CN101230195A - Nylon composite material and preparation method thereof - Google Patents
Nylon composite material and preparation method thereof Download PDFInfo
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- CN101230195A CN101230195A CNA2008100259010A CN200810025901A CN101230195A CN 101230195 A CN101230195 A CN 101230195A CN A2008100259010 A CNA2008100259010 A CN A2008100259010A CN 200810025901 A CN200810025901 A CN 200810025901A CN 101230195 A CN101230195 A CN 101230195A
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Abstract
The invention discloses nylon composite material and a preparation method thereof. The material is composed of nylon 66 slices, thermotropic liquid crystalline polymer, needle-like mineral fiber, coupling agent and antioxidant. The weight ratio of the nylon 66 slices, the thermotropic liquid crystalline polymer, the needle-like mineral fiber, the coupling agent and the antioxidant is 60-70: 10-15: 20-30: 4.5: 0.5. The preparation method comprises the following steps: the nylon 66 slices, the thermotropic liquid crystalline polymer, the needle-like mineral fiber, the coupling agent and the antioxidant with weight ratio of 60-70: 10-15: 20-30: 4.5: 0.5 are mixed evenly under the agitating condition, and then extruded, drawn and granulated at 280 DEG C or 295 DEG C, and molded by injection into the sample to obtain the nylon system composite material. The nylon system of the invention can attain the remarkable enhancement effect under the circumstance of a little thermotropic liquid crystalline, and can have the effects on lightening the warping of the product, reducing the roughness of the product surface and reducing the cost.
Description
Technical field
The present invention relates to nylon composite materials, particularly relate to a kind of nylon composite materials that contains TLCP and needle-like mineral filler and preparation method thereof.
Background technology
TLCP is owing to the polymer segment crystalline texture that added heat collapse and makes non-crystal structure enter molten state to be certain ordered arrangement and liquid crystal state occurs.It is a kind of novel high performance polymer material, be characterized in modulus height, intensity height, under liquid crystal state, present distinctive easy mobility, good thermostability, chemical proofing and weathering resistance, outstanding solvent resistance, excellent comprehensive performances such as lower linear expansivity and density.Utilize the characteristics of TLCP,, can improve the performance of thermoplastic engineering plastic itself and thermoplastic engineering plastic blending and modifying.In TLCP one thermoplastic engineering plastic blending modification system, TLCP has three kinds of obviously effects: the 1. effect of toughener, and the fibrillation surface of formation and length-to-diameter ratio are than the height of common fortifying fibre, thereby reinforced effects is very remarkable; 2. process the effect of flow ability modifying agent, can reduce the viscosity of blend melt, improve the flowability and the moulding processability of unmanageable thermoplastics; 3. save the forming process energy consumption.
In the modification of nylon 66, use TLCP can obviously improve comprehensive mechanical property, but its reinforced effects all falls far short from Theoretical Calculation at present, analyzes reason and is TLCP in matrix resin, is not fibrous arrangement fully.Develop a kind of matrix material for this reason, make TLCP can in nylon resin, become fine preferably, thereby obtain good reinforced effects, and reduce the consumption of thermotropic liquid crystal, reduce cost.Making TLCP enhanced nylon product to be accepted by market, drop into practical application as early as possible, is highly significant.
The needle-like mineral filler is natural mineral or the man-made mineral fiber that a class has high length-to-diameter ratio, length-to-diameter ratio is more than 20: 1, come the existing report of modified thermoplastic engineering plastics as filler, it mainly contains following advantage: 1. enhancement can strengthen the mechanical property of matrix resin significantly.2. Heat stability is good, thermal distortion is low, the product size good stability, these all are better than the fiber glass packing of using equally in the nylon of being everlasting.3. the product surface glossiness will be higher than the glass filling, and less to the wearing and tearing of processor in the processing.4. can alleviate the warpage properties of goods, improve the goods resistance toheat, reduce nylon products water absorbability etc.Itself and TLCP coupling are improved the become fine situation of TLCP in nylon resin report is not arranged.This needle-like mineral filler can interact with TLCP, produces synergistic effect, improves the fine effect of one-tenth of TLCP, and can significantly improve the over-all properties of matrix material.
