CN110229509A - A kind of long carbon chain nylon nanocomposite and preparation method thereof - Google Patents
A kind of long carbon chain nylon nanocomposite and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/041—Carbon nanotubes
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- C08K5/00—Use of organic ingredients
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- C08K5/03—Halogenated hydrocarbons aromatic, e.g. C6H5-CH2-Cl
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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Abstract
The present invention relates to field of nanocomposite materials, specifically, it is related to a kind of long carbon chain nylon 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 long carbon chain nylon 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 long carbon chain nylon 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 long carbon chain nylon 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 molten
Agent is not easily recycled, and can bring the variations such as environmental pollution.
Patent No. CN101081928A proposes a kind of preparation method of polyamide/nano montmorillonite masterbatch, using water
Auxiliary law prepares polyamide/nano montmorillonite masterbatch, and it is intercalator that preparation method, which is with deionized water, and the illiteracy of purifying is taken off
Mud is added step-wise to the polyamides that prescription amount melts completely by soil and deionized water mixing, fully dispersed obtained montmorillonite mud
Amine, then polyamide/nano montmorillonite masterbatch is obtained through extruding pelletization.Preparation method is simple, and production cost is low, but this method
It is to add montmorillonite mud after molten polyamide, will lead to montmorillonite mud and have not enough time to be thoroughly mixed with copolymer,
The water of interlayer just because of high-temperature gasification, causes polyamide to fail to timely enter interlayer, meanwhile, only by water generation
Energy, which is not enough to be completely exfoliated between cheating engaging layer, thus cannot obtain the composite material that type is completely exfoliated, properties of product
Receive strong 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 long carbon chain nylon, the nano material
The stretched processing in gap, do not need carry out intercalation in-situ polymerization, long carbon can be further increased while promoting intensity
The toughness of chain Nylon Nanocomposite material.
In order to achieve the above objectives, the present invention specifically adopts the following technical scheme that
A kind of long carbon chain nylon 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 to long carbon chain nylon particle by being combined with
Between formed.
In above scheme, the amide groups repeated in polyamide molecule segment is one with polar group, this collection
Hydrogen in group can form quite powerful hydrogen bond in conjunction with the oxygen on the carbonyl on the amide group segment of another molecule.
Hydrogen bond is formed such that the structure of polyamide easily crystallizes.And since intermolecular active force is larger, so that poly-
Amide has higher mechanical strength and high plasticization temperature.On the other hand the presence in polyamide molecule due to methylene makes
It is submissiveer to obtain strand, thus also toughness with higher, but during forming composite material with nano material,
Since nano material and the compatibility of polyamide are there are difference, the toughness that will lead to polyamide itself is declined, in addition, poly-
The major defect of amide is that hydrophily is too strong, and the dimensional stability after leading to water suction is deteriorated.
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, nanometer material
Material itself produce reunion in process, can not it is evenly dispersed in the composite, also result in certain mechanical properties
Missing.Nanocomposite provided by the invention is combined with liquid medium in nano material, and is combined with liquid for described
The nano material adherency of medium is wrapped in long carbon chain nylon particle surface and forms mixture, by said mixture through melt blending,
Liquid medium is enabled to undergo phase transition using processing temperature-rise period, so that nano material is dispersed in long carbon chain nylon, greatly
Improve the 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, second
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, ethylene glycol
Monomethyl ether, octane, morpholine, ethylene glycol monoethyl ether, dimethylbenzene, meta-xylene, acetic anhydride, ortho-xylene, N, N- dimethyl formyl
One or more of amine, cyclohexanone, cyclohexanol, furfural, N-METHYLFORMAMIDE；Preferably water.
In above scheme, staff of the invention it was unexpectedly observed that polyamide hydrophilic it is too strong and absorb water after size it is steady
Qualitative variation, although using the liquid medium based on water to infuse between nano material gap in the technical solution of the application
Liquid, but merged using the higher nano material of water content with polyamide 66 and its copolymer after fluid injection and mix and squeeze out
During processing, the dimensional stability of polyamide 66 is not impacted included in the interstitial water body of nano material, very
To also improving the impact strength of polyamide 66 composite material.
