.000 description 9
- 239000004952 Polyamide Substances 0.000 description 8
- 229920002647 polyamide Polymers 0.000 description 8
- 238000012360 testing method Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920002292 Nylon 6 Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 206010059866 Drug resistance Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006664 bond formation reaction Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 229920006126 semicrystalline polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of modified materials, and discloses a low-temperature-resistant nylon composite material, which comprises the following components: 40-50 parts of nylon, 30-40 parts of polyphenyl ether, 0.8-1.2 parts of heat stabilizer, 10-15 parts of toughening agent, 12-14 parts of modified montmorillonite, 10-16 parts of modified carbon fiber, 15-20 parts of inorganic mineral filler and 20-25 parts of compatilizer.
Description
Technical Field
The invention relates to the technical field of modified materials, in particular to a low-temperature-resistant nylon composite material.
Background
Nylon is polyamide fiber, namely nylon and nylon, the molecular main chain contains repeated amide groups, the polyamide fiber is the first synthetic fiber, long fiber or short fiber can be manufactured, the polyamide fiber has the most outstanding advantages of wear resistance higher than other fibers, elasticity, elastic recovery rate and wool compare favorably, the polyamide fiber is light in mass, the polyamide fiber can be processed into fine and smooth, nylon 6 is formed by ring-opening polycondensation of caprolactam, the macromolecular structure of the polyamide contains a large number of amide groups, and the macromolecular terminal is amino or carboxyl, so that the polyamide fiber is a semi-crystalline polymer with strong polarity, hydrogen bond formation and certain reactivity. PA6 is monoclinic system and takes on a plane 'zigzag' shape to form a and Y type crystals, and has extremely water absorption due to a large number of sub-coordination due to small crystallinity. The polyamide plastic has the performances of wear resistance, high toughness, light weight, drug resistance, heat resistance, cold resistance, easy molding and the like. As the literature 'research on the influence of filling polyethylene on the friction and abrasion performance of nylon', the polyethylene effectively improves the friction performance of nylon, but has poor low temperature resistance.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a nylon composite material with low temperature resistance and high toughness.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: the low-temperature-resistant nylon composite material comprises the following components in parts by weight: 40-50 parts of nylon, 30-40 parts of polyphenyl ether, 0.8-1.2 parts of heat stabilizer, 10-15 parts of toughening agent, 12-14 parts of modified montmorillonite, 10-16 parts of modified carbon fiber, 15-20 parts of inorganic mineral filler and 20-25 parts of compatilizer.
Preferably, the preparation method of the modified carbon fiber comprises the following steps:
(1) Winding carbon fibers in a stainless steel frame, putting the carbon fibers into an extraction device, adding a mixture of acetone and petroleum ether into the extraction device to extract for 70-80 hours, drying the extracted carbon fibers in an oven at 100-120 ℃ for 20-24 hours, putting the dried carbon fibers into a reaction kettle, locking the reaction kettle and a barometer by nuts, flushing carbon dioxide in the reaction kettle for 3-4 times, raising the pressure in the reaction kettle to critical pressure, and taking out the supercritical carbon fibers after reacting for 30-45 minutes;
(2) Adding 2.4-3.5g of polyvinyl alcohol and deionized water into a reactor, stirring for 30-50min, heating to 70-80 ℃, adding an initiator, methyl methacrylate and supercritical carbon fiber into the reactor, heating to 80-90 ℃, reacting for 2-3h, washing, suction filtering and drying to obtain the modified carbon fiber.
Preferably, the inorganic mineral filler is any one or more of fly ash, talcum powder, glass beads and wollastonite.
Preferably, the preparation method of the modified montmorillonite comprises the following steps: adding 12-14 parts of montmorillonite and deionized water into a reactor, stirring for 20-30min to form suspension, adding 2-4 parts of tetradecyl tributyl scale diluted by deionized water into the suspension, reacting at 60-80 ℃ for 5-8h, filtering, washing with ethanol, drying at 70-80 ℃ for 20-24h in a vacuum drying oven, and ball milling to obtain the modified montmorillonite.
Preferably, the heat stabilizer is any one or more of rare earth oxide, lead salt compound, antimony mercaptide, tribasic lead sulfate and dibasic stearic acid.
Preferably, the toughening agent is any one or more of liquid acrylate rubber, liquid polysulfide rubber, polybutadiene rubber, styrene-butadiene rubber, nitrile rubber and polyvinyl alcohol.
