CN105623248A - Polyamide composite material and preparation method thereof - Google Patents
Polyamide composite material and preparation method thereof Download PDFInfo
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- CN105623248A CN105623248A CN201610003527.9A CN201610003527A CN105623248A CN 105623248 A CN105623248 A CN 105623248A CN 201610003527 A CN201610003527 A CN 201610003527A CN 105623248 A CN105623248 A CN 105623248A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- 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
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/002—Physical properties
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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Abstract
The invention is applicable to the field of composite materials and provides a polyamide composite material and a preparation method thereof. The polyamide composite material contains the following ingredients in parts by weight: 30-90 parts of polyamide, 5-50 parts of zinc oxide, 0.1-1.0 part of coupling agent, 0.1-1.0 part of antioxidant, 0-1.0 part of heat resisting agent, 0.1-2.0 parts of lubricant and 0.1-2.0 parts of dispersant, wherein zinc oxide is quadru-acicular type zinc oxide whiskers. The preparation method comprises the following steps: weighing all the ingredients according to a formula of the polyamide composite material; carrying out first mixing treatment on all the ingredients except for zinc oxide and the coupling agent, so as to obtain a first mixed material; carrying out second mixing treatment zinc oxide and the coupling agent, so as to obtain a second mixed material; charging the first mixed material from a main feeding opening of a twin-screw extruder, charging the second mixed material from a side feeding opening of the twin-screw extruder, and carrying out melt extrusion and granulation.
Description
Technical field
The invention belongs to field of compound material, particularly relate to a kind of polyamide compoiste material and preparation method thereof.
Background technology
Polyamide has good mechanical property, chemical resistance, the premium properties such as wear-resisting, heat-resisting, is widely used to the fields such as automobile, Aero-Space, chemical industry, machinery, electronic apparatus, sports equipment at present. Owing to polyamide molecule existing a large amount of hydrogen, oxygen and nitrogen-atoms, thus intermolecular easy formation hydrogen bond, improve intermolecular force, this allows for polyamide material and has the feature of high intensity, high rigidity. Additionally, polyamide also has the advantages such as wear-resistant, corrosion-resistant.
But, polyamide molecule is linear dissymmetrical structure, and its strand is flexing state, so the degree of crystallinity of polyamide material is relatively low, generally only has 25%-45%. And owing to polyamide molecule structure containing substantial amounts of amido and carbonyl, therefore, its easy and hydrone formation hydrogen bond, cause that the material using this material easily absorbs water when using and deposit, and then generation plasticization effect, ultimately result in material volume expansion, modulus declines, and obvious creep occurs under mechanical force. And if material creep resisting ability is poor, the reduction of its mechanical performance, poor dimensional stability will be made, greatly limit the application of material, be not particularly well suited for as under hot and humid environment, there is the material of relatively high-mechanical property and dimensional stability requirements. Simultaneously as polyamide material itself does not have anti-microbial property, largely limit polyamide material use in household electrical appliance, kitchen guarding and hospital of school etc. Such as the CN203729669U a kind of anti-bacteria nylon door handle related to, using public arena frequently, owing to being subject to External Force Acting for a long time, it is easy to creep occurs, thus shortening the service life of material.
At present, mainly through adding various filler and antibacterial, overcome polyamide material creep and not antibacterial deficiency, improve polyamide material physical property simultaneously. Conventional filler mostly is inorganic particle and each fibrid, and wherein, the toughness of material is had large effect by the inorganic particle such as conventional Pulvis Talci, Kaolin, improves also undesirable to the intensity of material simultaneously; And glass fibre has bigger draw ratio, although the mechanical property of material is improved a lot, but, drawing abillity is had a certain impact by the interpolation of glass fibre, easily produces stress warpage, deforms and reduces product surface glossiness during relatively big especially for product, structure is more complicated product. And presently used antibacterial is relatively costly, is unfavorable for the control of composite cost.
Summary of the invention
It is an object of the invention to provide a kind of polyamide compoiste material with performances such as high mechanical properties, low creep, antibacterial, wear-resistant, heat-resisting, corrosion-resistant, good stability of the dimension, damping, noise reductions, it is intended to solve existing polyamide material creep-resistant property and the problem of anti-microbial property difference.
Another object of the present invention is to the preparation method that a kind of polyamide compoiste material is provided.
The present invention is achieved in that a kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
And, the preparation method of a kind of polyamide compoiste material, comprise the following steps:
Each component is weighed according to the formula of described polyamide compoiste material;
All components except zinc oxide and coupling agent is carried out the first mixed processing, obtains the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
Described first mixed material is added from side spout from the main spout charging of double screw extruder, described second mixed material, melt extrudes, pelletize.
