CN110229504A - A kind of nylon elastomer nanocomposite and preparation method thereof - Google Patents
A kind of nylon elastomer nanocomposite and preparation method thereof Download PDFInfo
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- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
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Abstract
The present invention relates to field of nanocomposite materials, specifically, it is related to a kind of nylon elastomer nanocomposite and preparation method thereof, the nanocomposite is as premix through made from melt blending, the premix is formed by being combined with full be adhered between nylon elastomer particle of the nano material of liquid medium.The preparation method includes that liquid medium and nano material are mixed to get paste, and the paste is adhered to nylon elastomer particle surface progress melt blending and obtains nanocomposite.Nanocomposite provided by the invention has excellent toughness, and process flow is short, at low cost, is suitble to promote the use of.
Description
Technical field
The present invention relates to field of nanocomposite materials, specifically, be related to a kind of nylon elastomer nanocomposite and
Preparation method.
Background technique
It is squeezed out in existing technology frequently with nano material and mixed with polymers, composite material is formed, although such is compound
The tensile strength of material is promoted, but the problems such as due to nano material and the poor compatibility of polymer, leads to such material
Impact resistance it is generally not high.
To solve the above problems, enabling polymer send out between the gap of nano material frequently with modes such as intercalation in-situ polymerizations
It is raw to react to improve the impact resistance of composite material, but the process is time-consuming longer, polymeric reaction condition is harsh, and solvent
It is not easily recycled, the variations such as environmental pollution can be brought.
Patent No. CN101081928A proposes a kind of preparation method of polyamide/nano montmorillonite masterbatch, auxiliary using water
Help method to prepare polyamide/nano montmorillonite masterbatch, it is intercalator that preparation method, which is with deionized water, by the montmorillonite of purifying and
Mud is added step-wise to the polyamide that prescription amount melts completely by deionized water mixing, fully dispersed obtained montmorillonite mud, then
Polyamide/nano montmorillonite masterbatch is obtained through extruding pelletization.Preparation method is simple, and production cost is low, but this method is poly-
Montmorillonite mud is added after amide melting, montmorillonite mud is will lead to and has not enough time to be thoroughly mixed with copolymer, interlayer
Water just because of high-temperature gasification, causes polyamide to fail to timely enter interlayer, meanwhile, it is insufficient only by the energy of water generation
Will be completely exfoliated between cheating engaging layer thus cannot obtain the composite material that type is completely exfoliated, properties of product are also received greatly
Influence.
In view of this, the present invention is specifically proposed.
Summary of the invention
The present invention is intended to provide a kind of nanocomposite, including nano material and nylon elastomer, the nano material
The stretched processing in gap, do not need carry out intercalation in-situ polymerization, nylon bullet can be further increased while promoting intensity
The toughness of property body nanocomposites.
In order to achieve the above objectives, the present invention specifically adopts the following technical scheme that
A kind of nylon elastomer nanocomposite, which is characterized in that the nanocomposite is by premix through molten
Melt made from blending, the premix is that the nano material of liquid medium is full to be adhered between nylon elastomer particle by being combined with
It is formed.
In above scheme, the nylon elastomer is mainly block or graft copolymer, the maximum of polymer chain structure
Feature is it while including chemical structure different " hard sections " and " soft segment ".The wherein T of hard sectiongAnd TmIt is higher, in macromolecular chain
In be in glassy state or semi-crystalline, the T of soft segmentgAnd TmIt is lower, polymer is imparted with flexibility and extendability.The nylon
The hard section of elastomer is divided into 12 system of 6 system of nylon, nylon66 fiber system or nylon etc. according to used polyamide type difference.
In above scheme, using macromolecule as the nanocomposite of base-material, in the mechanical property lifting process for representing intensity
In, it can be lost in terms of toughness, can even be lower than the toughness of base-material itself sometimes, reduce the scope of application of material；Study carefully
Its reason is due to poor compatibility between the part nano material component in composite material and part macromolecule, in addition, nano material
Itself produces reunions in process, can not it is evenly dispersed in the composite, also result in the scarce of certain mechanical properties
It loses.Nanocomposite provided by the invention is combined with liquid medium in nano material, and the liquid that is combined with is situated between
The nano material adherency of matter is wrapped in nylon elastomer particle surface and forms mixture, by said mixture through melt blending, benefit
It enables liquid medium undergo phase transition with processing temperature-rise period, so that nano material is dispersed in nylon elastomer, greatly mentions
The high toughness of composite material.
In above scheme, the liquid medium include at least water, can also include isopentane, pentane, petroleum ether, oneself
Alkane, hexamethylene, isooctane, trifluoroacetic acid, trimethylpentane, pentamethylene, heptane, butyl chloride, trichloro ethylene, carbon tetrachloride, three
Trichlorotrifluoroethane, propyl ether, toluene, paraxylene, chlorobenzene, o-dichlorohenzene, diethyl ether, benzene, isobutanol, ethylene dichloride, just
Butanol, butyl acetate, propyl alcohol, methylisobutylketone, tetrahydrofuran, ethyl acetate, isopropanol, ethyl alcohol, chloroform, methyl ethyl ketone,
Dioxane, pyridine, acetone, nitromethane, acetic acid, acetonitrile, dimethylformamide, methanol, methylamine, dimethylamine, ether,
Pentane, methylene chloride, carbon disulfide, 1,1- dichloroethanes, trifluoroacetic acid, 1,1,1- trichloroethanes, ethyl alcohol, butanone, 1,2-
Dichloroethanes, glycol dimethyl ether, triethylamine, propionitrile, 4-methyl-2 pentanone, ethylenediamine, butanol, acetic acid, one first of ethylene glycol
Ether, octane, morpholine, ethylene glycol monoethyl ether, dimethylbenzene, meta-xylene, acetic anhydride, ortho-xylene, N,N-dimethylformamide, ring
One or more of hexanone, cyclohexanol, furfural, N-METHYLFORMAMIDE；Preferably water.
