CN110452496A - A kind of modified glass-fiber reinforced resin laminate and preparation method thereof - Google Patents
A kind of modified glass-fiber reinforced resin laminate and preparation method thereof Download PDFInfo
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- CN110452496A CN110452496A CN201910832460.3A CN201910832460A CN110452496A CN 110452496 A CN110452496 A CN 110452496A CN 201910832460 A CN201910832460 A CN 201910832460A CN 110452496 A CN110452496 A CN 110452496A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/36—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and impregnating by casting, e.g. vacuum casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
Abstract
The invention discloses a kind of modified glass-fiber reinforced resin laminates and preparation method thereof, belong to wind turbine blade Material Field, the laminate is poured by several layers modified glass fibre peacekeeping resin by vacuum perfusion process, the several layers modified glass-fiber is tiled using 0 °/90 ° or 45 °/- 45 ° of ﹢ of direction, and the modified glass-fiber is to pass through silane coupler modified glass fibre.Laminate of the invention uses silane coupler modified glass fibre, the surface binding force of glass fibre and resin can be enhanced, to increase intensity, chemical resistance, water resistance and the weatherability of composite material.
Description
Technical field
The present invention relates to wind turbine blade Material Fields, more particularly to a kind of modified glass-fiber reinforced resin laminate
And preparation method thereof.
Background technique
With rapid development and current non-renewable resources (petroleum, natural gas, the gold of growth and the industry of population
Belong to mineral products) increasingly reduction, there is an urgent need to develop the renewable energy of clean type (wind energy, solar energy etc.) to meet current industry
Energy consumption needed for development process and life.A kind of renewable energy of the wind energy as clean type, is constantly subjected to domestic and international crowd
The concern of more Development institutions.Wind power generating set can will convert wind energy into the device of electric energy, by wind wheel, transmission system, power generation
The components such as machine, energy storage device, pylon and electrical system are constituted.In recent years, with continuous soaring, the wind of Wind turbines single-machine capacity
Electric blade is also gradually developing to enlargement, light-weighted direction.This is also to the composite material strength, rigid, tough for constituting blade
Property and density in terms of propose harsher requirement.
The main material for constituting blade includes: laminate, core material, coating, bonding agent etc., and wherein the performance of laminate is to determine
An important factor for fixed blade carrying and service life.Currently, laminate used in wind electricity blade is mostly by glass fibre and ring both at home and abroad
Oxygen resin is constituted.With riseing for Wind turbines capacity, the epoxy resin of common fiberglass reinforced is no longer satisfied high-power, big
The requirement of size wind electricity blade.Therefore, carbon fibre reinforcement is gradually applied to wind-powered electricity generation field, but due to the original of production cost
Cause, carbon fibre material do not obtain large-scale application in wind-powered electricity generation field.
In addition, having the experience of decades using Unidirectional Glass Fiber Reinforced Epoxy Composites manufacture wind electricity blade, paving cloth is filled
Note and curing process are all highly developed.How to be modified on the basis of original material, to improve glass fibre and ring
The interface binding power of oxygen resin is always that wind-powered electricity generation industry needs to be broken through to effectively improve the mechanical property of composite material
One of technical problem.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of modified glass-fiber reinforced resin laminate and its preparation sides
Method, by using the interface binding power of silane coupling agent high glass fibre and epoxy resin, to effectively improve composite material
Mechanical property.
In order to solve the above technical problems, technical solution provided by the invention is as follows:
On the one hand, the present invention provides a kind of modified glass-fiber reinforced resin laminate, and the laminate is changed by several layers
Property glass fibre and resin be poured by vacuum perfusion process, the several layers modified glass-fiber use 0 °/90 ° or ﹢
45 °/- 45 ° of direction tiling, the modified glass-fiber are to pass through silane coupler modified glass fibre.
Laminate of the invention uses silane coupler modified glass fibre, and the surface of glass fibre and resin can be enhanced
Binding force, to increase intensity, chemical resistance, water resistance and the weatherability of composite material.
