CN107652658A - A kind of nylon/polyketone alloy material and preparation method thereof - Google Patents
A kind of nylon/polyketone alloy material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L73/00—Compositions of macromolecular compounds obtained by reactions forming a linkage containing oxygen or oxygen and carbon in the main chain, not provided for in groups C08L59/00 - C08L71/00; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
Abstract
The invention discloses a kind of nylon/polyketone alloy material and preparation method thereof, the component and parts by weight of alloy material are：10 50 parts of nylon resin, 40 80 parts of polyketone resin, 10 30 parts of glass fibre, 0.1 0.2 parts of initiator, 13 parts of maleic anhydride, 26 parts of co-monomer, 0.2 1 parts of antioxidant, 0.2 0.8 parts of stabilizer, 0.3 0.6 parts of lubricant, 0.1 0.5 parts of nucleator.The alloy material of the present invention improves the performance of nylon material, improves the heat endurance of polyketone material, alternative glass fiber enhanced nylon, enhancing PPS and POM, is used applied to high-end extreme harsh environment.
Description
Technical field
The present invention relates to polymeric material field, more particularly to a kind of nylon/polyketone alloy material of excellent performance and its
Preparation method.
Background technology
Polyketone with excellent heat resistance, chemical resistance, barrier and wearability due to being widely used in more
Individual field, the low water absorbable of polyketone, high rigidity-toughness balanced performance, high heat distortion temperature, modification is combined with Other Engineering plastics
With potentiality.But shortcoming is that process window is narrow, temperature sensitive, easily degraded, and also intensity under dry state and rigidity are not so good as
Traditional engineering plastics.
Polyamide, i.e. nylon, there is excellent mechanical performance, chemical-resistant, machinability, heatproof air aging performance,
Softening point is high, and oil resistant, electrical insulating property is good, there is self-extinguishment, nontoxic, odorless, and dyeability is good, and coefficient of friction is low, wear-resistant, and has
Self lubricity, shock absorption and sound-deadening properties, while there is excellent machine-shaping characteristic；Shortcoming is that water imbibition is larger, influences size
Stability.Resin water absorption rate can be reduced to its alloying and enhancing modification, improve product stability, can be in high temperature, high humidity
Lower work, broader applications are enabled them in the harsher electronic apparatus of operating environment requirements, motor vehicle industry, wherein with
The application on motor car engine periphery is especially common.Therefore, a kind of new alloy material is developed, glass fiber enhanced nylon is substituted, increases
Strong PPS and POM is particularly urgent applied to high-end extreme harsh environment use.
The content of the invention
The invention provides the nylon of a kind of excellent performance/polyketone alloy material and preparation method thereof, its alloy prepared
Material has excellent heat endurance, case hardness, wearability, corrosion resistance and agent of low hygroscopicity energy.
The technical scheme is that a kind of nylon/polyketone alloy material, its component and parts by weight are：Nylon resin 10-
50 parts, polyketone resin 40-80 parts, glass fibre 10-30 parts, compatilizer 3-6 parts, lubricant 0.1-0.5 parts, antioxidant 0.2-1
Part, stabilizer 0.2-0.8 parts, nucleator 0.1-0.5 parts.
Further, the component of the compatilizer and parts by weight are：Polyketone resin 91-97 parts, co-monomer 2-6 parts, Malaysia
Acid anhydrides 1-3 parts, initiator 0.1-0.3 parts, stabilizer 0.1-0.4 parts.
Further, the co-monomer is styrene.
Further, the initiator is benzene cumyl peroxide DCP.
Further, the maleic anhydride is maleic anhydride.
Further, the stabilizer is that metal oxide, the acid group salt of metallic copper, Pb stabilizer or metal soap are steady
Determine agent.
Further, the preparation method of the compatilizer comprises the following steps：
(1) proportioning weighs each component in parts by weight；The maleic anhydride is dissolved in the co-monomer and is uniformly dispersed, then
Mixed with the polyketone resin, initiator and stabilizer, be placed in high mixer and stir 5-10min；
(2) mixture obtained in step (1) is placed in dual-screw-stem machine, through melting extrusion, be granulated.
Further, the glass fibre that the glass fibre infiltrated for the silane coupler containing epoxide group, diameter
For 5-24um, length 3-9mm.