Polyamide compoiste material provided by the invention, with the addition of four-needle-like zinc oxide component, described four-needle-like zinc oxide non-structure defect, its intensity is high, there is strengthening and toughening performance and the anti-microbial property of excellence, improve the intensity of polyamide material, creep-resistant property and anti-microbial property simultaneously. Concrete, owing to described four acicular type zinc oxide crystal whisker microcosmic is three-dimensional four needle-like stereochemical structures, namely whisker has a core, stretching out four acicular crystals from core radial direction, every spicule is monocrystal microfibre, and the angle of wantonly two spicules is 109 ��, centrosome diameter 0.7-1.4 ��m of whisker, spicule root diameter (RD) 0.5-14 ��m, spicule length is 3-200 ��m, has special stereoeffect. Described four-needle-like zinc oxide component is because of the solid four needle-like three dimensional structure of its uniqueness, it is easy to realize being uniformly distributed in matrix material, thus isotropically improving the physical property of material; Simultaneously because its four acicular texture, polyamide molecule chain in composite can consolidate winding on its four pins, each mutually homogeneous, eliminate the strand sliding in each direction, thus inherently and efficiently solving the creep of nylon, the creep-resistant property making polyamide compoiste material is remarkably reinforced, even if under hot and humid environment, also can have excellent mechanical performance and dimensional stability. Meanwhile, described four acicular type zinc oxide crystal whisker has good antibacterial action, it is possible to for kitchen guarding, public arena and the household electrical appliance product that such as the antibacterial requirement such as gear, valve, door handle, sports equipment, automobile component is higher, have good development prospect.
Polyamide compoiste material provided by the invention, there is good creep resistance, in use long-term stress and indeformable, also there is antibacterial ability simultaneously, it is prevented from antibacterial, viral growing and propagate, it is possible to for kitchen guarding's (such as washing machine, bowl components), public arena and hospital's communal facility and armarium (such as gear, valve, handle) etc.; Polyamide compoiste material provided by the invention, there is good damping property, absorbing property, thermostability, dimensional stability simultaneously, can be used in auto parts and components (such as engine bonnet, valve chamber cover, accelerator pedal etc.), apply also for electric tool and sports equipment simultaneously. Additionally, polyamide compoiste material provided by the invention, also there is the performances such as excellent mechanical strength, wear-resistant, corrosion-resistant, easy processing, and with low cost, have broad application prospects, it is possible to multi-field application, be particularly suited for household electrical appliances and kitchen products.
The preparation method of polyamide compoiste material provided by the invention, make as a whole after zinc oxide, coupling agent are sufficiently mixed, feeding is carried out from different spouts from the mixture that other compositions are formed, can ensure that described zinc oxide and coupling agent are fully dispersed uniformly, thus obtaining the joint product of function admirable. Additionally, the preparation method of polyamide compoiste material provided by the invention, only carry out melt granulation after each component need to be carried out mixed processing, simple to operate controlled, and melt granulation technical maturity, it is easy to accomplish industrialization.
Detailed description of the invention
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated. Should be appreciated that specific embodiment described herein is only in order to explain the present invention, is not intended to limit the present invention.
Embodiments provide a kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
Concrete, described polyamide, as the main body of embodiment of the present invention polyamide compoiste material, gives composite material high strength degree, high rigidity, advantage wear-resistant, corrosion resistant. In the embodiment of the present invention, described polyamide is a kind of of PA6, PA66 or two kinds of mixture formed. As the presently preferred embodiments, in order to obtain good mobility, high intensity, the superperformance such as wear-resistant, high temperature resistant, it is PA6, PA66 of 2.0-2.8 that described polyamide selects relative density to be 1.12-1.15, relative viscosity. In the embodiment of the present invention, the content of described polyamide is 30-90 part, can be the concrete numbers such as 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, 90 parts.