Further, the glass fibre using uniaxially, twin shaft or three axis glass fibres.
Further, the glass fibre size is 600mm × 600mm.
On the other hand, a kind of preparation method of modified glass-fiber reinforced resin composite material is provided, is included the following steps:
1) Muffle furnace high temperature calcination is put into after cutting glass fibre；
2) will be cooling by the glass fibre room temperature environment of high temperature sintering, it is then immersed in silane coupler solution；
3) take out the glass fibre after impregnating, put it into baking oven and dried at 45~55 DEG C, after baking oven is warming up to 120
DEG C, high-temperature process, which is carried out, so that silane coupling agent is chemically combined with glass fibre obtains modified glass-fiber；
4) fiber laying: modified glass-fiber is evenly laid out according to the direction of 0 °/90 ° or 45 °/- 45 ° of ﹢；
5) resin is perfused using vacuum perfusion process in fiber laying, resin is generally epoxy resin；
6) it after the completion of being perfused, keeps vacuum condition to be warming up to 70 DEG C perfusion part, completes resin solidification；
7) laminate is obtained after the completion of solidification, is then demoulded and is post-processed.
The present invention uses silane coupler modified glass fibre, and prepares the glass-fibre reinforced resin composite wood of coupling agent modification
Material, coupling agent have difunctional, and wherein amino or epoxy functionality can form chemical bond with glass fibre, and hydrophobic function
Group can be with resin-bonded, it is intended to improve intensity, chemical-resistant stability and the service life of composite material, and then improve wind electricity blade
Comprehensive performance.
Silane coupling agent is a kind of special low molecule organo-silicon compound, and molecular structural formula is general are as follows: Y-R-Si (OR)3
(Y-organic functional base, SiOR-siloxy in formula).Siloxy has reactivity to inorganic matter, has to organic matter anti-
Answering property or compatibility, the present invention make the hydroxyl in the siloxy and glass of coupling agent using silane coupling agent under the high temperature conditions
In conjunction with formation chemical bond.By improving multiple to the modified interfacial tension that glass fibre and epoxy resin can be enhanced of glass fibre
Intensity, chemical-resistant stability and the service life of condensation material, and then improve the comprehensive performance of wind electricity blade.
The present invention be directed in existing fiber-resin composite, or there are poor mechanical properties, or there are interface knots
Weak problem with joint efforts, or the problems such as there are product hickies, flaw.It is proposed that a kind of preparation process is simple, wellability is good, interface cohesion
Power is strong, excellent in mechanical performance glass-fibre reinforced resin composite material.
Further, in the step 1), the high temperature sintering time is 30-60min.
Further, glass fibre using uniaxially, twin shaft or three axis glass fibres.
Further, the cutting size of glass fibre is 600mm × 600mm.
Further, in the step 2), room temperature cooling time is 25~35min, and soaking time is 8~15min.
Further, the silane coupling agent selects one of KH-550, KH-560, KH-570, KH-792, DL-602
Or it is a variety of.
Further, in the step 3), 50 DEG C of drying 40min~1.5h, 120 DEG C of high-temperature process time in baking oven
For 2-4h.
Further, in the step 5), vacuum perfusion process are as follows: open vacuum pump, vacuumize, when pressure vacuum gauge reaches
After to -0.9, vacuum buffer valve is closed, checks that mold pressure vacuum gauge is then opened such as pressure gauge registration≤- 0.85 after 15min
The sealant of injecting glue pipe port is removed in beginning priming by vacuum, is put into the resin barrel prepared according to predetermined comparison, starts into glue, directly
To resin complete wetting, stop injecting glue, and after pressure maintaining 30min, then by glue inlet tube doubling and takes out glue inlet tube.
Further, in the step 6), in 70 DEG C of heat preservation 8h.
Further, demoulding and post-process includes: to remove the vacuum aided material on laminate surface, and by laminated plate surface
Sundries clean out, it is spare.
In another aspect, the application for the laminate that preparation method described in one kind is prepared is provided, for making wind-force hair
The blade of motor.
