CN101358011B - Polypropylene-Kevlar fiber composite material and preparation method thereof - Google Patents
Polypropylene-Kevlar fiber composite material and preparation method thereof Download PDFInfo
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- CN101358011B CN101358011B CN2008103047875A CN200810304787A CN101358011B CN 101358011 B CN101358011 B CN 101358011B CN 2008103047875 A CN2008103047875 A CN 2008103047875A CN 200810304787 A CN200810304787 A CN 200810304787A CN 101358011 B CN101358011 B CN 101358011B
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Abstract
The invention provides a polypropylene-Kevlar fiber composite material and a preparation method thereof. The invention adopts polypropylene, Kevlar fiber, PP-g-MAH-St graft and composite antioxidant as raw materials. The preparation process includes the following steps: ultrasound processing of Kevlar fiber; hydrolysis of Kevlar fiber; preparation of compatibilizer PP-g-MAH/St Graft and preparation of the polypropylene / Kevlar composite material. The invention adopts amidocyanogen of the surface of modified Kevlar fiber, which is capable of forming acid amide chemical bonds with compatibilizer PP-g-MAH/St, and solves the problem that the compatibility of fibers and polypropylene is poor, and greatly enhances interface bending strength of composite material, effectively improves the properties such as the tensile strength, the bending strength, the impact strength and the heat distortion temperature, etc, of the composite material. The composite material prepared with the method of the invention is applicable to the technical fields like aviation, astronavigation, military science, automobile, machinery, electrical and electronic field, petrochemical field, etc.
Description
Technical field
The invention belongs to technical field of polymer materials, more specifically relate to a kind of polypropylene-Kevlar fiber composite material and preparation method thereof.
Background technology
Polypropylene (PP) is because machine-shaping, product high comprehensive performance are enriched, are easy in original source, and purposes is very extensive, has become kind with fastest developing speed in the resins for universal use.In the research and development of general-purpose plastics through engineering approaches, PP has one of material of development potentiality most.But also there are some shortcomings in polypropylene,, shrinking percentage poor such as winter hardiness is big, creep resistance is poor, product size poor stability, suitability for secondary processing are poor, with the consistency difference of other polar polymers and mineral filler etc., thereby limited the further application of polypropylene through engineering approaches.In order to improve polyacrylic performance, prolong its work-ing life and broadened application scope, need it is carried out modification.
At present, compound enhancing modified is a kind of very effective, simple, economic, suitable method of polypropylene being carried out modification.Wherein, with the acrylic resin is base material, adopting fiber (glass fibre, natural fiber or synthon etc.) enhanced method, make it have better rigidity, shock resistance, creep resistance, thermostability and dimensional stability, is an importance of polypropylene material study on the modification and application.The fiber species that is used to make reinforced composite is a lot, mainly contains glass fibre, carbon fiber, aramid fiber, also has nylon, trevira and boron fibre, whisker etc. in addition.Glass fibre reinforced modified PP matrix material has become present widely used polymer matrix composites, but still has the deficiency of feasibility: the recycling difficulty, can cause environmental pollution; Forming process is difficulty relatively; For satisfying the requirement of a certain specified property, also must strengthen with the combination of fiber; Do not satisfy the occasion of mechanical property requirements at the chopped strand pellet, also must use macrofiber to strengthen.And polymer fiber not only has the general advantage of fiber reinforcement PP material, strengthens the incomparable advantage of PP matrix material but also have some common glasses.
Aramid fiber, the full name aromatic polyamide fibre is the novel polymeric fibres of a kind of high strength, high-modulus and light weight.Its representative kind is the Kevlar fiber of U.S. DuPont company exploitation, and chemical constitution is a PPTA.Kevlar fiber relative density only is 1.43～1.45, and specific tenacity is 5 times of steel wire, and has good thermostability.The aramid fiber reinforced composite has been successfully applied to fields such as aerospace, aircraft, boats and ships, sports goods, but the applied research of its reinforced polypropylene compound material report is less, so research preparation aramid fiber reinforced polypropylene compound material is that realistic meaning is arranged very much.
Summary of the invention
The invention provides a kind of polypropylene-Kevlar fiber composite material and preparation method thereof, solve the problem of polypropylene and Kevlar (aramid fiber) consistency difference, the preparation method is simple, practical, significantly improve composite materials property (as tensile strength, flexural strength, shock strength), the broadened application field.
