CN104151708B - A kind of fibre reinforced PP composite material and preparation method thereof - Google Patents
A kind of fibre reinforced PP composite material and preparation method thereof Download PDFInfo
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- CN104151708B CN104151708B CN201410410747.4A CN201410410747A CN104151708B CN 104151708 B CN104151708 B CN 104151708B CN 201410410747 A CN201410410747 A CN 201410410747A CN 104151708 B CN104151708 B CN 104151708B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of fibre reinforced PP composite material and preparation method thereof.The raw material of this fibre reinforced PP composite material comprises 39～97 parts of polypropylene, 1～40 part of carbon fiber, 1～8 part of modifying agent and 1～10 part of compatilizer according to mass parts, and described modifying agent comprises tetrafluoroborate ion liquid.The present invention uses the modifying agent containing tetrafluoroborate ion liquid that carbon fiber is carried out surface modification, drastically increases carbon fiber modifying effect.Modified carbon fiber is added to polypropylene, it is possible to increase carbon fiber is to polyacrylic reinforced effects so that composite has higher hot strength, bigger bending modulus and stronger notch impact strength, has higher comprehensive mechanical property.
Description
Technical field
The present invention relates to the technical field of carbon fiber, particularly relate to a kind of fibre reinforced polypropylene composite materials material
Material and preparation method thereof.
Background technology
Carbon fiber (carbon fiber, be called for short CF), be a kind of phosphorus content high intensity more than 95%,
The tencel material of high modulus fibre.It is along fiber axially side by organic fibers such as flake graphite crystallites
Form to piling up, the micro crystal graphite material obtained through carbonization and graphitization processing.Carbon fiber is " outer soft interior
Just ", quality is lighter than metallic aluminium, but intensity is higher than iron and steel, and has corrosion-resistant, the spy of high-modulus
Property, it is all important materials at defence and military and civilian aspect.
Owing to carbon fiber has high intensity, low-density, high-temperature resistant, the advantage such as water-fast, corrosion-resistant, can conduct
A kind of excellent reinforcing material.Carbon fiber interpolation is obtained to high polymer the high polymer composite material strengthened, can
To significantly improve the combination property of high polymer.
Polypropylene (PP), is a kind of thermoplastic resin prepared by propylene polymerization, Mechanical Properties of PP
Absolute value higher than polyethylene, thus the market share in plastic industry steps up.Carbon in prior art
TRPP material is poor with the polyacrylic compatibility due to carbon fiber, for improving carbon fiber in poly-third
Alkene mutually in associativity, generally carbon fiber is carried out surface modification.In prior art, often by modifying agent
Limiting etc. factor, the polyacrylic mechanical property of fibre reinforced of preparation is poor.
Summary of the invention
In view of this, one aspect of the present invention provides a kind of fibre reinforced PP composite material, this composite wood
Material has preferable mechanical property.
A kind of fibre reinforced PP composite material, its raw material comprises 39～97 parts poly-third according to mass parts
Alkene, 1～40 part of carbon fiber, 1～8 part of modifying agent and 1～10 part of compatilizer, described modifying agent comprises tetrafluoro
Borate ion liquid.
Modifying agent in the present invention is specially tetrafluoroborate ion liquid or the mixture with polyacrylonitrile.
Tetrafluoroborate is containing vinyl imidazole base, allyl imidazole base, acrylonitrile group imidazole radicals, styryl
Imidazole radicals, epoxy radicals imidazole radicals tetrafluoroborate in one or at least two.What deserves to be explained is, this
In the tetrafluoroborate ion liquid of described each substituent group all use and can buy on market, the present invention is not
Any improvement is made for it.
Wherein, raw material also comprises 0.05～3 part of processing aid in terms of raw material gross mass.Processing aid is antioxygen
Agent, lubricant and light stabilizer.
The raw material of the present invention is not limited to said components, and other component commonly used in the art is also suitable for adding
To this programme, do not repeat them here.
Wherein, carbon fiber is polyacrylonitrile-based carbon fibre or asphalt base carbon fiber.
