CN101696303B - Novel compatibilized polypropylene/glass fiber composite material and preparation method thereof - Google Patents
Novel compatibilized polypropylene/glass fiber composite material and preparation method thereof Download PDFInfo
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- CN101696303B CN101696303B CN2009100357836A CN200910035783A CN101696303B CN 101696303 B CN101696303 B CN 101696303B CN 2009100357836 A CN2009100357836 A CN 2009100357836A CN 200910035783 A CN200910035783 A CN 200910035783A CN 101696303 B CN101696303 B CN 101696303B
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Abstract
The invention relates to a novel compatibilized polypropylene/glass fiber composite material and a preparation method thereof. The polypropylene/glass fiber composite material is prepared from the following materials in percentage by weight: 10 to 15 percent of polypropylene 075, 15 to 20 percent of polypropylene P360, 30 to 35 percent of polypropylene 7032, 4 to 10 percent of epoxy resin, 20 to 30 percent of glass fiber, 0.1 to 0.4 percent of epoxy resin curing agent, 0.3 to 0.6 percent of antioxidant and 0.2 to 0.5 percent of lubricant. The preparation method comprises the following steps: firstly, drying the epoxy resin and the glass fiber; then, evenly mixing the components except the glass fiber inside a mixer according to the percentages; mixing the mixture in a double-screw extruder; adding the glass fiber from a glass fiber inlet of the double-screw extruder; and mixing, extruding, cooling and granulating the mixture in the double-screw extruder to obtain the dynamically cured polypropylene/epoxy resin/glass fiber composite material. The polypropylene/glass fiber composite material has excellent mechanical property and can be used for manufacturing parts such as automobile fan housings and interior trim panels and the like.
Description
Technical field
The present invention relates to polypropylene material, relate in particular to a kind of use dynamical cure Resins, epoxy compatibilized polypropylene/glass fiber composite material and preparation method thereof.
Background technology
In recent years, academia applies to the dynamical cure technology in the thermosetting resin modified thermoplastic resin, has obtained some progress.Show mainly that with the thermoplastics of linearity and thermosetting resin mixing handle through methods such as increase-volumes, the resin after the curing forms inierpeneirating network structure at the two-phase interface place, improve two alternate reactive forces, makes the high performance alloys material with reactive behavior.People such as Jiang Xueliang are applied to dynamical cure Resins, epoxy (EP) in polypropylene/talcum powder system, have prepared the matrix material of excellent property.
Resins, epoxy is a kind of raw material commonly used in the thermosetting resin modified thermoplastic resin, can not only be at the different alternate compatibilizations that play of polymer composites, improve the mechanical property of matrix material, it has good rigidity and intensity after solidifying simultaneously, be evenly distributed in the matrix resin, can improve the rigidity and the modulus of goods.Therefore, the reactive behavior of Resins, epoxy plays more and more important effect in polymer blending is filling-modified.
Summary of the invention
The purpose of this invention is to provide a kind of novel compatibilized polypropylene/glass fiber composite material and preparation method thereof, overcome the inconsistent problem of polypropylene and glass fibre.
Purpose of the present invention is achieved through the following technical solutions:
A kind of novel compatibilized polypropylene/glass fiber composite material, comprise following composition (weight percent): polypropylene 075:10～15%, polypropylene P360:15～20%, polypropylene 7032:30～35%, Resins, epoxy: 4～10%, glass fibre: 20～30%, epoxy curing agent: 0.1～0.4%, oxidation inhibitor: 0.3～0.6%, lubricant: 0.2～0.5%.
Above-mentioned a kind of novel compatibilized polypropylene/glass fiber composite material, optimum ratio is: polypropylene 075:14%, polypropylene P360:18%, polypropylene 7032:33%, Resins, epoxy: 4%, glass fibre: 30%, epoxy curing agent: 0.4%, oxidation inhibitor: 0.3%, lubricant: 0.3%.