Polypropylene-Kevlar fiber composite material of the present invention, it is characterized in that: the composition of raw materials of described polypropylene-Kevlar fiber composite material is: according to mass ratio: 100 parts of polypropylene PP, 3～5 parts of Kevlar fibers, 5～20 parts of PP-g-MAH-St graftss, 0.5～1 part of composite antioxidant.
Preparation method's technical scheme of the present invention is:
The supersound process of Kevlar is to wash the impurity that the Kevlar fiber surface adheres to off.
To place alkali lye through the Kevlar fiber of supersound process, processing is hydrolyzed.
The Kevlar fiber is after hydrolysis, and its surperficial amido quantity increases.
Preparation PP-g-MAH-St grafts is to be used as the expanding material in the matrix material.
By prepared in twin-screw extruder polypropylene/Kevlar fibre composite.
Preparation principle of the present invention and remarkable advantage are: at first the hydrolysis of Kevlar fiber produces amido, Kevlar fiber/PP-g-(MAH-co-St)/PP is by the twin screw extruder melt blending then, the amido of the Kevlar fiber surface of modification in this process can form the acid amides chemical bond with the anhydride group of expanding material PP-g-MAH/St, thereby fiber and polyacrylic consistency have been increased, strengthen the interface binding power of matrix material, and can improve the mechanical property (as tensile strength, flexural strength, shock strength) of matrix material effectively.
The PP/KF matrix material of modification organically combines the over-all properties of fortifying fibre and matrix resin, can be used for each field such as Aeronautics and Astronautics, military affairs, automobile, machinery, electric, petrochemical industry; And the preparation method is simple, fast efficient, is fit to apply on a large scale, has remarkable economic efficiency.
Embodiment
Preparation method's step is:
The supersound process of Kevlar fiber: the Kevlar fiber is put into encloses container, is solvent with ethanol, and supersound process 12～16h removes the fiber surface foreign material, then that the vacuum-drying of surface treated Kevlar fiber is standby;
The hydrolysis of Kevlar fiber: will place NaOH aqueous solution hydrolysis reaction 12～16h of 8～12% through the Kevlar fiber of step (1) supersound process, solution temperature is controlled at 90～100 ℃, and its product water is washed till neutrality, and vacuum-drying is standby then; Reaction mechanism is as follows:
The preparation of PP-g-MAH-St grafts: in the reactor that has agitator, add polypropylene PP, benzoyl peroxide BPO, dimethylbenzene, at N
2Leave standstill swelling 1～2h under the atmosphere; Add maleic anhydride MAH and vinylbenzene St then, be warming up to 120 ℃, start mechanical stirring, reaction 1～2h after reaction finishes, continues logical N
2For some time is till graft product cools off fully; Graft product is placed apparatus,Soxhlet's, with acetone extracting 24h, remove not grafted monomer homopolymer and multipolymer, 60 ℃ of vacuum-dryings are to constant weight then;
The preparation of polypropylene-Kevlar fiber composite material: the Kevlar fiber of crossing with polypropylene, through step (2) hydrolysis treatment, PP-g-MAH-St grafts and composite antioxidant thorough mixing in high-speed mixer of step (3) preparation, then in twin screw extruder melt blending extrude, granulation, prepare polypropylene-Kevlar fiber composite material.
The polypropylene-Kevlar fiber composite material pellet of gained is injected into the standard batten after drying, carries out Mechanics Performance Testing.
The length of Kevlar fiber is 5mm～6mm in the described step (1), and Kevlar fiber and consumption of ethanol are: the ethanol that adds 300～500ml according to 20～25gKevlar fiber.
The supersound process temperature is 60～80 ℃ in the described step (1), and power is 80～100w.
The Kevlar fiber that supersound process is crossed in the described step (2) with the consumption of the NaOH aqueous solution is: the NaOH aqueous solution of the Kevlar fiber adding 300～500ml that crosses according to 20～25g supersound process.
In the preparation of described step (3) PP-g-MAH-St grafts: polypropylene PP: benzoyl peroxide BPO: dimethylbenzene: maleic anhydride MAH: the mass ratio of vinylbenzene St is 1: 0.01～0.02: 1～1.5: 0.08～0.16: 0.10～0.20.
