CN1827671A - Continuous fiber reinforced composite materials, its production method and special equipment therefor - Google Patents
Continuous fiber reinforced composite materials, its production method and special equipment therefor Download PDFInfo
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Abstract
The invention relates to a glass fiberreinforced thermoplastic composite and a continuous fiber-reinforced composite, which are prepared with the following raw materials percentagewise by weight: 35-60 % of resin, 35-60 % of dip treated glass fiber and 0.5-5 % of auxiliary agent. The invention adopts resin and dip treated glass fiber as main raw materials, mixtures of antioxidant, ultraviolet absorbent and light-stability agent as main auxiliary agents, with logical formulations, eliminates the damage to glass fibrous surface caused by twin-screw with continuous fiber-reinforced composite producted by this manufacturing technique, improves product lustrous surface, binding properties between fiberglass and resins by a treatment for glass fibrous surface and mechanical properties of products, protects the materials for long periods from destruction because of addition of various stabilizing agents, and solves the limitation that general materials can not be used for a long time in extreme conditions such as high temperature, high humidity, radiation and so on.
Description
Technical field:
The present invention relates to glass fiber reinforced thermoplastics composite, also relate to the production method and the plant-scale equipment in addition.
Background technology:
Fibreglass reinforced thermoplastic (is called for short the fiber glass reinforced thermoplastics, GRTP), has accounted for more than 1/4 of glass reinforced plastic ultimate production in the world now, and steady-state growth in the recent period, according to document announcement, in the past few years in, GRTP market average annual growth rate is 5%～6%, and rate of growth surpasses thermosetting resin.And this material of continuous fiber reinforced thermoplastic plastic (LFT or LFRT) is one of material with fastest developing speed in the current composite markets, and the annual growth with 30% in the past 10 years rises.2002 annual consumptions reach 70000 tons, and current production rate has surpassed GMT (the glass felt strengthens thermoplastic sheets).
Glass fibre (roving) reinforced thermoplastics(RTP) has two types, a kind of is direct method, a kind of is the continuous fibre method, the former directly introduces long glass fibres at the cylindrical shell middle part of twin screw extruder, glass fibre enters forcing machine, with the fused mixing of materials, extrude by die head again behind the process segment that cuts into 0.3-1mm of twin screw.Because screw rod is to glass surface strong friction and shearing action, to such an extent as to the pre-treatment to the glass surface has caused destruction, the matrix material of producing has glass length inequality, orientation is inconsistent, staple length short, and resin and glass degree of adhesion are not high, the characteristics that the performance of material is not high.Owing to be subjected to the restriction of production unit, glass fiber content is not high again.
The latter is surrounded by resin fully owing to fiber, thereby be subjected to the damage of screw rod to drop to minimum level at fiber, and in end article, having kept long length, every mechanical property has all obtained improving significantly, advantages such as product surface is smooth, and cost is low, forming method is many.In fields such as automobile, aerospace, electronic apparatus, buildings wide application is arranged.But because prescription is had relatively high expectations, complex manufacturing, the production of this material and technology are in a few advanced country's technical monopoly situation always, and our country also has some mechanisms that it is studied at present.The manufacture method that the Shanghai outstanding company of outstanding thing has applied for the continuous fiber reinforced thermoplastic plastic of patent is to adopt the powder impregnation method to prepare the continuous fibre strongthener; This method fiber in actual production is difficult to effective dispersion, cause that glass and molten resin are difficult to that effective adhesive is arranged, fibre content and length are restricted, fill a prescription too simple.In goods, have the difficult floating fine problem of disperseing inhomogeneous, molten resin and glass degree of adhesion difference and producing of fiber equally, moreover this method production cost is higher.The Beijing Research Inst. of Aeronautic Material adopts the continuous fiber reinforced thermoplastic composite material of wet method preparation, has also applied for patent.This method still exists and is difficult to solve effectively dispersion of glass fibre, resin and the uneven problem of glass fibre; This kind method production efficiency is low in addition, is difficult to realize scale operation, can not satisfy industrial requirement.