Above-mentioned a kind of novel compatibilized polypropylene/glass fiber composite material, wherein, the oxirane value of described Resins, epoxy is 0.04～0.07eq/100g, and epoxy equivalent (weight) is 1425～2500g/eq, and softening point temperature is 110～135 ℃; Described glass fibre is an alkali-free glass fibre yarn, and diameter is 10～13 μ m; Described epoxy curing agent is 2-ethyl-4-methylimidazole (EMI-2,4); Described oxidation inhibitor is the compound of antioxidant 1010 and oxidation inhibitor 168, and compound proportion is 1: 2; Described lubricant is an ethylene bis stearamide.
The preparation method of novel compatibilized polypropylene/glass fiber composite material of the present invention may further comprise the steps:
1. raw material drying: with glass fibre and Resins, epoxy oven dry;
2. curing agent solution preparation: epoxy curing agent and acetone are mixed with solution in 1: 20 ratio (volume ratio);
3. raw material mixes: mix in mixing machine according to acetone soln, oxidation inhibitor and the lubricant of proportioning with polypropylene 075, polypropylene P360, polypropylene 7032, Resins, epoxy, solidifying agent;
4. glass fibre is reinforced: glass fiber yarn adds from the glass intake of twin screw extruder;
5. mixing in twin screw extruder: the mixture adding twin screw extruder that 3. step obtains is mixing with glass fibre, and the twin screw extruder temperature is set between 170～220 ℃, and the twin screw extruder screw speed is at 300～350r.min
-1
6. the material that obtains is extruded postcooling, pelletizing, promptly obtain dynamical cure polypropylene/epoxy resin/glass fiber compound material.
Further, the preparation method of above-mentioned a kind of novel compatibilized polypropylene/glass fiber composite material at first, 80 ℃ of oven dry, is mixed with solution with epoxy curing agent and acetone in 1: 20 ratio (volume ratio) with alkali free glass fibre and Resins, epoxy; Then, 075,18 parts of polypropylene P360 of 14 parts of polypropylene, 7032,4 parts of Resins, epoxy of 33 parts of polypropylene, 0.4 part of solidifying agent (form with acetone soln is added), 0.3 part of oxidation inhibitor and 0.3 part of lubricant are mixed in mixing machine, and 30 parts of alkali-free glass fibre yarns add from the glass intake of twin screw extruder; It is mixing with alkali free glass fibre that mixture adds twin screw extruder, and the temperature that twin screw extruder is every section is respectively: T
1=170 ℃, T
2=180 ℃, T
3=190 ℃, T
4=205 ℃, T
5=210 ℃, T
6=220 ℃, the twin screw extruder rotating speed is r=350r.min
-1, last, extrude, cooling, pelletizing promptly obtain, and promptly obtains dynamical cure polypropylene/epoxy resin/glass fiber compound material.
Substantive distinguishing features and obvious improvement that technical solution of the present invention is outstanding are mainly reflected in:
The employing polypropylene is a matrix resin, and glass fibre is a strongthener, and thermosetting epoxy resin is that compatilizer makes dynamical cure polypropylene/epoxy resin/glass fiber compound material.On the one hand, Resins, epoxy has certain polarity, with glass fibre consistency is preferably arranged; On the other hand, in the course of processing, Resins, epoxy solidifies under the effect of solidifying agent, form inierpeneirating network structure between solidified Resins, epoxy and the polypropylene molecular chain, effect by two aspects, play the effect that increases glass fibre and polypropylene interface interaction power, thereby improve the mechanical property of matrix material, this material is applicable to parts such as making automobile fan cover, trim panel.
Embodiment
The present invention is applied to dynamical cure Resins, epoxy in the polypropylene/glass fiber compound system, the Resins, epoxy of dynamical cure forms inierpeneirating network structure at the interface at polypropylene and glass fibre, reach the purpose that improves polypropylene and glass fibre interface interaction power, make dynamical cure PP/EP/GF matrix material.
