CN105295370A - High-glass-fiber-content reinforced nylon 66 material and preparation method thereof - Google Patents
High-glass-fiber-content reinforced nylon 66 material and preparation method thereof Download PDFInfo
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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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Abstract
The invention relates to the technical field of engineering plastic materials, in particular to a high-glass-fiber-content reinforced nylon 66 material, which is prepared from the following components in percentage by mass: 55 percent to 70 percent of glass fiber, 16 percent to 38 percent of nylon 66, 5 percent to 10 percent of nylon copolymer, 1 percent to 2 percent of lubricating auxiliary, 0.05 percent to 1 percent of star branching agent, 0.05 percent to 1 percent of end-capping agent and 0.05 percent to 1 percent of heat stabilizer; the nylon 66 and the nylon copolymer are chosen as main materials, and the star branching agent is added, so the materials are cheap and easy to obtain, and the prepared high-glass-fiber-content reinforced nylon 66 material has no white spot and is free of glass fiber exposure, the product overall performance is excellent, and extremely high mechanical strength, beneficial long-term heat resistance, excellent dimensional stability and high rigidity are obtained; the invention also relates to a preparation method of the high-glass-fiber-content reinforced nylon 66 material.
Description
Technical field
The present invention relates to engineering plastic materials technical field, particularly relate to a kind of high glass fiber content reinforced PA66 material and preparation method thereof.
Background technology
Nylon66 fiber (PA66) is poly-adipoyl diamines, antifatigue and rigid high, good heat resistance, frictional coefficient is low, wear resistance good, and stable chemical performance, but to temperature sensitive and water absorbability is large, cause poor dimensional stability, and dry state and low temperature impact strength low.Therefore usually medium load is applied to, the wear-resisting stressed driving parts worked under use temperature 100-120 DEG C of unlubricated or few lubricating condition.For improving the performances such as the tensile strength of nylon66 fiber, shock strength, modulus, wear resistance and dimensional stability, add toughener in the polymeric matrix of nylon66 fiber of being everlasting, as glass, nano silicon, carbon fiber and graphite fibre etc.; And due to the excellent properties of glass, in industry, generally all select glass as toughener.
Glass is also known as glass fibre (GF), it is a kind of ceramic of excellent performance, main component is silicon-dioxide, aluminum oxide, calcium oxide etc., it is formed through wire drawing cooling curing by the glass metal under the condition of high temperature, the diameter of general monofilament is 5-30 micron, every mass of fibers precursor is by hundreds of even thousands of monofilament compositions, become extraordinary metal substitute material at present, it is added in nylon 66 material, with the functional group reactions of nylon66 fiber, add interface binding power, improve the mechanical property of matrix material.
Along with the lifting of Industry Development Level and the raising of product quality requirement, general engineering plastic high performance is progressively brought into schedule, and becomes forward position and the primary study direction of the development of current modified plastics.The glass fibre modification of nylon that wherein massfraction is more than or equal to 50% has high mechanical strength, excellent long-term heat resistance, dimensional stability and high rigidity, the metallic substance such as alternative such as aluminium alloy.And the glass addition of current most of glass fiber enhanced nylon 66 material is all between 10-45wt%; Obvious mold deposit and white stubble can be produced in high-temperature injection process as being greater than nylon 66 material under 50wt% at high glass fiber content, the formation of mold deposit and white stubble is on the one hand because nylon 66 material itself causes, be on the other hand due to high glass fiber content causes processing temperature can corresponding raising, and more easily volatilization or decomposition cause after temperature raises to be retained in the lower small-molecule substance of some boiling points in glass; And content of glass fiber is when being greater than 50wt%, glass is not easily dispersed in nylon 66 material, when causing making, the poor and uneven GF that very easily causes on preparation surface that flows of system mobility exposes (floating fine), simultaneously, imperfect flow makes extrusion difficulty, and has serious disconnected bar phenomenon to occur.And in order to solve the cosmetic issue of high glass fiber content, mineral substance replacement part glass method is added abroad at present as the enterprises such as BASF, Du Pont, Asahi Chemical Industry all adopt, these enterprises have 60wt% glass and mineral substance mixing enhancing modified nylon material, and maturation is applied on numerous product, and the domestic research to this is also little.