Preferably, described polypropylene is HOPP and/or COPP；
Preferably, compatilizer is polypropylene grafted maleic anhydride, Research of Grafting Malaic Anhydride Onto Polyethylene, ethylene-pungent
One in alkene grafted maleic anhydride and ethene-vinyl acetate grafted maleic anhydride or at least two；
Preferably, the one during described antioxidant is antioxidant 1010, irgasfos 168, antioxidant 1098
Or at least two；
Preferably, lubricant stearic acid zinc and/or aluminium stearate.
Another aspect of the invention provides the preparation method of a kind of fibre reinforced PP composite material, and using should
The fibre reinforced PP composite material that preparation method prepares has preferable mechanical property.
The preparation method of above-mentioned fibre reinforced PP composite material, comprises the following steps:
(1) 1～8 mass parts modifying agent are carried out surface modification to 1～40 mass parts carbon fibers, changed
Property carbon fiber；
(2) by described modified carbon fiber light irradiate or heating under the conditions of carry out preliminary prepolymerization, obtain
Carbon fiber performed polymer；
(3) 39～97 mass parts polypropylene, 1～40 mass parts carbon fibers, 1～10 mass parts will be comprised
Insert after the raw material mixing of compatilizer and described carbon fiber performed polymer and comminutor carries out granulating and forming.
It is understood that " mass parts " described in above-mentioned steps refers both to fibre reinforced polypropylene multiple
The gross mass meter preparing raw material of condensation material.
Wherein, the mode of surface modification described in step (1) is that carbon fiber is inserted the diluent of modifying agent
Middle dipping, or the diluent of modifying agent is sprayed at carbon fiber surface；
Preferably, the diluent of the diluent of described modifying agent be water, methanol, ethanol, propanol, butanone,
One in toluene or at least two.Certainly other can be used to dilute the organic of tetrafluoroborate ion liquid
Solvent may be suitable for the present invention.
Preferably, the mass concentration of the diluent of described modifying agent is 10～80%, more preferably 20～
50%.Can be understood by one of ordinary skill in the art, here " mass concentration of the diluent of modifying agent "
Refer to modifying agent and account for the percent of diluent gross mass.
Wherein, also include between step (1) neutralization procedure (2) being dried modified carbon fiber；
Preferably, described drying mode is 50～120 DEG C of drying.
Wherein, light described in step (2) irradiates for using ultraviolet light to irradiate or heating prepolymerization mode；
Preferably, the light intensity that described ultraviolet light irradiates is less than 2KW；
Preferably, the time that described ultraviolet light irradiates is 2～15min；
Preferably, the equipment of heating is microwave oven or baking oven；
Preferably, the power of described microwave oven is 150～500W；
Preferably, the time of described microwave-oven-heating is less than 20min；
Preferably, the heating-up temperature of described baking oven is 80～120 DEG C；
Preferably, the heat time heating time of described baking oven is 0.5～2h.
Wherein, mixing described in step (3) uses homogenizer mixing 3～5min；
Preferably, described comminutor uses dual-screw-stem machine comminutor, district's temperature of described dual-screw-stem machine comminutor
Degree is 200～210 DEG C, and two district's temperature of described dual-screw-stem machine comminutor are 205～210 DEG C, described pair of spiral shell
Three district's temperature of bar machine comminutor are 210～215 DEG C, and four district's temperature of described dual-screw-stem machine comminutor are
215～220 DEG C, five district's temperature of described dual-screw-stem machine comminutor are 220～225 DEG C, and described dual-screw-stem machine is made
Grain Ji six district temperature is 220～230 DEG C, and the head temperature of described dual-screw-stem machine comminutor is 230～235
℃。
The routine operation that operation is polypropylene field of pelletize, those skilled in the art can not pass through the present invention
Loading also can obtain relevant technical information, do not repeat them here.
The present invention uses the modifying agent containing tetrafluoroborate ion liquid that carbon fiber is carried out surface modification, pole
The earth improves carbon fiber modifying effect.Modified carbon fiber is added to polypropylene, it is possible to increase carbon is fine
Dimension is to polyacrylic reinforced effects so that composite has higher hot strength, bigger bending modulus
And stronger notch impact strength, there is higher comprehensive mechanical property.
Detailed description of the invention
Technical scheme is further illustrated below in conjunction with embodiment.
