CN113789049B - Glass fiber reinforced nylon composite material with high welding strength and preparation method thereof - Google Patents
Glass fiber reinforced nylon composite material with high welding strength and preparation method thereof Download PDFInfo
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/10—Reinforcing macromolecular compounds with loose or coherent fibrous material characterised by the additives used in the polymer mixture
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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Abstract
The invention discloses a glass fiber reinforced nylon composite material with high welding strength and a preparation method thereof, and belongs to the field of nylon composite materials. The nylon composite material comprises the following components in parts by weight: 60-75 parts of nylon 66, 30-35 parts of short glass fiber, 1-10 parts of polar polyolefin resin, 6 0-20 parts of high-fluidity nylon, 0-10 parts of EVA block polyolefin, 0-10 parts of compatilizer and 0-5 parts of antioxidant. According to the invention, the polar polyolefin is added into the glass fiber reinforced nylon to endow polar groups, so that intermolecular acting force is greatly improved, intermolecular winding is facilitated, and fusion condition is facilitated. The high fluidity nylon 6, the compatilizer and the EVA block polyolefin improve the bonding degree of the base material and the interpenetrating crosslinked grid structure under the synergistic effect, and improve the weld mark strength of the material, and the weld mark strength of the obtained nylon composite material can reach 129MPa.
Description
Technical Field
The invention relates to the technical field of nylon composite materials, in particular to a glass fiber reinforced nylon composite material with high welding strength and a preparation method thereof.
Background
Nylon is the general plastic with the largest usage amount, nylon and fiber are added into the mixture for blending modification, and the obtained nylon composite material can be used as an application with higher strength, is widely applied to industries such as industry, automobiles and the like, and is an indispensable material for replacing steel with plastic. The integral strength of glass fiber added into nylon is greatly improved, but the welding line strength is not improved, and the application of glass fiber reinforced modified nylon is greatly limited, so that the improvement of the welding mark strength of glass fiber reinforced nylon is urgently needed, and the method is an important step for replacing the steel theme with plastic.
Glass fiber reinforced nylon melt is chaotic in glass fiber distribution at the weld mark, the fusion effect of the base material is poor, the strength of the weld mark of the product is only 40-60% of the overall tensile strength of the glass fiber reinforced nylon melt, so that the distribution and penetration rate of the glass fiber at the weld line and the fusion condition of the base material are improved, and the higher strength of the weld mark is endowed.
The weld mark strength is improved from the material angle direction, and published patent application numbers CN201911050576.8 (a high weld mark strength glass fiber reinforced polyamide composite material and a preparation method thereof) and CN101735577A (a high weld mark strength reinforced polybutylene terephthalate material and a preparation method thereof) are available, and the weld mark strength is improved in a higher degree from the material angle.
CN200810218925.8 discloses a polypropylene material with high weld mark strength and a preparation method thereof, in the patent, by improving interface bondability, the viscosity of a disperse phase is improved, the orientation of a polypropylene molecular chain and glass fiber along a vertical flow direction is hindered, and by reducing the orientation of the glass fiber, the bridging level of the glass fiber to an interface is improved, so that the weld mark strength is improved.
CN201811168956.7 discloses a permeation resistant air conditioning hose. The inner liner is a modified polyamide nylon alloy obtained by blending polyamide and modified polyolefin containing carboxyl, and the air hose has higher permeability resistance.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the glass fiber reinforced nylon composite material with high welding strength.
The invention also aims to provide a preparation method of the glass fiber reinforced nylon composite material with high welding strength.
The invention is realized by the following technical scheme.
The glass fiber reinforced nylon composite material with high welding strength comprises the following components in parts by weight:
preferably, the high-welding-strength glass fiber reinforced nylon composite material comprises the following components in parts by weight:
preferably, the high-welding-strength glass fiber reinforced nylon composite material comprises the following components in parts by weight:
preferably, the melt flow rate of the nylon 66 is 10-40 g/10min,2.16kg/230 ℃, and the testing method is GB/T3682.1-2018.
Preferably, the high fluidity nylon 6 is nylon 6 with the melting point below 200 ℃ and the intrinsic viscosity index of 2.0, and the test method is GB/T3682.1-2018. The high-flow nylon 6 is easier to flow to the front end of the melt under the injection molding condition, so that the glass fiber orientation and the penetration rate at the weld mark position are certain facilitated, and the fusion effect at the weld mark position is improved.