Further scheme of the invention are as follows: the nano material includes one kind of zero dimensional nanometer materials or monodimension nanometer material
Or it is a variety of, the liquid medium injects and fills the gap of nano material, forms the paste with tack.
Further scheme of the invention are as follows: the paste includes: that the consistency of the paste is 0~100mm, but is not
0mm；1 parts by weight of nano material, 0.02~100 parts by weight of liquid medium；Preferably, it is also preferable to include auxiliary agents 0 for the paste
~50 parts by weight, but be not 0.
In above scheme, compared to the prior art to nano-material modified filtering and dry process, nanometer of the invention
After material is between liquid medium is injected gap, paste continuous, and that there is certain tack, the paste are formd
With certain consistency, but consistency is not 0mm, represents the paste to be combined with liquid medium and having certain fluidity
Semisolid, therefore can be by the nano material paste uniform adhesion for being combined with liquid medium in nylon elastomer particle
Surface improves processability with the common feeding of nylon elastomer particle to the equipment of melt blending.Preferably, in order to mention
The amount of high the combined liquid medium of nano material, can also be added auxiliary agent.
Further scheme of the invention are as follows: the nylon elastomer includes polyamide, polyethers and dicarboxylic acids, the polyamide
Including one of PA6, PA66 or PA12.
In above scheme, the mass ratio of the polyamide and polyethers is 15~95:85~5, and the polyethers is by oxyalkylene list
Member composition, including but not limited to PEG, PPG, tetrahydrofuran, polytrimethylene ether glycol etc., the polyethers can be used to and contain
The polyamide-block polycondensation of carboxyl end group can also be changed into polyether diamine, and contract with the polyamide-block of carboxyl end group by amination
It is poly-.
Further scheme of the invention are as follows: the zero dimensional nanometer materials and monodimension nanometer material include nano silicon oxide, are received
Rice titanium oxide, nano zircite, nano zine oxide, nano aluminium oxide, nanogold, nano silver, nano-silicon, are received nano-nickel oxide
Rice carbon, carbon nano-fiber, carbon nanotube, nano-graphite, nano boron powder, nano-sulfur, nano lanthanum oxide, Nanometer-sized Neodymium Oxide, nanometer
Erbium oxide, nano-cerium oxide, nano oxidized praseodymium, nano yttrium oxide, nano europium oxide, nanometer tungsten oxide, nanometer silicon carbide, nanometer
One of tellurium oxide, nano oxidized niobium, nano-hafnium oxide or nanoscale molybdenum oxide are a variety of.
In above scheme, the ion exchange capacity between nano material and liquid medium is lower, and ion exchange does not almost occur, from
And liquid medium is made to enter the paste that nano material forms high viscosity containing large amount of liquid amount, convenient for further processing.
Further scheme of the invention are as follows: the mass ratio of the nano material and nylon elastomer is 0.1~20:100, excellent
It is selected as 1~10:100, more preferably 3~8:100.
The present invention also provides a kind of preparation methods of nylon elastomer nanocomposite, which is characterized in that the system
Preparation Method includes the following steps:
(1) liquid medium and nano material are mixed, obtain paste；
(2) paste will be obtained in step (1) to mix with nylon elastomer particle, enables paste is full to be adhered to nylon bullet
Premix is obtained between elastomer particles；
(3) premix in step (2) is subjected to melt blending, obtains nanocomposite；
Preferably, the step (1) further includes that liquid medium, nano material and auxiliary agent are mixed, and obtains paste.
In the above method, there is certain consistency semisolid paste since liquid medium and nano material to be mixed to get
Object, therefore slipping phenomenon will not occur for while being added to extrusion equipment after paste and nylon elastomer particle mixing, it can be direct
Feeding prepares nanocomposite, processing easy to produce, and avoids liquid medium in the prior art and receive caused by gasifying too early
The poor problem of nano composite material performance, through experiments, it was found that, it is compared with the prior art, nano combined made from mixing of the invention
Material property is more superior.
According to above-mentioned preparation method, in step (3), when melt blending, moulded in temperature greater than or equal to thermoplastic polymer
When changing temperature, liquid medium gasification in nanometer mixing material, the gasification separates the nano material of reunion, while the gasification
Heat is uniformly transferred in thermoplastic polymer and nano material；Preferably, the gasification softens thermoplastic polymer, and
Reduce the plasticization temperature of thermoplastic polymer.
According to above-mentioned preparation method, in step (3), it is higher than the boiling point of liquid medium in the temperature of melt blending and reaches Buddhist nun
During imperial elastomer plasticization temperature, liquid medium gasification separates the nano material of reunion；The boiling point of the liquid medium
Lower than the plasticization temperature of nylon elastomer, the boiling point is preferably not higher than 180 DEG C, and the liquid medium is preferably water；It is described
The weight ratio of liquid medium and nano material is 0.02~100:1, preferably 5~50:1, more preferably 5~20:1.
In the above method, the application use will add simultaneously in conjunction with the higher nano material of liquid medium amount with nylon elastomer
Enter process equipment, due to the lyophile media processes (forming paste) previously to nano material, so that nano material contains
Liquid measure improves, therefore when entering nylon elastomer melting zone, although system temperature is already higher than the boiling point of liquid medium, receives
Contained liquid medium is more between rice material void carry out the melting process of phase transformation evaporation process and nylon elastomer can simultaneously,
Just make molten state nylon elastomer that can smoothly enter into the gap of nano material, and improves the impact property of final products.And
In the prior art, the technical solution of the nano material containing liquid is added frequently with first carrying out melting to polymer, and due to receiving
The undertreatment of rice material lyophile medium reduces nano material and nylon elastic so that wherein liquid medium evaporation is too fast
The compatibility of body, so that the toughness of final products declines；On the other hand, in the prior art, first polymer melting is added and is received
Rice material undoubtedly extends the time of product preparation, wastes time cost.