In the embodiment of the present invention, described zinc oxide four acicular type zinc oxide crystal whisker. Described ZnOw microstructure is three-dimensional four needle-like stereochemical structures, namely whisker has a core, four acicular crystals are stretched out from core radial direction, the angle of wantonly two spicules is 109 ��, centrosome diameter 0.7-1.4 ��m of whisker, spicule root diameter (RD) 0.5-14 ��m, spicule length is 100-200 ��m. As the presently preferred embodiments, described four acicular type zinc oxide crystal whisker is the monocrystalline ZnOw that dislocation is little, lattice defect is few. In the embodiment of the present invention, the impurity content of described zinc oxide is few, purity >=99.95%, thus ensure that giving full play to of its function, respectively reaches 1.0 �� 10 as having high mechanical strength and elastic modelling quantity, hot strength and elastic modelling quantity4MPa and 3.5 �� 105MPa. Simultaneously because described ZnOw has the solid four needle-like three dimensional structure of uniqueness, described ZnOw is made to be capable of being uniformly distributed in matrix material, thus isotropy ground improves the physical property of material, give the various special performance of composite, as strengthened, wear-resisting, antibacterial, damping, noise reduction, suction ripple, the performance such as antistatic. Additionally, due to the three-dimensional four needle-like three dimensional structures of described zinc oxide uniqueness, on the pin being wrapped in its different directions that described polyamide molecule can be stable, owing to the angle between every pin is fixed as 109 ��, so polyamide molecule can be fixed up by more stable, thus after avoiding water suction, under the lubrication of hydrone, described polyamide molecule chain occur bigger sliding or strand to relax under external force, cause material generation creep, and then generating material deformation, affect it and use.
ZnOw described in the embodiment of the present invention also has excellent anti-microbial property, and described ZnOw can reach high-efficiency antimicrobial performance by photocatalysis antibacterial and two kinds of approach of contact sterilization. Concrete: owing to described ZnOw has stronger photo-catalysis capability, after ultra-vioket radiation, electrons in described zinc oxide valence band is energized into conduction band, form the hole of electronegative electronics and the positively charged moved freely, this hole and reactions such as being adsorbed on the oxygen of material surface, hydroxyl and water produce hydroxyl, negative oxygen ion and hydrogen peroxide etc. and have hydroxyl radical free radical and the active oxygen ion of reduction so that air and the oxygen in water become active oxygen. Active oxygen has extremely strong oxidation activity, they can react with the Organic substance (such as: hydroxyl etc.) in multiple-microorganism, multiple organic compound of degrading, and destroys the multiplication capacity of bacterial cell, and suppress or kill antibacterial, i.e. photocatalysis antibacterial. Contact sterilization refers to zinc oxide slow releasing zinc ion in moisture medium, and zinc ion little by little dissociates out. Owing to zinc ion has oxidation-reduction quality, when combining with bacterial cell membrane, zinc ion and Organic substance therein react, and can destroy the structure of memebrane protein so that it is lose activity, and reach sterilization purpose. Additionally, the hole on described ZnOw surface can produce electronics, directly participating in reaction, number of cavities is more many will produce more electronics, and its sterilizing ability is increased by. ZnOw described in the embodiment of the present invention can play antibacterial and two kinds of performances of sterilization simultaneously, and mutually play synergism, give described polyamide compoiste material height anti-microbial property, make described polyamide compoiste material be applicable to the aspects such as kitchen guarding, public arena equipment and household electrical appliance to use, guarantee equipment does not produce antibacterial when using and deposit, and is conducive to life health.
In the embodiment of the present invention, the content of described zinc oxide is relatively big to the influential effect of the present invention, when the content of described zinc oxide is very few, it is impossible to play creep resistant and anti-microbial property; When described zinc oxide content is too much, on the one hand, creep resistant and the anti-microbial property of its performance are saturated, it is difficult to further improve; On the other hand, add too much zinc oxide, can cause that its structure is destroyed in the course of processing, reduce creep resistant and anti-microbial property on the contrary. In view of this, in the embodiment of the present invention, the content of described zinc oxide is 5-50 part, can be the concrete numbers such as 5 parts, 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts.
In the embodiment of the present invention, in order to improve the compatibility between each component of composite, with the addition of coupling agent. As the presently preferred embodiments, described coupling agent is silane coupler. Further, described coupling agent is preferably gamma-aminopropyl-triethoxy-silane. Described ZnOw surface can be carried out surface treatment by this preferred coupling agent, thus the compatibility improved between described ZnOw and polyamide, and then produce firmly two-phase interface, improve the mechanical performance of material. In the embodiment of the present invention, the content of described coupling agent is 0.1-1.0 part, can be the concrete numbers such as 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1.0 parts.
In the embodiment of the present invention, bring impact to prevent the oxidation of composite to be used for the life-span, with the addition of antioxidant. As the presently preferred embodiments, described antioxidant is Hinered phenols antioxidant, it is preferred that N, N-1,6-methylene-two-[3,5-di-t-butyl-4-hydroxy benzenes propionic acid amide .]. Described polyamide not degradation can effectively be protected by this preferred antioxidant in the course of processing, it is to avoid material property declines. In the embodiment of the present invention, the content of described antioxidant is 0.1-1.0 part, can be the concrete numbers such as 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1.0 parts.
