CN100372885C - Continuous long fiber reinforced composite nylon/polyolefin material and its prepn - Google Patents
Continuous long fiber reinforced composite nylon/polyolefin material and its prepn Download PDFInfo
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Abstract
The present invention discloses a continuous long fiber reinforced composite nylon/polyolefin material and the preparation method thereof. The composite material is formed by mixing nylon resin and continuous long fiber reinforced polyolefin composite resin agglomerate with high fiber content, wherein the continuous long fiber reinforced polyolefin composite resin agglomerate is made from 30-80 weight percent of continuous long fiber and 20-70 weight percent of polyolefin composite resin with the adoption of pultruding method, and then the continuous long fiber reinforced polyolefin composite resin agglomerate is mixed with nylon resin to form the continuous long fiber reinforced composite nylon/polyolefin material. The mixing preparation method of the continuous long fiber reinforced composite nylon/polyolefin material overcomes the defects of the methods in the existing patents of inventions, and the composite material with excellent mechanical properties is obtained.
Description
Technical field
The present invention relates to polymeric material field, be specifically related to a kind of continuous long fiber reinforced composite nylon/polyolefin material and preparation method thereof.
Background technology
To be that a kind of fortifying fibre is unidirectional arrange and enhancing thermoplastic resin that its length is identical with resin granular material length continuous fiber reinforced thermoplastic resin.It strengthens thermoplastic resin with conventional staple fibre compares, and has excellent more mechanical property, dynamic fatigue resistance energy, creep-resistant property etc.; Particularly the shock resistance of material is very excellent.Therefore, be particularly suitable under some occasion, replacing cast iron, aluminium and thermosetting resin etc.
Although the continuous long fiber reinforced Nylon resin has excellent mechanical property and resistance toheat, strengthen polyolefine with continuous fiber and compare, its moisture absorption (water) rate, density and cost are higher; And the mechanical property of continuous fiber enhancing polyolefine material and resistance toheat are all far away from continuous fiber enhanced nylon resin.If the two is compound, then can reduce moisture absorption (water) rate, density and the cost of continuous long fiber reinforced Nylon resin significantly, also can keep good mechanical property and resistance toheat simultaneously; Thereby further widen the Application Areas of two kinds of continuous fiber reinforced thermoplastic resins.
Adopting conventional art to prepare fiber reinforced nylon/composite polyolefine material is that nylon resin, polyolefin resin, modified polyolefin resin are extruded and obtained with the twin screw extruder melt blending.Though this technology of preparing can realize lightweight, reduce moisture absorption (water) rate and cost, (staple length is generally 0.1～0.6mm), and can not obtain the Reinforced Nylon/composite polyolefine material of mechanical property excellence but because this technology of preparing itself is understood and to be sheared continuous rove fiber or chopped strand very short.
Disclosed preparation continuous long fiber reinforced Nylon resin/composite polyolefine material has been arranged, as Chinese patent CN1131427A.In this patent, first preparation continuous fiber reinforcing polyamide masterbatch then forms this masterbatch and the alloying diluent resin blending that contains polymeric amide, crystalline polyolefin resin and unsaturated carboxylic acid-modified olefin crystalline polymer.This preparation method's defective is: (1) will prepare two kinds of material (long fiber reinforced Nylon resin concentrates and alloying diluent resin), and process is comparatively loaded down with trivial details, has increased production cost; When (2) producing the long fiber reinforced Nylon masterbatch resin, because nylon resin is easy to xanthochromia, the technology controlling and process difficulty is not easy to guarantee colour stability.
Summary of the invention
The objective of the invention is to overcome the defective that existing continuous long fiber reinforced composite nylon/polyolefin material exists, provide that a kind of cost is low, the continuous long fiber reinforced composite nylon/polyolefin material of various stable performances.
Another object of the present invention provides the preparation method of above-mentioned matrix material, and this preparation method controls simply, cost is lower.
A kind of continuous long fiber reinforced composite nylon/polyolefin material is formed by continuous fiber enhancing polyolefine compound resin master batch and nylon resin blending; Both are not particularly limited by mixing proportion, decide on the predetermined fibre content of final continuous long fiber reinforced composite nylon/polyolefin material and the fibre content of continuous fiber enhancing polyolefine compound resin master batch; In whole continuous long fiber reinforced composite nylon/polyolefin material, the final content of continuous fiber is 5～60%.