Raw materials used prescription is in the described step (4): according to mass ratio: 100 parts of polypropylene PP, 3～5 parts of Kevlar fibers, 5～20 parts of PP-g-MAH-St graftss, 0.5～1 part of composite antioxidant.
Described composite antioxidant is the mixture of antioxidant 1010 and oxidation inhibitor 168, and its composite mass ratio is 2: 1.
The barrel zone temperature of twin screw extruder is 180 ℃～200 ℃ in the described step (4).
Adopt the percentage of grafting of the PP-g-MAH-St grafts of chemical titration step (2) preparation, concrete operations are: get 1～2g grafting purifying thing, place the single port flask, add dimethylbenzene, reflux 40～60min, add excessive KOH-ethanol standardized solution after cold slightly again, 4～6h again refluxes; The cooling back adds phenolphthalein as indicator, stirs fast on agitator, and with the excessive alkali of HCl-Virahol standardized solution back titration, alkali number and the used acid amount of back titration that record adds are calculated as follows percentage of grafting:
Wherein: M
KOH---potassium hydroxide-ethanol solution concentration, mol/L; M
HCl---hydrochloric acid aqueous isopropanol concentration, mol/L; V
KOH---add the amount of potassium hydroxide-ethanol solution, mL; V
HClThe consumption of hydrochloric acid aqueous isopropanol, mL; M---the quality of purifying thing, g.
Below be several specific embodiment of the present invention, further set forth the present invention, but the present invention be not limited only to this.
Embodiment 1
(1) raw material: polypropylene model T30S, Fujian Oil-Refining Chemical Co., Ltd.;
Kevlar fiber 5mm, du pont company;
Other raw materials are commercially available general goods level.
(2) concrete preparation method is as follows:
1. the supersound process of Kevlar fiber:
The Kevlar short fiber that is cut into 5mm is put into encloses container, is solvent with ethanol, and supersound process 12h under 60 ℃, 80w condition removes the fiber surface foreign material, and is then that the vacuum-drying of surface treated Kevlar fiber is standby.
2. the hydrolysis of Kevlar fiber:
A certain amount of Kevlar fiber through supersound process is placed 10% NaOH aqueous solution hydrolysis reaction 16h, and solution temperature is controlled at about 90 ℃, and its product water is washed till neutrality, and vacuum-drying is standby then.
3. the preparation of PP-g-MAH-St grafts:
In the reactor that has agitator, add 100 parts of polypropylene (PP), 2 parts of benzoyl peroxides (BPO), 10 parts of dimethylbenzene, at N
2Leave standstill swelling 1h under the atmosphere.Add 14 parts of maleic anhydrides (MAH) and 18 parts of vinylbenzene (St) then, be warming up to 120 ℃, start mechanical stirring, reaction 1h.After reaction finishes, continue logical N
2For some time is till graft product cools off fully.
Graft product is placed apparatus,Soxhlet's, with acetone extracting 24h, remove not grafted monomer homopolymer and multipolymer, 60 ℃ of vacuum-dryings are to constant weight then.
4. the preparation of polypropylene/Kevlar fibre composite:
With 100 parts of polypropylene, 3 parts of Kevlar fibers (hydrolysis treatment is crossed), 10 parts of PP-g-MAH/St, 0.5 part of composite antioxidant thorough mixing in high-speed mixer, then in twin screw extruder melt blending extrude, granulation, barrel zone temperature is respectively 180 ℃, 190 ℃, 200 ℃, 210 ℃, 210 ℃, 210 ℃.The gained pellet is injected into the standard batten after drying, carries out Mechanics Performance Testing.
The performance test contrast is as follows:
| ? | PP(T30S)? | The PP/Kevlar matrix material |
| Tensile strength (MPa) | 30? | 33? |
| Cantilever beam impact strength (J/m) | 25? | 28? |
| Modulus in flexure (GPa) | 1.6? | 1.8? |
| Heat-drawn wire (℃) | 100? | 130? |
| Melt flow rate (MFR) (g/10min) | 2? | 2? |
Embodiment 2
(1) raw material: polypropylene model T30S, Fujian Oil-Refining Chemical Co., Ltd.;
Kevlar fiber 6mm, du pont company;
Other raw materials are commercially available general goods level.
