CN101920587B - High-performance fire-retarding epoxy resin composite material and preparation thereof - Google Patents
High-performance fire-retarding epoxy resin composite material and preparation thereof Download PDFInfo
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- CN101920587B CN101920587B CN 201010276362 CN201010276362A CN101920587B CN 101920587 B CN101920587 B CN 101920587B CN 201010276362 CN201010276362 CN 201010276362 CN 201010276362 A CN201010276362 A CN 201010276362A CN 101920587 B CN101920587 B CN 101920587B
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Abstract
The invention discloses a fire-retarding epoxy resin composite material and a preparation method thereof. The composite material is divided into two parts which are a surface layer and a body respectively, wherein the surface layer is an aluminum foil; and the body part consists of fiberglass fabric, epoxy resin, a curing agent and a fire retardant. The preparation method for the composite material comprises the following steps of: performing fire-retarding treatment on the epoxy resin, preparing glue solution from the treated epoxy resin and the curing agent, performing surface treatment on the fiberglass fabric, impregnating the treated fiberglass fabric in the glue solution, draining water from the fiberglass fabric and drying the fiberglass fabric to prepare prepreg; performing the surface treatment on the aluminum foil with the ethanol solution of sodium hydroxide; combining the prepreg and the aluminum foil and placing the combination product on a hot press for molding; and finally cutting burrs and detecting the finished product. The composite material has the characteristics of economical, simple and convenient method, small added fire retardant amount, high performance, limited oxygen index higher than 40, capability of resisting the firing of acetylene flame for more than 10 minutes without through-burning, heat release and smoke release over 100 times lower than that of ordinary epoxy resin, no molten drop, and heat release and smoke release properties capable of satisfying the needs of aircraft and ship manufacture.
Description
Technical field
The present invention relates to a kind of lightweight, high-strength, fire-retarding epoxy resin composite material and preparation method thereof.
Background technology
Composite has the characteristics such as rigidity is large, intensity is high, quality is light; can design and make according to service condition; compare with metal material; has good endurance; required protection is few; parts can be integrated, and corrosion resistance is strong, carry out the advantages such as structure monitoring by utilizing intelligent fiber material and embedded type sensor.The material requirements that is used for aircraft manufacturing has higher specific strength and specific stiffness, to alleviate the construction weight of aircraft, improve flying quality, increase economic benefit, and has good machinability, be convenient to make needed part, the composite fast development has substituted metal material and has been used in a large number the aircraft manufacturing industry.
Epoxy resin is a kind of important resin kind, compares with other macromolecular materials, and epoxy resin has cure shrinkage low (only 1%-3%); Solidifying pressure is low, substantially non-volatile part; Adhesive property is good, the surface of metal and nonmetallic materials is had the characteristics such as adhesive strength of excellence, and Properties of Epoxy Resin is superior, is a kind of main matrices of composite material.Another key component of composite namely strengthens body, mainly is divided into fiber, whisker and particle etc., and the most frequently used fibre reinforcement is glass fibre.Glass fibre have cost low, do not burn, heat-resisting, chemical resistance good, hot strength and the characteristics such as impact strength is high, fracture elongation is little, thermal insulation is good.The composite material strength that is composited by epoxy resin and glass fabric is high, properties is superior, satisfy the aircraft material to the requirement of mechanical property, therefore, Unidirectional Glass Fiber Reinforced Epoxy Composites has been widely used in all trades and professions such as Aero-Space, automobile making.
Raising along with people's security against fire consciousness can require more and more higher to Flame Retardancy.But the inflammability of epoxy resin itself (limited oxygen index only is 19.8) can not satisfy it as the needs of advanced composite material, has limited greatly its application.Therefore, the development high-performance fire-retarding epoxy resin composite material is significant.