Preferably, the short glass fiber is a chopped glass fiber, the aspect ratio of the cross section of the chopped glass fiber is cylindrical glass fiber which tends to be 1:1, and the glass fiber treated by the surface treatment agent has the diameter of 10 mu m.
Preferably, the surface treatment agent is one or more of a silane coupling agent, a titanane coupling agent and an aluminate coupling agent.
Preferably, the polar polyolefin resin is an acrylate-acrylamide copolymer having a molecular weight of 9000 to 12000.
Preferably, the EVA block polyolefin is in the form of a block copolymer, is an ethylene-vinyl acetate copolymer, and has a melt index of 20-50 g/min under the test condition of 190 ℃ and 2.16 Kg.
Preferably, the compatilizer is one or a combination of more than one of EPDM (ethylene propylene diene monomer), POE (polyolefin elastomer) and SEBS (styrene-ethylene-butylene-styrene block copolymer) grafted by maleic anhydride.
Preferably, the antioxidant is one or more of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ], distearyl thiopropionate, dilauryl thiopropionate, ditridecyl thiopropionate and octadecyl-3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate.
Of course, it is also possible to add some aids for improving the processing adjustment, such as lubricants, and some uv-resistant agents, high temperature stabilizers, and the like, for improving other weather resistance.
The method for preparing the high-welding-strength glass fiber reinforced nylon composite material comprises the following steps of:
the raw materials are weighed according to the proportion, nylon 66, polar polyolefin resin, high-fluidity nylon 6, EVA block polyolefin, compatilizer and antioxidant are fed from a main feeding port of a double-screw extruder, short glass fibers are added from a side feeding port, after melt blending extrusion in the double-screw extruder, the glass fiber reinforced nylon composite material with high welding strength is obtained through cooling, air drying and granulating, the extrusion temperature is set to 270-280 ℃, the rotating speed of a host screw is 300-600rpm, and the length-diameter ratio of the screw is 56:1.
The invention adopts a 56:1 large length-diameter ratio double screw extruder so as to arrange a plurality of side feeds, so that glass fibers are subjected to 'pre-infiltration', and the retention length and the glass fiber addition amount are increased.
The polar polyolefin resin is added into the invention to be the resin containing polar groups, which is one or two of acrylic ester-acrylamide copolymer or sulfonated polyolefin wax, the polar groups are enriched and tightly combined at the front end of melt flow, so that the concentration of ionic bonds of base materials at two ends of a weld mark is endowed, the composite material obtains higher intermolecular acting force, the intermolecular winding at two ends of the weld mark is facilitated, the fusion condition of the molten material is improved, and the strength of the weld mark is improved. The nylon base material contains polar amide groups, hydrogen bonds are formed, the hydrogen bonds are also intermolecular acting force, and the weld mark strength can be improved, so that the reason that the weld mark strength of the glass fiber modified nylon 66 base material is slightly higher than that of a pure material can be laterally described. The ionic bond contained in the polar polyolefin resin added by the invention belongs to one of chemical bonds, is stronger than hydrogen bond and weaker than Van der Waals force, so that higher intermolecular acting force can be given to weld marks, the intermolecular acting force is greatly improved, intermolecular winding is facilitated, the bonding degree of a base material is higher, and fusion is facilitated.
According to the invention, the combination degree of the base material and the orientation of glass fibers are researched and modified at the weld mark in the aspect of materials, and the strength of the weld mark is greatly improved.
Because two kinds of nylon are added, the strength of weld marks is affected certainly due to the problem of compatibility, and the improvement of mechanical properties is limited. The invention adopts the POE grafted by maleic anhydride and is matched with polar polyolefin resin and EVA block copolymer. The polar polyolefin resin contains carboxyl which can react with hydroxyl and anhydride groups of a coupling agent on the surface of the fiber respectively, so that the grafting rate of maleic anhydride grafted POE is improved, the compatibilization effect of two kinds of nylon at the injection molding front end is improved, the strength of nylon base materials at weld marks is improved, and the carboxyl reacts with anhydride to generate mono/di-grease, so that EVA and lipid substances are subjected to esterification and transesterification, and long-chain hydrocarbon groups and o-phenyl groups with more complex space structures are simultaneously introduced into the PA, thereby being beneficial to the formation of more complex interpenetrating crosslinked grid structures of the PA base materials and the EVA.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the polar polyolefin is added into the glass fiber reinforced nylon to endow polar groups, so that intermolecular acting force at weld marks is greatly improved, intermolecular winding is facilitated, the substrate bonding degree is higher, and fusion is facilitated. The high fluidity nylon 6, the compatilizer and the EVA block polyolefin improve the bonding degree of the base material and the interpenetrating crosslinked grid structure under the synergistic effect, and improve the weld mark strength of the material.