In sum, domestic continuous fiber reinforced composite materials all exists effectively dispersion of glass fibre, resin and the uneven defective of glass fibre at present, and is especially complicated at article construction, and size is easy to generate problems such as warpage especially when big.Also there are problems such as the low-cost height of production efficiency simultaneously, all are difficult to satisfy industrial requirement.Invent a kind of can scale operation technology and one can be advanced prescription just by being important.
Summary of the invention:
The present invention seeks to overcome above-mentioned not enough problem, a kind of continuous fiber reinforced composite materials is provided, characteristics with mechanical property excellence, heat-drawn wire height, anticorrosive, good weatherability, its production method also is provided in addition, improve product surface glossiness and mechanical property, provide production institute specific equipment at last, the structure uniqueness, be convenient to operation, improve effect.
The technical scheme that the present invention is adopted for achieving the above object is: continuous fiber reinforced composite materials, formulated by following raw materials by weight:
Resin 35-60%
Soak into and handle glass fibre 35-60%
Auxiliary agent 0.5-5%.
Described resin is selected from polypropylene, nylon, the polyethylene and plants arbitrarily.
Described infiltration is handled glass fibre for to make by following weight percent:
Roving 95-98
Treating compound 2-5;
Wherein glass fibre is the non-twist glass roving of E type, and filament diameter is 7.4 μ m; Treating compound is organosilicon alkanes coupling agent and membrane-forming agent, and coupling agent is selected modified amido silane, peroxy silane, azido-silane for use or planted mixture arbitrarily.
Described auxiliary agent is that following raw material is prepared by described weight percent:
Antioxidant 0.3-1
UV light absorber 0.1-1
Photostabilizer 0.1-1
Lubricating auxiliary agent 0.3-2;
Wherein antioxidant is 3,5-di-tert-butyl-hydroxy phenyl propionic acid octadecanol ester, tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester, four phenmethyls (3,5-di-t-butyl-4-hydroxy phenylpropionic acid) methyl esters or wherein two kinds or three kinds of mixtures; UV light absorber is an Octabenzone, 2,2 '-dihydroxyl-4-methyl oxygen base benzophenone, 2 (2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-5-chlorinated benzotriazoles or wherein two kinds or three kinds of mixtures; Photostabilizer is two (2,2,6, the agent of 6-tetramethyl-benzene piperidines) sebates and/or two (1,2,2,6,6-penta methyl-4-piperidyl) certain herbaceous plants with big flowers diacid salt; Lubricating auxiliary agent can be selected the stearic acid auxiliary agent for use.
The production method of continuous fiber reinforced composite materials of the present invention: soak into treating compound earlier and handle fibre glass roving, disperse to soak into the fibre glass roving of handling with the glass fibre dispersion system again, rove after the dispersion is introduced by an inlet of special cross slit forcing machine die head, resin by another inlet evenly flow into die head, rove further is forced to disperse in die head, molten resin is abundant covered fiber evenly; The glass fibre that molten resin fully coats is extruded by die head exit, be configured as the continuous fiber reinforced composite materials that needs shape through former, after matrix material tension system, cooling granulation system, form the continuous fiber reinforced composite materials that pellet length can be selected on demand.
Interface shear strength between described resin and the glass fibre is greater than 9Mpa.
The present invention produces the special-purpose cross slot die of continuous fiber reinforced composite materials, two opening for feeds are arranged, be respectively resin feeding mouth and fiber feed mouth, the resin feeding mouth adopts the design of multiple-limb melt flow channel, the runner design is about die head medullary ray symmetry, and the infiltration runner of resin and fiber adopts serpentine design, along certain gradient bending, vertex and lower-most point are arranged respectively, and the vertex that at first arrives of fiber is than the vertex height of fiber outlet.