Improve the most frequently used method of epoxy resin (EP) fire resistance and be divided into two kinds of additive flame combustion technology and reaction-type flame-retarding technology.So-called additive flame combustion technology is that fire retardant is scattered among the EP with physical form, thereby obtains fire-retardant EP.Used fire retardant can be divided into Halogen, phosphorous, boracic, contain antimony and other metal fire retardant etc. by contained element.And the ignition-proof element (such as halogen, P, Si, N etc.) in reaction-type flame-retarding (also the claiming active flame-proof) technology finally all is attached in the macromolecular chain of EP, it has the advantages such as anti-migration, heat endurance and good stability of the dimension, but because its cost is high, be not easy to realize, limited the application in industrial production.The additive flame combustion technology has the characteristics such as simple process, raw material sources be extensive, is present the most frequently used ethoxyline resin antiflaming method.The additive flame retardant that uses at present can be divided into inorganic combustion inhibitor (comprising filler), organic fire-retardant.The most frequently used inorganic combustion inhibitor of preparation halogen-free flameproof EP has metal oxide (such as aluminium hydroxide, magnesium hydroxide), boride (such as Firebrake ZB), Phos system (mainly comprising red phosphorus, phosphate and APP) etc.The addition that but the shortcoming of additive flame combustion technology maximum is exactly the flame retardant level that will reach certain to be needed is very large (such as Al (OH)
3Addition usually to reach 50%-200%), this just produces greatly impact to the mechanical property of composite.Present industrial multiplex halogen containing flame-retardant, but because the dispute of halogen containing flame-retardant aspect toxicity and environment, halogen flame is eliminated.The present invention adopts interpolation halogen-free flame retardants and material surface to cover the mode that fireprotection layer is assisted mutually, and by surface modification raising material mechanical performance, obtain excellent flame retarding and smoke suppressing properties on the basis that guarantees material mechanical performance, and have eco-friendly characteristics.The epoxy resin composite material mechanical property of developing and security performance are excellent, can be used for the aspects such as manufacturing of aircraft, automobile, steamer, yacht and large-scale games for play.
Summary of the invention
Make the poor problem of fire resistance in order to solve present epoxy resin composite material as Sealing Arrangements such as car and boat, the present invention aims to provide a kind of lightweight that space flight and aviation needs, high-strength, fire-retarding epoxy resin composite material and preparation method thereof of being applicable to.
Epoxy resin composite material structure of the present invention is divided into two parts: (1) is the top layer up and down, and (2) are the main body between the top layer up and down; The top layer is aluminium foil up and down, main body is comprised of following raw material: glass fabric 50-70 weight portion, and epoxy resin 20-40 weight portion accounts for the fire retardant of the weight portion of epoxy resin 10%-40%, account for the curing agent of the weight portion of epoxy resin 8%-12%, account for the promoter of epoxy resin 0.1%-1% weight portion.Described glass fabric kind is one or both in twill, the plain.
Described fire retardant prescription is: APP and boric acid in mass ratio 1:1 form, and amount of flame-retardant agent is 25% weight portion of epoxy resin.The fire retardant mechanism of these two kinds of fire retardants of APP and boric acid is different, and two kinds of fire retardants can replenish mutually at different combustion phases performance flame retardant effects in the combustion process of material, and flame retardant effect is better than using merely a kind of fire retardant.
Described curing agent is dicyandiamide, and consumption is the weight portion of 10 % of epoxy resin; Described promoter is glyoxal ethyline, and consumption is the weight portion of 0.2 % of epoxy resin;
The preparation method of a kind of high-performance fire-retarding epoxy resin composite material of the present invention is: epoxy resin carries out flame treatment by fire retardant, be mixed with glue with curing agent, promoter, diluent according to the proportioning of prescription, glass fabric is through surface treatment, immersing to take out in the glue places drying box to heat, be prepared into prepreg, time is 1-2h, and temperature is 120 ℃-150 ℃.Adopt the NaOH ethanolic solution of 28%-32% that aluminium foil is carried out preliminary treatment.Epoxy prepreg and aluminium foil combination place moulding on the hot press, and temperature is 140 ℃-160 ℃, and pressure is 0.5-3.0MPa, cuts away at last burr, detects finished product.
Described flame treatment process is with the fire retardant porphyrize, sieves, mixes, and adds in the epoxy resin to stir.
Described diluent is acetone, and content is the weight portion of the 10-40% of epoxy resin.
A kind of high-performance fire-retarding epoxy resin composite material material of main part of the present invention is processed through halogen-free flame retardants, the Surface mulch aluminium foil, and required fire retardant addition is few, limited oxygen index surpasses 40, be difficult to for a long time under the high heat radiation light, and drip without melting, flue dust is few; By the means of surface modification, improved fire retardant and epoxy resin compatibility, quality of materials is light, intensity is high; And have method economy, easy, characteristics such as environmental friendliness.
Description of drawings
Fig. 1 is the epoxy resin composite material structural representation.