Embodiment 1
Fibre reinforced PP composite material prepare raw material according to mass parts, its composition is as follows:
The ethanol dilution liquid of the allyl imidazole tetrafluoroborate ion liquid that carbon fiber is inserted 10% soaks
Stain, filters out carbon fiber after complete wetting.The carbon fiber processed through aforesaid way is it at 50 DEG C
Drying, and carry out preliminary prepolymerization in baking oven, oven temperature controls at 80 DEG C, and the time is 0.5～2 little
Time, obtain carbon fiber performed polymer.
Polypropylene, modifying agent, compatilizer and processing aid are mixed 3～5 minutes in high speed machine high speed
After, carbon fiber is entered from entering fine mouth, is then passed through dual-screw-stem machine and carries out pelletize, wherein a district of screw machine
Temperature is 200 DEG C, two district's temperature are 205 DEG C, three district's temperature are 210 DEG C, four district's temperature are 215 DEG C, five
District's temperature is 220 DEG C, six district's temperature are 220 DEG C, head temperature is 230 DEG C, and extrusion bar passes through circulating water chennel
It is cooled to room temperature, enters pelleter pelletize after drying through hair-dryer, obtain a kind of carbon fiber reinforced poly-third
Alkene composite.
Embodiment 2
Fibre reinforced PP composite material prepare raw material according to mass parts, its composition is as follows:
The ethanol dilution liquid of the allyl imidazole tetrafluoroborate ion liquid by 80% is at blender high speed rotating
Time uniformly spray in carbon fiber surface.It is the carbon fiber processed through aforesaid way at 120 DEG C to be baked to,
And carrying out preliminary prepolymerization under ultraviolet light, the prepolymerized light intensity of ultraviolet light is less than 2KW, during irradiation
Between be 2 minutes, obtain carbon fiber performed polymer.
By polypropylene, modifying agent, compatilizer and processing aid after high speed machine high speed mixes 5 minutes, by carbon
Fiber enters from entering fine mouth, is then passed through dual-screw-stem machine and carries out pelletize, and wherein district's temperature of screw machine is 210
DEG C, two district's temperature be 210 DEG C, three district's temperature be 215 DEG C, four district's temperature be 220 DEG C, five district's temperature be
225 DEG C, six district's temperature be 230 DEG C, head temperature be 235 DEG C, extrusion bar is cooled to room by circulating water chennel
Temperature, enters pelleter pelletize after drying through hair-dryer, obtains a kind of carbon fiber reinforced polypropylene composite materials material
Material.
Embodiment 3
Fibre reinforced PP composite material prepare raw material according to mass parts, its composition is as follows:
The water diluent of the allyl imidazole tetrafluoroborate ion liquid that carbon fiber is inserted 35% impregnates,
Carbon fiber is filtered out after complete wetting.The carbon fiber processed through above two mode is it at 85 DEG C
Drying, and carry out preliminary prepolymerization in microwave oven, the power of microwave oven is 150W, is placed in microwave oven
20 minutes response time within, obtain carbon fiber performed polymer.
By polypropylene, modifying agent, compatilizer and processing aid after high speed machine high speed mixes 4 minutes,
Carbon fiber is entered from entering fine mouth, is then passed through dual-screw-stem machine and carries out pelletize, wherein district's temperature of screw machine
Be 205 DEG C, two district's temperature be 207 DEG C, three district's temperature be 218 DEG C, four district's temperature be 218 DEG C, five district's temperature
Degree is 223 DEG C, six district's temperature are 225 DEG C, head temperature is 232 DEG C, and extrusion bar is cooled down by circulating water chennel
To room temperature, enter pelleter pelletize after drying through hair-dryer, obtain a kind of carbon fiber reinforced polypropylene multiple
Condensation material.
Embodiment 4
Fibre reinforced PP composite material prepare raw material according to mass parts, its composition is as follows:
The ethanol dilution liquid of the allyl imidazole tetrafluoroborate ion liquid by 45% is at blender high-speed rotary
Uniformly spray in carbon fiber surface when turning.It is the carbon fiber processed through aforesaid way at 70 DEG C to be dried
Dry, and carry out preliminary prepolymerization under ultraviolet light, the prepolymerized light intensity of ultraviolet light is less than 2KW, shines
The time of penetrating is 8 minutes, obtains carbon fiber performed polymer.