(2) concrete preparation method is as follows:
1. the supersound process of Kevlar fiber:
The Kevlar short fiber that is cut into 6mm is put into encloses container, with ethanol is that (Kevlar fiber and consumption of ethanol are solvent: the ethanol that adds 300ml according to the 20gKevlar fiber), supersound process 13h under 80 ℃, 100w condition, remove the fiber surface foreign material, then that the vacuum-drying of surface treated Kevlar fiber is standby.
2. the hydrolysis of Kevlar fiber:
A certain amount of Kevlar fiber through supersound process is placed 8% the NaOH aqueous solution (the Kevlar fiber of crossing according to the 20g supersound process adds the NaOH aqueous solution of 300ml) hydrolysis reaction 12h, solution temperature is controlled at about 90 ℃, its product water is washed till neutrality, and vacuum-drying is standby then.
3. the preparation of PP-g-MAH-St grafts:
In the reactor that has agitator, add 100 parts of polypropylene (PP), 1 part of benzoyl peroxide (BPO), 10 parts of dimethylbenzene, at N
2Leave standstill swelling 1h under the atmosphere.Add 8 parts of maleic anhydrides (MAH) and 10 parts of vinylbenzene (St) then, be warming up to 120 ℃, start mechanical stirring, reaction 1h.After reaction finishes, continue logical N
2For some time is till graft product cools off fully.
Graft product is placed apparatus,Soxhlet's, with acetone extracting 24h, remove not grafted monomer homopolymer and multipolymer, 60 ℃ of vacuum-dryings are to constant weight then.
4. the preparation of polypropylene/Kevlar fibre composite:
With 100 parts of polypropylene, 3 parts of Kevlar fibers (hydrolysis treatment is crossed), 5 parts of PP-g-MAH-St graftss, 0.5 part of composite antioxidant thorough mixing in high-speed mixer, then in twin screw extruder melt blending extrude, granulation, barrel zone temperature is respectively 180 ℃, 190 ℃, 200 ℃, 210 ℃, 210 ℃, 210 ℃.
Embodiment 3
(1) raw material: polypropylene model T30S, Fujian Oil-Refining Chemical Co., Ltd.;
Kevlar fiber 5mm, du pont company;
Other raw materials are commercially available general goods level.
(2) concrete preparation method is as follows:
1. the supersound process of Kevlar fiber:
The Kevlar short fiber that is cut into 5mm is put into encloses container, with ethanol is that (Kevlar fiber and consumption of ethanol are solvent: the ethanol that adds 500ml according to the 25gKevlar fiber), supersound process 16h under 80 ℃, 100w condition, remove the fiber surface foreign material, then that the vacuum-drying of surface treated Kevlar fiber is standby.
2. the hydrolysis of Kevlar fiber:
A certain amount of Kevlar fiber through supersound process is placed 10% the NaOH aqueous solution (the Kevlar fiber of crossing according to the 25g supersound process adds the NaOH aqueous solution of 500ml) hydrolysis reaction 16h, solution temperature is controlled at about 100 ℃, its product water is washed till neutrality, and vacuum-drying is standby then.
3. the preparation of PP-g-MAH-St grafts:
In the reactor that has agitator, add 100 parts of polypropylene (PP), 2 parts of benzoyl peroxides (BPO), 15 parts of dimethylbenzene, at N
2Leave standstill swelling 1h under the atmosphere.Add 16 parts of maleic anhydrides (MAH) and 20 parts of vinylbenzene (St) then, be warming up to 120 ℃, start mechanical stirring, reaction 1h.After reaction finishes, continue logical N
2For some time is till graft product cools off fully.
Graft product is placed apparatus,Soxhlet's, with acetone extracting 24h, remove not grafted monomer homopolymer and multipolymer, 60 ℃ of vacuum-dryings are to constant weight then.
4. the preparation of polypropylene/Kevlar fibre composite:
With 100 parts of polypropylene, 5 parts of Kevlar fibers (hydrolysis treatment is crossed), 20 parts of PP-g-MAH-St graftss, 1 part of composite antioxidant thorough mixing in high-speed mixer, then in twin screw extruder melt blending extrude, granulation, barrel zone temperature is respectively 180 ℃, 190 ℃, 200 ℃, 210 ℃, 210 ℃, 210 ℃.