Preferably, the compatilizer is any one or more of ethylene-octene copolymer, ethylene-vinyl acetate copolymer, styrene-maleic anhydride, styrene-acrylonitrile-maleic anhydride copolymer, ethylene-methacrylic acid-isobutyl acrylic acid terpolymer and rare earth neutralized copolymer.
Preferably, the preparation method of the low-temperature-resistant nylon composite material comprises the following steps:
(1) Fully mixing 40-50 parts of nylon, 30-40 parts of polyphenyl ether, 0.8-1.2 parts of heat stabilizer, 12-14 parts of modified montmorillonite, 15-20 parts of inorganic mineral filler and 20-25 parts of compatilizer to obtain a primary mixture, uniformly mixing the primary mixture with 10-15 parts of toughening agent to obtain a mixture, and adding the mixture into a high-speed mixer for mixing for 5-8min at 200-300 r/min;
(2) And adding the mixture into a double-screw extruder for melting and extruding, simultaneously adding 10-16 parts of modified carbon fibers through a glass fiber port of the double-screw extruder, extruding, cooling, drying and granulating to obtain the low-temperature-resistant nylon composite material, wherein the temperature of each region of the extruder is 230-250 ℃, and the screw speed of the double-screw extruder is 120-300r/min.
(III) beneficial technical effects
The invention can improve the physical and chemical properties of polymer resin after modifying carbon fiber and blending polymer matrix resin, and the reinforcing effect mainly depends on the firm bonding of fiber material and polymer matrix to transfer the load borne by the polymer matrix to high-strength fiber material, and the load is transferred to a larger range from local part to even the whole composite material. The inorganic filler can improve the mechanical property of the low temperature resistant nylon composite material, and the compatibility between nylon and the inorganic filler can be improved by using the compatilizer of the ethylene-octene copolymer, the ethylene-vinyl acetate copolymer, the styrene-maleic anhydride, the styrene-acrylonitrile-maleic anhydride copolymer, the ethylene-methacrylic acid-isobutyl acrylic acid terpolymer and the rare earth neutralized copolymer, so that the morphological structure of the mixture can be improved, and the composite material can resist lower temperature.
Detailed Description
Example 1
(1) Winding carbon fibers in a stainless steel frame, putting the carbon fibers into an extraction device, adding a mixture of acetone and petroleum ether into the extraction device for extraction for 70 hours, drying the extracted carbon fibers in a baking oven at 100 ℃ for 20 hours, putting the dried carbon fibers into a reaction kettle, locking the reaction kettle and a barometer by nuts, flushing carbon dioxide in the reaction kettle for 3 times, raising the pressure in the reaction kettle to critical pressure, and taking out the supercritical carbon fibers after 30 minutes of reaction;
(2) Adding 2.4g of polyvinyl alcohol and deionized water into a reactor, stirring for 30min, heating to 70 ℃, adding an initiator, methyl methacrylate and supercritical carbon fiber into the reactor, heating to 80 ℃, reacting for 2h, washing, suction filtering and drying to obtain modified carbon fiber;
the preparation method of the modified montmorillonite comprises the following steps: adding 12 parts of montmorillonite and deionized water into a reactor, stirring for 20min to form a suspension, adding 2 parts of tetradecyl tributyl scale diluted by deionized water into the suspension, reacting at 60 ℃ for 5h, filtering, washing with ethanol, drying at 70 ℃ for 20h in a vacuum drying oven, and performing ball milling to obtain modified montmorillonite;
the preparation method of the low-temperature-resistant nylon composite material comprises the following steps:
(1) Fully mixing nylon, polyphenyl ether, a heat stabilizer, modified montmorillonite, an inorganic mineral filler and a compatilizer to obtain a primary mixture, uniformly mixing the primary mixture with a toughening agent to obtain a mixture, and adding the mixture into a high-speed mixer for mixing for 5min at 200 r/min;
(2) Adding the mixture into a double-screw extruder for melting and extruding, adding modified carbon fibers through a glass fiber port of the double-screw extruder, extruding, cooling, drying and granulating to obtain a low-temperature-resistant nylon composite material, wherein the temperature of each region of the extruder is 230 ℃, and the screw speed of the double-screw extruder is 120r/min;
the low temperature resistant nylon composite comprises: 40 parts of nylon, 30 parts of polyphenyl ether, 0.8 part of heat stabilizer, 10 parts of toughening agent, 12 parts of modified montmorillonite, 10 parts of modified carbon fiber, 15 parts of inorganic mineral filler and 20 parts of compatilizer.