By polypropylene, modifying agent, compatilizer and processing aid after high speed machine high speed mixes 4 minutes,
Carbon fiber is entered from entering fine mouth, is then passed through dual-screw-stem machine and carries out pelletize, wherein district's temperature of screw machine
Be 205 DEG C, two district's temperature be 208 DEG C, three district's temperature be 213 DEG C, four district's temperature be 218 DEG C, five district's temperature
Degree is 222 DEG C, six district's temperature are 225 DEG C, head temperature is 232 DEG C, and extrusion bar is cooled down by circulating water chennel
To room temperature, enter pelleter pelletize after drying through hair-dryer, obtain a kind of carbon fiber reinforced polypropylene multiple
Condensation material.
Embodiment 5
Fibre reinforced PP composite material prepare raw material according to mass parts, its composition is as follows:
In addition to above-mentioned condition, other are with embodiment 4.
The fibre reinforced PP composite material that embodiment 1～5 obtains is carried out hot strength, bending by force
Degree, bending modulus and the test of notch impact strength, what deserves to be explained is, these tests are art technology
The means of testing that personnel are familiar with, concrete method of testing does not repeats at this.Its test result such as following table:
Table 1
Applicant states, the present invention illustrates detailed process equipment and the technique of the present invention by above-described embodiment
Flow process, but the invention is not limited in above-mentioned detailed process equipment and technological process, i.e. do not mean that the present invention
Have to rely on above-mentioned detailed process equipment and technological process could be implemented.Person of ordinary skill in the field should
This understands, any improvement in the present invention, and the equivalence of raw material each to product of the present invention is replaced and auxiliary element
Interpolation, concrete way choice etc., within the scope of all falling within protection scope of the present invention and disclosure.
Claims (25)
1. a fibre reinforced PP composite material, it is characterized in that, its raw material comprises 39～97 parts of polypropylene, 1～40 part of carbon fiber, 1～8 part of modifying agent and 1～10 part of compatilizer according to mass parts, and described modifying agent is the mixture of tetrafluoroborate ion liquid and polyacrylonitrile；Described tetrafluoroborate ion liquid be containing vinyl imidazole base, allyl imidazole base, acrylonitrile group imidazole radicals, styryl imidazole radicals, epoxy radicals imidazole radicals tetrafluoroborate ion liquid in one or at least two.
Fibre reinforced PP composite material the most according to claim 1, it is characterised in that its raw material also comprises 0.05～3 part of processing aid in terms of raw material gross mass.
Fibre reinforced PP composite material the most according to claim 2, it is characterised in that described processing aid is antioxidant, lubricant and light stabilizer.
Fibre reinforced PP composite material the most according to claim 3, it is characterised in that described lubricant is zinc stearate and/or aluminium stearate.
Fibre reinforced PP composite material the most according to claim 1, it is characterised in that described carbon fiber is polyacrylonitrile-based carbon fibre or asphalt base carbon fiber.
Fibre reinforced PP composite material the most according to claim 1, it is characterised in that described polypropylene is HOPP and/or COPP.
Fibre reinforced PP composite material the most according to claim 1, it is characterized in that, compatilizer is the one in polypropylene grafted maleic anhydride, Research of Grafting Malaic Anhydride Onto Polyethylene, ethylene-octene grafted maleic anhydride and ethene-vinyl acetate grafted maleic anhydride or at least two.
Fibre reinforced PP composite material the most according to claim 3, it is characterised in that described antioxidant is the one in antioxidant 1010, irgasfos 168, antioxidant 1098 or at least two.
9. the method preparing fibre reinforced PP composite material as claimed in claim 1, it is characterised in that comprise the following steps:
(1) 1～8 mass parts modifying agent are carried out surface modification to 1～40 mass parts carbon fibers, obtain modified carbon fiber；
(2) by described modified carbon fiber light irradiate or heating under the conditions of carry out preliminary prepolymerization, obtain carbon fiber performed polymer；
(3) by comprise 39～97 mass parts polypropylene, 1～10 mass parts compatilizer and described carbon fiber performed polymer raw material mixing after insert comminutor carry out granulating and forming.
Method the most according to claim 9, it is characterised in that the mode of surface modification described in step (1) is to impregnate in the diluent that carbon fiber is inserted modifying agent, or the diluent of modifying agent is sprayed at carbon fiber surface.