According to above-mentioned preparation method, in step (3), premix that the paste and nylon elastomer particle are mixed to get
Feeding to hot melt process equipment carries out melt blending under the conditions of no pressure.
In the above method, hot melt process equipment includes but is not limited to mixer, open mill or screw extruder (parallel/cone
Shape/mono-/bis -/tri- screw rods), when using screw extruder, premix that the shape object and nylon elastomer particle are mixed to get
Material realizes the charging under the conditions of no pressure from without pressure feed zone charging.In the present invention, can by nano material directly with nylon bullet
Elastomer particles directly mix and carry out feeding, have benefited from nano material and form the cream with certain consistency in conjunction with liquid medium
Shape object, it is therefore prevented that slipping phenomenon, on the other hand the content of the liquid medium as contained by nano material is higher, logical in premix
When crossing the first melting zone, liquid medium therein will not too early phase transformation gasification, allow melting nylon elastomer preferably
It infiltrates between the gap of nano material and forms the nanocomposite of good mechanical properties.
According to above-mentioned preparation method, the step (1) further includes auxiliary agent being added in nano material to improve nano material
Liquid content, the liquid medium for enabling the nano material be combined accounts for the 50~98% of paste gross mass, preferably 60~
98%, more preferably 80~98%.
According to above-mentioned preparation method, the mass ratio of the auxiliary agent and nano material is 0.01~50:1, preferably 0.1~
5:1, more preferably 0.2~1:1, the auxiliary agent include carboxylate surface active agent, sulfate salt surfactant, sulfonate table
Face activating agent, phosphate ester salt surfactant, amine salt surfactant, quaternary surfactant, heterocyclic type surfactant,
Nonionic surfactant, natural water soluble high molecular, one or more of synthetic water soluble high molecular and its prepolymer.
In the above method, the premix in the present invention during the preparation process, using nylon elastomer as base-material, is used lower
The auxiliary agent of content, its purpose is to form the environment of lyophile medium between the gap of nano material, to improve paste
Liquid content；It is multiple to nanometer to significantly reduce auxiliary agent for high-content intercalator used in intercalation polymeric compared to the prior art
The influence of condensation material overall performance.
In above scheme, the ability that liquid medium enters nano material is can be improved in the addition of auxiliary agent, to increase nanometer
The consistency of material blends；In addition, the addition of auxiliary agent can also improve the boiling point of liquid medium, prevent liquid medium from gasifying in advance
Evolution.Due in the present invention generate gel nano material reaction temperature at room temperature, the requirement to auxiliary agent is not
Height, therefore it is wider to be suitable for the invention the alternative range of auxiliary agent.
The auxiliary agent includes but is not limited to one or more of following component:
A. surfactant:
1, anionic surfactant: it is divided into carboxylate, sulfuric acid, sulfonate and phosphate ester salt.
(1) soap kind is higher fatty acid salt, and general formula of molecular structure is (RCOO)-nMn+.With stearic acid, oleic acid, laurel
Acid etc. is more common.According to the difference of its metal ion (Mn+), there are alkali metal soap, alkaling earth metal base and organic amine soap etc..
(2) hydrosulphate is mainly the sulfuric acid ester of sulfated oil and higher aliphatic, general formula of molecular structure ROSO3-
M+, there are commonly lauryl sodium sulfate (also known as " sldium lauryl sulfate "), sodium hexadecyl sulfate (also known as " cetanol sulfuric acid
Sodium "), sodium stearyl sulfate (also known as " stearyl alcohol sodium sulphate ") etc..
(3) sulphonic acid compound mainly has aliphatic sulfonic compound, sulfo group aryl sulfonic acid compound, sulfo group naphthalene sulfonic acids compound etc.
2, cationic surfactant: containing nitrogen-atoms in the hydrophilic group ion of cationic surfactant, according to nitrogen original
The position difference of son in the molecule is divided into amine salt, quaternary ammonium salt and heterocyclic type three classes.Such as benzalkonium chloride (trade name " geramine "), benzene
Prick bromine ammonium (trade name " bromogeramine "), chlorination (bromination) cetyl pyridinium (trade name " Xi Bailin ") etc.
3, zwitterionic surfactant: lecithin, amino acid pattern, betaine type
4, nonionic surfactant: fatty glyceride, fatty acid sorbitan (sapn), polysorbate (tween), alkane
Base phenol polyethenoxy ether, fatty alcohol polyoxyethylene ether, fatty acid methyl ester APEO, detergent series.
B. water soluble polymer includes:
1, natural class macromolecule
Starch
Seaweeds: sodium alginate, agar-agar.
Natural plant gum class: Arabic gum, tragacanth gum, locust bean gum, tamarind seed polysaccharide glue, sesbania gum, carrageenan, guar gum, fruit
Glue.
Animal glue class: gelatin, casein, chitosan.
Microbiological gum: xanthan gum, gellan gum, hyaluronic acid.
2, class macromolecule and its prepolymer are synthesized
(1) polymeric type water soluble polymer and its prepolymer
Polyacrylamide, polyacrylic acid, polymethylacrylic acid and its copolymer, polyvinyl alcohol, polyethylene glycol, polyoxyethylene
Alkene, polyvinylpyrrolidone, polymaleic anhydride, polydimethyl diallyl ammonium chloride, polyvinylamine, poly- divinyl imidazoles
Quinoline, sulfonate styrene maleic anhydride copolymer, opens Pu Shi resin at kayexalate.
