CN108264758A - A kind of high dielectric property and wear-resisting nylon composite materials and preparation method thereof - Google Patents
A kind of high dielectric property and wear-resisting nylon composite materials and preparation method thereof Download PDFInfo
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- CN108264758A CN108264758A CN201611270094.XA CN201611270094A CN108264758A CN 108264758 A CN108264758 A CN 108264758A CN 201611270094 A CN201611270094 A CN 201611270094A CN 108264758 A CN108264758 A CN 108264758A
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- 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
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
- B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
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- 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
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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
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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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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Abstract
The invention discloses a kind of high dielectric property and wear-resisting nylon composite materials, which is made of the component for including following parts by weight：60 94 parts of nylon resin, polyvinylidene fluoride resin 5 25, compatilizer 1 15,0.02 0.5 parts of antioxidant.Each component is sufficiently mixed by the preparation of above-mentioned nylon composite materials using conical twin-screw mixer, then using double screw extruder extruding pelletization.Nylon composite materials of the present invention and preparation method thereof solve the problems, such as the poor compatibility between two kinds of resins of the nylon being primarily present at present and Kynoar, the excellent dielectric properties of Kynoar and good wearability are utilized simultaneously, the dielectric constant and wearability of nylon are improved, obtained composite material can be widely applied to need high abrasion, the auto industry of high-k and electric field.
Description
Technical field
The invention belongs to high-dielectric composite material fields, are related to a kind of wear-resisting nylon composite materials of high dielectric and its preparation
Method can be applied to high abrasion requirement, the auto industry of high-k and electric field.
Background technology
Nylon (PA) is the high polymer containing amide group in macromolecular main chain repetitive unit, is produced in five large-engineering plastics
The kind that amount is maximum, kind is most, purposes is most wide.Due to excellent mechanical property, excellent heat resistance and electrical isolation
Performance, excellent weatherability, nylon are widely used in machinery, automobile, electric appliance, textile material, chemical industry equipment, aviation, electric
The fields of grade, become indispensable structural material in all trades and professions.
Kynoar (PVDF) serves many purposes and moderate as a kind of physics, chemical synthesis function admirable
Thermoplastic fluoroelastomer plastics, at present its yield second is accounted in fluororesin, be only second to polytetrafluoroethylene (PTFE).Due on polymer chain
CH2 and CF2 are alternately arranged, and make it have polarity, and the dielectric constant of Kynoar is especially high.Low (the 160-185 of PVDF fusing points
DEG C), fluidity of molten is good, has most outstanding processing performance in fluoroplastics, can by the process equipment of resins for universal use into
Row squeezes out, blending, is molded and is blow molded, and is processed into various products.
In recent years, in polymer matrix composite research field, requirement of the people for high dielectric property is increasingly paid attention to,
Typically the ceramic with high-k is added to as function ingredients in polymer, high-k is prepared
Ceramic/polymer composites, but since the adhesive property between ceramic and polymer composites is poor,
The high-dielectric composite material of good mechanical properties just can not be obtained when ceramic additive amount is more, simultaneously because ceramic particle
The influence of scale limits the application of ceramic/polymer composites to a certain extent.Attempt other high-ks
Material substitution ceramic becomes one of solution.
The dielectric constant of Kynoar is especially high, but Kynoar strand has the bond energy height of F-C keys, and fluorine is former
Son has the characteristics of barrier action to the C-C keys in molecular backbone, therefore the regularity of strand is very high, and polymer has higher
Crystallinity, constitute close physical barrier so that any other atom or group hardly enter its structure and compatible,
Therefore the poor compatibility of polyvinylidene fluoride material and other materials is also resulted in.And use the preparation of twin-screw progress plastic alloy
When, it is necessary first to the key component in system will have good compatibility, therefore Kynoar is in the polymer alloy system of progress
The obstacle incompatible with other resins is encountered when standby.
The more existing research for nylon/Kynoar is mainly carried out in research institutions, is concentrated on being compression molded into
Type prepares composite material sheet or film using the method for melting/solution blending, for studying the crystal property of compound system.
It there is no the research report of the actual processing and application aspect in the range of industrialization to nylon/polyvinylidene fluoride composite material at present
Road.
Invention content
The high dielectric wear resistant nylon that the present invention provides a kind of filler with matrix compatibility is good, mechanical performance is high, heat-resist
Composite material and preparation method thereof.
The present invention adopts the following technical scheme that：
A kind of high dielectric property and wear-resisting nylon composite materials, are made of the component for including following parts by weight：
Wherein, the sum of parts by weight of the nylon resin, polyvinylidene fluoride resin and the compatilizer are kept for 100 parts.