Further scheme of the invention are as follows: the nano material includes the one of zero dimensional nanometer materials or monodimension nanometer material
Kind is a variety of, and the liquid medium injects and fill the gap of nano material, forms the paste with tack.
Further scheme of the invention are as follows: the consistency of the paste is 0~100mm, but is not 0mm；The paste
It include: 1 parts by weight of nano material, 0.02~100 parts by weight of liquid medium；Preferably, it is also preferable to include help the paste
0~50 parts by weight of agent, 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
Object has certain consistency, but consistency is not 0mm, represents the paste to be combined with liquid medium and having a constant current
The semisolid of dynamic property, therefore can be by the nano material paste uniform adhesion for being combined with liquid medium in Long carbon chain Buddhist nun
Imperial particle surface improves processability with the common feeding of long carbon chain nylon particle to the equipment of melt blending.Preferably,
In order to improve the amount of the combined liquid medium of nano material, auxiliary agent can also be added.
Further scheme of the invention are as follows: the long carbon chain nylon includes the nylon that carbon atom number is greater than 10 in carbochain
Molecule, including PA11, PA12, PA1212, PA1010, PA612 or PA610.
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 oxidized praseodymium, nano yttrium oxide, nano europium oxide, nanometer tungsten oxide, nanometer silicon carbide, is received nano-cerium oxide
One of rice 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,
So that liquid medium enters 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 long carbon chain nylon is 0.1~20:100,
Preferably 1~10:100, more preferably 4:100.
The present invention also provides a kind of preparation methods of long carbon chain nylon 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 long carbon chain nylon particle, enables paste is full to be adhered to long carbon
Premix is obtained between chain nylon 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
Object.
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 long carbon chain nylon 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, compared with the prior art, nanometer made from mixing of the invention is multiple
Condensation material performance 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 gas
Change uniformly transfers heat in thermoplastic polymer and nano material；Preferably, the gasification is soft by thermoplastic polymer
Change, and reduces 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
During long carbon chain nylon plasticization temperature, liquid medium gasification separates the nano material of reunion；The liquid medium
Boiling point is lower than the plasticization temperature of long carbon chain nylon, and the boiling point is preferably not higher than 180 DEG C, and the liquid medium is preferably water；
The weight ratio of the 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 combine the higher nano material of liquid medium amount and long carbon chain nylon simultaneously
Process equipment is added, due to the lyophile media processes (forming paste) previously to nano material, so that nano material
Liquid content improves, therefore when entering long carbon chain nylon melting zone, although system temperature is already higher than the boiling point of liquid medium,
But the more melting process for making phase transformation evaporation process and long carbon chain nylon of contained liquid medium can be simultaneously between nano material gap
It carries out, just makes molten state long carbon chain nylon that can smoothly enter into the gap of nano material, and improve the impact of final products
Energy.And in the prior art, the technical solution of the nano material containing liquid, Er Qieyou are added frequently with first melting is carried out to polymer
In the undertreatment to nano material lyophile medium, so that wherein liquid medium evaporation is too fast, nano material and length are reduced
The compatibility of carbon chain nylon, so that the toughness of final products declines；On the other hand, in the prior art, first to polymer melting again
The time that nano material undoubtedly extends product preparation is added, wastes time cost.
According to above-mentioned preparation method, in step (3), premix that the paste and long carbon chain nylon particle are mixed to get
Material feeding to hot melt process equipment under the conditions of no pressure carries out melt blending.
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 long carbon chain nylon 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 long carbon
Chain nylon particles directly mix and carry out feeding, have benefited from nano material and are formd in conjunction with liquid medium with certain consistency
Paste, it is therefore prevented that slipping phenomenon, on the other hand the content of the liquid medium as contained by nano material is higher, pre-
When mixing passes through the first melting zone, liquid medium therein will not the gasification of phase transformation too early so that the long carbon chain nylon of melting can be with
It preferably 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
Surfactant, phosphate ester salt surfactant, amine salt surfactant, quaternary surfactant, heterocyclic type surface-active
Agent, nonionic surfactant, natural water soluble high molecular, one or more of synthetic water soluble high molecular and its prepolymer.