(2) polycondensation class water soluble polymer and its prepolymer
Water soluble amino resin, water soluble phenol resin, water soluble alkyd resin, water-soluble epoxy resin, water-soluble poly
Urethane resin, polyethylene imine, poly-aspartate, poly-epoxy succinic acid, polyamine epichlorohydrin resin, polyamide second two
Urea formaldehyde, ammonia-epichlorohydrin resin, heavy polyamine epichlorohydrin resin, ammonia-dimethylamine-epichlorohydrin resin, N, N-
Dimethyl 1,3- propane diamine and epichlorohydrin resin.
(3) other
Water Soluble Maleic Anhydride oil, dicyandiamide formaldehyde resin, rosin amine-ethylene oxide condensate, poly N-ethylene yl acetamide, water
Dissolubility ficoll.
3, semi-synthetic class macromolecule
Modified cellulose and converted starch.
Preferably synthetic class macromolecule and its prepolymer.
According to above-mentioned preparation method, nano material and the adding manner of auxiliary agent include being added at one time in the step (1)
It is added in batches；It is respectively 0.01-100g/min that speed, which is added, preferably 5-10g/min, more preferable 7g/min.
According to above-mentioned preparation method, the step (1) further includes implementing physical dispersion, the physical dispersion to nano material
Including but not limited to colloid mill, ball milling, ultrasound, vortex, etching auxiliary, gas shock etc.；Preferably, the physical dispersion is super
Sound, the frequency of the ultrasonic field are 800~1000Hz, and power is 200~1000W.
According to above-mentioned preparation method, the preparation method further includes addition latex shape in the paste made from step (1)
The mass ratio of resulting mixture, the later mixture and nylon elastomer melt blending, the latex and paste is 0.1~
10:1, the latex include styrene-acrylic emulsion, acrylic acid ester emulsion, acrylic emulsion, silicone acrylic emulsion, aqueous polyurethane emulsion, fluorine
Carbon emulsion, rosin resin lotion, terpinol, acrylate and vinyl acetate emulsion, aqueous epoxy resin emulsion, styrene-butadiene latex, Heveatex, white glue
One of cream, polychloroprene latex, pure C latex, carboxylic styrene butadiene latex, styrene-acrylic latex are a variety of.
In the above method, after the completion of prepared by the nano material paste for being combined with liquid medium, latex can also be utilized
Mixed processing is carried out to paste precast body, and the paste after latex mixed processing is melted simultaneously with nylon elastomer
It is blended and carries out following process, above-mentioned mixed processing has greatly delayed the release rate of liquid medium between gap, effectively prevent liquid
Phase transformation occurs to early in body medium, and on the other hand, the mixed processing of latex and paste further improves liquid medium phase transformation
When nano material gap expansion scale, be conducive to polymer travel further into nano material gap realize filling.
According to above-mentioned preparation method, the preparation method further includes before or during melt blending to paste and nylon
The weight ratio of the age resister being added in the premix that elastomer particles are formed, the age resister and nylon elastomer is 0.1
~1:100, preferably 0.3:100；The age resister is selected from amine antioxidants, phenolic antioxidant, and thio-2 acid vinegar class resists
One or more of oxygen agent and phosphorous vinegar kind antioxidant.
In the above method, the age resister includes:
Amine antioxidants: there are ketoamine condensation product, secondary diarylamine, substituted p-phenylenediamine, hindered amine；
Phenolic antioxidant: alkylation monophenols, alkylation polyphenol, thiobisphenol and polyphenol can be divided into.Alkylation monophenols and
Polyphenol antioxidant principal item has antioxidant 264,1076,2246,1035,1010,3114 and 1790；Thiobisphenol it is main
Kind has antioxidant 2246 and 300；Polyatomic phenol antioxidant principal item has 2,5 1 di-t-butyl hydroquinones and 2,5 12 uncles penta
Base quinhydrones；
Thio-2 acid vinegar and phosphorous vinegar kind antioxidant；Its principal item has anti-aging agent TNP, Ultranox624 and Asia
Tricresyl phosphate (2,4 1 di-tert-butyl) ester.
Other type antioxidants: 2 one coloured glaze base benzo miaow trade name antioxidant MBs, nickel dibutyl dithiocarbamate
Trade name antioxidant NBC, there are also zinc dialkyl dithiophosphates.
The age resister specifically includes: anti-aging agent RD, antioxidant A W, antioxidant BLE, antioxidant A, anti-aging agent OD, 4,
4 '-bis- (α-methylbenzyl) diphenylamines, 4,4 '-bis- (α, α-methylbenzyl) diphenylamines, N, N ,-di-sec-butyl-p-phenyl enediamine prevent
Old agent 4030, antioxidant 4010, antioxidant 4010NA, antioxidant 4020, antioxidant 264, antioxidant 1076, antioxidant 2216,
Antioxidant 1035, antioxidant 1010, antioxidant 3114, antioxidant 1790, antioxidant 2246, DBH 2,5 di tert butylhydroquinone, antioxygen
Agent DLTP, antioxidant TNP, Ultranox624, phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, antioxidant MB, anti-aging agent
NBC, zinc dialkyl dithiophosphate.
The present invention also provides a kind of premix, the premix includes paste and nylon elastomer；The paste
Include: 1 parts by weight of nano material, liquid medium 5-100 parts by weight, auxiliary agent 0-50 parts by weight, but is not 0；The paste is viscous
It overlays on nylon elastomer particle surface and forms premix；Preferably, during preparing paste, successively by nano material and
Auxiliary agent is added into liquid medium and is dispersed；It is furthermore preferred that the dispersion includes ultrasound, shearing, stirring, ball milling, colloid
Mill, vortex, etching auxiliary or gas shock；It is further preferred that nano material and the adding manner of auxiliary agent include disposable add
Enter and is added in batches.