In some embodiments, the nylon resin be selected from PA6, PA7, PA8, PA9, PA10, PA11, PA12,
One or more of PA610, PA612, PA613, PA1010, PA1212, PA1313.Preferably, nylon resin choosing
From one or more of PA6, PA10, PA1010, PA11, PA12, PA1212, PA610, PA612.It is it is highly preferred that described
Nylon resin is selected from one or more of PA10, PA11, PA12, PA1010, PA1212.
In some embodiments, the polyvinylidene fluoride resin is Kynoar powder.It is it is highly preferred that described
The molecular weight of polyvinylidene fluoride resin is in the range of 250,000~500,000.
In some embodiments, the compatilizer is selected from dimethyl sulfoxide (DMSO) (DSMO), methyl propenoic acid glycidyl
Ester (GMA), Kynoar grafted maleic anhydride (PVDF-g-MAH), styrene-maleic anhydride copolymer (SMA), polyamide
One or more of grafted maleic anhydride (PA-g-MAH).Preferably, it is sweet to be selected from Glycidyl methacrylate for the compatilizer
One in grease (GMA), Kynoar grafted maleic anhydride (PVDF-g-MAH), styrene-maleic anhydride copolymer (SMA)
Kind is several.
In a preferred embodiment, the antioxidant is selected from β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid positive ten
Eight carbon alcohol esters (1076), N, N '-bis--(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine (1098) and three
One kind or their compositions in [2.4- di-tert-butyl-phenyls] phosphite ester.
In a preferred embodiment, the nylon resin in the high dielectric property and wear-resisting nylon composite materials is adding
Work precedent is such as dried in vacuo 6-10H at 110 DEG C, its water absorption rate is made to be less than 0.05%.
In a preferred embodiment, each component of the high dielectric property and wear-resisting nylon composite materials is in conical double ribbon
Rotation mixing machine is mixed.
The preparation method of a kind of above-mentioned high dielectric property and wear-resisting nylon composite materials, includes the following steps：
(1) nylon resin of the water absorption rate less than 0.05% is added in together with Kynoar powder, compatilizer, antioxidant
It is sufficiently mixed into conical twin-screw mixer；
(2) mixed component is added in the loading hopper of double screw extruder, squeezes out pelletizing, it is wear-resisting that high dielectric is made
Nylon composite materials particle.
Wherein, double screw extruder used is processed, corrosion-resistant nickel alloy must be used for the part for touching melt
Material.
Above-mentioned preparation method further includes pre-treatment step：Nylon resin is dried in vacuo before processing, usually 110
DEG C dry 6-10H, makes its water absorption rate be less than 0.05%.
In step (1), other auxiliary agents can also be added according to the actual needs, such as：Toughener, fire retardant, stabilization
Agent, glass fibre or other mineral fillers etc. for further improving the properties of this system, expand its use scope.
Compared with prior art, beneficial effects of the present invention are as follows：
First, the compatilizer used in the present invention can increase the compatibility between nylon and Kynoar, reduce two
Surface tension between system boundary improves dispersion degree and Kynoar and nylon phase of the Kynoar in nylon
Binding force between interface；
Second, each component is sufficiently mixed by this patent using conical twin-screw mixer, then using double screw extruder
Extruding pelletization solves the consistency problem between two kinds of resins of the nylon being primarily present at present and Kynoar, while profit
With the excellent dielectric properties of Kynoar and good wearability, the dielectric constant and wearability of nylon, Ke Yiguang are improved
It is general to be applied to high abrasion, the auto industry of high-k and electric field.
Certainly, the either a program for implementing the present invention does not need to reach all the above advantage.
Specific embodiment
The present invention provides a kind of high dielectric property and wear-resisting nylon composite materials and preparation method thereof.
The present invention, which selects, has highly polar compatilizer such as Kynoar grafted maleic anhydride, polyvinylidene fluoride in compatilizer
Olefinic constituent can be fully compatible with resin matrix Kynoar, while present invention selection Kynoar powdered resin, powder
Form is in the contact area for macroscopically increasing Kynoar and compatilizer, nylon resin；Also, present invention selection uses cone
Mixture system is fully blended in shape double-spiral mixer, using the variation in batch mixer space, increases Kynoar
With the mixing uniformity of nylon.Therefore, the present invention solves the problems, such as that Kynoar can not be compatible with other resins, using this
When Kynoar and nylon resin are carried out a step melt blending by the technical solution of invention, preferable compatible effect will be reached
Fruit.
The present invention solves the problems, such as that existing Kynoar industrial at present can not be compatible with other resins, passes through this
Invention can reach obtains Kynoar/nylon blending material using relatively simple method, expands Kynoar
Application range.
With reference to specific embodiment, the present invention is further explained.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than restriction protection scope of the present invention.Technical staff is according to the improvement of the invention made and tune in practical applications
It is whole, still fall within protection scope of the present invention.