Example 2
(1) Winding carbon fibers in a stainless steel frame, putting the carbon fibers into an extraction device, adding a mixture of acetone and petroleum ether into the extraction device for extraction for 80 hours, drying the extracted carbon fibers in a baking oven at 120 ℃ for 24 hours, putting the dried carbon fibers into a reaction kettle, locking the reaction kettle and a barometer by nuts, flushing carbon dioxide in the reaction kettle for 4 times, raising the pressure in the reaction kettle to critical pressure, and taking out the supercritical carbon fibers after reacting for 45 minutes;
(2) Adding 3.5g of polyvinyl alcohol and deionized water into a reactor, stirring for 50min, heating to 80 ℃, adding an initiator, methyl methacrylate and supercritical carbon fiber into the reactor, heating to 90 ℃, reacting for 3h, washing, suction filtering and drying to obtain modified carbon fiber;
the preparation method of the modified montmorillonite comprises the following steps: adding 14 parts of montmorillonite and deionized water into a reactor, stirring for 30min to form a suspension, adding 4 parts of tetradecyl tributyl scale diluted by deionized water into the suspension, reacting at 80 ℃ for 8h, filtering, washing with ethanol, drying at 80 ℃ for 24h in a vacuum drying oven, and performing ball milling to obtain modified montmorillonite;
the preparation method of the low-temperature-resistant nylon composite material comprises the following steps:
(1) Fully mixing nylon, polyphenyl ether, a heat stabilizer, modified montmorillonite, an inorganic mineral filler and a compatilizer to obtain a primary mixture, uniformly mixing the primary mixture with a toughening agent to obtain a mixture, and adding the mixture into a high-speed mixer for mixing for 8min at 300r/min;
(2) Adding the mixture into a double-screw extruder for melting and extruding, adding modified carbon fibers through a glass fiber port of the double-screw extruder, extruding, cooling, drying and granulating to obtain a low-temperature-resistant nylon composite material, wherein the temperature of each area of the extruder is 250 ℃, and the screw speed of the double-screw extruder is 300r/min;
the low temperature resistant nylon composite comprises: 50 parts of nylon, 40 parts of polyphenyl ether, 1.2 parts of heat stabilizer, 15 parts of toughening agent, 14 parts of modified montmorillonite, 16 parts of modified carbon fiber, 20 parts of inorganic mineral filler and 25 parts of compatilizer.
Example 3
(1) Winding carbon fibers in a stainless steel frame, putting the carbon fibers into an extraction device, adding a mixture of acetone and petroleum ether into the extraction device for extraction for 75 hours, drying the extracted carbon fibers in a baking oven at 110 ℃ for 22 hours, putting the dried carbon fibers into a reaction kettle, locking the reaction kettle and a barometer by nuts, flushing carbon dioxide in the reaction kettle for 3.5 times, raising the pressure in the reaction kettle to critical pressure, and taking out the supercritical carbon fibers after reaction for 37.5 minutes;
(2) Adding 2.95g of polyvinyl alcohol and deionized water into a reactor, stirring for 40min, heating to 75 ℃, adding an initiator, methyl methacrylate and supercritical carbon fiber into the reactor, heating to 85 ℃, reacting for 2.5h, washing, suction filtering and drying to obtain modified carbon fiber;
the preparation method of the modified montmorillonite comprises the following steps: 13 parts of montmorillonite and deionized water are added into a reactor, stirred for 25min to form suspension, 3 parts of tetradecyl tributyl scale diluted by deionized water are added into the suspension, the reaction temperature is 70 ℃, the reaction time is 6.5h, filtration, ethanol washing and drying are carried out for 22h at 75 ℃ in a vacuum drying oven, and the modified montmorillonite is obtained after ball milling;
the preparation method of the low-temperature-resistant nylon composite material comprises the following steps:
(1) Fully mixing nylon, polyphenyl ether, a heat stabilizer, modified montmorillonite, an inorganic mineral filler and a compatilizer to obtain a primary mixture, uniformly mixing the primary mixture with a toughening agent to obtain a mixture, and adding the mixture into a high-speed mixer for mixing at 250r/min for 6.5min;
(2) Adding the mixture into a double-screw extruder for melting and extruding, adding modified carbon fibers through a glass fiber port of the double-screw extruder, extruding, cooling, drying and granulating to obtain a low-temperature-resistant nylon composite material, wherein the temperature of each region of the extruder is 240 ℃, and the screw speed of the double-screw extruder is 210r/min;
the low temperature resistant nylon composite comprises: 45 parts of nylon, 35 parts of polyphenyl ether, 1 part of heat stabilizer, 12.5 parts of toughening agent, 13 parts of modified montmorillonite, 13 parts of modified carbon fiber, 17.5 parts of inorganic mineral filler and 22.5 parts of compatilizer.