The preparation method of above-mentioned nylon elastic composite material specifically comprises the following steps:
(1) liquid medium is stirred, while nano material is added with the speed of 0.01~100g/min and is persistently stirred
It is uniformly dispersed, the weight ratio of liquid medium and nano material is 0.02~100:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) in batches or once with the speed of 0.01~100g/min,
Obtain paste, the consistency of the paste is 0~100mm, and the weight ratio of the auxiliary agent and nano material is 0.001~50:
1；
(3) paste and nylon elastomer particle that step (2) obtains are mixed to get premix；
(4) by the premix of step (3), feeding hot melting equipment, melt blending simultaneously carry out subsequent add under the conditions of no pressure
Work obtains nanocomposite.
According to the above method, when the hot melting equipment is screw extruder, engine speed is 30~80Hz, and main feeding hopper turns
Speed is 10~30Hz, and extrusion temperature is 260~290 DEG C of an area, two 260~290 DEG C of areas, three 280~290 DEG C of areas, four areas 280
~290 DEG C, five 280~290 DEG C of areas.The linear velocity of screw speed is 0.6~1m/s.
It further include carrying out mixed processing using latex and paste afterwards in step (2), then carry out step according to the above method
(3) technique.
The invention has the benefit that
1. nylon elastomer nanocomposite provided by the invention is in terms of mechanical property, especially in terms of impact property
With biggish promotion, and simple process is easy to operate, and the used time is short, is suitable for promoting；
2. the present invention melts the higher nano material of liquid content with nylon elastomer simultaneously, composite processing mistake is utilized
Heat in journey improves the molecular energy of the liquid medium combined between nano material gap, promotes liquid medium between gap that phase occurs
Become, expanded the gap of nano material, realizes filling so that the nylon elastomer of molten state enters gap；
3. nano material provided by the invention through auxiliary agent processing formed have compared with containing large amount of liquid amount paste, with nylon bullet
Property body simultaneously during melt-processed, when the time and nylon elastomer that the liquid medium combined between gap is undergone phase transition melt
Between match, enter the gap of nano material conducive to the nylon elastomer of molten state and be filled；
4. nano material provided by the invention is while using liquid medium phase transformation expansion gap, also playing prevents from receiving
The effect that rice material is reunited.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with implementation of the invention
Example, is clearly and completely described the technical solution in embodiment, the following examples are intended to illustrate the invention, but is not used to
It limits the scope of the invention.
Embodiment 1
In the present embodiment, the mass ratio of nano material and nylon elastomer is 15:100, and the nylon elastomer is PA6
The mass ratio of system, PA6 and polyether block is 95:5, and the liquid medium used is water, and the auxiliary agent used for lecithin, receive by use
Rice material is nano oxidized praseodymium, is prepared as follows nanocomposite:
(1) liquid medium is stirred, while nano material is added with the speed of 8g/min and is persistently dispersed with stirring
Uniformly, the weight ratio of liquid medium and nano material is 16:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) in batches or once with the speed of 0.1g/min, obtains cream
Shape object, the consistency of the paste are 31mm, and the weight ratio of the auxiliary agent and nano material is 20:1；
(3) paste and nylon elastomer that step (2) obtains are mixed to get premix；
(4) by the premix of step (3) from without pressure feed zone feed screw extruder, melt blending simultaneously carries out subsequent add
Work obtains nanocomposite.
The engine speed of the extrusion equipment is 30Hz, and main feeding hopper revolving speed is 10Hz, and extrusion temperature is 260 DEG C of an area,
Two 290 DEG C of areas, three 280 DEG C of areas, four 285 DEG C of areas, five 280 DEG C of areas, the linear velocity of screw speed are 0.8m/s.
The tensile strength for the nylon elastomer nanocomposite that final extruding pelletization obtains is 54MPa, and bending strength is
88MPa, impact strength 52kgcm/cm.
Embodiment 2
In the present embodiment, the mass ratio of nano material and nylon elastomer is 10:100, and the nylon elastomer is PA66
The mass ratio of system, PA66 and polyether block is 95:5, and used liquid medium is glycol dimethyl ether and water, glycol dinitrate
The mass ratio of ether and water be 6:4, used auxiliary agent be polyacrylic acid and heavy polyamine epichlorohydrin resin, weight ratio 1:
1, the nano material used is prepared as follows nanocomposite for nano zine oxide:
(1) liquid is stirred, while nano material is added with the speed of 10g/min and is persistently dispersed with stirring
Even, the weight ratio of liquid medium and nano material is 100:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 0.5g/min, obtains paste, it is described
The consistency of paste is 24mm, and the weight ratio of the auxiliary agent and nano material is 50:1；
(3) paste and nylon elastomer that step (2) obtains are mixed to get premix；
(4) by the premix of step (3) from without pressure feed zone feed screw extruder, melt blending simultaneously carries out subsequent add
Work obtains nanocomposite.
The engine speed of the extrusion equipment is 80Hz, and main feeding hopper revolving speed is 30Hz, and one area of extrusion temperature is 270 DEG C,
Two 285 DEG C of areas, three 280 DEG C of areas, four 280 DEG C of areas, five 285 DEG C of areas；The linear velocity of screw speed is 1m/s.
The tensile strength for the nylon elastomer nanocomposite that final extruding pelletization obtains is 55MPa, and bending strength is
87MPa, impact strength 52kgcm/cm.
Embodiment 3
In the present embodiment, the mass ratio of nano material and nylon elastomer is 0.1:100, and the nylon elastomer is PA12
The mass ratio of system, PA12 and polyether block is 95:5, and the liquid medium used for water, adopt to open Pu Shi resin by the auxiliary agent used
Nano material is nanometer silicon carbide and nano oxidized erbium, and mass ratio 9:1 is prepared as follows nano combined material
Material:
(1) liquid medium is stirred, while nano material is added with the speed of 0.01g/min and carries out continuing stirring point
It dissipates uniformly, the weight ratio of liquid medium and nano material is 50:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 10g/min, obtains paste, the cream
The consistency of shape object is 69mm, and the weight ratio of the auxiliary agent and nano material is 0.1:1；
(3) paste and nylon elastomer that step (2) obtains are mixed to get premix；
(4) by the premix of step (3) from without pressure feed zone feed screw extruder, melt blending simultaneously carries out subsequent add
Work obtains nanocomposite.