Chinese patent 03126409.3 discloses a kind of matrix material that contains granular filler and TLCP, and its preparation method is with granular fillers such as hollow glass micro-ball and the complete fragrant liquid crystalline polymer blend modification of main chain, at 260～280 ℃ of following extruding pelletizations; Thereby the matrix material that acquisition has good dimensional stability, this matrix material can be used for making the meticulous plastic part of structure.
Chinese patent CN1168395A discloses liquid crystalline polymers and oxy-poly-arylene sulfide mixed and modified, has the material of good anti-nonferromagnetic substance with preparation, and this material can be used for making parts such as gear, tooth bar, bearing.
Chinese patent CN1454934 discloses polyamide 66 through polynite and the collaborative matrix material of filling of wollastonite and preparation method thereof.This matrix material modulus height, heat resistance is good, has reduced cost simultaneously again.But difficulty of processing is bigger, and is more serious to the wearing and tearing of processing machine.
But above three patents are not to be used to prepare the nylon composite materials that contains TLCP and needle-like mineral fibre.Prepare nylon composite materials of the present invention if directly use for reference above-mentioned patent, the direct compatibility problem of each component can't solve, and will cause being separated, and composite property obviously descends.
Summary of the invention
The object of the present invention is to provide a kind of advantageous property that utilizes TLCP, the needle-like mineral filler is good strengthens the property and cheap price prepares the nylon composite materials that actual application value is arranged.
Purpose of the present invention can realize by following technical solution.
The nylon composite materials that contains TLCP and needle-like mineral fibre of the present invention is by nylon 66 slice, TLCP, and the needle-like mineral fibre, coupling agent, oxidation inhibitor is formed.Weight ratio is 60～70: 10～15: 15～25: 4.5: 0.5
Described nylon 66 slice is the section of engineering plastics grade nylon 66.
Described TLCP is the Vectra A type TLCP of U.S. Goodfellow company production or the Zenite type TLCP that U.S. Dupont company produces.
Described needle-like mineral fibre is carbon fiber, halloysite nanotubes, acicular wollastonite, Kevlar fiber or whisker.
Described coupling agent is the A-1100 type coupling agent of U.S.'s union carbide corporation production, the Fusabond type coupling agent of U.S. Dupont company, the EPON type coupling agent of U.S. Aldrich company, or the maleic anhydride of last maritime affairs Bi Da company, styrene copolymerized type coupling agent.
Described oxidation inhibitor is the Lunchemao-R type hindered phenol antioxygen that U.S. big lake company produces.
The preparation method who contains the nylon composite materials of TLCP and needle-like mineral fibre of the present invention mainly contains following step:
(1) be 60～70: 10～15 with weight part ratio: 20～30: 4.5: 0.5 nylon 66 slice, TLCP, the needle-like mineral fibre, coupling agent, oxidation inhibitor mixes under agitation condition;
(2) under 280 ℃ or 295 ℃, extrude, traction, granulation, and injection moulding is made sample and is obtained the ternary nylon composite materials.
The present invention utilizes coupling agent to improve consistency between TLCP and Nylon 66, consistency between needle-like mineral filler and Nylon 66, reduced being separated between each component, improved the boundary strength between each component, thereby improved the tensile strength of matrix material, flexural strength, mechanical properties such as modulus in flexure, and make article shape even, improved dimensional stability.The nylon 66 composite material of the present invention's preparation can be used for making multiple plastic components.