Therefore, how to improve above-mentioned situation and eliminate the white patches on surface of high GF content modified product and floating fibre, becoming one of the difficult point and focus of each large modifying plastics business research; Develop the high glass fiber content reinforced PA66 material with Good All-around Property more, wide market, and have very important practical significance.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of high glass fiber content reinforced nylon 6 material.Obtain rigidity and the good matrix material of toughness
To achieve these goals, technical scheme of the present invention is as follows:
A kind of high glass fiber content reinforced PA66 material, by mass percentage, comprising:
Wherein, the structure of described star-branched dose is:
Wherein, R is aromatic series segment, aliphatics segment or alicyclic segment, and R ' is amino, carboxyl, epoxy group(ing) or the hydroxy functional group that can react with the end amido of nylon66 fiber, R ' number of functional groups >=3.
More preferably, the content of described glass fibre is 56%-61%, preferably 60%.
Add nylon copolymer in nylon66 fiber of the present invention, structural regularity that end-capping reagent and star-branched dose destroy PA66, form star-branched nylon, reduce degree of crystallinity, improve the mobility of nylon66 fiber, reduce the post crystallization temperature of material significantly, impel glass fibre better to disperse in nylon material, be convenient to processing; The tensile strength of obtained high glass fiber content reinforced PA66 material significantly improves, and Young's modulus and modulus in flexure significantly improve, and its tensile strength reaches more than 240MPa, and modulus in flexure is more than more than 20GPa.
The diameter of described glass fibre is 5 ~ 30 μm, and described glass fibre is alkali-free short glass fiber; Particularly, described glass fibre is the alkali-free short glass fiber after fiberglass surface treating agent soaks, and described fiberglass surface treating agent is silane coupling agent, is specially KH560.Described alkali-free short glass fiber, surface-coated has silane type treating compound, through the alkali-free short glass fiber of this special processing and nylon resin intermiscibility good, there is good dispersiveness and mobility, be conducive to the coated fusion of nylon to glass fibre, ensure product size stability and physical strength.
Described nylon copolymer is the PA6/66 multipolymer that nylon 6 and nylon66 fiber reaction dehydration polymerization form containing amide group, the surface smoothness of common PA66 glass fiber reinforced materials over-all properties and goods can be improved comprehensively, preferably, by mass percentage, content is 6% ~ 10% to nylon copolymer.
Described lubricating auxiliary agent is one or more mixtures in polyamide wax (C wax), SEED, TAF-A, above-mentioned three kinds of materials are all as polar lubricant, wherein, the long-chain end of the silane coupling agent in the polar group of polyamide wax and glass fibre produces very strong magnetism by Fan get Hua Li, this magnetism is enough to two thing phase interfacies are disappeared, and forming a phase, C wax and nylon66 fiber also have certain consistency, play compatilizer effect; SEED, TAF-A are anti-glass emergence on the surface agent, and its effect is similar with C wax, and it is more high temperature resistant; Like this, between glass, base nylon (nylon66 fiber), define similar anchoring node, i.e. cross-linking set, improve the bond state of glass and nylon.Because the mechanical function layer thickness between the surface of glass and nylon increases, make the matrix being in glass near surface be easier to shear yielding occurs, increase the absorption to striking energy and dissipative effect, promote that glass is to the activeness and quietness effect of base nylon.Because glass obtains coated well in nylon, in the course of processing, glass and nylon synchronously flow, and not easily rip, reduce the floating fibre of fiberglass reinforced modification of nylon, fine, the white problem such as stubble, flow liner of dew widely, make its goods can have good surface smoothness.