Described continuous fiber strengthens polyolefine compound resin master batch and is made up of the polyolefine compound resin of continuous long fiber peacekeeping 20～70 weight % of 30～80 weight %.Described continuous fiber monofilament is arranged in parallel with each other along master batch particle length direction, and length is identical with the master batch particle, is 3～30mm.
Above-mentioned continuous fiber is a kind of inorganic fibre that is made of glass fibre, steel fiber, carbon fiber and boron fibre at least, and/or at least a organic fibre that is made of all aromatic polyamide fibres and all aromatic polyester fibers.
The said polyolefins compound resin is made up of 70～100% polyolefin resin and 0～30% modified polyolefin resin.
The said polyolefins resin is crystalline polypropylene (Co-PP, Homo-PP), polyethylene (HDPE, LDPE, LLDPE), one or more the mixture in the ethylene-octene copolymer (POE), ethylene-propylene-diene terpolymer (EPDM), ethylene-propylene copolymer.
Above-mentioned modified polyolefin resin is meant with in the crystalline polypropylene of unsaturated carboxylic acid or its acid anhydrides or derivatives thereof (below be referred to as unsaturated carboxylic acid) modification, polyethylene, ethylene-octene copolymer, ethylene-propylene-diene terpolymer, the ethylene-propylene copolymer one or more, but is not limited only to these modified polyolefin resins.
Above-mentioned nylon resin comprises as in nylon 6 (PA6), nylon 66 (PA66), Ni Long11 (PA11), nylon 12 (PA12), NYLON610 (PA610), the nylon 612 (PA612) one or more, but is not limited only to these nylon resins.
The preparation method of above-mentioned continuous long fiber reinforced composite nylon/polyolefin material comprises the steps:
(1) continuous long fiber peacekeeping polyolefine compound resin is adopted pultrusion method make continuous fiber and strengthens polyolefine compound resin master batch:
(2) continuous fiber is strengthened polyolefine compound resin master batch and nylon resin and be blended into continuous long fiber reinforced composite nylon/polyolefin material.
The moulding process of above-mentioned steps (1) described " pultrude process (Pultrusion) " is: a branch of continuous fiber is introduced in the independent runner of dipping former by the continuous fiber access road; This bundle continuous fiber advances along broken line after alternately walking around in groups tensioning roller, at this moment, cause that because of the tensioning roller rotation that longitudinally has circular groove the enough turbulent flows of thermoplastic resin melt that flow in the independent runner by the slit runner flood the continuous fiber that is come by the tensioning roller homodisperse effectively; Continuous fiber behind the dipping along the outlet the center by forming the fiber reinforced thermoplastic resin of predetermined shape; At last, fiber reinforced thermoplastic resin being become length through cooling, pelletizing is the continuous fiber reinforced thermoplastic resin particle of 3～30mm.In this resin particle, continuous fiber is arranged in parallel with each other, and its length is identical with particle length.
Above-mentioned content is weight percentage.
Compared with prior art, the present invention has following beneficial effect:
The present invention is the first long fiber-reinforced polyolefin compound resin master batch of the high fibre content of preparation, then directly and commercialization nylon resin blending and obtain continuous long fiber reinforced composite nylon/polyolefin material.Compare with method described in the aforementioned patent (CN1131427A), the described method of patent of the present invention with the obvious advantage: (1) only needs a kind of material of preparation, it is long fiber-reinforced polyolefin compound resin master batch, and method described in the patent CN1131427A will be produced two kinds of material, be continuous fiber reinforcing polyamide masterbatch and the alloying resin used as thinner, the present invention has saved production cost greatly; (2) compare with production long fiber reinforced Nylon masterbatch resin, the processing temperature of producing long fiber-reinforced polyolefin compound resin master batch is low, and polyolefin resin is difficult for hot oxygen variable color, and controlling of production process is much easier, also just can guarantee the colour stability of product and the stability of other performance.This matrix material is applicable to injection moulding, and continuous fiber is uniformly dispersed in goods, and product surface does not have " revealing fine " phenomenon fully; And the mechanical property of this matrix material, as tensile strength, flexural strength, especially resistance to impact shock etc. is very excellent.