Embodiment 4
(1) raw material: polypropylene model T30S, Fujian Oil-Refining Chemical Co., Ltd.;
Kevlar fiber 6mm, du pont company;
Other raw materials are commercially available general goods level.
(2) concrete preparation method is as follows:
1. the supersound process of Kevlar fiber:
The Kevlar short fiber that is cut into 6mm is put into encloses container, with ethanol is that (Kevlar fiber and consumption of ethanol are solvent: the ethanol that adds 400ml according to the 25gKevlar fiber), supersound process 13-15h under 70 ℃, 90w condition, remove the fiber surface foreign material, then that the vacuum-drying of surface treated Kevlar fiber is standby.
2. the hydrolysis of Kevlar fiber:
A certain amount of Kevlar fiber through supersound process is placed 10% the NaOH aqueous solution (the Kevlar fiber of crossing according to the 20-25g supersound process adds the NaOH aqueous solution of 400ml) hydrolysis reaction 16h, solution temperature is controlled at about 95-100 ℃, its product water is washed till neutrality, and vacuum-drying is standby then.
3. the preparation of PP-g-MAH-St grafts:
In the reactor that has agitator, add 100 parts of polypropylene (PP), 1.5 parts of benzoyl peroxides (BPO), 13 parts of dimethylbenzene, at N
2Leave standstill swelling 1h under the atmosphere.Add 15 parts of maleic anhydrides (MAH) and 18 parts of vinylbenzene (St) then, be warming up to 120 ℃, start mechanical stirring, reaction 1h.After reaction finishes, continue logical N
2For some time is till graft product cools off fully.
Graft product is placed apparatus,Soxhlet's, with acetone extracting 24h, remove not grafted monomer homopolymer and multipolymer, 60 ℃ of vacuum-dryings are to constant weight then.
4. the preparation of polypropylene/Kevlar fibre composite:
With 100 parts of polypropylene, 4 parts of Kevlar fibers (hydrolysis treatment is crossed), 15 parts of PP-g-MAH-St graftss, 0.5 part of composite antioxidant thorough mixing in high-speed mixer, then in twin screw extruder melt blending extrude, granulation, barrel zone temperature is respectively 180 ℃, 190 ℃, 200 ℃, 210 ℃, 210 ℃, 210 ℃.
The matrix material that this method makes has mechanical property and higher heat-drawn wires such as good stretching, bending, shock resistance.
Claims (8)
1. the preparation method of a polypropylene-Kevlar fiber composite material, it is characterized in that: described preparation method's step is:
(1) supersound process of Kevlar fiber: the Kevlar fiber is put into encloses container, is solvent with ethanol, and supersound process 12～16h removes the fiber surface foreign material, then that the vacuum-drying of surface treated Kevlar fiber is standby;
(2) hydrolysis of Kevlar fiber: will place mass concentration through the Kevlar fiber of step (1) supersound process is NaOH aqueous solution hydrolysis reaction 12～16h of 8～12%, solution temperature is controlled at 90～100 ℃, its product water is washed till neutrality, and vacuum-drying is standby then;
(3) preparation of PP-g-MAH-St grafts: in the reactor that has agitator, add polypropylene PP, benzoyl peroxide BPO, dimethylbenzene, at N
2Leave standstill swelling 1～2h under the atmosphere; Add maleic anhydride MAH and vinylbenzene St then, be warming up to 120 ℃, start mechanical stirring, reaction 1～2h after reaction finishes, continues logical N
2For some time is till graft product cools off fully; Graft product is placed apparatus,Soxhlet's, with acetone extracting 24h, remove not grafted monomer homopolymer and multipolymer, 60 ℃ of vacuum-dryings are to constant weight then;
(4) preparation of polypropylene-Kevlar fiber composite material: 3～5 parts of the Kevlar fibers of crossing with 100 parts of polypropylene, through step (2) hydrolysis treatment, 5～20 parts of the PP-g-MAH-St graftss and the composite antioxidant of step (3) preparation place the high-speed mixer thorough mixing for 0.5～1 part, described composite antioxidant is the mixture of antioxidant 1010 and oxidation inhibitor 168, and its composite mass ratio is 2: 1; Then in twin screw extruder melt blending extrude, granulation, prepare polypropylene-Kevlar fiber composite material.