In the embodiment of the present invention, in order to improve the heat resistance of composite, with the addition of heat-resistant agent. As the presently preferred embodiments, described heat-resistant agent is the mixture of cupric antioxidant and synergist. Wherein, the copper ion in described cupric antioxidant and described polyamide bond chelating form more stable structure, described synergist be can the material of reinforced polyamide key Stability of Chelate, include but not limited to potassium iodide. By preferred described heat-resistant agent, copper ion forms amido link chelate with described polyamide bond chelating, described synergist such as potassium iodide can coordinate the stability of reinforced polyamide key chelate with copper simultaneously, described polyamide is made to be not easy to when the attack of the oxygen groups that is heated fracture degraded, thus ensureing that composite is in the stability of hot environment Middle molecule chain for a long time, it is to avoid material embrittlement. In the embodiment of the present invention, the content of described heat-resistant agent is 0-1.0 part, can be the concrete numbers such as 0.01 part, 0.05 part, 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1.0 parts.
In the embodiment of the present invention, in order to improve the processing type between each component of composite, with the addition of lubricant. As the presently preferred embodiments, the described lubricant mixture of one or more in stearate, silicone. It is preferred that pentaerythritol stearic acid ester 2. This preferred lubricant has good heat resistance, the polyamide course of processing is not decomposed, the compatibility of described pentaerythritol stearic acid ester 2 and described polyamide is good simultaneously, the lubricant effect having concurrently inside and outside playing, the melted of each component can be promoted, it is efficiently modified described Composite Melt mobility, reduces the friction between melt and equipment in the course of processing. Described pentaerythritol stearic acid ester 2 molecular weight is relatively big simultaneously, will not precipitate out, without influence on materials'use and product appearance, additionally aid the demolding performace of material simultaneously in follow-up use procedure. In the embodiment of the present invention, the content of described lubricant is 0.1-2.0 part, can be the concrete numbers such as 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1.0 parts, 1.2 parts, 1.5 parts, 1.8 parts, 2.0 parts.
In the embodiment of the present invention, in order to promote the dispersion of described zinc oxide, thus ensureing that it gives full play to its effect, with the addition of dispersant in the composite. As the presently preferred embodiments, described dispersant is at least one in montanin wax, ethylene bis stearic acid amide. Further, the brown coal cerinic acid-1-methyl isophthalic acid in the preferred montanin wax of described dispersant, the blend of 3-glyceryl ester and fatty acid-lignite wax calcium salt. Preferred described dispersant can be effectively improved four acicular type zinc oxide crystal whisker peptizaiton in described polyamide substrate resin, it is ensured that the uniform and stable property of material, improves the physical property of material. In the embodiment of the present invention, the content of described dispersant is 0.1-2.0 part, can be the concrete numbers such as 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1.0 parts, 1.2 parts, 1.5 parts, 1.8 parts, 2.0 parts.
In the embodiment of the present invention, described polyamide compoiste material can also add other auxiliary agents according to actual needs.
The polyamide compoiste material that the embodiment of the present invention provides, with the addition of four-needle-like zinc oxide component, described four-needle-like zinc oxide non-structure defect, its intensity is high, there is strengthening and toughening performance and the anti-microbial property of excellence, improve the intensity of polyamide material, creep-resistant property and anti-microbial property simultaneously. Concrete, owing to described four acicular type zinc oxide crystal whisker microcosmic is three-dimensional four needle-like stereochemical structures, namely whisker has a core, stretching out four acicular crystals from core radial direction, every spicule is monocrystal microfibre, and the angle of wantonly two spicules is 109 ��, centrosome diameter 0.7-1.4 ��m of whisker, spicule root diameter (RD) 0.5-14 ��m, spicule length is 3-200 ��m, has special stereoeffect. Described four-needle-like zinc oxide component is because of the solid four needle-like three dimensional structure of its uniqueness, it is easy to realize being uniformly distributed in matrix material, thus isotropically improving the physical property of material; Simultaneously because its four acicular texture, polyamide molecule chain in composite can consolidate winding on its four pins, each mutually homogeneous, eliminate the strand sliding in each direction, thus inherently and efficiently solving the creep of nylon, the creep-resistant property making polyamide compoiste material is remarkably reinforced, even if under hot and humid environment, also can have excellent mechanical performance and dimensional stability. Meanwhile, described four acicular type zinc oxide crystal whisker has good antibacterial action, it is possible to for kitchen guarding, public arena and the household electrical appliance product that such as the antibacterial requirement such as gear, valve, door handle, sports equipment, automobile component is higher, have good development prospect.