Embodiment 1
The present embodiment provides a kind of high dielectric property and wear-resisting nylon composite materials, preparation method it is as follows：
Weigh 60 parts by weight nylon 10, the Kynoar powder that 25 parts by weight molecular weight are 250,000,15 parts by weight of compatible
Agent Kynoar grafted maleic anhydride (PVDF-g-MAH), 0.1 parts by weight antioxidant β-(3,5- di-t-butyl -4- hydroxy benzenes
Base) the positive octadecanol ester (1076) of propionic acid and three [2.4- di-tert-butyl-phenyls] phosphite esters (168) composition (weight ratio
For 1: 1)；
10 resin of nylon is dried in vacuo 10H at 110 DEG C before processing first, its water absorption rate is made to be less than 0.05%；
Dried 10 resin of nylon is added to taper together with above-mentioned Kynoar powder, compatilizer, antioxidant
Double worm mixer is sufficiently mixed；
Mixed component is added in the loading hopper of double screw extruder, squeezes out pelletizing, the high wear-resisting Buddhist nun of dielectric is made
Imperial composite particles.
Embodiment 2
The present embodiment provides a kind of high dielectric property and wear-resisting nylon composite materials, preparation method it is as follows：
Weigh 70 parts by weight nylon 11s, the Kynoar powder that 20 parts by weight molecular weight are 350,000,10 parts by weight of compatible
Agent Kynoar grafted maleic anhydride (PVDF-g-MAH), 0.2 parts by weight antioxidant β-(3,5- di-t-butyl -4- hydroxy benzenes
Base) the positive octadecanol ester (1076) of propionic acid and three [2.4- di-tert-butyl-phenyls] phosphite esters (168) composition (weight ratio
For 1: 1)；
Nylon 11 resin is dried in vacuo 10H at 110 DEG C before processing first, its water absorption rate is made to be less than 0.05%；
Dried nylon resin is added to taper pair together with above-mentioned Kynoar powder, compatilizer, antioxidant
Mixing screw is sufficiently mixed；
Mixed component is added in the loading hopper of double screw extruder, squeezes out pelletizing, the high wear-resisting Buddhist nun of dielectric is made
Imperial composite particles.
Embodiment 3
The present embodiment provides a kind of high dielectric property and wear-resisting nylon composite materials, preparation method it is as follows：
Weigh 80 parts by weight nylon 12,13 parts by weight molecular weight be 400,000 Kynoar powder, 7 parts by weight of compatible agent
Poly (glycidyl methacrylate) (GMA), 0.3 parts by weight antioxidant β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid is just
The composition (weight ratio 1: 1) of octadecanol ester (1076) and three [2.4- di-tert-butyl-phenyls] phosphite esters (168)；
12 resin of nylon is dried in vacuo 9H at 110 DEG C before processing first, its water absorption rate is made to be less than 0.05%；
Dried nylon resin is added to taper pair together with above-mentioned Kynoar powder, compatilizer, antioxidant
Mixing screw is sufficiently mixed；
Mixed component is added in the loading hopper of double screw extruder, squeezes out pelletizing, high dielectric nylon is made and answers
Condensation material particle.
Embodiment 4
The present embodiment provides a kind of high dielectric property and wear-resisting nylon composite materials, preparation method it is as follows：
Weigh 90 parts by weight nylon 1010s, the Kynoar powder that 8 parts by weight molecular weight are 450,000,2 parts by weight of compatible
Agent styrene-maleic anhydride copolymer (SMA), 0.4 parts by weight antioxidant β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid is just
The composition (weight ratio 1: 1) of octadecanol ester (1076) and three [2.4- di-tert-butyl-phenyls] phosphite esters (168)；
Nylon 1010 resin is dried in vacuo 8H at 110 DEG C before processing first, its water absorption rate is made to be less than 0.05%；
Dried nylon resin is added to taper pair together with above-mentioned Kynoar powder, compatilizer, antioxidant
Mixing screw is sufficiently mixed；
Mixed component is added in the loading hopper of double screw extruder, squeezes out pelletizing, the high wear-resisting Buddhist nun of dielectric is made
Imperial composite particles.
Embodiment 5
The present embodiment provides a kind of high dielectric property and wear-resisting nylon composite materials, preparation method it is as follows：
Weigh 94 parts by weight nylon 1212s, the Kynoar that 5 parts by weight molecular weight are 500,000,1 parts by weight of compatible agent benzene
Ethylene maleic acid anhydride copolymer (SMA), 0.5 parts by weight antioxidant β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid positive 18
The composition (weight ratio 1: 1) of carbon alcohol ester (1076) and three [2.4- di-tert-butyl-phenyls] phosphite esters (168)；
Its water absorption rate is made to be less than 0.05% before processing in 110 DEG C of dry vacuum 8H 10 resin of nylon first；
Dried nylon resin is added to conical double ribbon rotation together with Kynoar powder, compatilizer, antioxidant
Mixing machine is sufficiently mixed；
Mixed component is added in the loading hopper of double screw extruder, squeezes out pelletizing, the high wear-resisting Buddhist nun of dielectric is made
Imperial composite particles.