Example 4
(1) Winding carbon fibers in a stainless steel frame, putting the carbon fibers into an extraction device, adding a mixture of acetone and petroleum ether into the extraction device for extraction for 75 hours, drying the extracted carbon fibers in a baking oven at 110 ℃ for 22 hours, putting the dried carbon fibers into a reaction kettle, locking the reaction kettle and a barometer by nuts, flushing carbon dioxide in the reaction kettle for 3.5 times, raising the pressure in the reaction kettle to critical pressure, and taking out the supercritical carbon fibers after reaction for 37.5 minutes;
(2) Adding 2.95g of polyvinyl alcohol and deionized water into a reactor, stirring for 40min, heating to 75 ℃, adding an initiator, methyl methacrylate and supercritical carbon fiber into the reactor, heating to 85 ℃, reacting for 2.5h, washing, suction filtering and drying to obtain modified carbon fiber;
the preparation method of the modified montmorillonite comprises the following steps: adding 12 parts of montmorillonite and deionized water into a reactor, stirring for 20min to form a suspension, adding 2 parts of tetradecyl tributyl scale diluted by deionized water into the suspension, reacting at 60 ℃ for 5h, filtering, washing with ethanol, drying at 70 ℃ for 20h in a vacuum drying oven, and performing ball milling to obtain modified montmorillonite;
the preparation method of the low-temperature-resistant nylon composite material comprises the following steps:
(1) Fully mixing nylon, polyphenyl ether, a heat stabilizer, modified montmorillonite, an inorganic mineral filler and a compatilizer to obtain a primary mixture, uniformly mixing the primary mixture with a toughening agent to obtain a mixture, and adding the mixture into a high-speed mixer for mixing for 5min at 200 r/min;
(2) Adding the mixture into a double-screw extruder for melting and extruding, adding modified carbon fibers through a glass fiber port of the double-screw extruder, extruding, cooling, drying and granulating to obtain a low-temperature-resistant nylon composite material, wherein the temperature of each region of the extruder is 230 ℃, and the screw speed of the double-screw extruder is 120r/min;
the low temperature resistant nylon composite comprises: 40 parts of nylon, 30 parts of polyphenyl ether, 0.8 part of heat stabilizer, 10 parts of toughening agent, 12 parts of modified montmorillonite, 10 parts of modified carbon fiber, 15 parts of inorganic mineral filler and 20 parts of compatilizer.
Example 5
(1) Winding carbon fibers in a stainless steel frame, putting the carbon fibers into an extraction device, adding a mixture of acetone and petroleum ether into the extraction device for extraction for 70 hours, drying the extracted carbon fibers in a baking oven at 100 ℃ for 20 hours, putting the dried carbon fibers into a reaction kettle, locking the reaction kettle and a barometer by nuts, flushing carbon dioxide in the reaction kettle for 3 times, raising the pressure in the reaction kettle to critical pressure, and taking out the supercritical carbon fibers after 30 minutes of reaction;
(2) Adding 2.4g of polyvinyl alcohol and deionized water into a reactor, stirring for 30min, heating to 70 ℃, adding an initiator, methyl methacrylate and supercritical carbon fiber into the reactor, heating to 80 ℃, reacting for 2h, washing, suction filtering and drying to obtain modified carbon fiber;
the preparation method of the modified montmorillonite comprises the following steps: adding 14 parts of montmorillonite and deionized water into a reactor, stirring for 30min to form a suspension, adding 4 parts of tetradecyl tributyl scale diluted by deionized water into the suspension, reacting at 80 ℃ for 8h, filtering, washing with ethanol, drying at 80 ℃ for 24h in a vacuum drying oven, and performing ball milling to obtain modified montmorillonite;
the preparation method of the low-temperature-resistant nylon composite material comprises the following steps:
(1) Fully mixing nylon, polyphenyl ether, a heat stabilizer, modified montmorillonite, an inorganic mineral filler and a compatilizer to obtain a primary mixture, uniformly mixing the primary mixture with a toughening agent to obtain a mixture, and adding the mixture into a high-speed mixer for mixing for 8min at 300r/min;
(2) Adding the mixture into a double-screw extruder for melting and extruding, adding modified carbon fibers through a glass fiber port of the double-screw extruder, extruding, cooling, drying and granulating to obtain a low-temperature-resistant nylon composite material, wherein the temperature of each region of the extruder is 240 ℃, and the screw speed of the double-screw extruder is 210r/min;
the low temperature resistant nylon composite comprises: 45 parts of nylon, 35 parts of polyphenyl ether, 1 part of heat stabilizer, 12.5 parts of toughening agent, 13 parts of modified montmorillonite, 13 parts of modified carbon fiber, 17.5 parts of inorganic mineral filler and 22.5 parts of compatilizer.