The polyamide compoiste material that the embodiment of the present invention provides, there is good creep resistance, in use long-term stress and indeformable, also there is antibacterial ability simultaneously, it is prevented from antibacterial, viral growing and propagate, it is possible to for kitchen guarding's (such as washing machine, bowl components), public arena and hospital's communal facility and armarium (such as gear, valve, handle) etc.; The polyamide compoiste material that the embodiment of the present invention provides, there is good damping property, absorbing property, thermostability, dimensional stability simultaneously, can be used in auto parts and components (such as engine bonnet, valve chamber cover, accelerator pedal etc.), apply also for electric tool and sports equipment simultaneously. Additionally, the polyamide compoiste material that the embodiment of the present invention provides, also there is the performances such as excellent mechanical strength, wear-resistant, corrosion-resistant, easy processing, and it is with low cost, have broad application prospects, it is possible to multi-field application, be particularly suited for household electrical appliances and kitchen products.
The polyamide compoiste material that the embodiment of the present invention provides can be prepared by following method.
Accordingly, the preparation method embodiments providing a kind of polyamide compoiste material, comprise the following steps:
S01. each component is weighed according to the formula of described polyamide compoiste material;
S02. all components except zinc oxide and coupling agent is carried out the first mixed processing, obtain the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
S03. described first mixed material is added from side spout from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize.
Concrete, in above-mentioned steps S01, the recipe ingredient of described polyamide compoiste material and preferable case thereof as described above, in order to save length, repeat no more herein.
In above-mentioned steps S02, described first mixed processing is by mix homogeneously such as polyamide, antioxidant, heat-resistant agents, and concrete, the first mixed processing mode includes but not limited to high-speed mixer mixing 1-5 minute, uniform to protect material mixing; Described zinc oxide and described coupling agent are sufficiently mixed by described second mixed processing, concrete, described second mixed processing mode includes but not limited to: described ZnOw is added high-speed mixer, temperature 75 DEG C, described coupling agent is joined in powder body in the way of sprinkling, mix 10-20 minute, to guarantee that described coupling agent is evenly coated at described ZnOw surface, described ZnOw is carried out surface modification simultaneously. Wherein, adopt the mode sprayed to add coupling agent, fully dispersed when being conducive to described coupling agent in subsequent steps with described first mixing of materials mix.
In above-mentioned steps S03, described first mixed material is added from the main spout charging of double screw extruder, described second mixed material from side spout such as five side, district spouts, it is possible to by fully dispersed uniformly to described zinc oxide and coupling agent and described first mixed material. As the presently preferred embodiments, the described process conditions that melt extrude are: temperature 180-210 DEG C of a district, two temperature 220-250 DEG C of districts, three temperature 230-280 DEG C of districts, four temperature 240-290 DEG C of districts, five temperature 240-295 DEG C of districts, six temperature 240-290 DEG C of districts, seven temperature 230-280 DEG C of districts, eight temperature 220-280 DEG C of districts, nine temperature 200-290 DEG C of districts. This preferred melt zone temperature can guarantee that described polyamide is fully melted, reduces melt strength; Meanwhile, after adding described ZnOw, contribute to the dispersion of described ZnOw, protect its four acicular texture not to be destroyed in the course of processing, it is ensured that the mechanical property of material simultaneously.
The preparation method of the polyamide compoiste material that the embodiment of the present invention provides, make as a whole after zinc oxide, coupling agent are sufficiently mixed, feeding is carried out from different spouts from the mixture that other compositions are formed, can ensure that described zinc oxide and coupling agent are fully dispersed uniformly, thus obtaining the joint product of function admirable. Additionally, the preparation method of polyamide compoiste material provided by the invention, only carry out melt granulation after each component need to be carried out mixed processing, simple to operate controlled, and melt granulation technical maturity, it is easy to accomplish industrialization.
Below in conjunction with specific embodiment, the invention will be further described. The scope of the present invention is not restricted by the embodiments.