The present invention compares with prior art, has following advantage and beneficial effect:
(1) TLCP during nylon composite materials of the present invention is formed with the nylon 66 slice extrusion in, in the Nylon 66 matrix, form microfibrillar structure, thereby reduce the melt viscosity of Nylon 66, improve melt flow rate (MFR), and then improve processing characteristics;
(2) multiple improvement effect has been played in the adding of needle-like mineral filler, compares with filler glass fibre commonly used, and it has following advantage: 1. the needle-like mineral filler is better mobile, is higher than fiber glass packing.2. needle-like mineral filler Heat stability is good, thermal distortion is low, and dimensional stability is better than glass.3. surface gloss will be higher than the glass filling.4. the needle-like mineral filler can solve the surface floating fiber that the glass filler causes and the problem of the easy warpage of goods.5. easily form microscopic capillary between the needle-like mineral filler, can promote the one-tenth fibre of TLCP.
(3) adding of coupling agent has not only improved the consistency between TLCP and nylon 66 matrix resins, has also improved needle-like mineral fibre and matrix resin, and the consistency between needle-like mineral fibre and the TLCP.These all help forming homodisperse phase structure, avoid the generation that is separated, thereby make prepared matrix material can fully show the excellent comprehensive performance of thermotropic liquid crystal.
(4) adding of oxidation inhibitor can avoid material oxidative degradation and consequent degradation to occur in the course of processing.
Embodiment
In order to understand technical characterstic of the present invention better,, need to prove that embodiment is not a limiting the scope of the invention below in conjunction with the present invention being further described by embodiment.
Embodiment 1
By weight, take by weighing 60 parts of nylon 66 slices (the engineering plastics grade nylon 66 section that Chinese refreshing horse Group Co.,Ltd produces), 10 parts of Vectra A type TLCP (productions of U.S. Goodfellow company), 25 parts of acicular wollastonites (Jiangxi Xinyu City south wollastonite industrial corporation produces), 4.5 parts of maleic anhydrides and styrol copolymer type coupling agent (upward maritime affairs Bi Da company production), 0.5 part of Lunchemao-R type hindered phenol antioxygen (production of U.S. big lake company); Under agitation condition, said components is mixed, then the mixture of gained is extruded under 290 ℃ in forcing machine, traction, granulation, and injection moulding makes sample, carry out performance test.The mechanical property of sample is according to following standard testing, and the result is as shown in table 1, by table as seen, compare pure nylon 66, tensile strength improves 13%, and flexural strength improves 3%, modulus in flexure remains basically stable, and notched Izod impact strength improves 25%, and heat-drawn wire improves 40 ℃.Over-all properties increases.I think and cause this raising mainly to be the mutual enhancing of filler and liquid crystalline resin that liquid crystal well is orientated to fibre under the help of needle-like mineral, make the mechanical property of material improve a lot.Along with the increase of liquid crystal consumption and amount of filler, the raising of this performance is also remarkable all the more.
Table 1
| 5.Izod notched Izod impact strength (J/m) | 50 | ASTM D256 |
| Heat-drawn wire (℃, 1.82MPa) | 220 | ASTM D648 |
| 7. proportion (g/cm3) | 1.6 | ASTM D792 |
Embodiment 2
By weight, take by weighing 70 parts of nylon 66 slices (the engineering plastics grade nylon 66 section that Chinese refreshing horse Group Co.,Ltd produces), 10 parts of Zenite type TLCP (productions of U.S. Dupont company), 15 parts of acicular wollastonites (Jiangxi Xinyu City south wollastonite industrial corporation produces), 4.5 parts of maleic anhydrides and styrol copolymer type coupling agent (upward maritime affairs Bi Da company production), 0.5 part of Lunchemao-R type hindered phenol antioxygen (production of U.S. big lake company); Under agitation condition, said components is mixed, then the mixture of gained is extruded under 285 ℃ in forcing machine, traction, granulation, and injection moulding makes sample, carry out performance test.The mechanical property of sample is according to following standard testing, and the result is as shown in table 2: by table as seen, compare pure nylon 66, tensile strength improves 18%, and flexural strength improves 3%, and modulus in flexure improves 30%, notched Izod impact strength improves 75%, and heat-drawn wire improves 10 ℃.Over-all properties improves a lot.