By adopting such a design, the present invention has at least the following advantages:
The present invention utilizes silane coupler modified glass fibre, and coupling agent has difunctional, wherein amino or epoxy group
Functional group can form chemical bond with glass fibre, and hydrophobic functional group can be with resin-bonded, to improve the interface of fiber and resin
Binding performance promotes the abundant infiltration of resin in the fibre, improves the adhesive strength of resin and fiber and the mechanics of composite material
Performance.And should preparation method is simple, it is at low cost, for develop the application with higher of high-performance wind-power blade composite
Value.Material properties test shows to may make layer using coupling agent modified compared with unmodified glass-fibre reinforced resin laminate
The tensile strength of plate improves 20% or more, and compressive strength and shear strength improve 15% or more.
Detailed description of the invention
The above is merely an overview of the technical solutions of the present invention, in order to better understand the technical means of the present invention, below
In conjunction with attached drawing, the present invention is described in further detail with specific embodiment.
Fig. 1 is the structural schematic diagram of one embodiment of modified glass-fiber reinforced resin laminate of the invention；
Fig. 2 is process flow chart of the invention；
Fig. 3 is the structural formula of silane coupling agent of the invention；Wherein, (a) gamma-aminopropyl-triethoxy-silane KH-550,
(b) γ-glycidyl ether oxygen propyl trimethoxy silicane KH-560, (c) γ-(methacryloxypropyl) propyl trimethoxy silicon
Alkane, (d) N- (mono- aminoethyl of β)-γ-aminopropyl front three (second) oxysilane KH-792, (e) N- β-(aminoethyl)-γ-aminopropyl
Methyl dimethoxysilane DL-602.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but the present invention is not limited to following embodiments, Ren He
The identical or similar product with the present invention obtained under enlightenment of the invention, within protection scope.
The present invention provides a kind of embodiment of modified glass-fiber reinforced resin laminate, if as shown in Figure 1, laminate by
Dried layer modified glass-fiber 1 and resin are poured by vacuum perfusion process, and several layers modified glass-fiber uses 0 °/90 °
Or 45 °/- 45 ° of ﹢ of direction is tiled, modified glass-fiber is to pass through silane coupler modified glass fibre.Glass fibre can be with
Using uniaxially, twin shaft or three axis glass fibres.The size that glass fibre is cut is generally 600mm × 600mm.
Laminate of the invention uses silane coupler modified glass fibre, and the surface of glass fibre and resin can be enhanced
Binding force, to increase intensity, chemical resistance, water resistance and the weatherability of composite material.
The flow chart of one embodiment of preparation method of the invention, as shown in Figure 2 and Figure 3, one for can enumerating are specific
Embodiment is as follows:
Embodiment 1
The first step uniaxially will be cut into the square of 600 × 600mm by glass fabric, be placed in Muffle furnace, 150
Calcination 1h at DEG C removes surface treating agent.Then glass is taken out to and is placed at room temperature for 30min, then be dipped in 1wt.%KH550
In amino silicane coupling agent aqueous solution, 10min is impregnated, takes out the glass fibre after impregnating, puts it into baking oven and is dried at 50 DEG C
Dry 1h, after baking oven will be warming up to 120 DEG C, and high-temperature process 2-4h.In the drying process, hydrolysis can occur for KH-550,
And O-Si-O key is formed with glass fibre.
Second step, using 0 °/90 °, uniaxial cloth both ends alignment of fibers, uniform ground are layered on system by 0 °/90 ° ply sequences
On sample platform.
Third step is opened vacuum pump, is vacuumized, and after pressure vacuum gauge reaches -0.9, closes vacuum buffer valve,
After 15min check mold pressure vacuum gauge, such as pressure gauge registration≤- 0.85, then the sealant of injecting glue pipe port removes, be put by
According to the resin barrel that predetermined comparison prepares, start into glue, when resin complete wetting, stops injecting glue, and after keeping 30min, then
By glue inlet tube doubling and take out glue inlet tube.