Embodiment
Following embodiment indication content is weight percentage.
Embodiment 1
Co-polypropylene with 36% (Co-PP) resin, 4% polypropylene grafted maleic anhydride (PP-g-MAH) are mixed, and adopting pultrude process to make content of glass fiber is 60% continuous glass fiber reinforced polypropylene compound resin master batch.Then, with the ratio blending of this master batch and nylon 6 (PA6) resin, and be injection molded into the test of standard mechanics test bars with 1: 1.In final matrix material, the content of Co-PP resin is 18%, and the content of PP-g-MAH is 2%, and the content of PA6 resin is 50%, and the content of glass fibre is 30%.
Embodiment 2
Homo-polypropylene with 46.5% (Homo-PP), 3.5% ethylene-octene copolymer (POE) grafted maleic anhydride (POE-g-MAH) are mixed, and adopting pultrude process to make content of glass fiber is 50% continuous glass fiber reinforced polypropylene compound resin master batch.Then, with the ratio blending of this master batch and nylon 66 (PA66) resin, and be injection molded into the test of standard mechanics test bars with 3: 2.In final matrix material, the content of Homo-PP resin is 27.9%, and the content of POE-g-MAH is 2.1%, and the PA66 resin content is 40%, and the content of glass fibre is 30%.
Embodiment 3
High density polyethylene(HDPE) with 45% (HDPE), 5% polyethylene to graft glycidyl methacrylate (PE-g-GMA) are mixed, and adopting pultrude process to make content of glass fiber is that 50% continuous glass fibre strengthens polyethylene compound resin master batch.Then, with the ratio blending of this master batch and nylon 6 (PA6) resin, and be injection molded into the test of standard mechanics test bars with 2: 3.In final matrix material, the HDPE resin content is 18%, and PE-g-GMA content is 2%, and the PA6 resin content is 60%, and the content of glass fibre is 20%.
Embodiment 4
High density polyethylene(HDPE) with 36% (HDPE), 4% polycthylene grafted acryhic (PE-g-AA) are mixed, and adopting pultrude process to make content of glass fiber is that 60% continuous glass fibre strengthens polyethylene compound resin master batch.Then, with the ratio blending of this master batch and nylon 66 (PA66), nylon 6 (PA6) resin, and be injection molded into the test of standard mechanics test bars with 1: 1: 1.In final matrix material, the HDPE resin content is 12%, and PE-g-AA content is 1.4%, and the PA66 resin content is 33.3%, and the PA6 resin content is 33.3%, and the content of glass fibre is 20%.
Embodiment 5
Homo-polypropylene with 34% (Homo-PP) resin, 6% polypropylene grafted maleic anhydride (PP-g-MAH) are mixed, and adopting pultrude process to make aromatic polyamide fibre (Aramid fiber) content is 50% continuous Aramid fiber reinforced polypropylene compound resin master batch.Then, with the ratio blending of this master batch and nylon 6 (PA6) resin, and be injection molded into the test of standard mechanics test bars with 3: 2.In final matrix material, the content of Homo-PP resin is 20.4%, and the content of PP-g-MAH is 3.6%, and the content of PA6 resin is 46%, and the content of Aramid fiber is 30%.
Comparative example 1
Copolymerization with 18% gather polypropylene (Co-PP), 2% polypropylene grafted maleic anhydride (PP-g-MAH), 50% nylon 6 (PA6) mixed after, adopting traditional expressing technique method to prepare content of glass fiber is that 30% short glass fiber strengthens the PA6/Co-PP matrix material, and is injection molded into the test of standard mechanics test bars.
Comparative example 2
Homopolymerization with 27.9% gather polypropylene (Homo-PP), 2.1% ethylene-octene copolymer (POE) grafted maleic anhydride (POE-g-MAH), 40% nylon 66 (PA66) mixed after, adopting traditional expressing technique method to prepare content of glass fiber is that 30% short glass fiber strengthens the PA66/Homo-PP matrix material, and is injection molded into the test of standard mechanics test bars.