Table 2
Embodiment 3
By weight, take by weighing 60 parts of nylon 66 slices (the engineering plastics grade nylon 66 section that Chinese refreshing horse Group Co.,Ltd produces), 10 parts of Vectra A type TLCP (productions of U.S. Goodfellow company), 25 parts of acicular wollastonites (production of Jiangxi Xinyu City south wollastonite industrial corporation), 4.5 parts of EPON coupling agents (production of U.S. Aldrich company), 0.5 part of Lunchemao-R type hindered phenol antioxygen (production of U.S. big lake company); Under agitation condition, said components is mixed, then the mixture of gained is extruded under 290 ℃ in forcing machine, traction, granulation, and injection moulding makes sample, carry out performance test.The mechanical property of sample is according to following standard testing, and the result is as shown in table 3: by table as seen, compare pure nylon 66, tensile strength improves 18%, and flexural strength improves 10%, and modulus in flexure improves 20%, notched Izod impact strength improves 50%, and heat-drawn wire improves 40 ℃.Over-all properties improves a lot.
Table 3
Embodiment 4
By weight, take by weighing 70 parts of nylon 66 slices (the engineering plastics grade nylon 66 section that Chinese refreshing horse Group Co.,Ltd produces), 10 parts of Vectra A type TLCP (productions of U.S. Goodfellow company), 15 parts of halloysite nanotubes (self-control), 4.5 parts of A-1100 type coupling agents (U.S.'s union carbide corporation production), 0.5 part of Lunchemao-R type hindered phenol antioxygen (production of U.S. big lake company); Under agitation condition, said components is mixed, then the mixture of gained is extruded under 285 ℃ in forcing machine, traction, granulation, and injection moulding makes sample, carry out performance test.The mechanical property of sample is according to following standard testing, and the result is as shown in table 4: by table as seen, compare pure nylon 66, tensile strength improves 25%, and flexural strength improves 6%, and modulus in flexure improves 50%, notched Izod impact strength improves 100%, and heat-drawn wire improves 20 ℃.Over-all properties improves a lot.
Table 4
Embodiment 5
By weight, take by weighing 65 parts of nylon 66 slices (the engineering plastics grade nylon 66 section that Chinese refreshing horse Group Co.,Ltd produces), 15 parts of Zenite type TLCP (productions of U.S. Dupont company), 15 parts of acicular wollastonites (production of Jiangxi Xinyu City south wollastonite industrial corporation), EPON coupling agent (production of U.S. Aldrich company), 0.5 part of Lunchemao-R type hindered phenol antioxygen (production of U.S. big lake company); Under agitation condition, said components is mixed, then the mixture of gained is extruded under 285 ℃ in forcing machine, traction, granulation, and injection moulding makes sample, carry out performance test.The mechanical property of sample is according to following standard testing, and the result is as shown in table 5: by table as seen, compare pure nylon 66, tensile strength improves 25%, and flexural strength does not have increase, and modulus in flexure improves 50%, notched Izod impact strength improves 87%, and heat-drawn wire improves 15 ℃.Over-all properties improves a lot.