A kind of preparation method of nylon/polyketone alloy material, comprises the following steps：
1) the accurate each component for weighing formula ratio, nylon and polyketone resin are well mixed to obtain component A, by compatilizer, profit
Lubrication prescription, antioxidant, stabilizer, nucleator are well mixed, and obtain component B；Glass fibre is added by side feeding.
2) by component A and component B, while subregion is added in double screw extruder and extruded, and by water cooling, pelletizing, property is made
Excellent nylon/polyketone the alloy material of energy.
Further, the double screw extruder selection draw ratio 25-44:1..
Beneficial effects of the present invention：The present invention is compounded using polyketone resin and nylon resin, greatly reduces nylon material
Water absorption rate so that alloy material has good mobility, excellent anti-flammability, has further expanded the application of nylon material
Field.The present invention also optimizes the component and preparation method of compatilizer, is with the excellent polyketone grafted maleic anhydride of chemical resistance
Gained, it is fully compatible with base material polyketone resin, preferably promote nylon, glass fibre compatible scattered in polyketone；Not only carry
The high impact property of nylon material, chemically-resistant hydrolysis property so that the anti-wear performance of nylon material, case hardness are into several times
Increase；And the heat endurance of polyketone material is further improved, extend its application；Enable the present invention alloy material
Fiber glass reinforcement is substituted, for strengthening nylon, enhancing PPS and POM, is made applied to high-end extreme harsh environment
With.
Embodiment
In order that technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only explaining
The present invention, it is not intended to limit the present invention.
The deficiency aimed to overcome that in prior art of the present embodiment, there is provided a kind of excellent heat endurance, surface are hard
Degree, wearability, corrosion resistance and agent of low hygroscopicity can nylon/polyketone alloy material, its component and parts by weight are nylon resin
10-50 parts, polyketone resin 40-80 parts, glass fibre 10-30 parts, compatilizer 3-6 parts, lubricant 0.1-0.5 parts, antioxidant
0.2-1 parts, stabilizer 0.2-0.8 parts, nucleator 0.1-0.5 parts.
The nylon resin PA be selected from PA46, PA66, PA6, PA11, PA12, PA610, PA612, PA1010, PA1012,
In PA1212, PA4T, PA6T, PA9T, PA10T, PA6I, PAMXD6, PA6I, PA66/6, PA6/66, PA6T/6I, PA6T/66
One or more；One kind or several preferably in PA66, PA6, PA610, PA612, PA1010, PA11, PA12, PA66/6
Kind；More preferably PA6, PA610, PA612, PA1010, PA11, PA12.
The polyketone resin POK, which is selected from, to be contained derived from olefinic comonomer repeat unit and is repeated derived from carbon monoxide
The compound of the ketone unit of units alternately structure；The comonomer is selected from ethene, propylene, butylene, hexene, octene, decene, ten
One or more in diene, tetradecene, hexadecylene, octadecylene；Preferably ethene and/or propylene.
The glass fibre is continuous long glass fiber, short glass fiber or flat glass fiber, preferably comprises epoxy radicals
The glass fibre that the silane coupler of group infiltrated, its a diameter of 5-24 μm, preferably 10-15 μm, length 3-9mm, preferably
For 5-7mm.
The preparation method of the nylon/polyketone alloy material comprises the following steps：
1) the accurate each component for weighing formula ratio, nylon and polyketone resin are well mixed to obtain component A, by compatilizer, profit
Lubrication prescription, antioxidant, stabilizer, nucleator are well mixed, and obtain component B；Glass fibre is added by side feeding；
2) by component A and component B, while subregion is added in double screw extruder and extruded, and by water cooling, pelletizing, property is made
Excellent nylon/polyketone the alloy material of energy.
Wherein, double screw extruder is followed successively by by the temperature of feed zone to head：One 160 DEG C -180 DEG C of area's temperature, 2nd area
230 DEG C -250 DEG C of temperature, 230 DEG C -250 DEG C of three area's temperature, 210 DEG C -230 DEG C of four area's temperature, 210 DEG C -230 DEG C of five area's temperature,
Six 180 DEG C -210 DEG C of area's temperature, 180 DEG C -210 DEG C of seven area's temperature, the temperature of die head is 230 DEG C -250 DEG C.