Comparative example 3
After high density polyethylene(HDPE) with 18% (HDPE) resin, 2% polycthylene grafted acryhic glycidyl ester (PE-g-GMA), 60% nylon 6 (PA6) resin are mixed, adopting traditional expressing technique method to prepare content of glass fiber is 20% short glass fiber enhanced PA6/HDPE matrix material, and is injection molded into the test of standard mechanics test bars.
Comparative example 4
After high density polyethylene(HDPE) with 12% (HDPE) resin, 1.4% polycthylene grafted acryhic (PE-g-AA), 33.3% nylon 66 (PA66) resin, 33.3% nylon 6 (PA6) resin are mixed, adopting traditional expressing technique method to prepare content of glass fiber is 20% short glass fiber enhanced PA66/PA6/HDPE matrix material, and is injection molded into the test of standard mechanics test bars.
Comparative example 5
After homo-polypropylene with 20.4% (Homo-PP) resin, 3.6% polypropylene grafted maleic anhydride (PP-g-MAH), 46% nylon 6 (PA6) mixed with resin, adopting traditional expressing technique method to prepare the Aramid fibre content is 30% the fibre-reinforced PA6/Homo-PP matrix material of short Aramid, and is injection molded into the test of standard mechanics test bars.
Comparative example 6
Adopting the pultrude process method to make content of glass fiber nylon 6 (PA6) and continuous fiber is that 60% long glass fibres strengthens the PA6 masterbatch resin; After PA6 with 60%, 36% Co-polypropylene (Co-PP), 4% polypropylene grafted maleic anhydride (PP-g-MAH) are mixed, adopt traditional expressing technique method to make the alloying diluent resin.Then, the long glass fibres that obtains is strengthened PA6 masterbatch resin and the ratio blending of alloying diluent resin with 1: 1, and be injection molded into standard mechanics test bars and test.In final matrix material, the content of Co-PP resin is 18%, and the content of PP-g-MAH is 2%, and the content of PA6 resin is 50%, and the content of glass fibre is 30%.
Comparative example 7
It is that 60% long glass fibres strengthens the PA66 masterbatch resin that nylon 66 (PA66) with 40% and continuous fiber adopt the pultrude process method to make content of glass fiber; After PA66 with 30%, 50% nylon 6 (PA6), 18% high density polyethylene(HDPE) (HDPE), 2% polycthylene grafted acryhic (PE-g-AA) are mixed, adopt traditional expressing technique method to make the alloying diluent resin.Then, the long glass fibres that obtains is strengthened PA66 masterbatch resin and the ratio blending of alloying diluent resin with 1: 2, and be injection molded into standard mechanics test bars and test.In final matrix material, the PA66 resin content is 33.3%, and the PA6 resin content is 33.3%, and HDPE content is 12%, and PE-g-AA content is 1.4%, and content of glass fiber is 20%.
Table 1 has been listed the The performance test results of the foregoing description and comparative example.
Table 1
| Project | Tensile strength (MPa) | Notched Izod impact strength (KJ/m 2) | Flexural strength (MPa) | Modulus in flexure (MPa) | Heat-drawn wire (℃) | Color and stability |
| Embodiment 1 | 145 | 36 | 203 | 6800 | 190 | Good |
| Embodiment 2 | 136 | 22 | 195 | 6000 | 188 | Good |
| Embodiment 3 | 135 | 26 | 200 | 6200 | 186 | Good |
| Embodiment 4 | 142 | 24 | 200 | 6400 | 195 | Good |
| Embodiment 5 | 86 | 13 | 130 | 4500 | 189 | Good |
| Comparative example 1 | 117 | 14 | 178 | 6300 | 188 | Fine |
| Comparative example 2 | 109 | 12 | 167 | 5780 | 185 | Fine |
| Comparative example 3 | 105 | 16 | 164 | 5950 | 184 | Fine |
| Comparative example 4 | 114 | 13 | 174 | 6030 | 194 | Fine |
| Comparative example 5 | 63 | 8 | 94 | 4320 | 184 | Fine |
| Comparative example 6 | 147 | 37 | 205 | 6850 | 190 | Difference |
| Comparative example 7 | 145 | 23 | 203 | 6390 | 195 | Very poor |
Claims (8)
1. a continuous long fiber reinforced composite nylon/polyolefin material is characterized in that being formed by continuous fiber enhancing polyolefine compound resin master batch and nylon resin blending.