Novel compatibilized polypropylene/glass fiber composite material, prescription is: polypropylene 075:10～15%, polypropylene P360:15～20%, polypropylene 7032:30～35%, Resins, epoxy: 4～10%, glass fibre: 20～30%, epoxy curing agent: 0.1～0.4%, oxidation inhibitor: 0.3～0.6%, lubricant: 0.2～0.5%.Screening formulation is: polypropylene 075:14%, and polypropylene P360:18%, polypropylene 7032:33%, Resins, epoxy: 4%, glass fibre: 30%, epoxy curing agent: 0.4%, oxidation inhibitor: 0.3%, lubricant: 0.3%.
Wherein, the oxirane value of Resins, epoxy is 0.04～0.07eq/100g, and epoxy equivalent (weight) is 1425～2500g/eq, and softening point temperature is 110～135 ℃; Glass fibre is an alkali-free glass fibre yarn, and diameter is 10～13 μ m; Epoxy curing agent is 2-ethyl-4-methylimidazole (EMI-2,4); Lubricant is ethylene bis stearamide, Zinic stearas, polyethylene wax, Poly Propylene Wax; Oxidation inhibitor is the compound (antioxidant 1010 is 1: 2 with the composite ratio of oxidation inhibitor 168) of antioxidant 1010 and oxidation inhibitor 168.
Concrete preparation technology is: 1. raw material drying: with glass fibre and Resins, epoxy oven dry; 2. curing agent solution preparation: epoxy curing agent and acetone are mixed with solution in 1: 20 ratio (volume ratio); 3. raw material mixes: mix in mixing machine according to acetone soln, oxidation inhibitor and the lubricant of proportioning with polypropylene 075, polypropylene P360, polypropylene 7032, Resins, epoxy, solidifying agent; 4. glass fibre is reinforced: glass fiber yarn adds from the glass intake of twin screw extruder; 5. mixing in twin screw extruder: the mixture adding twin screw extruder that 3. step obtains is mixing with glass fibre, and the twin screw extruder temperature is set between 170～220 ℃, and the twin screw extruder screw speed is at 300～350r.min
-16. the material that obtains is extruded postcooling, pelletizing, promptly obtain dynamical cure polypropylene/epoxy resin/glass fiber compound material.
With specific embodiment, the present invention will be further described below.
Embodiment 1:
With 14 parts of polypropylene 075,18 parts of polypropylene P360,33 parts of polypropylene 7032,4 parts of Resins, epoxy, 0.4 part 2-ethyl-4-methylimidazole, 0.3 part of oxidation inhibitor and 0.3 part of ethylene bis stearamide mix in high-speed mixer, and mixture is mixing in twin screw extruder, extrude, 30 parts of glass fibre add from the glass intake of forcing machine, and every section temperature of forcing machine is set at T
1=170 ℃, T
2=180 ℃, T
3=190 ℃, T
4=205 ℃, T
5=210 ℃, T
6=220 ℃, rotating speed 350r/min promptly obtains dynamical cure polypropylene/epoxy resin/glass fiber pellets after the cooling and dicing.
Embodiment 2:
With 10 parts of polypropylene 075,20 parts of polypropylene P360,35 parts of polypropylene 7032,9 parts of Resins, epoxy, 0.1 part 2-ethyl-4-methylimidazole, 0.4 part of oxidation inhibitor and 0.5 part of Zinic stearas mix in high-speed mixer, and mixture is mixing in twin screw extruder, extrude, 25 parts of glass fibre add from the glass intake of forcing machine, and every section temperature of forcing machine is set at T
1=170 ℃, T
2=190 ℃, T
3=195 ℃, T
4=200 ℃, T
5=205 ℃, T
6=210 ℃, rotating speed 300r/min promptly obtains dynamical cure polypropylene/epoxy resin/glass fiber pellets after the cooling and dicing.
Embodiment 3:
With 15 parts of polypropylene 075,15 parts of polypropylene P360,35 parts of polypropylene 7032,6 parts of Resins, epoxy, 0.1 part 2-ethyl-4-methylimidazole, 0.6 part of oxidation inhibitor and 0.3 part of polyethylene wax mix in high-speed mixer, and mixture is mixing in twin screw extruder, extrude, 28 parts of glass fibre add from the glass intake of forcing machine, and every section temperature of forcing machine is set at T
1=180 ℃, T
2=190 ℃, T
3=200 ℃, T
4=205 ℃, T
5=215 ℃, T
6=220 ℃, rotating speed is 300r/min, promptly obtains dynamical cure polypropylene/epoxy resin/glass fiber pellets after the cooling and dicing.