The double screw extruder selection draw ratio 25-44:1, preferably draw ratio is 30:1.Selection 30:1 draw ratio can
Shorten residence time of the material in body, and can completes the scattered enhancing of the mixed melting and glass of alloy material.
The application especially optimizes component of compatilizer and preparation method thereof, and the component and parts by weight of the compatilizer are：
Polyketone resin 91-97 parts, co-monomer 2-6 parts, maleic anhydride 1-3 parts, initiator 0.1-0.3 parts, stabilizer 0.1-0.4 parts.
Wherein, main body of the polyketone resin as compatilizer, can be fully compatible with the polyketone end of alloy material, improves polyketone
With the compatibility of nylon；Because polyketone chemical resistance is fabulous, long hydrocarbon chain again be present, be especially suitable for grafted maleic anhydride.
Wherein co-monomer is preferably styrene, on the one hand, the fusible cis maleic anhydride of grafting of styrene, improves melt and adds
Work, play and help scattered effect；On the other hand, styrene may also suppress the decomposition of polyketone material, improve connecing for graft reaction
Branch rate.
Wherein cis maleic anhydride is highly polar reactive group, can be used as macromolecule interfacial coupling agent, compatilizer, disperses
Accelerator, make polyketone grafted maleic anhydride material that there is high polarity and reactivity, the compatibility of alloy material can also be improved
Energy.
Wherein initiator is preferably benzene cumyl peroxide DCP, in the compatilizer component for the application that is particularly suitable for use in, is made
With being to be catalyzed to trigger to maleic anhydride, it is set to be grafted in polyketone strand.
The stabilizer can be the acid group salt of metal oxide or metallic copper, preferably zinc oxide, cuprous iodide etc., can
To be Pb stabilizer, such as lead sulfate tribasic, dibasic lead stearate, or metal soap stabilizer, such as zinc stearate
(ZnSt), lead stearate (PbSt) etc., of course, it is possible to be substituted with the other kinds of stabilizer of this area.Further, it is described
Stabilizer is zinc oxide and lead sulfate tribasic compound, activated zinc oxide of the preferable particle size in 1-1000nm.Zinc oxide can be with
Acidic materials reaction, plays a part of stabilizing material color and performance caused by material decomposition.And Pb stabilizer can play
Improve the heat endurance of polyketone, the defects of improving its processing temperature window narrows.
The preparation method of the compatilizer, including step：
(1) proportioning weighs each component in parts by weight；
(2) maleic anhydride in the component that will be weighed in step (1) is dissolved among the co-monomer, then is gathered with described
Ketone, initiator and stabilizer are placed in stirring 5-10 minutes in high mixer；
(3) mixture obtained in step (2) is placed in dual-screw-stem machine, through melting extrusion, be granulated, process conditions are：
One 130-150 DEG C of area's temperature, two 180-200 DEG C of area's temperature, three 180-200 DEG C of area's temperature, four 160-180 DEG C of area's temperature, 5th area
160-180 DEG C of temperature, 190-210 DEG C of head temperature material, cylinder residence time are 1-3 minutes, melt pressure 10-20MPa.
One detailed elaboration is done to the present invention with reference to specific embodiment.
Embodiment 1-3
Compatilizer maleic anhydride grafting polyketone is prepared, it, which forms to match in parts by weight, is：
The preparation method of the compatilizer, including step：
(1) proportioning weighs each component in parts by weight；
(2) maleic anhydride in the component that will be weighed in step (1) is dissolved among the co-monomer, then is gathered with described
Ketone, initiator and stabilizer are placed in stirring 5-10 minutes in high mixer；
(3) mixture obtained in step (2) is placed in dual-screw-stem machine, through melting extrusion, be granulated, process conditions are：
One 130-150 DEG C of area's temperature, two 180-200 DEG C of area's temperature, three 180-200 DEG C of area's temperature, four 160-180 DEG C of area's temperature, 5th area
160-180 DEG C of temperature, 190-210 DEG C of head temperature material, cylinder residence time are 1-3 minutes, melt pressure 10-20MPa.
The grafting rate highest of maleic anhydride grafting polyketone compatilizer, wherein embodiment 2 is finally given through above-mentioned steps.