It is main raw material that the present invention handles glass fibre with resin and treating compound; with antioxidant; UV light absorber; the photostabilizer mixture is main auxiliary agent; prescription rationally; the comprehensive glass fibre dispersion system that adopts; fiberglass surfacing special processing technology; and the continuous glass fibre reinforced composite of the design of special cross slot die production; the continuous fiber reinforced composite materials of producing; staple length reaches 15mm in the pellet; fibre content can reach 40-60%; the present invention eliminates the destruction of twin screw to fiberglass surfacing by this prescription and the continuous fiber reinforced composite materials of explained hereafter; improved the surface luster of goods; the processing of fiberglass surfacing has been improved the binding property of glass fibre and resin; improved mechanical performance of products; the adding of various stablizers has protected the performance of material not to be damaged for a long time, and having solved general material cannot be at high temperature; high humidity; the limitation of life-time service under the mal-conditions such as radiation.
The special-purpose dispersion system of glass fibre of the present invention is made of stationary roll and mobile roller, and a mobile roller that moves perpendicular to the fiber working direction is arranged between two stationary rolls.Roving is incorporated in this equipment by the fiber inlet pipe, the rove that is drawn passes through stationary roll, mobile roller, stationary roll successively, the to-and-fro movement on of mobile in addition roller perpendicular to the rove lead, rove is subjected to two tension force on the vertical direction each other, and rove is effectively disperseed and uniform distribution.
The special-purpose cross slot die of the present invention has two opening for feeds, is respectively resin feeding mouth and fiber feed mouth.The resin feeding mouth flows for avoiding instabilities such as melt turbulent flow, adopt the design of multiple-limb melt flow channel, the runner design is about die head medullary ray symmetry, this design has reduced inhomogeneous the extruding that the difference owing to pressure causes, resin through several branch's runners laggard go in the slit soak into fiber.The infiltration runner of resin and fiber adopts serpentine design, and by this structure, therefore the tension force maximum that vertex that continuous fibre arrives first or lower-most point are subjected to obtains maximum fiber dispersion and infiltration.Along with the reduction of vertex (or lower-most point) height, fiber is subjected to the infiltration of relatively little degree, has therefore stoped the destruction that fiber is chaotic and reduced fibrous bundle.Compare with rectilinear runner on the other hand, fiber and resin melt have bigger contact surface in this runner, can guarantee to soak into more fully.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the special-purpose cross slot die of the present invention flow passage structure synoptic diagram.
Fig. 3 soaks into the flow passage structure synoptic diagram for the special-purpose cross slot die of the present invention.
Embodiment:
Embodiment 1
According to following raw material weight (continuous fiber reinforced composite materials of kg preparation,
Acrylic resin 50
Soak into and handle glass fibre 47
3,5-di-tert-butyl-hydroxy phenyl propionic acid octadecanol ester 1
Octabenzone 0.5
Two (1,2,2,6,6-penta methyl-4-piperidyl) certain herbaceous plants with big flowers diacid salt 0.5
Magnesium Stearate 1.
At first utilize electronic scale and platform balance to take by weighing desired raw material respectively by formula rate, will join in the low speed mixer that volume is 100L except that soaking into the various raw materials of handling the glass fibre, stir, it is even to make it blending dispersion.How much compounding time is determined according to the batch mixing amount, about 3-5Min, and the compounding temperature is a room temperature, at last that compounding is good material is put in the TE-65 twin screw extruder hopper.Start and extrude unit, the material that compounding is finished carries out melting mixing.
Its processing parameter sees the following form:
| Processing parameter | ||||||||
| Temperature ℃ | 1 district | 200±10 | Main frame electric current (A) | 110-130 | Feeding (HZ) | 12-16 | ||
| 2 districts | 200±10 | |||||||
| 3 districts | 210±10 | |||||||
| 4 districts | 210±10 | Pulling speed (r/min) | 600-800 | Screw speed | 200- 300 | |||
| 5 districts | 210±10 | Head | 210±10 | |||||
| 6 districts | 220±10 | Material | 210±10 | |||||
In mixing process, drain air, avoid the defective that causes owing to air.