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, liquid medium gas in advance is prevented
Change evolution.Due to generating the reaction temperature of gel nano material in the present invention at room temperature, requirement to auxiliary agent
It is not high, therefore it is wider to be suitable for the invention the alternative range of auxiliary agent.
In the above method, the present invention in premix during the preparation process, using long carbon chain nylon as base-material, use compared with
The auxiliary agent of low content, its purpose is to form the environment of lyophile medium between the gap of nano material, to improve paste
The liquid content of object；High-content intercalator used in intercalation polymeric compared to the prior art, significantly reduces auxiliary agent to nanometer
The influence of composite material overall performance.
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.As benzalkonium chloride (trade name " geramine "),
Benzalkonium bromide (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, polyoxygenated
Ethylene, polyvinylpyrrolidone, polymaleic anhydride, polydimethyl diallyl ammonium chloride, polyvinylamine, poly- divinyl miaow
Oxazoline, 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 formaldehydes, 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-soluble poly-sucrose.
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 physics point to nano material
Dissipate includes but is not limited to colloid mill, ball milling, ultrasound, vortex, etching auxiliary, gas shock etc.；Preferably, the physical dispersion
For ultrasound, the frequency of the ultrasonic field is 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 long carbon chain nylon 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 long carbon chain nylon
Melt blending and carry out following process, above-mentioned mixed processing has greatly delayed the release rate of liquid medium between gap, effectively prevent
Phase transformation occurs to early in liquid medium, and on the other hand, the mixed processing of latex and paste further improves liquid medium phase
The scale that nano material gap is expanded when change is conducive to the gap realization filling that polymer travels further into nano material.
According to above-mentioned preparation method, the preparation method further includes before or during melt blending to paste and length
The weight ratio of the age resister that is added in the premix that carbon chain nylon particle is formed, the age resister and long carbon chain nylon is
0.1~1:100, preferably 0.3:100；The age resister is selected from amine antioxidants, phenolic antioxidant, thio-2 acid vinegar
One or more of kind antioxidant 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, dibutyl dithiocaarbamate
Nickel 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,
Anti-aging agent 4030, antioxidant 4010, antioxidant 4010NA, antioxidant 4020, antioxidant 264, antioxidant 1076, antioxidant
2216, antioxidant 1035, antioxidant 1010, antioxidant 3114, antioxidant 1790, antioxidant 2246,2,5- di-t-butyl hydrogen
Quinone, antioxidant TNP, Ultranox624, phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, antioxidant MB, is prevented anti-oxidant DLTP
Old agent NBC, zinc dialkyl dithiophosphate.
The present invention also provides a kind of premix, the premix includes paste and long carbon chain nylon；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 long carbon chain nylon particle surface and forms premix；Preferably, during preparing paste, successively by nano material
It is added into liquid medium and is dispersed with auxiliary agent；It is furthermore preferred that the dispersion includes ultrasound, shearing, stirring, ball milling, glue
Body mill, vortex, etching auxiliary or gas shock；It is further preferred that nano material and the adding manner of auxiliary agent include disposable
It is added and is added in batches.
The preparation method of above-mentioned long carbon chain nylon 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) it is once added in batches or into the lasting agitating solution of step (1) and helps with the speed of 0.01~100g/min
Agent, obtains paste, and 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 long carbon chain nylon 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, main feeding hopper
Revolving 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, 4th area
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 walked according to the above method
Suddenly the technique of (3).