(2) The invention optimizes the proportion of polar polyolefin and high fluidity nylon 6, and the welding mark strength of the obtained nylon composite material can reach 129MPa under the action of the compatibility agent and EVA block polyolefin.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The following examples and comparative examples were prepared from the following raw materials:
nylon 66;
short glass fibers;
polar polyolefin resin: acrylate-acrylamide copolymer with molecular weight 9000-12000;
high fluidity nylon 6 resin (new mermenda M2000);
EVA block copolymer (trade name E1051);
and (3) a compatilizer: maleic anhydride grafted POE;
an antioxidant: tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ].
The preparation method of the glass fiber reinforced nylon composite material with high welding strength comprises the following steps: raw materials are weighed according to the proportion, auxiliary agents such as nylon resin, polyolefin resin, compatilizer, curing agent, antioxidant and the like are fed from a main feeding port of a double-screw extruder, short glass fibers are added from a side feeding port, and after being melted, blended and extruded in the double-screw extruder, the glass fiber reinforced polyamide/polypropylene alloy composite material with high weld mark strength is obtained through cooling, air drying and granulating, the extrusion temperature is set at 270-280 ℃, the rotating speed of a main screw is 300-600rpm, and the length-diameter ratio of the screw is 56:1.
The performance testing method comprises the following steps:
(1) Weld mark strength: the test is carried out according to the national standard GB/T1040.2-2008 method, and the test sample bars are cast at two ends.
(2) Tensile strength: the test is carried out according to the method of national standard GB/T1040.2-2008.
(3) Flexural strength: the test is carried out according to the method of national standard GB/T9341-2008.
TABLE 1
TABLE 2
As is clear from examples 1 to 9, the polar polyolefin resin and EVA block copolymer were blended with the compatibilizer to prepare a nylon 6 resin having high fluidity, and both of these systems contributed to the weld strength of the substrate, but the weld strength was rather lowered with the addition of the amount. It is understood from examples 1 to 6 and examples 10 and 12 that the amount of the high-fluidity nylon 6 is required to be controlled within the range of 1 to 5 parts, and that the effect is better when 1 to 2 parts are preferable, and that the polar polyolefin resin works best when 2 parts are used.
As is clear from examples 9, 15 and 16, it is preferable that no compatibilizing agent is added to the components, the compatibility of the components is poor, and the compatibility with glass fibers is reduced at the weld line. As can be seen from the combination of examples 8, 14 and 16, the addition of the EVA block copolymer can improve the weld mark strength of the substrate, and the block copolymer can form a dense network structure on the substrate at the weld mark, thereby improving the bonding degree of the substrate.
The weld mark strength of examples 7 and 13, when combined with the EVA polyolefin and the compatibilizer, the polar polyolefin resin and the nylon 6 resin act together, will result in a higher improvement in the weld mark strength of the substrate, probably because the polar polyolefin resin acts on the weld mark, which results in an improved degree of bonding of the weld mark substrate, an improved fusion, and a higher intermolecular force, while the high flowability nylon 6 is advantageous for improving the glass fiber orientation, and increasing the glass fiber penetration rate, thereby improving the weld mark strength. And when the content is 2:2, the effect is optimal, and the weld mark strength of the material is improved.
Claims (9)
1. The glass fiber reinforced nylon composite material with high welding strength is characterized by comprising the following components in parts by weight:
60-75 parts of nylon 66
30-35 parts of short glass fiber
1-10 parts of polar polyolefin resin
6 1-5 parts of high-fluidity nylon
EVA block polyolefin 0-10 parts
0-10 parts of compatilizer
0-5 parts of antioxidant, wherein the EVA block polyolefin and the compatilizer are 0 part at different time;
the polar polyolefin resin is an acrylate-acrylamide copolymer having a molecular weight of 9000 to 12000.