In the polyamide compoiste material that the embodiment of the present invention and comparative example provide, polyamide can be PA6 and/or PA66, and relative density is that 1.13-1.15, PA6 fusing point is 215-225 DEG C, and PA66 fusing point is 255-265 DEG C, and relative viscosity is 2.0-2.5; The four acicular type zinc oxide crystal whisker of the trade mark T-ZnOw that described four acicular type zinc oxide crystal whisker can produce for PANASONIC; Glass fibre is alkali-free short glass fiber, the short glass fiber that the trade mark is ECS301HP that concretely the multiple material in Chongqing produces; Described heat-resistant agent can for the mixture of the cupric antioxidant of the Lv Geman trade mark H3373 produced and synergist; Described antioxidant can be suffocated amine antioxidant, concretely for the suffocated amine antioxidant of BASF AG's product (trade mark is 1098); Described lubricant can be pentaerythritol stearate, concretely sends out the pentaerythritol stearate that the trade mark is PETS-AHS that base produces; Described dispersant can be montanin wax, the montanin wax that the trade mark is OPwax that concretely Clariant produces.
Embodiment 1
A kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
S11. each component is weighed according to the formula of described polyamide compoiste material;
S22. all components except zinc oxide and coupling agent is carried out the first mixed processing, obtain the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
S13. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 180 DEG C, two district's temperature 220 DEG C, three district's temperature 230 DEG C, four district's temperature 240 DEG C, five district's temperature 240 DEG C, six district's temperature 240 DEG C, seven district's temperature 230 DEG C, eight district's temperature 220 DEG C, nine district's temperature 240 DEG C.
Embodiment 2
A kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
S21. each component is weighed according to the formula of described polyamide compoiste material;
S22. all components except zinc oxide and coupling agent is carried out the first mixed processing, obtain the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
S23. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 180 DEG C, two district's temperature 230 DEG C, three district's temperature 240 DEG C, four district's temperature 250 DEG C, five district's temperature 250 DEG C, six district's temperature 220 DEG C, seven district's temperature 210 DEG C, eight district's temperature 200 DEG C, nine district's temperature 250 DEG C.
Embodiment 3
A kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
S31. each component is weighed according to the formula of described polyamide compoiste material;
S32. all components except zinc oxide and coupling agent is carried out the first mixed processing, obtain the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
S33. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 200 DEG C, two district's temperature 220 DEG C, three district's temperature 235 DEG C, four district's temperature 250 DEG C, five district's temperature 260 DEG C, six district's temperature 270 DEG C, seven district's temperature 260 DEG C, eight district's temperature 240 DEG C, nine district's temperature 270 DEG C.
Embodiment 4
A kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
S41. each component is weighed according to the formula of described polyamide compoiste material;
S42. all components except zinc oxide and coupling agent is carried out the first mixed processing, obtain the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
S43. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 180 DEG C, two district's temperature 210 DEG C, three district's temperature 230 DEG C, four district's temperature 250 DEG C, five district's temperature 260 DEG C, six district's temperature 250 DEG C, seven district's temperature 240 DEG C, eight district's temperature 220 DEG C, nine district's temperature 260 DEG C.
Embodiment 5
A kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
S51. each component is weighed according to the formula of described polyamide compoiste material;
S52. all components except zinc oxide and coupling agent is carried out the first mixed processing, obtain the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
S53. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 220 DEG C, two district's temperature 240 DEG C, three district's temperature 260 DEG C, four district's temperature 290 DEG C, five district's temperature 295 DEG C, six district's temperature 295 DEG C, seven district's temperature 280 DEG C, eight district's temperature 270 DEG C, nine district's temperature 260 DEG C.
Embodiment 6
A kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
S61. each component is weighed according to the formula of described polyamide compoiste material;
S62. all components except zinc oxide and coupling agent is carried out the first mixed processing, obtain the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
S63. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 210 DEG C, two district's temperature 230 DEG C, three district's temperature 250 DEG C, four district's temperature 260 DEG C, five district's temperature 280 DEG C, six district's temperature 270 DEG C, seven district's temperature 260 DEG C, eight district's temperature 230 DEG C, nine district's temperature 280 DEG C.
Embodiment 7
A kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
S71. each component is weighed according to the formula of described polyamide compoiste material;
S72. all components except zinc oxide and coupling agent is carried out the first mixed processing, obtain the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
S73. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 180 DEG C, two district's temperature 230 DEG C, three district's temperature 250 DEG C, four district's temperature 270 DEG C, five district's temperature 280 DEG C, six district's temperature 260 DEG C, seven district's temperature 240 DEG C, eight district's temperature 220 DEG C, nine district's temperature 280 DEG C.
Embodiment 8
A kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
S81. each component is weighed according to the formula of described polyamide compoiste material;
S82. all components except zinc oxide and coupling agent is carried out the first mixed processing, obtain the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
S83. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 220 DEG C, two district's temperature 240 DEG C, three district's temperature 260 DEG C, four district's temperature 280 DEG C, five district's temperature 295 DEG C, six district's temperature 275 DEG C, seven district's temperature 275 DEG C, eight district's temperature 275 DEG C, nine district's temperature 290 DEG C.