Described star-branched dose is one or more mixtures in triethylene tetramine, diethylenetriamine, triaminotriphenyl methylmethane; Particularly, star-branched dose that the structure of nylon66 fiber can be made to be changed into by straight-chain is netted, greatly promote the mechanical property of materials, because the star-branched agent of uniqueness is to the effect of molecular structure, plasticize process Middle molecule is roller motion, matrix resin mobility significantly promotes, and has remarkable effect to the dispersion of glass, is conducive to the stability of modification and injection molding.
Described end-capping reagent is one or more mixtures in phenylformic acid, acetic acid, propionic acid.
Described thermo-stabilizer is metal halide, is selected from one or more mixtures in cuprous iodide, cuprous chloride, potassiumiodide, Potassium Bromide; Add the weathering resistance that thermo-stabilizer can promote material greatly, ensure work-ing life and the permanent stability of material.
A preparation method for high glass fiber content reinforced PA66 material as above, comprises the steps:
1) by nylon66 fiber, nylon copolymer, lubricating auxiliary agent, thermo-stabilizer, end-capping reagent, star-branched dose mix by formula ratio, obtain raw material A;
2) soak glass fibre 10 ~ 15 hours with fiberglass surface treating agent, the vacuum drying oven being then placed in 50 ~ 60 DEG C is dried to constant weight and is obtained raw material B;
3) by step 2) the raw material B that obtains joins in the hopper of side feeding, step 1) raw material A that obtains joins in main feeding hopper, by the demarcation of master, side feeding motor, ensure that the content of glass fibre reaches more than 55%, then granulation after melt blending in twin screw extruder, obtains high glass fiber content reinforced PA66 material after dry constant weight.
The invention provides the preparation method of high glass fiber enhanced nylon 66 material, the method is adopted glass fibre to be added by the mode of side feeding and melt extrudes the reinforced PA66 material of the high glass fiber content of preparation at 55-70%.High fiber glass reinforced polyamide 66 material is jointly prepared by the polyamide material A and short glass fiber B and processing aid C that prepare high workability energy; This material is by the special processing of raw material, material is made to have excellent intensity and rigidity, its tensile strength can reach more than 240MPA, modulus in flexure can reach more than 20GPA, material has splendid mobility, even so the finished surface unusual light that high glass fiber content is made, this material has high mechanical strength and rigidity than glass fibre and breeze compound, can alternative metals material.
Beneficial effect of the present invention: obtained product selects nylon66 fiber and nylon copolymer as major ingredient, and its material is cheap and easy to get; And obtained high glass fiber content reinforced PA66 material is without the situation of hickie and glass emergence on the surface, product high comprehensive performance, has high mechanical strength, useful long-term heat resistance, excellent dimensional stability and high rigidity; When making this material, the mixed good fluidity of raw material, extrudes easily, and occurs without serious disconnected bar phenomenon in extrusion.
Embodiment
Below the specific embodiment of the present invention is described in further detail.
Embodiment 1
A kind of high glass fiber content reinforced PA66 material, by mass percentage, comprising:
Wherein select triethylene tetramine for star-branched dose, end-capping reagent selects phenylformic acid, and lubricating auxiliary agent is C wax, and thermo-stabilizer is cuprous iodide, and glass fibre is the alkali-free short glass fiber after silane coupling agent (KH560) soaks, and diameter is 5 ~ 30 μm.
The preparation method of this kind high glass fiber content reinforced PA66 material, comprises the steps:
1) by nylon66 fiber, nylon copolymer, lubricating auxiliary agent, thermo-stabilizer, end-capping reagent, star-branched dose mix by formula ratio, obtain raw material A;
2) soak glass fibre 10 ~ 15 hours with KH560, the vacuum drying oven being then placed in 50 ~ 60 DEG C is dried to constant weight and is obtained raw material B;
3) by step 2) the raw material B that obtains joins in the hopper of side feeding, step 1) raw material A that obtains joins in main feeding hopper, by the demarcation of master, side feeding motor, ensure that the content of glass fibre reaches 55%, then granulation after melt blending in twin screw extruder, obtains high glass fiber content reinforced PA66 material after dry constant weight.