Embodiment 4-8
The compatilizer that embodiment 2 is obtained is used for the preparation of nylon and polyketone alloy material, specific as follows：
Performance test and evaluation：
First 100-120 DEG C of the condition in convection oven of particle material prepared by above-described embodiment 4-8 and comparative example 1-3
Lower drying 4 hours, standard testing batten then is made with injection (mo(u)lding) machine in dried particle material and is tested.
Wherein, tensile strength is tested by ASTM D-638 standards.Specimen types are I types, batten size (mm)：(176
± 2) (length) × (12.6 ± 0.2) (end portion width) × (3.05 ± 0.2) (thickness), draw speed 50mm/min；
Notch impact strength is tested by ASTM D-256 standards.Specimen types are I types, specimen size (mm)：(63±
2)×(12.45±0.2)×(3.1±0.2)；Breach type is A classes, and breach residual thickness is 1.9mm；
Corrosion resistance test is that 24h is persistently soaked in 5% hydrochloric acid, 5% sodium hydroxide, 5% sodium chloride solution, without obvious
Swelling and corrosion phenomenon；
Abrasion test method is as follows：Experiment carried out on XM-1 type abrasion wear test machines, load 210N, rotating speed 180RPM,
Time 630min.Material is processed into 10mm × 20mm × 20mm sample, is 45# steel to flour milling, both use flour milling
NO.900 emery papers polishing 100 times in advance, with electronics balance measurement frictional dissipation.
Embodiment 1-5 and comparative example 1-3 material properties test data such as table 1 below：
PA6 contents 20% can determine that by above table, alloy property is optimal during glass 30%, increases well beyond equal glass
Strong PA6 materials.Pass through embodiment 6 and comparative example 3, it can be seen that the compatilizer of this patent independent development preferably improves alloy
Compatibility, make alloy property shock resistance improve more than 30%, intensity improves more than 20%.
Alloy material provided by the present invention and preparation method thereof is described in detail above, tool used herein
Body example is set forth to the principle and embodiment of the present invention, and the explanation of above example is only intended to help and understands this hair
Bright method and its core concept；Meanwhile for those of ordinary skill in the art, according to the thought of the present invention, specific real
There will be changes in mode and application are applied, in summary, this specification content should not be construed as the limit to the present invention
System.
Claims (10)
1. a kind of nylon/polyketone alloy material, it is characterised in that its component and parts by weight are：
Nylon resin 10-50 parts
Polyketone resin 40-80 parts
Glass fibre 10-30 parts
Compatilizer 3-6 parts
Lubricant 0.1-0.5 parts
Antioxidant 0.2-1 parts
Stabilizer 0.2-0.8 parts
Nucleator 0.1-0.5 parts.
A kind of 2. nylon/polyketone alloy material as claimed in claim 1, it is characterised in that the component of the compatilizer and again
Measuring part is：
Polyketone resin 91-97 parts
Co-monomer 2-6 parts
Maleic anhydride 1-3 parts
Initiator 0.1-0.3 parts
Stabilizer 0.1-0.4 parts.
3. a kind of nylon/polyketone alloy material as claimed in claim 2, it is characterised in that the co-monomer is styrene.
4. a kind of nylon/polyketone alloy material as claimed in claim 2, it is characterised in that the initiator is benzene peroxidating
Diisopropylbenzene (DIPB) DCP.
5. a kind of nylon/polyketone alloy material as claimed in claim 2, it is characterised in that the maleic anhydride is maleic
Dicarboxylic anhydride.
6. a kind of nylon/polyketone alloy material as claimed in claim 2, it is characterised in that the stabilizer is metal oxidation
Acid group salt, Pb stabilizer or the metal soap stabilizer of thing, metallic copper.
7. a kind of nylon/polyketone alloy material as described in claim any one of 2-6, it is characterised in that the compatilizer
Preparation method comprises the following steps：
(1) proportioning weighs each component in parts by weight；The maleic anhydride is dissolved in the co-monomer and is uniformly dispersed, then with institute
Polyketone resin, initiator and stabilizer mixing are stated, is placed in high mixer and stirs 5-10min；
(2) mixture obtained in step (1) is placed in dual-screw-stem machine, through melting extrusion, be granulated.
A kind of 8. nylon/polyketone alloy material as described in claim any one of 1-6, it is characterised in that the glass fibre
The glass fibre infiltrated for the silane coupler containing epoxide group, a diameter of 5-24um, length 3-9mm.