The invention has the benefit that
1. long carbon chain nylon nanocomposite provided by the invention is in terms of mechanical property, especially bending modulus side
Face has 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 long carbon chain nylon simultaneously, composite processing is utilized
Heat in the process improves the molecular energy of the liquid medium combined between nano material gap, and liquid medium between gap is promoted to send out
Raw phase transformation, has expanded the gap of nano material, realizes filling so that the long carbon chain nylon 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 long carbon
For chain nylon simultaneously during melt-processed, the time and long carbon chain nylon that the liquid medium combined between gap is undergone phase transition are molten
Melting the time matches, and enters the gap of nano material conducive to the long carbon chain nylon of molten state and is filled；
4. nano material provided by the invention is while using liquid medium phase transformation expansion gap, also playing is prevented
The effect that nano material is reunited.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be to the technology in embodiment
Scheme is clearly and completely described, and the following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
In the present embodiment, the mass ratio of nano material and long carbon chain nylon is 16:100, and the long carbon chain nylon is selected from
PA1010, the liquid medium used for water, the auxiliary agent used for o-dichlorohenzene, the nano material used for carbon nanotube, according to
Following method prepares nanocomposite:
(1) liquid medium is stirred, while nano material is added with the speed of 3g/min and is persistently dispersed with stirring
Uniformly, the weight ratio of liquid medium and nano material is 18:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) in batches or once with the speed of 0.1g/min, obtained
Paste, the consistency of the paste are 96mm, and the weight ratio of the auxiliary agent and nano material is 20:1；
(3) paste and long carbon chain nylon 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 280 DEG C of areas, five 285 DEG C of areas, the linear velocity of screw speed are 0.8m/s.
The tensile strength for the long carbon chain nylon nanocomposite that final extruding pelletization obtains is 50MPa, and bending strength is
62MPa, impact strength 36kgcm/cm, bending modulus 1610GPa.
Embodiment 2
In the present embodiment, the mass ratio of nano material and long carbon chain nylon is 10:100, and the long carbon chain nylon is selected from
PA610, used liquid medium are trimethylpentane and water, and the mass ratio of trimethylpentane and water is 3:1, used
Auxiliary agent is polyacrylic acid and pectin, and weight ratio 1:1, the nano material used is prepared as follows for nano lanthanum oxide
Nanocomposite:
(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 85mm, and the weight ratio of the auxiliary agent and nano material is 40:1；
(3) paste and long carbon chain nylon 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 260 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 long carbon chain nylon nanocomposite that final extruding pelletization obtains is 49MPa, and bending strength is
63MPa, impact strength 37kgcm/cm, bending modulus 1590GPa.
Embodiment 3
In the present embodiment, the mass ratio of nano material and long carbon chain nylon is 0.1:100, and the long carbon chain nylon is selected from
PA612, the liquid medium used is water, and the auxiliary agent used is dicyandiamide formaldehyde resin, and the nano material used is nano oxidized
Zirconium and nano oxidized erbium, mass ratio 1:1 are prepared as follows nanocomposite:
(1) liquid medium is stirred, while nano material is added with the speed of 0.01g/min and carries out continuing stirring
It is uniformly dispersed, 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 10g/min, obtains paste, it is described
The consistency of paste is 42mm, and the weight ratio of the auxiliary agent and nano material is 50:1；
(3) paste and long carbon chain nylon 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 260 DEG C,
Two 265 DEG C of areas, three 280 DEG C of areas, four 290 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 long carbon chain nylon nanocomposite that final extruding pelletization obtains is 48MPa, and bending strength is
60MPa, impact strength 38kgcm/cm, bending modulus 1600GPa.
Embodiment 4
In the present embodiment, the mass ratio of nano material and long carbon chain nylon is 7:100, and the long carbon chain nylon is selected from
PA1010, the liquid medium used for isobutanol, adopt for polyamine epichlorohydrin resin and its prepolymer by the auxiliary agent used
Nano material is carbon nano-fiber, and the age resister used is N, N ,-di-sec-butyl-p-phenyl enediamine, as follows
Prepare nanocomposite:
(1) liquid medium is stirred, while nano material is added with the speed of 15g/min and carries out continuing stirring point
Dissipate that uniformly to apply frequency simultaneously be 800~1000Hz, power is the ultrasound of 200~1000W, liquid medium and nano material
Weight ratio is 45:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 70g/min, obtains paste, it is described
The consistency of paste is 64mm, and the weight ratio of the auxiliary agent and nano material is 5:1；
(3) paste and long carbon chain nylon 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 long carbon chain nylon nanocomposite is 51MPa, bending strength 65MPa, punching
Hit intensity is 35kgcm/cm, bending modulus 1640GPa.