Embodiment 2
A kind of high glass fiber content reinforced PA66 material, by mass percentage, comprising:
Wherein, select diethylenetriamine for star-branched dose, end-capping reagent selects acetic acid, and lubricating auxiliary agent is C wax, and thermo-stabilizer is Potassium Bromide, and glass fibre is the alkali-free short glass fiber after KH560 soaks, and diameter is 5 ~ 30 μm.
The preparation method of this kind high glass fiber content reinforced PA66 material, comprises the steps:
1) by nylon66 fiber, nylon copolymer, lubricating auxiliary agent, thermo-stabilizer, end-capping reagent, star-branched dose mix by formula ratio, obtain raw material A;
2) soak glass fibre 10 ~ 15 hours with KH560, the vacuum drying oven being then placed in 50 ~ 60 DEG C is dried to constant weight and is obtained raw material B;
3) by step 2) the raw material B that obtains joins in the hopper of side feeding, step 1) raw material A that obtains joins in main feeding hopper, by the demarcation of master, side feeding motor, ensure that the content of glass fibre reaches more than 60%, then granulation after melt blending in twin screw extruder, obtains high glass fiber content reinforced PA66 material after dry constant weight.
Embodiment 3
A kind of high glass fiber content reinforced PA66 material, by mass percentage, comprising:
Wherein, star-branched dose is triaminotriphenyl methylmethane, and end-capping reagent is propionic acid, lubricating auxiliary agent is the mixture of C wax and SEED, thermo-stabilizer is the mixture of cuprous iodide and potassiumiodide, and glass fibre is the alkali-free short glass fiber after silane coupling agent soaks, and its diameter is 5 ~ 30 μm.
The preparation method of this kind high glass fiber content reinforced PA66 material, comprises the steps:
1) by nylon66 fiber, nylon copolymer, lubricating auxiliary agent, thermo-stabilizer, end-capping reagent, star-branched dose mix by formula ratio, obtain raw material A;
2) soak glass fibre 10 ~ 15 hours with silane coupling agent, the vacuum drying oven being then placed in 50 ~ 60 DEG C is dried to constant weight and is obtained raw material B;
3) by step 2) the raw material B that obtains joins in the hopper of side feeding, step 1) raw material A that obtains joins in main feeding hopper, by the demarcation of master, side feeding motor, ensure that the content of glass fibre reaches 65%, then granulation after melt blending in twin screw extruder, obtains high glass fiber content reinforced PA66 material after dry constant weight.
Embodiment 4
A kind of high glass fiber content reinforced PA66 material, by mass percentage, comprising:
Wherein, star-branched dose is the mixture in triethylene tetramine and triaminotriphenyl methylmethane, and end-capping reagent is acetic acid, lubricating auxiliary agent is C wax, thermo-stabilizer is cuprous chloride, and glass fibre is the alkali-free short glass fiber after silane coupling agent (KH560) soaks, and its diameter is 5 ~ 30 μm.
The preparation method of this kind high glass fiber content reinforced PA66 material, comprises the steps:
1) by nylon66 fiber, nylon copolymer, lubricating auxiliary agent, thermo-stabilizer, end-capping reagent, star-branched dose mix by formula ratio, obtain raw material A;
2) soak glass fibre 10 ~ 15 hours with silane coupling agent, the vacuum drying oven being then placed in 50 ~ 60 DEG C is dried to constant weight and is obtained raw material B;
3) by step 2) the raw material B that obtains joins in the hopper of side feeding, step 1) raw material A that obtains joins in main feeding hopper, by the demarcation of master, side feeding motor, ensure that the content of glass fibre reaches 70%, then granulation after melt blending in twin screw extruder, obtains high glass fiber content reinforced PA66 material after dry constant weight.