2. continuous long fiber reinforced composite nylon/polyolefin material according to claim 1 is characterized in that described continuous fiber strengthens polyolefine compound resin master batch and is made up of the polyolefine compound resin of continuous long fiber peacekeeping 20～70 weight % of 30～80 weight %; Wherein the continuous fiber monofilament is arranged in parallel with each other along master batch particle length direction, and length is identical with the master batch particle, is 3～30mm; In whole continuous long fiber reinforced composite nylon/polyolefin material, the content of continuous fiber is 5～60 weight %.
3. continuous long fiber reinforced composite nylon/polyolefin material according to claim 1 and 2 is characterized in that described continuous fiber is a kind of inorganic fibre or at least a organic fibre that is made of all aromatic polyamide fibres and all aromatic polyester fibers that is made of glass fibre, steel fiber, carbon fiber and boron fibre at least.
4. continuous long fiber reinforced composite nylon/polyolefin material according to claim 1 and 2 is characterized in that described polyolefine compound resin is made up of the polyolefin resin of 70～100 weight % and the modified polyolefin resin of 0～30 weight %.
5. continuous long fiber reinforced composite nylon/polyolefin material according to claim 4 is characterized in that described polyolefin resin is one or more the mixture in crystalline polypropylene, polyethylene, ethylene-octene copolymer, ethylene-propylene-diene terpolymer, the ethylene-propylene copolymer.
6. continuous long fiber reinforced composite nylon/polyolefin material according to claim 4 is characterized in that described modified polyolefin resin is meant one or more the mixture in crystalline polypropylene with unsaturated carboxylic acid or its acid anhydrides or derivatives thereof modification, polyethylene, ethylene-octene copolymer, ethylene-propylene-diene terpolymer, the ethylene-propylene copolymer.
7. continuous long fiber reinforced composite nylon/polyolefin material according to claim 1 is characterized in that described nylon resin is one or more the mixture in nylon 6, nylon 66, Ni Long11, nylon 12, NYLON610, the nylon 612.
8. the preparation method of the described continuous long fiber reinforced composite nylon/polyolefin material of claim 1 is characterized in that comprising the steps:
(1) continuous long fiber peacekeeping polyolefine compound resin is adopted pultrusion method make continuous fiber and strengthens polyolefine compound resin master batch:
(2) continuous fiber is strengthened polyolefine compound resin master batch and nylon resin and be blended into continuous long fiber reinforced composite nylon/polyolefin material.
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| CN100372885C true CN100372885C (en) | 2008-03-05 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: JINFA TECHNOLOGY CO., LTD.; SHANGHAI JINFA TECHNOL Free format text: FORMER NAME OR ADDRESS: GUANGZHOU JINFA SCIENCE + TECHNOLOGY CO. LTD.; SHANGHAI JINFA TECHNOLOGY DEVELOPMENT CO., LTD. |
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| CP03 | Change of name, title or address |
Address after: Ke Feng Lu Science City high tech Industrial Development Zone of Guangzhou City, Guangdong Province, No. 33 zip code: 510520 Co-patentee after: Shanghai Kingfa Science and Technology Development Co., Ltd. Patentee after: Blonde Polytron Technologies Inc Address before: Guangdong city of Guangzhou province Tianhe District blonde Ke Mu Lang Industrial Zone Gaotang Polytron Technologies Inc zip code: 510520 Co-patentee before: Shanghai Kingfa Science and Technology Development Co., Ltd. Patentee before: Guangzhou blonde Polytron Technologies Inc |
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Mianyang Dongfang Special Engineering Plastic Co., Ltd. Assignor: Shanghai Blonde Technology Development Co., Ltd.|Blonde Technology Co., Ltd Contract record no.: 2010440001088 Denomination of invention: Continuous long fiber reinforced composite nylon/polyolefin material and its prepn Granted publication date: 20080305 License type: Exclusive License Open date: 20060802 Record date: 20100803 |