Embodiment 4:
With 15 parts of polypropylene 075,20 parts of polypropylene P360,34 parts of polypropylene 7032,10 parts of Resins, epoxy, 0.3 part solidifying agent, 0.5 part of oxidation inhibitor and 0.2 part of Poly Propylene Wax mix in high-speed mixer, and mixture is mixing in twin screw extruder, extrude, 20 parts of glass fibre add from the glass intake of forcing machine, and every section temperature of forcing machine is set at T
1=175 ℃, T
2=185 ℃, T
3=195 ℃, T
4=205 ℃, T
5=210 ℃, T
6=220 ℃, rotating speed 350r/min promptly obtains dynamical cure polypropylene/epoxy resin/glass fiber pellets after the cooling and dicing.
Embodiment 5:
With 12 parts of polypropylene 075,20 parts of polypropylene P360,30 parts of polypropylene 7032,7 parts of Resins, epoxy, 0.2 part solidifying agent, 0.4 part of oxidation inhibitor and 0.4 part of lubricant mix in high-speed mixer, and mixture is mixing in twin screw extruder, extrude, 30 parts of glass fibre add from the glass intake of forcing machine, and every section temperature of forcing machine is set at T
1=170 ℃, T
2=180 ℃, T
3=190 ℃, T
4=195 ℃, T
5=200 ℃, T
6=210 ℃, rotating speed 320r/min promptly obtains dynamical cure polypropylene/epoxy resin/glass fiber pellets after the cooling and dicing.
Be injection molded into the standard batten after the above embodiment gained pellet drying, be used for performance test, adopt the testing method of national standard, the gained result is as shown in table 1.
Table 1 embodiment performance test table
Can find out that from above-mentioned The performance test results its performance is very excellent.
In sum, the present invention adopts the expanding material of Resins, epoxy as polypropylene and glass fibre, adopt the dynamical cure technology, Resins, epoxy solidifies when extruding blend, Resins, epoxy after the curing forms inierpeneirating network structure at the interface at glass fibre and polypropylene, reaches the purpose of Reinforced Polypropylene and glass fibre interface interaction power.The mechanical property excellence of this matrix material is an ideal material of making parts such as automobile fan cover, trim panel.
Below only be concrete exemplary applications of the present invention, protection scope of the present invention is not constituted any limitation.All employing equivalents or equivalence are replaced and the technical scheme of formation, all drop within the rights protection scope of the present invention.
Claims (9)
1. compatibilized polypropylene/glass fiber composite material, it is characterized in that comprising following weight percent composition: polypropylene 075:10～15%, polypropylene P360:15～20%, polypropylene 7032:30～35%, Resins, epoxy: 4～10%, glass fibre: 20～30%, epoxy curing agent: 0.1～0.4%, oxidation inhibitor: 0.3～0.6%, lubricant: 0.2～0.5%.
2. a kind of compatibilized polypropylene/glass fiber composite material according to claim 1, it is characterized in that its component has following weight percent: polypropylene 075:14%, polypropylene P360:18%, polypropylene 7032:33%, Resins, epoxy: 4%, glass fibre: 30%, epoxy curing agent: 0.4%, oxidation inhibitor: 0.3%, lubricant: 0.3%.
3. a kind of compatibilized polypropylene/glass fiber composite material according to claim 1 and 2 is characterized in that: the oxirane value of described Resins, epoxy is 0.04～0.07eq/100g, and epoxy equivalent (weight) is 1425～2500g/eq, and softening point temperature is 110～135 ℃.
4. a kind of compatibilized polypropylene/glass fiber composite material according to claim 1 and 2 is characterized in that: described glass fibre is an alkali-free glass fibre yarn, and diameter is 10～13 μ m.
5. a kind of compatibilized polypropylene/glass fiber composite material according to claim 1 and 2 is characterized in that: described epoxy curing agent is a 2-ethyl-4-methylimidazole.