Embodiment 5
A kind of high glass fiber content reinforced PA66 material, by mass percentage, comprising:
Wherein, star-branched dose is triethylene tetramine, and end-capping reagent is the mixture of phenylformic acid and acetic acid, lubricating auxiliary agent is C wax, thermo-stabilizer is potassiumiodide, and glass fibre is the alkali-free short glass fiber after silane coupling agent (KH560) soaks, and its diameter is 5 ~ 30 μm.
The preparation method of this kind high glass fiber content reinforced PA66 material, comprises the steps:
1) by nylon66 fiber, nylon copolymer, lubricating auxiliary agent, thermo-stabilizer, end-capping reagent, star-branched dose mix by formula ratio, obtain raw material A;
2) soak glass fibre 10 ~ 15 hours with KH560, the vacuum drying oven being then placed in 50 ~ 60 DEG C is dried to constant weight and is obtained raw material B;
3) by step 2) the raw material B that obtains joins in the hopper of side feeding, step 1) raw material A that obtains joins in main feeding hopper, by the demarcation of master, side feeding motor, ensure that the content of glass fibre reaches more than 60%, then granulation after melt blending in twin screw extruder, obtains high glass fiber content reinforced PA66 material after dry constant weight.
Embodiment 6
A kind of high glass fiber content reinforced PA66 material, by mass percentage, comprising:
Wherein, star-branched dose is the mixture of triethylene tetramine and diethylenetriamine, and end-capping reagent is propionic acid, and lubricating auxiliary agent is SEED, and thermo-stabilizer is cuprous chloride, and glass fibre is the alkali-free short glass fiber after KH560 soaks, and its diameter is 5 ~ 30 μm.
The preparation method of this kind high glass fiber content reinforced PA66 material, comprises the steps:
1) by nylon66 fiber, nylon copolymer, lubricating auxiliary agent, thermo-stabilizer, end-capping reagent, star-branched dose mix by formula ratio, obtain raw material A;
2) soak glass fibre 10 ~ 15 hours with KH560, the vacuum drying oven being then placed in 50 ~ 60 DEG C is dried to constant weight and is obtained raw material B;
3) by step 2) the raw material B that obtains joins in the hopper of side feeding, step 1) raw material A that obtains joins in main feeding hopper, by the demarcation of master, side feeding motor, ensure that the content of glass fibre reaches 65%, then granulation after melt blending in twin screw extruder, obtains high glass fiber content reinforced PA66 material after dry constant weight.
Embodiment 7
A kind of high glass fiber content reinforced PA66 material, by mass percentage, comprising:
Wherein, star-branched dose is triaminotriphenyl methylmethane, and end-capping reagent is acetic acid, lubricating auxiliary agent is the mixture of C wax and TAF-A, thermo-stabilizer is the mixture of cuprous chloride and potassiumiodide, and glass fibre is the alkali-free short glass fiber after silane coupling agent soaks, and its diameter is 5 ~ 30 μm.
The preparation method of this kind high glass fiber content reinforced PA66 material, comprises the steps:
1) by nylon66 fiber, nylon copolymer, lubricating auxiliary agent, thermo-stabilizer, end-capping reagent, star-branched dose mix by formula ratio, obtain raw material A;
2) soak glass fibre 10 ~ 15 hours with silane coupling agent, the vacuum drying oven being then placed in 50 ~ 60 DEG C is dried to constant weight and is obtained raw material B;
3) by step 2) the raw material B that obtains joins in the hopper of side feeding, step 1) raw material A that obtains joins in main feeding hopper, by the demarcation of master, side feeding motor, ensure that the content of glass fibre reaches more than 60%, then granulation after melt blending in twin screw extruder, obtains high glass fiber content reinforced PA66 material after dry constant weight.
Performance test is carried out to the high glass fiber content reinforced PA66 material made in above-described embodiment, wherein, Performance Detection mainly concentrates on: outward appearance, dimensional stability, thermotolerance, tensile strength, flexural strength, modulus in flexure, and its record result is as shown in table 1 below:
Table 1
As shown above, the high glass fiber content reinforced PA66 material prepared by the present invention occurs without floating fibre and hickie, and good stability of the dimension, its tensile strength reaches more than 240MPa, and modulus in flexure is more than 20GPa.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, its framework form can be flexible and changeable, can subseries product.Just make some simple deduction or replace, all should be considered as belonging to the scope of patent protection that the present invention is determined by submitted to claims.