Table 5
| 1. tensile strength (MPa) | 100 | ASTM D638 |
| 2. elongation at break (%) | 3.1 | ASTM D638 |
| 3. flexural strength (MPa) | 125 | ASTM D790 |
| 4. modulus in flexure (MPa) | 45000 | ASTM D790 |
| 5.Izod notched Izod impact strength (J/m) | 75 | ASTM D256 |
| Heat-drawn wire (℃, 1.82MPa) | 195 | ASTM D648 |
| 7. proportion (g/cm3) | 1.60 | ASTM D792 |
Embodiment 6
By weight, take by weighing 60 parts of nylon 66 slices (the engineering plastics grade nylon 66 section that Chinese refreshing horse Group Co.,Ltd produces), 20 parts of Vectra A type TLCP (productions of U.S. Goodfellow company), 15 parts of acicular wollastonites (Jiangxi Xinyu City south wollastonite industrial corporation produces), 4.5 parts of maleic anhydrides and styrol copolymer type coupling agent (upward maritime affairs Bi Da company production), 0.5 part of Lunchemao-R type hindered phenol antioxygen (production of U.S. big lake company); Under agitation condition, said components is mixed, then the mixture of gained is extruded under 290 ℃ in forcing machine, traction, granulation, and injection moulding makes sample, carry out performance test.The mechanical property of sample is according to following standard testing, and the result is as shown in table 6: by table as seen, compare pure nylon 66, tensile strength improves 37.5%, and flexural strength improves 18%, and modulus in flexure improves 30%, notched Izod impact strength improves 75%, and heat-drawn wire improves 45 ℃.Over-all properties improves a lot.
Table 6
| Heat-drawn wire (℃, 1.82MPa) | 225 | ASTM D648 |
| 7. proportion (g/cm3) | 1.65 | ASTM D792 |
Embodiment 7
By weight, take by weighing 60 parts of nylon 66 slices (the engineering plastics grade nylon 66 section that Chinese refreshing horse Group Co.,Ltd produces), 20 parts of Zenite type TLCP (productions of U.S. Dupont company), 15 parts of halloysite nanotubes (self-control), 4.5 parts of maleic anhydrides and styrol copolymer type coupling agent (production of last maritime affairs Bi Da company), 0.5 part of Lunchemao-R type hindered phenol antioxygen (production of U.S. big lake company); Under agitation condition, said components is mixed, then the mixture of gained is extruded under 285 ℃ in forcing machine, traction, granulation, and injection moulding makes sample, carry out performance test.The mechanical property of sample is according to following standard testing,, the result is as shown in table 7: by table as seen, compare pure nylon 66, tensile strength improves 37.5%, and flexural strength improves 3%, modulus in flexure improves 60%, and notched Izod impact strength improves 105%, and heat-drawn wire improves 20 ℃.Over-all properties improves a lot.
Table 7
Embodiment 8
By weight, take by weighing 60 parts of nylon 66 slices (the engineering plastics grade nylon 66 section that Chinese refreshing horse Group Co.,Ltd produces), 20 parts of Vectra A type TLCP (production of U.S. Goodfellow company), 15 parts of halloysite nanotubes (self-control), 4.5 parts of EPON coupling agents (production of U.S. Aldrich company), 0.5 part of Lunchemao-R type hindered phenol antioxygen (production of U.S. big lake company); Under agitation condition, said components is mixed, then the mixture of gained is extruded under 285 ℃ in forcing machine, traction, granulation, and injection moulding makes sample, carry out performance test.The mechanical property of sample is according to following standard testing,, the result is as shown in table 8: by table as seen, compare pure nylon 66, tensile strength improves 50%, and flexural strength improves 18.1%, modulus in flexure improves 83.3%, and notched Izod impact strength improves 125%, and heat-drawn wire improves 40 ℃.Over-all properties improves a lot.
Table 8
Claims (7)
1. a nylon composite materials is characterized in that, nylon composite materials is by nylon 66 slice, TLCP, needle-like mineral fibre, coupling agent, and the antioxidant material mixing granulation makes; The weight ratio of nylon 66 slice, TLCP, needle-like mineral fibre, coupling agent and oxidation inhibitor is 60～70: 10～15: 20～30: 4.5: 0.5.
2. nylon composite materials according to claim 1 is characterized in that, described nylon 66 slice is the section of engineering plastics grade nylon 66.
3. nylon composite materials according to claim 1 and 2 is characterized in that described TLCP is Vectra type TLCP or Zenite type TLCP.
4. nylon composite materials according to claim 1 is characterized in that described needle-like mineral fibre is carbon fiber, halloysite nanotubes, acicular wollastonite, Kevlar fiber or whisker.