The engine speed of the extrusion equipment is 60Hz, and main feeding hopper revolving speed is 20Hz, and one area of extrusion temperature is 270 DEG C,
Two 275 DEG C of areas, three 290 DEG C of areas, four 285 DEG C of areas, five 290 DEG C of areas；The linear velocity of screw speed is 0.9m/s.
The tensile strength for the nylon elastomer nanocomposite that final extruding pelletization obtains is 53MPa, and bending strength is
89MPa, impact strength 51kgcm/cm.
Embodiment 4
In the present embodiment, the mass ratio of nano material and nylon elastomer is 7:100, and the nylon elastomer is PA6
The mass ratio of system, PA6 and polyether block is 70:30, and for propyl ether, the auxiliary agent used uses the liquid medium used for chitosan
Nano material be carbon nano-fiber, the age resister used is prepared as follows nano combined for antioxidant 4010NA
Material:
(1) liquid medium is stirred, while nano material is added with the speed of 20g/min and is persistently dispersed with stirring
Uniformly applying frequency simultaneously is 800~1000Hz, and power is the ultrasound of 200~1000W, the weight of liquid medium and nano material
Than for 5:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 80g/min, obtains paste, the cream
The consistency of shape object is 71mm, and the weight ratio of the auxiliary agent and nano material is 5:1；
(3) paste and nylon elastomer that step (2) obtains are mixed to get premix；
(4) by the premix feeding mixer of step (3), melt blending simultaneously carries out following process, obtains nano combined material
Material.
The tensile strength of finally obtained nylon elastomer nanocomposite is 52MPa, bending strength 84MPa, punching
Hit intensity is 53kgcm/cm.
Embodiment 5
In the present embodiment, the mass ratio of nano material and nylon elastomer is 4:100, and the nylon elastomer is PA66
The mass ratio of system, PA66 and polyether block is 70:30, and for chlorotrifluoroethane and water, mass ratio is the liquid medium used
1:15, for benzalkonium chloride, the nano material used is prepared as follows nano combined the auxiliary agent used for Nanometer-sized Neodymium Oxide
Material:
(1) liquid medium is stirred, while nano material is added with the speed of 40g/min and is persistently dispersed with stirring
Uniformly, the weight ratio of liquid medium and nano material is 0.8:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 16g/min, obtains paste, the cream
The consistency of shape object is 45mm, and the weight ratio of the auxiliary agent and nano material is 0.8:1；
(3) paste and nylon elastomer that step (2) obtains are mixed to get premix；
(4) by the premix feeding open mill of step (3), melt blending simultaneously carries out following process, obtains nano combined material
Material.
The tensile strength of finally obtained nylon elastomer nanocomposite is 53MPa, bending strength 85MPa, punching
Hit intensity is 54kgcm/cm.
Embodiment 6
In the present embodiment, the mass ratio of nano material and nylon elastomer is 4:100, and the nylon elastomer is PA12
The mass ratio of system, PA12 and polyether block is 70:30, and the liquid medium used is water, and the auxiliary agent used is polyamide glyoxal
Resin and its prepolymer, the nano material used is nano silicon oxide, and the age resister used is Ultranox624, according to such as
Lower section method prepares nanocomposite:
(1) liquid medium is stirred, while nano material is added with the speed of 0.2g/min and carries out continuing stirring point
It dissipates uniformly, the weight ratio of liquid medium and nano material is 20:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 60g/min, obtains paste, the cream
The consistency of shape object is 68mm, and the weight ratio of the auxiliary agent and nano material is 30:1, further, by paste and acrylate
Lotion mixed processing；
(3) paste mixed with acrylic acid ester emulsion and nylon elastomer that step (2) obtains are mixed to get premix
Material；
(4) by the premix of step (3) from without pressure feed zone feed screw extruder, melt blending simultaneously carries out subsequent add
Work obtains nanocomposite.
The engine speed of the extrusion equipment is 60Hz, and main feeding hopper revolving speed is 30Hz, and one area of extrusion temperature is 270 DEG C,
Two 285 DEG C of areas, three 280 DEG C of areas, four 285 DEG C of areas, five 280 DEG C of areas；The linear velocity of screw speed is 0.7m/s.
The tensile strength for the nylon elastomer nanocomposite that final extruding pelletization obtains is 53MPa, and bending strength is
86MPa, impact strength 53kgcm/cm.
Embodiment 7
In the present embodiment, the mass ratio of nano material and nylon elastomer is 2:100, and the nylon elastomer is PA6
The mass ratio of system, PA6 and polyether block is 15:85, and the liquid medium used is water and dioxane, water and dioxane
The mass ratio 10:1 of hexane, used auxiliary agent are fatty acid methyl ester APEO, and the nano material used is nano oxidized
Hafnium is prepared as follows nanocomposite:
(1) liquid medium is stirred, while nano material is added with the speed of 20g/min and is persistently dispersed with stirring
Uniformly, the weight ratio of liquid medium and nano material is 40:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 4g/min, obtains paste, the cream
The consistency of shape object is 74mm, and the weight ratio of the auxiliary agent and nano material is 15:1；
(3) paste and nylon elastomer that step (2) obtains are mixed to get premix；
(4) by the premix feeding open mill of step (3), melt blending simultaneously carries out following process, obtains nano combined material
Material.