Comparative example 1
The preparation method of the modified montmorillonite comprises the following steps: 13 parts of montmorillonite and deionized water are added into a reactor, stirred for 25min to form suspension, 3 parts of tetradecyl tributyl scale diluted by deionized water are added into the suspension, the reaction temperature is 70 ℃, the reaction time is 6.5h, filtration, ethanol washing and drying are carried out for 22h at 75 ℃ in a vacuum drying oven, and the modified montmorillonite is obtained after ball milling;
the preparation method of the low-temperature-resistant nylon composite material comprises the following steps:
(1) Fully mixing nylon, polyphenyl ether, a heat stabilizer, modified montmorillonite, an inorganic mineral filler and a compatilizer to obtain a primary mixture, uniformly mixing the primary mixture with a toughening agent to obtain a mixture, and adding the mixture into a high-speed mixer for mixing at 250r/min for 6.5min;
(2) Adding the mixture into a double-screw extruder for melting and extruding, adding modified carbon fibers through a glass fiber port of the double-screw extruder, extruding, cooling, drying and granulating to obtain a low-temperature-resistant nylon composite material, wherein the temperature of each region of the extruder is 240 ℃, and the screw speed of the double-screw extruder is 210r/min;
the low temperature resistant nylon composite comprises: 45 parts of nylon, 35 parts of polyphenyl ether, 1 part of heat stabilizer, 12.5 parts of toughening agent, 13 parts of modified montmorillonite, 13 parts of modified carbon fiber, 17.5 parts of inorganic mineral filler and 22.5 parts of compatilizer.
Comparative example 2
(1) Winding carbon fibers in a stainless steel frame, putting the carbon fibers into an extraction device, adding a mixture of acetone and petroleum ether into the extraction device for extraction for 70 hours, drying the extracted carbon fibers in a baking oven at 100 ℃ for 20 hours, putting the dried carbon fibers into a reaction kettle, locking the reaction kettle and a barometer by nuts, flushing carbon dioxide in the reaction kettle for 3 times, raising the pressure in the reaction kettle to critical pressure, and taking out the supercritical carbon fibers after 30 minutes of reaction;
(2) Adding 2.4g of polyvinyl alcohol and deionized water into a reactor, stirring for 30min, heating to 70 ℃, adding an initiator, methyl methacrylate and supercritical carbon fiber into the reactor, heating to 80 ℃, reacting for 2h, washing, suction filtering and drying to obtain modified carbon fiber;
the preparation method of the low-temperature-resistant nylon composite material comprises the following steps:
(1) Fully mixing nylon, polyphenyl ether, a heat stabilizer, modified montmorillonite, an inorganic mineral filler and a compatilizer to obtain a primary mixture, uniformly mixing the primary mixture with a toughening agent to obtain a mixture, and adding the mixture into a high-speed mixer for mixing at 250r/min for 6.5min;
(2) Adding the mixture into a double-screw extruder for melting and extruding, adding modified carbon fibers through a glass fiber port of the double-screw extruder, extruding, cooling, drying and granulating to obtain a low-temperature-resistant nylon composite material, wherein the temperature of each region of the extruder is 240 ℃, and the screw speed of the double-screw extruder is 210r/min;
the low temperature resistant nylon composite comprises: 45 parts of nylon, 35 parts of polyphenyl ether, 1 part of heat stabilizer, 12.5 parts of toughening agent, 13 parts of modified montmorillonite, 13 parts of modified carbon fiber, 17.5 parts of inorganic mineral filler and 22.5 parts of compatilizer.
The tensile property of the low-temperature-resistant nylon composite material is referred to GB/T1040.1-2018 standard, the bending strength is referred to GB/T9341-2008 standard, an electronic universal testing machine is adopted for testing, the tensile rate is 50mm/min, and the sample is 10cm long, 5cm wide and 3mm high; cold resistance test: low temperature fold test (HG 2-161-65); notched impact strength was tested with reference to ISO180 and the test results are shown in table 1.