Secondly soak into and handle glass fibre, by the non-twist glass roving 95-98% of following weight percent raw materials weighing E type, filament diameter is 7.4 μ m, treating compound 2-5%.The effective sized glass fibres for the treatment of compound in room temperature environment, the even preheating of warming apparatus makes treating compound be coated to every monofilament.Glass fibre is incorporated in the glass fibre dispersion system by the fiber inlet pipe after infiltration, the glass fibre that is drawn passes through stationary roll, mobile roller, stationary roll successively, the to-and-fro movement on of mobile in addition roller perpendicular to the glass fibre lead, glass fibre is subjected to two tension force on the vertical direction each other, and glass fibre is effectively disperseed and uniform distribution.
Fibre glass roving after disperseing is at last introduced by an inlet of special-purpose cross slit forcing machine die head, melting mixing material such as resin evenly flow into die head by another inlet, through several branch's runners laggard go in the slit fully soak into fiber, rove further is forced to disperse in die head, evenly abundant covered fiber such as molten resin is extruded by die head exit, be configured as the continuous fiber reinforced composite materials that needs shape through former, through the matrix material tension system, form the continuous fiber reinforced composite materials that pellet length can be selected (being generally 10-15mm) on demand after the cooling granulation system.
Used matrix material tension system is the tension roll that the tape loop up and down of elastomeric material constitutes.The rotation of take-up device by take-up roll transmits the matrix material that comes out after being shaped.
Used cooling granulation system is made up of tank, air knife, dicing machine.
Produce continuous fiber reinforced composite materials according to embodiment 1 described method, concrete material and weight (kg is as described in Table 1:
| Raw material | Example 2 | Example 3 | Example 4 | Example 5 |
| | 3 | 40 | 16 | |
| Nylon | 50 | 44 | ||
| Polyethylene | 35 | 12 | ||
| Tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester | 0.1 | 0.3 | 0.2 | |
| Four phenmethyls (3,5-di-t-butyl-4-hydroxy phenylpropionic acid) methyl esters | 0.6 | 0.2 | 0.2 | |
| 3,5-di-tert-butyl-hydroxy phenyl propionic acid octadecanol ester | 0.1 | 0.6 | 0.2 | |
| 2,2 '-dihydroxyl-4-methyl oxygen base benzophenone | 0.1 | 0.2 | 0.2 | |
| 2 (2 '-hydroxyl-3,5 '-di-tert-butyl-phenyl)-5-chlorinated benzotriazoles | 0.2 | 0.1 | 0.3 | |
| Octabenzone | 0.5 | 0.1 | 0.3 | |
| Two (2,2,6, the agent of 6-tetramethyl-benzene piperidines) sebate | 0.2 | 0.3 | 0.5 | |
| Two (1,2,2,6,6-penta methyl-4-piperidyl) certain herbaceous plants with big flowers diacid salt | 0.5 | 0.1 | 0.3 | |
| Magnesium Stearate | 0.6 | 1.2 | 1.8 | 0.4 |
| The non-twist glass roving of E type | 58 | 44 | 40 | 50.8 |
| Modified amido silane | 1.0 | 0.5 | 0.6 | |
| Azido-silane | 0.7 | 0.9 | 1 | |
| Peroxy silane | 0.6 | 0.5 | 1 |
The products obtained therefrom performance sees Table 2
| Project | Unit | Test result | Testing method |
| Tensile strength tension fracture elongation rate flexural strength bending elastic modulus socle girder notched Izod impact strength heat-drawn wire (0.45Mpa) | Mpa ％ Mpa Gpa Kj/m 2 ℃ | 225 6 237 8.96 18.9 252.0 | GB/T1040-1992 GB/T1040-1992 GB/T9341-2000 GB/T1041-2000 GB/T1843-1996 GB/T1634-20047 |
Produce the special-purpose cross slot die of the said products shown in Fig. 2 and 3, die head 2 has two opening for feeds, be respectively resin feeding mouth 3 and fiber feed mouth 5, the resin feeding mouth adopts 1 design of multiple-limb melt flow channel, the runner design is about die head medullary ray symmetry, the infiltration runner 6 of resin and fiber adopts serpentine design, along certain gradient bending, 4 have vertex and lower-most point respectively from opening for feed 5 to discharge port, and the vertex that fiber at first arrives is than the vertex height of fiber outlet, promptly the height of Wan Qu vertex descends successively, wherein h
2=h
3, h
4=h
5, h
3＞h
4, h
1＞h
6
Claims (12)
1, a kind of continuous fiber reinforced composite materials is characterized in that: formulated by following raw materials by weight:
Resin 35-60%
Soak into and handle glass fibre 35-60%
Auxiliary agent 0.5-5%.