The tensile strength of finally obtained nylon elastomer nanocomposite is 51MPa, bending strength 85MPa, punching
Hit intensity is 50kgcm/cm.
Embodiment 8
In the present embodiment, the mass ratio of nano material and nylon elastomer is 6:100, and the nylon elastomer is PA66
The mass ratio of system, PA66 and polyether block is 15:85, and for water, the auxiliary agent used uses the liquid medium used for sodium alginate
Nano material be nano zine oxide, be prepared as follows nanocomposite:
(1) liquid medium is stirred, while nano material is added with the speed of 0.5g/min and carries out continuing stirring point
It dissipates and applies frequency simultaneously uniformly as 800~1000Hz, power is the ultrasound of 200~1000W, the weight of liquid medium and nano material
Amount is than being 6.5:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 9g/min, obtains paste, the cream
The consistency of shape object is 53mm, and the weight ratio of the auxiliary agent and nano material is 45:1；
(3) paste and nylon elastomer that step (2) obtains are mixed to get premix；
(4) by the premix of step (3) from without pressure feed zone feed screw extruder, melt blending simultaneously carries out subsequent add
Work obtains nanocomposite.
The engine speed of the extrusion equipment is 70Hz, and main feeding hopper revolving speed is 20Hz, and one area of extrusion temperature is 290 DEG C,
Two 290 DEG C of areas, three 285 DEG C of areas, four 285 DEG C of areas, five 290 DEG C of areas；The linear velocity of screw speed is 0.6m/s.
The tensile strength for the nylon elastomer nanocomposite that final extruding pelletization obtains is 50MPa, and bending strength is
84MPa, impact strength 51kgcm/cm.
Embodiment 9
In the present embodiment, the mass ratio of nano material and nylon elastomer is 18:100, and the nylon elastomer is PA12
The mass ratio of system, PA12 and polyether block is 15:85, and the liquid medium used is water, and the auxiliary agent used is polyamide glyoxal
The mass ratio of resin and poly-aspartate, polyamide glyoxal resin and poly-aspartate is 3:1, and used nano material is
Carbon nanotube is prepared as follows nanocomposite:
(1) liquid medium is stirred, while nano material is added with the speed of 10g/min and is persistently dispersed with stirring
Uniformly applying frequency simultaneously is 800~1000Hz, and power is the ultrasound of 200~1000W, the weight of liquid medium and nano material
Than for 30:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 15g/min, obtains paste, the cream
The consistency of shape object is 67mm, and the weight ratio of the auxiliary agent and nano material is 9:1, further, by paste and Carboxy
Latex mixed processing；
(3) paste mixed with carboxylic styrene butadiene latex and nylon elastomer that step (2) obtains are mixed to get premix
Material；
(4) by the premix of step (3) from without pressure feed zone feed screw extruder, melt blending simultaneously carries out subsequent add
Work obtains nanocomposite.
The engine speed of the extrusion equipment is 70Hz, and main feeding hopper revolving speed is 30Hz, and one area of extrusion temperature is 285 DEG C,
Two 290 DEG C of areas, three 285 DEG C of areas, four 280 DEG C of areas, five 280 DEG C of areas；The linear velocity of screw speed is 1m/s.
The tensile strength for the nylon elastomer nanocomposite that final extruding pelletization obtains is 52MPa, and bending strength is
83MPa, impact strength 50kgcm/cm.
Comparative example 1
In this comparative example, on the basis of embodiment 1, the position of extruder is added in adjustment nano material containing liquid, in no pressure
Feeding nylon elastomer under the conditions of power is pressurizeed in nylon elastomer after melting zone by receiving containing liquid medium between gap
Rice material feeding is mixed with the nylon elastomer of molten state.
The difference of comparative example 1 and embodiment is: the nano material between nylon elastomer and gap containing liquid medium is not
Feeding simultaneously, but first feeding nylon elastomer and after nylon elastomer melting, are combined with liquid between feeding gap of pressurizeing
The nano material of medium is processed.
The tensile strength for the nylon elastomer nanocomposite that final extruding pelletization obtains is 43MPa, and bending strength is
72MPa, impact strength 47kgcm/cm.
Mechanics Performance Testing is carried out to Examples 1 to 9 and comparative example 1, respectively obtains tensile strength, bending strength and impact
The performance parameter of intensity is as shown in the table:
As seen from the above table, the mechanical property of nanocomposite obtained by Examples 1 to 9 is above the performance ginseng of comparative example 1
Number, to find out its cause, being that the present invention using the phase transformation of liquid medium has carried out divergence process to nano material, so that and nano material
The nylon elastomer of melting is filled between entering gap simultaneously, is added when polymer melting is utilized in divergence process between above-mentioned gap
The heat that work generates enables liquid medium evaporation generate implosion and struts gap, while using the shearing force for squeezing out processing, further shelling
Gap is opened, so that molten state nylon elastomer realizes filling, to improve the mechanical property of product.
The above is only a better embodiment of the present invention and the applied technical principle.It will be appreciated by those skilled in the art that this hair
It is bright to be not limited to specific embodiment described here, be able to carry out for a person skilled in the art it is various it is apparent variation, again
Adjustment and substitution are without departing from protection scope of the present invention.Therefore, although by above embodiments to the present invention carried out compared with
For detailed description, but the present invention is not limited to the above embodiments only, without departing from the inventive concept, can be with
Including more other equivalent embodiments, and the scope of the invention is determined by the scope of the appended claims.
Claims (10)
1. a kind of nylon elastomer nanocomposite, which is characterized in that
The nanocomposite is as premix through made from melt blending, the premix is by being combined with liquid medium
Nano material is full to be adhered to and is formed between nylon elastomer particle.