A kind of 9. preparation method of nylon/polyketone alloy material as described in claim any one of 1-8, it is characterised in that bag
Include following steps：
1）The accurate each component for weighing formula ratio, to obtain component A by nylon and polyketone resin are well mixed, by compatilizer, lubricant,
Antioxidant, stabilizer, nucleator are well mixed, and obtain component B；Glass fibre is added by side feeding；
2）By component A and component B, while subregion is added in double screw extruder and extruded, and by water cooling, pelletizing, it is excellent that performance is made
Different nylon/polyketone alloy material.
A kind of 10. preparation method of nylon/polyketone alloy material as claimed in claim 9, it is characterised in that the twin-screw
Extruder selection draw ratio 25-44:1.
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| CN109280322A (en) * | 2018-09-21 | 2019-01-29 | 新钻塑料科技（上海）有限公司 | A kind of ultra-toughness POK polyketone material and preparation method thereof |
| CN109370194A (en) * | 2018-10-25 | 2019-02-22 | 新钻塑料科技（上海）有限公司 | A kind of rigidity and the tertiary blending alloy material of toughness equilibrium and preparation method thereof |
| CN109749397A (en) * | 2018-12-29 | 2019-05-14 | 上海日之升科技有限公司 | A kind of high shrinkage polyketone material and preparation method thereof |
| CN109852033A (en) * | 2019-01-23 | 2019-06-07 | 上海延锋金桥汽车饰件系统有限公司 | A kind of preparation method of moulding and thus obtained moulding |
| CN110172241A (en) * | 2019-05-16 | 2019-08-27 | 宁波公牛精密制造有限公司 | Polyamide and polyketone alloy composite materials and preparation method thereof |
| CN111171550A (en) * | 2019-12-24 | 2020-05-19 | 厦门颜盛塑化科技有限公司 | Modified nylon material and preparation method thereof |
| CN111875947A (en) * | 2020-08-03 | 2020-11-03 | 湖南工业大学 | Modified polyketone resin and preparation method thereof, nylon composite film and preparation method and application thereof |
| CN112175345A (en) * | 2020-10-09 | 2021-01-05 | 横店集团得邦工程塑料有限公司 | High-impact-resistance wear-resistance glass fiber reinforced POK-HDPE composite material and preparation method thereof |
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| CN109280322B (en) * | 2018-09-21 | 2021-08-20 | 新钻塑料科技（上海）有限公司 | Super-tough POK polyketone material and preparation method thereof |
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| CN110172241B (en) * | 2019-05-16 | 2021-09-14 | 公牛集团股份有限公司 | Polyamide and polyketone alloy composite material and preparation method thereof |
| CN111171550A (en) * | 2019-12-24 | 2020-05-19 | 厦门颜盛塑化科技有限公司 | Modified nylon material and preparation method thereof |
| CN111875947B (en) * | 2020-08-03 | 2022-06-07 | 湖南工业大学 | Modified polyketone resin and preparation method thereof, nylon composite film and preparation method and application thereof |
| CN111875947A (en) * | 2020-08-03 | 2020-11-03 | 湖南工业大学 | Modified polyketone resin and preparation method thereof, nylon composite film and preparation method and application thereof |
| CN112175345A (en) * | 2020-10-09 | 2021-01-05 | 横店集团得邦工程塑料有限公司 | High-impact-resistance wear-resistance glass fiber reinforced POK-HDPE composite material and preparation method thereof |
| CN112175345B (en) * | 2020-10-09 | 2022-06-14 | 横店集团得邦工程塑料有限公司 | High-impact-resistance wear-resistance glass fiber reinforced POK-HDPE composite material and preparation method thereof |
| CN113150538A (en) * | 2021-02-06 | 2021-07-23 | 广州辰东新材料有限公司 | Regenerated PA6/POK alloy reinforced wear-resistant material for automobile suspension plane bearing and preparation method thereof |
| CN113563593A (en) * | 2021-08-14 | 2021-10-29 | 科艾斯化学有限公司 | Core-shell toughening agent, preparation method thereof and toughened nylon applied by core-shell toughening agent |
| CN113563593B (en) * | 2021-08-14 | 2023-02-28 | 科艾斯化学有限公司 | Core-shell toughening agent, preparation method thereof and toughened nylon applied by core-shell toughening agent |
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