2, continuous fiber reinforced composite materials according to claim 1 is characterized in that: resin is selected from polypropylene, nylon, the polyethylene and plants arbitrarily.
3, continuous fiber reinforced composite materials according to claim 1 is characterized in that: soak into and handle glass fibre for to make by following weight percent:
Roving 95-98
Treating compound 2-5.
4, continuous fiber reinforced composite materials according to claim 3 is characterized in that: glass fibre is the non-twist glass roving of E type, and filament diameter is 7.4 μ m.
5, continuous fiber reinforced composite materials according to claim 3 is characterized in that: treating compound is organosilicon alkanes coupling agent and membrane-forming agent, and coupling agent is selected modified amido silane, peroxy silane, azido-silane for use or planted mixture arbitrarily.
6, continuous fiber reinforced composite materials according to claim 1 is characterized in that: auxiliary agent is that following raw material is prepared by described weight percent:
Antioxidant 0.3-1
UV light absorber 0.1-1
Photostabilizer 0.1-1
Lubricating auxiliary agent 0.3-2.
7, continuous fiber reinforced composite materials according to claim 6, it is characterized in that: antioxidant is 3,5-di-tert-butyl-hydroxy phenyl propionic acid octadecanol ester, tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester, four phenmethyls (3,5-di-t-butyl-4-hydroxy phenylpropionic acid) methyl esters or wherein two kinds or three kinds of mixtures.
8, continuous fiber reinforced composite materials according to claim 6, it is characterized in that: UV light absorber is an Octabenzone, 2,2 '-dihydroxyl-4-methyl oxygen base benzophenone, 2 (2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-5-chlorinated benzotriazoles or wherein two kinds or three kinds of mixtures.
9, continuous fiber reinforced composite materials according to claim 6 is characterized in that: photostabilizer is two (2,2,6, the agent of 6-tetramethyl-benzene piperidines) sebate and/or two (1,2,2,6,6-penta methyl-4-piperidyl) certain herbaceous plants with big flowers diacid salt.
10, the production method of continuous fiber reinforced composite materials according to claim 1, it is characterized in that: soak into treating compound earlier and handle fibre glass roving, disperse to soak into the fibre glass roving of handling with the glass fibre dispersion system again, rove after the dispersion is introduced by an inlet of special cross slit forcing machine die head, resin by another inlet evenly flow into die head, rove further is forced to disperse in die head, molten resin is abundant covered fiber evenly; The glass fibre that molten resin fully coats is extruded by die head exit, be configured as the continuous fiber reinforced composite materials that needs shape through former, after matrix material tension system, cooling granulation system, form the continuous fiber reinforced composite materials that pellet length can be selected on demand.
11, the production method of continuous fiber reinforced composite materials according to claim 1 is characterized in that: the interface shear strength between resin and the glass fibre is greater than 9Mpa.
12, the special-purpose cross slot die of production continuous fiber reinforced composite materials according to claim 1, it is characterized in that: special-purpose cross slot die has two opening for feeds, be respectively resin feeding mouth and fiber feed mouth, the resin feeding mouth adopts the design of multiple-limb melt flow channel, the runner design is about die head medullary ray symmetry, the infiltration runner of resin and fiber adopts serpentine design, along certain gradient bending, vertex and lower-most point are arranged respectively, and the vertex that at first arrives of fiber is than the vertex height of fiber outlet.
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|---|---|---|---|
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