2. The high-weld-strength glass fiber reinforced nylon composite according to claim 1, which is characterized by comprising the following components in parts by weight:
60-75 parts of nylon 66
30-35 parts of short glass fiber
1-2 parts of polar polyolefin resin
6 1-5 parts of high-fluidity nylon
EVA block polyolefin 0-5 parts
0-10 parts of compatilizer
0-5 parts of antioxidant, and 0 part of EVA block polyolefin and compatilizer at different time.
3. The high-weld-strength glass fiber reinforced nylon composite according to claim 2, which is characterized by comprising the following components in parts by weight:
70 parts of nylon 66
30 parts of short glass fiber
Polar polyolefin resin 2 parts
6 2 parts of high-fluidity nylon
EVA block polyolefin 5 parts
10 parts of compatilizer
0.2 parts of antioxidant.
4. A high weld strength glass fiber reinforced nylon composite as claimed in any one of claims 1 to 3, wherein the high flow nylon 6 is nylon 6 having a melting point below 200 ℃ and an intrinsic viscosity index of 2.0.
5. The high weld strength glass fiber reinforced nylon composite of any of claims 1-3, wherein the EVA block polyolefin is an ethylene-vinyl acetate copolymer having a melt index of 20-50 g/min under test conditions of 190 ℃ and 2.16 Kg.
6. The high weld strength glass fiber reinforced nylon composite of any of claims 1-3, wherein the nylon 66 has a melt flow rate of 10-40 g/10min,2.16kg/230 ℃.
7. A high weld strength glass fiber reinforced nylon composite according to any of claims 1-3, wherein the short glass fibers are cylindrical glass fibers having a cross-section aspect ratio of 1:1, and are surface treated with a surface treatment agent having a diameter of 10 μm; the surface treating agent is one or more of silane coupling agent, titanane coupling agent and aluminate coupling agent.
8. A high weld strength glass fiber reinforced nylon composite according to any of claims 1-3, wherein the compatibilizer is a maleic anhydride grafted polyolefin elastomer; the antioxidant is one or more of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ], distearyl thiopropionate, dilauryl thiopropionate, ditridecyl thiopropionate and octadecyl-3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate.
9. A method for preparing the high weld strength glass fiber reinforced nylon composite of any one of claims 1-8, comprising the steps of:
raw materials are weighed according to the proportion, nylon 66, polar polyolefin resin, high-fluidity nylon 6, EVA block polyolefin, compatilizer and antioxidant are fed from a main feeding port of a double-screw extruder, short glass fibers are added from a side feeding port, after melt blending extrusion in the double-screw extruder, the glass fiber reinforced nylon composite material with high welding strength is obtained through cooling, air drying and granulating, the extrusion temperature is set to 270-280 ℃, the rotating speed of a host screw is 300-600rpm, and the length-diameter ratio of the screw is 56:1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153860A (en) * | 2011-04-22 | 2011-08-17 | 江苏金发科技新材料有限公司 | Modified nylon material with high weld line strength and preparation method thereof |
| CN103242649A (en) * | 2012-02-06 | 2013-08-14 | 金发科技股份有限公司 | Glass fiber reinforced nylon material used for extrusion molding, preparation method and application |
| CN103665838A (en) * | 2012-09-12 | 2014-03-26 | 滁州格美特科技有限公司 | Reinforced impact-resistant nylon composite material and preparation method thereof |
| CN106009655A (en) * | 2016-06-16 | 2016-10-12 | 曹晓宏 | High-surface low-wraping glass fiber reinforced PA composite material and preparation method thereof |
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- 2021-08-26 CN CN202110985045.9A patent/CN113789049B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153860A (en) * | 2011-04-22 | 2011-08-17 | 江苏金发科技新材料有限公司 | Modified nylon material with high weld line strength and preparation method thereof |
| CN103242649A (en) * | 2012-02-06 | 2013-08-14 | 金发科技股份有限公司 | Glass fiber reinforced nylon material used for extrusion molding, preparation method and application |
| CN103665838A (en) * | 2012-09-12 | 2014-03-26 | 滁州格美特科技有限公司 | Reinforced impact-resistant nylon composite material and preparation method thereof |
| CN106009655A (en) * | 2016-06-16 | 2016-10-12 | 曹晓宏 | High-surface low-wraping glass fiber reinforced PA composite material and preparation method thereof |
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