Perfusion part after the completion of perfusion, is kept vacuum condition and is warming up to 70 DEG C of heat preservation 8h by the 4th step, solid to complete resin
Change.
5th step after the completion of solidification, removes the vacuum aided material on laminate surface, and the sundries of laminated plate surface is clear
Reason is clean, spare.
Compared with unmodified laminate, laminate prepared by the present embodiment, 0 ° of tensile strength improves 21%
(1280MPa v.s.1059MPa), 0 ° of compressive strength improve 18% (1017MPa v.s.862MPa), and in-plane shear strength mentions
High 16% (54.7MPa v.s.47.2MPa).
Embodiment 2
The first step uniaxially will be cut into the square of 600 × 600mm by glass fabric, be placed in Muffle furnace, 150
Calcination 1h at DEG C removes surface treating agent.Then glass is taken out to and is placed at room temperature for 30min, then be dipped in 1wt.%KH-
In 560 epoxy silane coupling aqueous solutions, and a small amount of acetic acid is added and adjusts solution ph 5.5, impregnates 10min, take out and impregnate
Glass fibre afterwards is put it into baking oven in 50 DEG C of drying 1h, after baking oven is warming up to 120 DEG C, and high-temperature process 2-4h.
Second step, using 0 °/90 °, uniaxial cloth both ends alignment of fibers, uniform ground are layered on system by 0 °/90 ° ply sequences
On sample platform.
Third step is opened vacuum pump, is vacuumized, and after pressure vacuum gauge reaches -0.9, closes vacuum buffer valve,
Check that the sealant of injecting glue pipe port is then removed, be put into such as pressure gauge registration≤- 0.85 by mold pressure vacuum gauge after 15min
According to the resin barrel that predetermined comparison prepares, start into glue, when resin complete wetting, stop injecting glue, and after keeping 30min,
By glue inlet tube doubling and take out glue inlet tube again.
Perfusion part after the completion of perfusion, is kept vacuum condition and is warming up to 70 DEG C of heat preservation 8h by the 4th step, solid to complete resin
Change.
5th step after the completion of solidification, removes the vacuum aided material on laminate surface, and the sundries of laminated plate surface is clear
Reason is clean, spare.
Compared with unmodified laminate, laminate prepared by the present embodiment, 0 ° of tensile strength improves 23%
(1302MPa v.s.1059MPa), 0 ° of compressive strength improve 19% (1025MPa v.s.862MPa), and in-plane shear strength mentions
High 15% (54.3MPa v.s.47.2MPa).
In above-described embodiment, by the type of silane coupling agent, KH-550, KH-560, KH-570, KH-792, DL- are replaced with
One of 602 or a variety of, it can also obtain preferable result.
The object of the present invention is to improve glass-fibre reinforced resin composite materials property used in current wind electricity blade, solve
The problems such as interface binding power certainly between resin and glass is weak and resin infiltration is poor.
The present invention handles glass fibre using silane coupling agent, effectively raises the wellability between resin and fiber,
Avoid the probability for occurring hickie and defect in product.Meanwhile the introducing of coupling agent significantly improves the boundary between glass and resin
Face binding force, so that the stretching of composite material, compression, bending, cutting performance be greatly improved.Through silane coupler modified
Afterwards, 0 ° of tensile strength of the laminate improves 20% or more, and 0 ° of compressive strength improves 15% or more, and in-plane shear strength mentions
It is high by 15% or more.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, this
Field technical staff makes a little simple modification, equivalent variations or modification using the technology contents of the disclosure above, all falls within this hair
In bright protection scope.
Claims (10)
1. a kind of modified glass-fiber reinforced resin laminate, which is characterized in that the laminate is by several layers modified glass fibre
Peacekeeping resin is poured by vacuum perfusion process, and the several layers modified glass-fiber uses 0 °/90 ° or 45 °/- 45 ° of ﹢
Direction tiling, the modified glass-fiber be pass through silane coupler modified glass fibre.
2. modified glass-fiber reinforced resin laminate according to claim 1, which is characterized in that the glass fibre is adopted
With uniaxially, twin shaft or three axis glass fibres.