Embodiment 5
In the present embodiment, the mass ratio of nano material and long carbon chain nylon is 4:100, and the long carbon chain nylon is selected from
PA1212, the liquid medium used is trifluoroacetic acid and water, and mass ratio 1:15, the auxiliary agent used is alkylphenol-polyethenoxy
Ether, the nano material used are prepared as follows nanocomposite for nano oxidized niobium:
(1) liquid medium is stirred, while nano material is added with the speed of 40g/min and carries out continuing stirring point
It dissipates 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, it is described
The consistency of paste is 37mm, and the weight ratio of the auxiliary agent and nano material is 0.8:1；
(3) paste and long carbon chain nylon 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 long carbon chain nylon nanocomposite is 52MPa, bending strength 64MPa, punching
Hit intensity is 34kgcm/cm, bending modulus 1650GPa.
Embodiment 6
In the present embodiment, the mass ratio of nano material and long carbon chain nylon is 4:100, and the long carbon chain nylon is selected from
PA610, the liquid medium used for water, the auxiliary agent used for hyaluronic acid, the nano material used for nano-sulfur, use
Age resister is antioxidant 1035, is prepared as follows nanocomposite:
(1) liquid medium is stirred, while nano material is added with the speed of 0.02g/min and carries out continuing stirring
It is uniformly dispersed, 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 0.1g/min, obtains paste, it is described
The consistency of paste is 77mm, and the weight ratio of the auxiliary agent and nano material is 2:1, further, by paste and white glue cream
Mixed processing；
(3) paste mixed with white glue cream and long carbon chain nylon 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 30Hz, and one area of extrusion temperature is 270 DEG C,
Two 265 DEG C of areas, three 290 DEG C of areas, four 280 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 long carbon chain nylon nanocomposite that final extruding pelletization obtains is 50MPa, and bending strength is
63MPa, impact strength 36kgcm/cm, bending modulus 1580GPa.
Embodiment 7
In the present embodiment, the mass ratio of nano material and long carbon chain nylon is 2:100, and the long carbon chain nylon is selected from
PA612, the liquid medium used is water and 1,2- dichloroethanes, water and 1, the mass ratio 10:1 of 2- dichloroethanes, used
Auxiliary agent is sulfo group aryl sulfonic acid compound, and the nano material used is prepared as follows nano combined material for nano boron powder
Material:
(1) liquid medium is stirred, while nano material is added with the speed of 20g/min and carries out continuing stirring point
It dissipates 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 44mm, and the weight ratio of the auxiliary agent and nano material is 16:1；
(3) paste and long carbon chain nylon 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 long carbon chain nylon nanocomposite is 49MPa, bending strength 62MPa, punching
Hit intensity is 35kgcm/cm, bending modulus 1590GPa.
Embodiment 8
In the present embodiment, the mass ratio of nano material and long carbon chain nylon is 6:100, and the long carbon chain nylon is selected from
PA1212, the liquid medium used is water, and the auxiliary agent used for sodium alginate, press for nano oxidized tellurium by the nano material used
Nanocomposite is prepared according to following method:
(1) liquid medium is stirred, while nano material is added with the speed of 0.5g/min and carries out continuing stirring point
Dissipate that uniformly to apply frequency simultaneously be 800~1000Hz, power is the ultrasound of 200~1000W, liquid medium and nano material
Weight ratio is 5.5:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 37g/min, obtains paste, it is described
The consistency of paste is 15mm, and the weight ratio of the auxiliary agent and nano material is 37:1；
(3) paste and long carbon chain nylon 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 260 DEG C,
Two 265 DEG C of areas, three 270 DEG C of areas, four 275 DEG C of areas, five 280 DEG C of areas；The linear velocity of screw speed is 0.6m/s.