5. nylon composite materials according to claim 1 is characterized in that described coupling agent is silane type coupling agent, ethylene-acrylic acid copolymer type coupling agent or maleic anhydride, styrene copolymerized type coupling agent.
6. nylon composite materials according to claim 1 is characterized in that described oxidation inhibitor is hindered phenol type antioxidant.
7. method for preparing the described nylon composite materials of claim 1 is characterized in that step is as follows:
(1) be 60～70: 10～15 with weight part ratio: 20～30: 4.5: 0.5 nylon 66 slice, TLCP, needle-like mineral fibre, coupling agent and oxidation inhibitor mix under agitation condition;
(2) under 280 ℃ or 295 ℃, extrude, traction, granulation, and injection moulding is made sample and is obtained nylon composite materials.
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| CN102079869A (en) * | 2010-12-20 | 2011-06-01 | 金发科技股份有限公司 | Preparation method of liquid crystal nylon alloy |
| CN102219994A (en) * | 2011-05-24 | 2011-10-19 | 华南理工大学 | Heat conducting nanometer material and preparation method and application thereof |
| CN102250347A (en) * | 2011-05-04 | 2011-11-23 | 中国地质大学（武汉） | Preparation method of chelating type ion exchange resin with natural halloysite nanotube (HNT) as matrix |
| CN103289394A (en) * | 2013-06-24 | 2013-09-11 | 苏州新区佳合塑胶有限公司 | Antistatic reinforced Nylon 66 composite |
| CN104098890A (en) * | 2013-04-10 | 2014-10-15 | 上海杰事杰新材料(集团)股份有限公司 | HPN (high temperature resistant nylon)/(thermotropic liquid crystal polymer) / HNTs (halloysite nanotubes) composite material and preparation method thereof |
| CN104448814A (en) * | 2014-11-27 | 2015-03-25 | 湖北洋田塑料制品有限公司 | High-strength and high-rigidity liquid crystal polymer reinforced nylon 66 composite and preparation method thereof |
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| CN102250347A (en) * | 2011-05-04 | 2011-11-23 | 中国地质大学（武汉） | Preparation method of chelating type ion exchange resin with natural halloysite nanotube (HNT) as matrix |
| CN102250347B (en) * | 2011-05-04 | 2012-11-21 | 中国地质大学（武汉） | Preparation method of chelating type ion exchange resin with natural halloysite nanotube (HNT) as matrix |
| CN102219994A (en) * | 2011-05-24 | 2011-10-19 | 华南理工大学 | Heat conducting nanometer material and preparation method and application thereof |
| CN104098890A (en) * | 2013-04-10 | 2014-10-15 | 上海杰事杰新材料(集团)股份有限公司 | HPN (high temperature resistant nylon)/(thermotropic liquid crystal polymer) / HNTs (halloysite nanotubes) composite material and preparation method thereof |
| CN103289394A (en) * | 2013-06-24 | 2013-09-11 | 苏州新区佳合塑胶有限公司 | Antistatic reinforced Nylon 66 composite |
| CN104629356A (en) * | 2013-11-12 | 2015-05-20 | 上海杰事杰新材料(集团)股份有限公司 | Enhanced semi-aromatic nylon/liquid crystal polymer alloy material and preparation method thereof |
| CN104448814A (en) * | 2014-11-27 | 2015-03-25 | 湖北洋田塑料制品有限公司 | High-strength and high-rigidity liquid crystal polymer reinforced nylon 66 composite and preparation method thereof |
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| CN109251520A (en) * | 2018-09-25 | 2019-01-22 | 广东顾纳凯材料科技有限公司 | A kind of low water absorption, LCP enhancing PA composite material and preparation method |
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| CN112795181A (en) * | 2020-12-30 | 2021-05-14 | 金发科技股份有限公司 | Polyamide composition and preparation method and application thereof |
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