3. modified glass-fiber reinforced resin laminate according to claim 1 or 2, which is characterized in that the glass fibers
Dimension size is 600mm × 600mm.
4. a kind of preparation method of modified glass-fiber reinforced resin composite material, which comprises the steps of:
1) Muffle furnace high temperature calcination is put into after cutting glass fibre；
2) will be cooling by the glass fibre room temperature environment of high temperature sintering, it is then immersed in silane coupler solution；
3) take out the glass fibre after impregnating, put it into baking oven and dried at 45~55 DEG C, after baking oven is warming up to 120 DEG C,
It carries out high-temperature process and obtains modified glass-fiber so that silane coupling agent is chemically combined with glass fibre；
4) fiber laying: modified glass-fiber is evenly laid out according to the direction of 0 °/90 ° or 45 °/- 45 ° of ﹢；
5) resin is perfused using vacuum perfusion process in fiber laying；
6) it after the completion of being perfused, keeps vacuum condition to be warming up to 70 DEG C perfusion part, completes resin solidification；
7) laminate is obtained after the completion of solidification, is then demoulded and is post-processed.
5. the preparation method of modified glass-fiber reinforced resin composite material according to claim 4, which is characterized in that institute
It states in step 1), the high temperature sintering time is 30-60min.
And/or glass fibre using uniaxially, twin shaft or three axis glass fibres；
And/or the cutting size of glass fibre is 600mm × 600mm.
6. the preparation method of modified glass-fiber reinforced resin composite material according to claim 4 or 5, feature exist
In in the step 2), room temperature cooling time is 25~35min, and soaking time is 8~15min；
And/or the silane coupling agent selects one of KH-550, KH-560, KH-570, KH-792, DL-602 or a variety of.
7. according to the preparation method of any modified glass-fiber reinforced resin composite material of claim 4 to 6, feature
It is, in the step 3), 50 DEG C of drying 40min~1.5h in baking oven, 120 DEG C of high-temperature process time is 2-4h.
8. according to the preparation method of any modified glass-fiber reinforced resin composite material of claim 4 to 7, feature
It is, in the step 5), vacuum perfusion process are as follows: open vacuum pump, vacuumize, after pressure vacuum gauge reaches -0.9, close
Vacuum buffer valve is closed, checks that mold pressure vacuum gauge then starts priming by vacuum such as pressure gauge registration≤- 0.85 after 15min,
The sealant of injecting glue pipe port is removed, the resin barrel prepared according to predetermined comparison is put into, is started into glue, until resin soaks completely
Profit stops injecting glue, and after pressure maintaining 30min, then by glue inlet tube doubling and takes out glue inlet tube；
And/or the resin is epoxy resin.
9. according to the preparation method of any modified glass-fiber reinforced resin composite material of claim 4 to 8, feature
It is, in the step 6), in 70 DEG C of heat preservation 8h；
And/or demoulding and post-processing include: the vacuum aided material for removing laminate surface, and by the sundries of laminated plate surface
It cleans out, it is spare.
10. the application for the laminate that a kind of any preparation method of claim 4~9 is prepared, which is characterized in that use
In the blade of production wind-driven generator.
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| CN112012013B (en) * | 2020-09-07 | 2021-06-01 | 湖南大学 | Nano-cellulose toughened mixed fiber yarn composite material laminated plate and preparation method thereof |
| CN114163773A (en) * | 2021-10-30 | 2022-03-11 | 贵州通用航空有限责任公司 | High-stability carbon fiber cloth coating material for light aircraft and manufacturing method thereof |
| CN115196889A (en) * | 2022-08-01 | 2022-10-18 | 中国科学院合肥物质科学研究院 | Method for modifying surface and enhancing insulation of glass fiber subjected to heat treatment of superconducting magnet |
| CN115196889B (en) * | 2022-08-01 | 2024-01-30 | 中国科学院合肥物质科学研究院 | Glass fiber surface modification and insulation enhancement method used after superconducting magnet heat treatment |
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