TABLE 1
As shown in Table 1, the flexural strength of the low temperature resistant nylon composite material reaches 41.6-46.8Mpa, the tensile strength reaches 34.9-36.8Mpa, the lowest temperature resistance reaches-180-165 ℃, and the notch impact strength reaches 25-35KJ/m 2 。
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (8)
1. The low-temperature-resistant nylon composite material is characterized by comprising the following components in parts by weight: 40-50 parts of nylon, 30-40 parts of polyphenyl ether, 0.8-1.2 parts of heat stabilizer, 10-15 parts of toughening agent, 12-14 parts of modified montmorillonite, 10-16 parts of modified carbon fiber, 15-20 parts of inorganic mineral filler and 20-25 parts of compatilizer.
2. The low temperature resistant nylon composite of claim 1, wherein the modified carbon fiber is prepared by the following steps:
(1) Winding carbon fibers in a stainless steel frame, putting the carbon fibers into an extraction device, adding a mixture of acetone and petroleum ether into the extraction device to extract for 70-80 hours, drying the extracted carbon fibers in an oven at 100-120 ℃ for 20-24 hours, putting the dried carbon fibers into a reaction kettle, locking the reaction kettle and a barometer by nuts, flushing carbon dioxide in the reaction kettle for 3-4 times, raising the pressure in the reaction kettle to critical pressure, and taking out the supercritical carbon fibers after reacting for 30-45 minutes;
(2) Adding 2.4-3.5g of polyvinyl alcohol and deionized water into a reactor, stirring for 30-50min, heating to 70-80 ℃, adding an initiator, methyl methacrylate and supercritical carbon fiber into the reactor, heating to 80-90 ℃, reacting for 2-3h, washing, suction filtering and drying to obtain the modified carbon fiber.
3. The low temperature resistant nylon composite of claim 1, wherein the inorganic mineral filler is any one or more of fly ash, talcum powder, glass beads and wollastonite.
4. The low temperature resistant nylon composite of claim 1, wherein the modified montmorillonite is prepared by the following steps: adding 12-14 parts of montmorillonite and deionized water into a reactor, stirring for 20-30min to form suspension, adding 2-4 parts of tetradecyl tributyl scale diluted by deionized water into the suspension, reacting at 60-80 ℃ for 5-8h, filtering, washing with ethanol, drying at 70-80 ℃ for 20-24h in a vacuum drying oven, and ball milling to obtain the modified montmorillonite.
5. The low temperature resistant nylon composite material according to claim 1, wherein the heat stabilizer is any one or more of rare earth oxide, lead salt compound, antimony mercaptide, tribasic lead sulfate and dibasic stearic acid.
6. The low temperature resistant nylon composite material according to claim 1, wherein the toughening agent is any one or more of liquid acrylate rubber, liquid polysulfide rubber, polybutadiene rubber, styrene-butadiene rubber, nitrile rubber and polyvinyl alcohol.
7. The low temperature resistant nylon composite of claim 1, wherein the compatibilizer is any one or more of ethylene-octene copolymer, ethylene-vinyl acetate copolymer, styrene-maleic anhydride, styrene-acrylonitrile-maleic anhydride copolymer, ethylene-methacrylic acid-isobutyl acrylic acid terpolymer and rare earth neutralized copolymer.
8. The method for producing a low temperature resistant nylon composite according to any one of claims 1 to 7, characterized in that the method for producing:
(1) Fully mixing 40-50 parts of nylon, 30-40 parts of polyphenyl ether, 0.8-1.2 parts of heat stabilizer, 12-14 parts of modified montmorillonite, 15-20 parts of inorganic mineral filler and 20-25 parts of compatilizer to obtain a primary mixture, uniformly mixing the primary mixture with 10-15 parts of toughening agent to obtain a mixture, and adding the mixture into a high-speed mixer for mixing for 5-8min at 200-300 r/min;
(2) And adding the mixture into a double-screw extruder for melting and extruding, simultaneously adding 10-16 parts of modified carbon fibers through a glass fiber port of the double-screw extruder, extruding, cooling, drying and granulating to obtain the low-temperature-resistant nylon composite material, wherein the temperature of each region of the extruder is 230-250 ℃, and the screw speed of the double-screw extruder is 120-300r/min.
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| CN117659696B (en) * | 2024-02-01 | 2024-05-07 | 河北铁科翼辰新材科技有限公司 | Anti-fatigue low-temperature-resistant nylon composite material and preparation method and application thereof |
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