Comparative example 1
A kind of polyamide compoiste material, including the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
D11. each component is weighed according to the formula of described polyamide compoiste material;
D12. all components except zinc oxide is carried out the first mixed processing, obtain the first mixed material; Zinc oxide is carried out the second mixed processing, obtains the second mixed material;
D13. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 200 DEG C, two district's temperature 220 DEG C, three district's temperature 235 DEG C, four district's temperature 240 DEG C, five district's temperature 250 DEG C, six district's temperature 240 DEG C, seven district's temperature 230 DEG C, eight district's temperature 220 DEG C, nine district's temperature 250 DEG C.
Comparative example 2
A kind of polyamide compoiste material, including the following component of following parts by weight:
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
D21. each component is weighed according to the formula of described polyamide compoiste material;
D22. all components except zinc oxide is carried out the first mixed processing, obtain the first mixed material; Zinc oxide is carried out the second mixed processing, obtains the second mixed material;
D23. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 180 DEG C, two district's temperature 210 DEG C, three district's temperature 230 DEG C, four district's temperature 250 DEG C, five district's temperature 270 DEG C, six district's temperature 250 DEG C, seven district's temperature 230 DEG C, eight district's temperature 220 DEG C, nine district's temperature 250 DEG C.
Comparative example 3
A kind of polyamide compoiste material, including the following component of following parts by weight:
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
D31. each component is weighed according to the formula of described polyamide compoiste material;
D32. all components except zinc oxide is carried out the first mixed processing, obtain the first mixed material; Zinc oxide is carried out the second mixed processing, obtains the second mixed material;
D33. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 220 DEG C, two district's temperature 240 DEG C, three district's temperature 260 DEG C, four district's temperature 280 DEG C, five district's temperature 270 DEG C, six district's temperature 260 DEG C, seven district's temperature 260 DEG C, eight district's temperature 260 DEG C, nine district's temperature 280 DEG C.
Comparative example 4
A kind of polyamide compoiste material, including the following component of following parts by weight:
The preparation method of above-mentioned polyamide compoiste material, comprises the following steps:
D41. each component is weighed according to the formula of described polyamide compoiste material;
D42. all components except zinc oxide is carried out the first mixed processing, obtain the first mixed material; Zinc oxide is carried out the second mixed processing, obtains the second mixed material;
D43. described first mixed material is added from five side, district spouts from the main spout charging of double screw extruder, described second mixed material, melt extrude, pelletize, wherein, one district's temperature 230 DEG C, two district's temperature 250 DEG C, three district's temperature 270 DEG C, four district's temperature 290 DEG C, five district's temperature 270 DEG C, six district's temperature 250 DEG C, seven district's temperature 230 DEG C, eight district's temperature 230 DEG C, nine district's temperature 280 DEG C.
The polyamide compoiste material of embodiment 1-8 and comparative example 1-4 gained is carried out performance test, the test result of its impact strength, hot strength, bending strength, anti-microbial property and fungicidal properties such as table 1 below, the test result of its creep-resistant property such as table 2 below. Wherein, what deserves to be explained is, numerical values recited and the anti-microbial property of antibacterial activity value are directly proportional, and namely numerical value is more big, represent that anti-microbial property is more good; The numerical value of mildew-resistant grade is more little then represents that fungicidal properties is more good; Melt flows direction time laterally for being perpendicular to injection moulding, longitudinal direction is for being parallel to melt flows direction.
Table 1
Table 2
From the above 1 and the test result of comparative example 1 known, after it is carried out surface treatment (surface modification) by described four acicular type zinc oxide crystal whisker coupling agent, the surface modification four acicular type zinc oxide crystal whisker obtained and polyamide have better boundary strength, impact flexibility and the hot strength of material all improve a lot, and the creep-resistant property of material is also improved simultaneously.
From the above 2 and the test result of comparative example 2, it is found that the addition of described four acicular type zinc oxide crystal whisker, greatly improve material mechanical performance, anti-microbial property and creep-resistant property.
The relatively test result of the above embodiments 5 and comparative example 3, it appeared that, the physical property of the mechanical property of described four acicular type zinc oxide crystal whisker reinforced polyamide and the glass-fiber-reinforced polyamide of equal number is suitable, but the polyamide compoiste material that described four acicular type zinc oxide crystal whisker strengthens has excellent anti-microbial property. Simultaneously, owing to its four acicular texture is horizontal, longitudinal creep-resistant property is all excellent, therefore, the polyamide compoiste material that the embodiment of the present invention 5 provides is respectively provided with good creep-resistant property under different temperatures, different humidity, different force, and comparative example 3 adopts the polyamide compoiste material that glass fibre obtains, only close with the creep-resistant property of ZnOw in a longitudinal direction, horizontal direction is substantially much lower.