6. a kind of compatibilized polypropylene/glass fiber composite material according to claim 1 and 2 is characterized in that: described oxidation inhibitor is the compound of antioxidant 1010 and oxidation inhibitor 168.
7. a kind of compatibilized polypropylene/glass fiber composite material according to claim 1 and 2 is characterized in that: described lubricant is an ethylene bis stearamide.
8. the preparation method of the described a kind of compatibilized polypropylene/glass fiber composite material of claim 1 is characterized in that may further comprise the steps:
1. raw material drying: with glass fibre and Resins, epoxy oven dry;
2. curing agent solution preparation: epoxy curing agent and acetone are mixed with solution by 1: 20 volume ratio;
3. raw material mixes: mix in mixing machine according to acetone soln, oxidation inhibitor and the lubricant of proportioning with polypropylene 075, polypropylene P360, polypropylene 7032, Resins, epoxy, solidifying agent;
4. glass fibre is reinforced: glass fiber yarn adds from the glass intake of twin screw extruder;
5. mixing in twin screw extruder: the mixture adding twin screw extruder that 3. step obtains is mixing with glass fibre, and the twin screw extruder temperature is set between 170～220 ℃, and the twin screw extruder screw speed is at 300～350r.min
-1
6. the material that obtains is extruded postcooling, pelletizing, promptly obtain dynamical cure polypropylene/epoxy resin/glass fiber compound material.
9. the preparation method of a kind of compatibilized polypropylene/glass fiber composite material according to claim 8, it is characterized in that: at first, alkali free glass fibre and Resins, epoxy 80 ℃ of oven dry, are mixed with solution with epoxy curing agent and acetone by 1: 20 volume ratio; Then, 075,18 parts of polypropylene P360 of 14 parts of polypropylene, 7032,4 parts of Resins, epoxy of 33 parts of polypropylene, the acetone soln of 0.4 part of epoxy curing agent, 0.3 part of oxidation inhibitor and 0.3 part of lubricant are mixed in mixing machine, and 30 parts of alkali-free glass fibre yarns add from the glass intake of twin screw extruder; It is mixing with alkali free glass fibre that mixture adds twin screw extruder, and the temperature that twin screw extruder is every section is respectively: T
1=170 ℃, T
2=180 ℃, T
3=190 ℃, T
4=205 ℃, T
5=210 ℃, T
6=220 ℃, the twin screw extruder rotating speed is r=350r.min
-1, last, extrude, cooling, pelletizing promptly obtain dynamical cure polypropylene/epoxy resin/glass fiber compound material.
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| CN2009100357836A CN101696303B (en) | 2009-10-14 | 2009-10-14 | Novel compatibilized polypropylene/glass fiber composite material and preparation method thereof |
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| CN101696303B true CN101696303B (en) | 2011-09-14 |
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| CN106397982A (en) * | 2016-09-07 | 2017-02-15 | 芜湖德鑫汽车部件有限公司 | High-temperature resistant fan impeller and preparation method thereof |
| CN108794884A (en) * | 2018-05-25 | 2018-11-13 | 宁波星陆汽车部件有限公司 | Nano modification Anti-aging, high-strength degree wheel cover preparation process |
| CN114891320B (en) * | 2022-05-07 | 2023-09-19 | 重庆国际复合材料股份有限公司 | Epoxy resin/chopped glass fiber composite material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583867A (en) * | 2004-05-27 | 2005-02-23 | 上海交通大学 | Preparation of electrostatic resistant and conductive polypropylene blend |
| CN1854180A (en) * | 2005-04-26 | 2006-11-01 | 华德塑料制品有限公司 | Modification of engineering plastics (PP) for vehicle |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583867A (en) * | 2004-05-27 | 2005-02-23 | 上海交通大学 | Preparation of electrostatic resistant and conductive polypropylene blend |
| CN1854180A (en) * | 2005-04-26 | 2006-11-01 | 华德塑料制品有限公司 | Modification of engineering plastics (PP) for vehicle |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2003-201165A 2003.07.15 |
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