2. nanocomposite according to claim 1, which is characterized in that the nano material includes zero dimensional nanometer materials
Or monodimension nanometer material is one or more, the liquid medium injects and fills the gap of nano material, and being formed has self-adhesion
The paste of property；Preferably, the zero dimensional nanometer materials and monodimension nanometer material include nano silicon oxide, and nano-titanium oxide is received
Rice zirconium oxide, nano zine oxide, nano aluminium oxide, nano-nickel oxide, nanogold, nano silver, nano-silicon, nano-sized carbon, carbon nanometer
Fiber, carbon nanotube, nano-graphite, nano boron powder, nano-sulfur, nano lanthanum oxide, Nanometer-sized Neodymium Oxide, nano oxidized erbium, nanometer
Cerium oxide, nano oxidized praseodymium, nano yttrium oxide, nano europium oxide, nanometer tungsten oxide, nanometer silicon carbide, nano oxidized tellurium, nanometer
One of niobium oxide, nano-hafnium oxide or nanoscale molybdenum oxide are a variety of.
3. composite material according to claim 1 or 2, which is characterized in that the consistency of the paste is 0~100mm, but
It is not 0mm；
The paste includes:
1 parts by weight of nano material
0.02~100 parts by weight of liquid medium；
The paste it is also preferable to include,
0~50 parts by weight of auxiliary agent, but be not 0.
4. composite material according to any one of claims 1 to 3, which is characterized in that the nylon elastomer includes poly-
Amide, polyethers and dicarboxylic acids, the polyamide include one of PA6, PA66 or PA12.
5. composite material described in any one according to claim 1~4, which is characterized in that the nano material and nylon bullet
Property body mass ratio be 0.1~20:100, preferably 1~10:100, more preferably 3~8:100.
6. a kind of preparation method of nylon elastomer nanocomposite, which is characterized in that the preparation method includes following step
It is rapid:
(1) liquid medium and nano material are mixed, obtain paste；
(2) paste will be obtained in step (1) to mix with nylon elastomer particle, enables paste is full to be adhered to nylon elastomer
Premix is obtained between particle；
(3) premix in step (2) is subjected to melt blending, obtains nanocomposite；
Preferably, the step (1) further includes that liquid medium, nano material and auxiliary agent are mixed, and obtains paste.
7. preparation method according to claim 6, which is characterized in that high in the temperature of melt blending in the step (3)
In liquid medium boiling point and during reaching nylon elastomer plasticization temperature, liquid medium gasification, by the nanometer material of reunion
Material separation；The boiling point of the liquid medium is lower than the plasticization temperature of nylon elastomer, and the boiling point is preferably not higher than 180 DEG C,
The liquid medium is preferably water；The weight ratio of the liquid medium and nano material be 0.02~100:1, preferably 5~50:
1, more preferably 5~20:1.
8. preparation method according to claim 6 or 7, which is characterized in that the step (1) further includes in nano material
Auxiliary agent is added to improve the liquid content of nano material, the liquid medium for enabling the nano material be combined accounts for paste gross mass
50~98%, preferably 60~98%, more preferably 80~98%；The auxiliary agent and the mass ratio of nano material be 0.01~
50:1, preferably 0.1~5:1, more preferably 0.2~1:1, the auxiliary agent include carboxylate surface active agent, sulfuric acid table
Face activating agent, sulfosalt surfactant, phosphate ester salt surfactant, amine salt surfactant, quaternary surfactant,
Heterocyclic type surfactant, nonionic surfactant, natural water soluble high molecular, in synthetic water soluble high molecular and its prepolymer
It is one or more of.
9. preparation method according to any one of claims 6 to 8, which is characterized in that the preparation method further include
Latex is added in paste made from step (1) and forms mixture, later the mixture and nylon elastomer melt blending, institute
The mass ratio for stating latex and paste is 0.1~10:1, and the latex includes styrene-acrylic emulsion, acrylic acid ester emulsion, propylene yogurt
Liquid, silicone acrylic emulsion, aqueous polyurethane emulsion, fluorine carbon emulsion, rosin resin lotion, terpinol, acrylate and vinyl acetate emulsion, aqueous epoxy resins
One of lotion, styrene-butadiene latex, Heveatex, white glue cream, polychloroprene latex, pure C latex, carboxylic styrene butadiene latex, styrene-acrylic latex
Or it is a variety of.
10. a kind of premix characterized by comprising
The premix includes paste and nylon elastomer；
The paste includes: 1 parts by weight of nano material, liquid medium 5-100 parts by weight, auxiliary agent 0-50 parts by weight, but is not
0；
The paste, which is covered, forms premix in nylon elastomer particle surface；
Preferably, during preparing paste, successively nano material and auxiliary agent are added into liquid medium and are divided
It dissipates；
It is furthermore preferred that the dispersion includes ultrasound, shearing, stirring, ball milling, colloid mill, vortex, etching auxiliary or gas shock；
It is further preferred that nano material and the adding manner of auxiliary agent include being added at one time and being added in batches.
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| CN1752112A (en) * | 2004-09-20 | 2006-03-29 | 中国科学院化学研究所 | Montmorillonoid in-situ organises and prepares the method for nano composite polymer-montmorillonoid material |
| CN106832913A (en) * | 2017-02-28 | 2017-06-13 | 苏州博利迈新材料科技有限公司 | A kind of hydrophobicity nylon 66 composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1752112A (en) * | 2004-09-20 | 2006-03-29 | 中国科学院化学研究所 | Montmorillonoid in-situ organises and prepares the method for nano composite polymer-montmorillonoid material |
| CN106832913A (en) * | 2017-02-28 | 2017-06-13 | 苏州博利迈新材料科技有限公司 | A kind of hydrophobicity nylon 66 composite material and preparation method thereof |
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| CN110229501A (en) * | 2018-03-06 | 2019-09-13 | 中国科学院化学研究所 | A kind of nylon elastomer nanocomposite and preparation method thereof |
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