The relatively test result of above-described embodiment 7 and comparative example 4, it appeared that, adopt 40 parts of four acicular type zinc oxide crystal whisker reinforced polyamide composites, longitudinal creep resistant that its longitudinal creep-resistant property relatively adopts 40 parts of glass fiber-reinforced polyamide composite materials is on the low side on the contrary, this is excessive mainly due to the addition of ZnOw, in the course of processing, four acicular textures are destroyed, and cause that the creep-resistant property of material is on the low side.
From embodiment 1-8 and comparative example test result, the addition of four-needle-like zinc oxide can improve anti-microbial property and the anti-fungi performance of material greatly, and along with the addition of four acicular type zinc oxide crystal whisker increases, antibacterial and anti-fungi performance improves therewith, this mainly due to four acicular type zinc oxide crystal whisker itself as antibacterial. But addition more than 30 parts after, anti-microbial property promotes little;
The impact flexibility of described polyamide compoiste material and hot strength all improve with the addition of four acicular type zinc oxide crystal whisker and improve. But when addition to 30 part, impact and stretching reaches maximum, when improving the addition of four acicular type zinc oxide crystal whisker again, the physical property of material begins to decline on the contrary, when this is mainly the addition of ZnOw to 30 parts, reach capacity, if continue to improve ZnOw, ZnOw is too much, causes that in the course of processing, material melt intensity is excessive, this makes ZnOw acicular texture be more easily damaged so that four pins are easily broken off;
The processing temperature improving front 6th district can make material molten plasticizing more abundant, reduces melt strength simultaneously, four acicular type zinc oxide crystal whisker acicular texture in the course of processing can be protected preferably not to be destroyed.
Polyamide compoiste material of the present invention has excellent mechanical property, creep-resistant property, anti-microbial property, heat resistance, abrasion resistance properties etc., can meet the requirement of the aspects such as gear, medical apparatus and instruments, communal facility, automobile component, electric tool, sports equipment.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent replacement and improvement etc. made within the spirit and principles in the present invention, should be included within protection scope of the present invention.
Claims (10)
1. a polyamide compoiste material, it is characterised in that include the following component of following parts by weight:
Wherein, described zinc oxide is four acicular type zinc oxide crystal whisker.
2. polyamide compoiste material as claimed in claim 1, it is characterised in that described four acicular type zinc oxide crystal whisker is monocrystalline ZnOw.
3. polyamide compoiste material as claimed in claim 1, it is characterised in that purity >=99.95% of described zinc oxide.
4. the polyamide compoiste material as described in as arbitrary in claim 1-3, it is characterised in that described coupling agent is silane coupler.
5. polyamide compoiste material as claimed in claim 4, it is characterised in that described coupling agent is gamma-aminopropyl-triethoxy-silane.
6. the polyamide compoiste material as described in as arbitrary in claim 1-3, it is characterised in that described antioxidant is Hinered phenols antioxidant.
7. the polyamide compoiste material as described in as arbitrary in claim 1-3, it is characterised in that described heat-resistant agent is the mixture of cupric antioxidant and synergist.
8. the polyamide compoiste material as described in as arbitrary in claim 1-3, it is characterised in that described dispersant is at least one in montanin wax, ethylene bis stearic acid amide.
9. a preparation method for polyamide compoiste material, comprises the following steps:
Each component is weighed according to the formula of the arbitrary described polyamide compoiste material of claim 1-8;
All components except zinc oxide and coupling agent is carried out the first mixed processing, obtains the first mixed material; Zinc oxide and coupling agent are carried out the second mixed processing, obtains the second mixed material;
Described first mixed material is added from side spout from the main spout charging of double screw extruder, described second mixed material, melt extrudes, pelletize.
10. the preparation method of polyamide compoiste material as claimed in claim 9, it is characterized in that, the described process conditions that melt extrude are: temperature 180-210 DEG C of a district, two temperature 220-250 DEG C of districts, three temperature 230-280 DEG C of districts, four temperature 240-290 DEG C of districts, five temperature 240-295 DEG C of districts, six temperature 240-290 DEG C of districts, seven temperature 230-280 DEG C of districts, eight temperature 220-280 DEG C of districts, nine temperature 200-290 DEG C of districts.
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