The tensile strength for the long carbon chain nylon nanocomposite that final extruding pelletization obtains is 51MPa, and bending strength is
63MPa, impact strength 37kgcm/cm, bending modulus 1640GPa.
Embodiment 9
In the present embodiment, the mass ratio of nano material and long carbon chain nylon is 18:100, and the long carbon chain nylon is selected from
PA1010, the liquid medium used is water, and the auxiliary agent used is rosin amine-ethylene oxide condensate and poly N-vinyl acetyl
The mass ratio of amine, rosin amine-ethylene oxide condensate and poly N-ethylene yl acetamide is 3:1, and used nano material is to receive
Rice cerium oxide, 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 applying frequency simultaneously is 800~1000Hz, and power is the ultrasound of 200~1000W, the weight of liquid medium and nano material
Amount is than being 55:1；
(2) auxiliary agent is added into the lasting agitating solution of step (1) with the speed of 15g/min, obtains paste, it is described
The consistency of paste is 21mm, and the weight ratio of the auxiliary agent and nano material is 15:1, further, by paste and rosin
Resin emulsion mixed processing；
(3) paste mixed with rosin resin lotion and long carbon chain nylon 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 280 DEG C,
Two 285 DEG C of areas, three 290 DEG C of areas, four 290 DEG C of areas, five 280 DEG C of areas；The linear velocity of screw speed is 1m/s.
The tensile strength for the long carbon chain nylon nanocomposite that final extruding pelletization obtains is 49MPa, and bending strength is
61MPa, impact strength 38kgcm/cm, bending modulus 1630GPa.
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 long carbon chain nylon under the conditions of power pressurizes in long carbon chain nylon after melting zone by receiving containing liquid medium between gap
Rice material feeding is mixed with the long carbon chain nylon of molten state.
The difference of comparative example 1 and embodiment is: the nano material between long carbon chain nylon and gap containing liquid medium is not
Feeding simultaneously, but first feeding long carbon chain nylon and after long carbon chain nylon melting, are combined with liquid between feeding gap of pressurizeing
The nano material of medium is processed.
The tensile strength for the long carbon chain nylon nanocomposite that final extruding pelletization obtains is 39MPa, and bending strength is
55MPa, impact strength 28kgcm/cm, bending modulus 1390GPa.
Mechanics Performance Testing is carried out to Examples 1 to 9 and comparative example 1, respectively obtains tensile strength, bending strength, impact
The performance parameter of intensity and bending modulus 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, especially there is promotion by a relatively large margin in bending modulus, to find out its cause, being the phase transformation pair that the present invention utilizes liquid medium
Nano material has carried out divergence process, is filled so that entering between gap with the long carbon chain nylon that nano material melts simultaneously,
The heat that processing generates when polymer melting is utilized in divergence process between above-mentioned gap enables liquid medium evaporation generate implosion support
Gap is opened, while using the shearing force for squeezing out processing, further peeling off gap, so that molten state long carbon chain nylon 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
To be described in detail, but the present invention is not limited to the above embodiments only, without departing from the inventive concept, may be used also
To include 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 long carbon chain nylon 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 long carbon chain nylon 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 long carbon chain nylon includes carbon
Carbon atom number is greater than 10 nylon molecules, including PA11, PA12, PA1212, PA1010, PA612 or PA610 in chain.
5. composite material described in any one according to claim 1~4, which is characterized in that the nano material and Long carbon chain
The mass ratio of nylon is 0.1~20:100, preferably 1~10:100, more preferably 4:100.
6. a kind of preparation method of long carbon chain nylon 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 long carbon chain nylon particle, enables paste is full to be adhered to long carbon chain nylon
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 long carbon chain nylon 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 long carbon chain nylon, 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 long carbon chain nylon 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 long carbon chain nylon；
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 long carbon chain nylon 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|---|---|---|---|
| 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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