11. methods according to claim 10, it is characterised in that the diluent of the diluent of described modifying agent is the one in water, methanol, ethanol, propanol, butanone, toluene or at least two.
12. methods according to claim 10, it is characterised in that the mass concentration of the diluent of described modifying agent is 10～80%.
13. methods according to claim 10, it is characterised in that the mass concentration of the diluent of described modifying agent is 20～50%.
14. methods according to claim 9, it is characterised in that also include between step (1) neutralization procedure (2) being dried modified carbon fiber.
15. methods according to claim 14, it is characterised in that described drying mode is 50～120 DEG C of drying.
16. methods according to claim 9, it is characterised in that light described in step (2) irradiates for using ultraviolet light to irradiate.
17. methods according to claim 16, it is characterised in that the light intensity that described ultraviolet light irradiates is less than 2KW.
18. methods according to claim 16, it is characterised in that the time that described ultraviolet light irradiates is 2～15min.
19. methods according to claim 9, it is characterised in that the equipment of heating is baking oven or microwave oven.
20. methods according to claim 19, it is characterised in that the power of described microwave oven is 150～500W.
21. methods according to claim 19, it is characterised in that the time of described microwave oven is less than 20min.
22. methods according to claim 19, it is characterised in that the heating-up temperature of described baking oven is 80～120 DEG C.
23. methods according to claim 19, it is characterised in that the heat time heating time of described baking oven is 0.5～2h.
24. methods according to claim 9, it is characterised in that mixing described in step (3) uses homogenizer mixing 3～5min.
25. methods according to claim 9, it is characterized in that, described comminutor uses dual-screw-stem machine comminutor, one district's temperature of described dual-screw-stem machine comminutor is 200～210 DEG C, two district's temperature of described dual-screw-stem machine comminutor are 205～210 DEG C, three district's temperature of described dual-screw-stem machine comminutor are 210～215 DEG C, four district's temperature of described dual-screw-stem machine comminutor are 215～220 DEG C, five district's temperature of described dual-screw-stem machine comminutor are 220～225 DEG C, six district's temperature of described dual-screw-stem machine comminutor are 220～230 DEG C, the head temperature of described dual-screw-stem machine comminutor is 230～235 DEG C.
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| CN104774437B (en) * | 2015-04-07 | 2017-07-04 | 北京汽车股份有限公司 | A kind of carbon fiber enhancement polylactic acid composite and its preparation method and application |
| CN105199234A (en) * | 2015-11-11 | 2015-12-30 | 贵州凯科特材料有限公司 | Carbon fiber reinforced polypropylene composite and preparation method thereof |
| CN105670162B (en) * | 2016-01-20 | 2018-05-11 | 林家豪 | A kind of preparation method of high tenacity anti-static PVC composite sole material |
| KR20220152582A (en) | 2016-08-12 | 2022-11-16 | 다우 글로벌 테크놀로지스 엘엘씨 | The propylene system composition including the carbon fiber and thermoplastic polyolefin elastomer |
| SG11201901113QA (en) | 2016-08-12 | 2019-03-28 | Dow Global Technologies Llc | Compositions comprising carbon fibers and at least one thermoplastic polyolefin elastomer |
| CN106366405A (en) * | 2016-08-30 | 2017-02-01 | 盐城市艾斯特体育器材有限公司 | Polymer composition for manufacturing high-elasticity table tennis ball |
| CN114213751B (en) * | 2021-12-09 | 2022-07-15 | 福建师范大学泉港石化研究院 | Carbon fiber reinforced polypropylene composite material and preparation method thereof |
| CN114752152B (en) * | 2022-06-02 | 2024-04-12 | 福建师范大学泉港石化研究院 | Modified carbon fiber reinforced high-filling nano calcium carbonate polypropylene composite material and preparation method thereof |
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| CN102180458A (en) * | 2011-03-25 | 2011-09-14 | 深圳市贝特瑞纳米科技有限公司 | Nano-carbon material dispersion liquid and preparation method and equipment thereof |
| CN102604232A (en) * | 2011-01-20 | 2012-07-25 | 合肥杰事杰新材料股份有限公司 | Antistatic polypropylene material and preparation method thereof |
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| CN102604232A (en) * | 2011-01-20 | 2012-07-25 | 合肥杰事杰新材料股份有限公司 | Antistatic polypropylene material and preparation method thereof |
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