Claims (9)
1. a high glass fiber content reinforced PA66 material, is characterized in that, by mass percentage, comprising:
Wherein, the structure of described star-branched dose is:
Wherein, R is aromatic series segment, aliphatics segment or alicyclic segment, and R ' is amino, carboxyl, epoxy group(ing) or the hydroxy functional group that can react with the end group of nylon66 fiber, R ' number of functional groups >=3.
2. high glass fiber content reinforced PA66 material according to claim 1, is characterized in that: described star-branched dose is one or more mixtures in triethylene tetramine, diethylenetriamine, triaminotriphenyl methylmethane.
3. high glass fiber content reinforced PA66 material according to claim 1, is characterized in that: described end-capping reagent is one or more mixtures in phenylformic acid, acetic acid, propionic acid.
4. high glass fiber content reinforced PA66 material according to claim 1, is characterized in that: described lubricating auxiliary agent is one or more mixtures in polyamide wax, SEED, TAF-A.
5. high glass fiber content reinforced PA66 material according to claim 1, is characterized in that: the diameter of described glass fibre is 5 ~ 30 μm.
6. high glass fiber content reinforced PA66 material according to claim 1, is characterized in that: described glass fibre is alkali-free short glass fiber.
7. high glass fiber content reinforced PA66 material according to claim 1, is characterized in that: described glass fibre is the alkali-free short glass fiber after fiberglass surface treating agent soaks.
8. high glass fiber content reinforced PA66 material according to claim 7, is characterized in that: described fiberglass surface treating agent is silane coupling agent.
9. a preparation method for the high glass fiber content reinforced PA66 material as described in any one of claim 1 ~ 8, is characterized in that, comprise the steps:
1) by nylon66 fiber, nylon copolymer, lubricating auxiliary agent, thermo-stabilizer, end-capping reagent, star-branched dose mix by formula ratio, obtain raw material A;
2) soak glass fibre 10 ~ 15 hours with fiberglass surface treating agent, then obtain raw material B in lower oven dry to the constant weight of 50 ~ 60 DEG C;
3) by step 2) the raw material B that obtains joins in the hopper of side feeding, step 1) raw material A that obtains joins in main feeding hopper, then granulation after melt blending in twin screw extruder, obtains high glass fiber content reinforced PA66 material after dry constant weight.
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| CN105802206A (en) * | 2016-04-15 | 2016-07-27 | 浙江亚太机电股份有限公司 | Nylon 66 glass fiber composite material with high glass fiber content and preparing method thereof |
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| CN110079084A (en) * | 2019-05-29 | 2019-08-02 | 辰东意普万新材料(广东)有限公司 | Nylon composite materials and preparation method thereof |
| CN112080140A (en) * | 2020-09-22 | 2020-12-15 | 上海盈固化工有限公司 | Glass fiber reinforced polyamide resin material and preparation method thereof |
| CN114716821A (en) * | 2022-03-21 | 2022-07-08 | 江苏博云塑业股份有限公司 | Glass fiber reinforced nylon material and preparation method thereof |
| CN114716821B (en) * | 2022-03-21 | 2024-02-02 | 江苏博云塑业股份有限公司 | Glass fiber reinforced nylon material and preparation method thereof |
| CN115260760A (en) * | 2022-09-15 | 2022-11-01 | 辰东新材料(江苏)有限公司 | Polyamide composite with high heat resistance, high modulus and low dielectric constant, preparation and application thereof |
| CN115260760B (en) * | 2022-09-15 | 2023-12-12 | 辰东新材料(江苏)有限公司 | Polyamide composite with high heat resistance, high modulus and low dielectric constant, and preparation and application thereof |
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