The high dielectric property and the performance test results of wear-resisting nylon composite materials that above-described embodiment 1-5 is obtained see the table below
1。
Table 1
As can be seen from the above table, the high-k and wear-resisting nylon composite materials that prepared by the present invention, compared with PA12,
Its dielectric constant is improved significantly, while its coefficient of kinetic friction is also significantly reduced.The high dielectric property and resistance to of the present invention
The nylon composite materials of mill have high-k and the low coefficient of kinetic friction, can be widely used in auto industry and electronics electricity
Gas field is especially needed in wear-resisting, high dielectric property Material Field.
It is understood that the above description of the embodiments is intended to facilitate those skilled in the art and using this hair
It is bright.Person skilled in the art obviously easily can make various modifications, and described herein to these embodiments
General Principle is applied in other embodiment without having to go through creative labor.
Therefore, the present invention is not limited to embodiment here, those skilled in the art's announcement according to the present invention does not depart from this
The improvement and modification that invention scope is made all should be within protection scope of the present invention.
Claims (10)
1. a kind of high dielectric property and wear-resisting nylon composite materials, which is characterized in that by the component system for including following parts by weight
Into：
Wherein, the sum of parts by weight of the nylon resin, polyvinylidene fluoride resin and the compatilizer are 100 parts.
2. high dielectric property as described in claim 1 and wear-resisting nylon composite materials, which is characterized in that the nylon tree
Fat is in PA6, PA7, PA8, PA9, PA10, PA11, PA12, PA610, PA612, PA613, PA1010, PA1212, PA1313
One or more.
3. high dielectric property as described in claim 1 and wear-resisting nylon composite materials, which is characterized in that the poly- inclined fluorine
Vinyl is Kynoar powder.
4. high dielectric property and wear-resisting nylon composite materials as described in claim 1 or 3, which is characterized in that described is poly-
The molecular weight of pvdf resin is in the range of 250,000~500,000.
5. high dielectric property as described in claim 1 and wear-resisting nylon composite materials, which is characterized in that the compatilizer
It is common selected from dimethyl sulfoxide (DMSO), glycidyl methacrylate, Kynoar grafted maleic anhydride, phenylethylene-maleic anhydride
One or more of polymers, polyamide grafts maleic anhydride.
6. high dielectric property as described in claim 1 and wear-resisting nylon composite materials, which is characterized in that the antioxidant
Selected from β-the positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyl) propionic acid, N, N '-bis--(3- (3,5- di-t-butyl -4- hydroxyls
Base phenyl) propiono) one kind or their compositions in hexamethylene diamine and three [2.4- di-tert-butyl-phenyls] phosphite esters.
7. high dielectric property as described in claim 1 and wear-resisting nylon composite materials, which is characterized in that the high dielectric
When performance and the preparation of wear-resisting nylon composite materials, nylon resin is dried in vacuo before processing, its water absorption rate is made to be less than 0.05%.
8. high dielectric property as described in claim 1 and wear-resisting nylon composite materials, which is characterized in that the high dielectric property
When energy and the preparation of wear-resisting nylon composite materials, each component is mixed in conical twin-screw mixer.
9. a kind of preparation method of high dielectric property described in claim 1 and wear-resisting nylon composite materials, which is characterized in that
Include the following steps：
(1) nylon resin of the water absorption rate less than 0.05% is added to cone together with Kynoar powder, compatilizer, antioxidant
It is sufficiently mixed in shape double worm mixer；
(2) mixed component is added in the loading hopper of double screw extruder, squeezes out pelletizing, high dielectric wear resistant nylon is made
Composite particles.
10. the preparation method of high dielectric property as claimed in claim 9 and wear-resisting nylon composite materials, which is characterized in that
Further include pre-treatment step：Nylon resin is dried in vacuo before processing, its water absorption rate is made to be less than 0.05%.
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|---|---|---|---|---|
| CN111269448A (en) * | 2020-03-20 | 2020-06-12 | 清华大学 | Dielectric film, preparation method thereof and film capacitor |
| CN112316756A (en) * | 2020-11-12 | 2021-02-05 | 艾克飞膜材(嘉兴)有限公司 | High-strength and high-retention TIPS hollow fiber membrane and preparation method thereof |
| CN112940495A (en) * | 2020-12-31 | 2021-06-11 | 华南理工大学 | Nylon dielectric composite material with high resistance stability and preparation method and application thereof |
| CN115322562A (en) * | 2022-08-08 | 2022-11-11 | 江阴市龙山合成材料有限公司 | Low-moisture-absorption, heat-conduction and insulation PA66 composite material and preparation method thereof |
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