2. the preparation method of polypropylene-Kevlar fiber composite material according to claim 1, it is characterized in that: the polypropylene-Kevlar fiber composite material pellet of gained is injected into the standard batten after drying, carries out Mechanics Performance Testing.
3. the preparation method of polypropylene-Kevlar fiber composite material according to claim 1 is characterized in that: the length of Kevlar fiber is 5mm～6mm in the described step (1); Kevlar fiber and consumption of ethanol are: the ethanol that adds 300～500ml according to 20～25gKevlar fiber.
4. the preparation method of polypropylene-Kevlar fiber composite material according to claim 1 is characterized in that: the supersound process temperature is 60～80 ℃ in the described step (1), and power is 80～100w.
5. the preparation method of polypropylene-Kevlar fiber composite material according to claim 1 is characterized in that: the Kevlar fiber that supersound process is crossed in the described step (2) with the consumption of the NaOH aqueous solution is: the NaOH aqueous solution of the Kevlar fiber adding 300～500ml that crosses according to 20～25g supersound process.
6. the preparation method of polypropylene-Kevlar fiber composite material according to claim 1, it is characterized in that: in the preparation of described step (3) PP-g-MAH-St grafts: polypropylene PP: benzoyl peroxide BPO: dimethylbenzene: maleic anhydride MAH: the mass ratio of vinylbenzene St is 1: 0.01～0.02: 1～1.5: 0.08～0.16: 0.10～0.20.
7. the preparation method of polypropylene-Kevlar fiber composite material according to claim 1 is characterized in that: the barrel zone temperature of twin screw extruder is 180 ℃～200 ℃ in the described step (4).
8. the preparation method of polypropylene-Kevlar fiber composite material according to claim 1, it is characterized in that: the percentage of grafting that adopts the PP-g-MAH-St grafts of chemical titration step (3) preparation, concrete operations are: get 1～2g grafting purifying thing, place the single port flask, add dimethylbenzene, reflux 40～60min adds excessive KOH-ethanol standardized solution after cold slightly again, and 4～6h again refluxes; The cooling back adds phenolphthalein as indicator, stirs fast on agitator, and with the excessive alkali of HCl-Virahol standardized solution back titration, alkali number and the used acid amount of back titration that record adds are calculated as follows percentage of grafting:
Wherein:
M KOH-potassium hydroxide-ethanol solution concentration, mol/L;
M HCl-hydrochloric acid aqueous isopropanol concentration, mol/L;
V KOHThe amount of-adding potassium hydroxide-ethanol solution, mL;
V HClThe consumption of-hydrochloric acid aqueous isopropanol, mL;
m--the quality of purifying thing, g.
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| CN101838423B (en) * | 2010-06-10 | 2012-07-04 | 南京聚隆科技股份有限公司 | Modified polypropylene material for thin-wall bumper and preparation method thereof |
| CN101875790B (en) * | 2010-08-09 | 2012-07-04 | 东北林业大学 | Preparation method of surface hydrolysis modified aramid fiber enhanced wood plastic composite material |
| CN107286294B (en) * | 2017-06-23 | 2019-12-31 | 常州大学 | Compatilizer for PP/PS extrusion molding and preparation method thereof |
| CN110048036B (en) * | 2019-04-19 | 2024-05-17 | 桑顿新能源科技有限公司 | Reinforcing rib sheet and preparation method thereof, battery cell and preparation method thereof, and soft package battery |
| CN110751986A (en) * | 2019-10-15 | 2020-02-04 | 山东省科学院能源研究所 | Calculation model and detection method of polyolefin grafting rate based on artificial neural network |
| CN110964248A (en) * | 2019-11-29 | 2020-04-07 | 苏州润佳高分子材料有限公司 | Soft touch polypropylene composite material for automobile |
| CN115124782B (en) * | 2021-03-29 | 2023-06-13 | 广州汽车集团股份有限公司 | Environment-friendly regenerated polypropylene material with high thermo-oxidative aging resistance and preparation method thereof |
| CN116178846B (en) * | 2023-04-06 | 2023-10-20 | 青岛中新华美塑料有限公司 | Anti-fatigue PP alloy material and preparation method thereof |
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