Fig. 2 is the influence curve (testing by GB/T2406) that amount of flame-retardant agent refers to epoxy resin limit oxygen.
Fig. 3 is that amount of flame-retardant agent is to the influence curve (testing by GB/T1447) of epoxy resin stretching intensity.
Fig. 4 is that (caloradiance is 35kW/m for the HRR HRR curve of epoxy resin composite material sample
2).
Fig. 5 is that (caloradiance is 35kW/m for the living cigarette rate curve of epoxy resin composite material sample
2).
Fig. 6 is that (caloradiance is 35kW/m for the accumulation smoke release curve of epoxy resin composite material sample
2).
The specific embodiment
The invention will be further described below in conjunction with chart and embodiment.
Epoxy resin composite material structure of the present invention is divided into two parts: as shown in Figure 1, the aluminium foil top layer 1 up and down, up and down the main body between the top layer 2.
Embodiment 1
Epoxy resin by by APP and boric acid in mass ratio the fire retardant that forms of 1:1 carry out flame treatment, amount of flame-retardant agent is the weight portion of epoxy resin 25%, then be the dicyandiamide of the weight portion of epoxy resin 10% with consumption, consumption is the glyoxal ethyline of the weight portion of epoxy resin 0.2%, consumption is that the acetone of the weight portion of epoxy resin 30% is mixed with glue, glass fabric is through surface treatment, immerse to take out in the glue and place the drying box heating, drying, be prepared into prepreg, be 1h heat time heating time, and temperature is 130 ℃; Adopt 30% NaOH ethanolic solution to clean the aluminium foil top layer, clean with 95% ethanol again, for subsequent use.With prepreg and aluminium foil combination, place moulding on the hot press, forming temperature is 150 ℃, pressure is 1.0Mpa, cuts away at last burr, detects finished product.By the performance impact of each factor of a series of Experimental Research to material of the present invention.
At first inquire into APP and boric acid proportioning to the impact of epoxy resin limited oxygen index, when APP and boric acid proportioning were 1:1, flame retardant effect relatively other proportioning will be got well as can be seen from Table 1.
Table 1 APP and boric acid proportioning are on the impact of epoxy resin limited oxygen index
| Mass ratio | 100:0 | 80:20 | 60:40 | 50:50 | 40:60 | 20:80 | 0:100 |
| LOI（%） | 27.6 | 26.9 | 26.3 | 28.4 | 25.0 | 24.9 | 27.8 |
Then the fire retardant of selecting is the in mass ratio compound composition of 1:1 of APP and boric acid, for obtaining optimum amount of flame-retardant agent, and the research amount of flame-retardant agent is on the impact of mechanical performance, 5%, 10%, 15%, 20%, 25%, 30%, 35% and 40% a series of different amounts have been selected respectively, be prepared under the same conditions batten, hot strength is tested according to the GB/T1447 standard, and limited oxygen index is tested according to the GB/T2406 standard.Fig. 2 is that amount of flame-retardant agent is to the influence curve of epoxy resin limited oxygen index; Fig. 3 is that amount of flame-retardant agent is to the influence curve of epoxy resin stretching intensity; Analysis-by-synthesis Fig. 2 and Fig. 3 obtain a conclusion: along with the increase of amount of flame-retardant agent, the oxygen index (OI) of epoxy resin is in rising trend, and up to 40, but hot strength is under some influence.After adding APP, epoxy resin stretching intensity descends, and when the addition of fire retardant was less than 25%, hot strength increased and increases gradually with amount of flame-retardant agent, and after amount of flame-retardant agent surpassed 25%, along with the increase of consumption, hot strength sharply descended.Analyzing its reason should be powdery flame retardent and is added to epoxy resin as decentralized photo and has affected its adhesive power, cause hot strength to descend, and fire retardant can promote epoxy resin cure to a certain extent, strengthen the hot strength of solidfied material, after addition surpasses 25%, be equivalent to curing agent excessive, cause solidfied material to burn, hot strength sharply descends.Comprehensive two indexs, on the basis that affects composite materials property within reason, selecting the fire retardant addition is 25%.
The aluminium foil fire retardation of material surface is remarkable, adopts cone calorimeter to study the fire resistance of the high-performance fire-retarding epoxy resin composite material of the present invention's preparation.GB/T16172-2007 tests according to standard, and sample all faces except heating surface are wrapped up with aluminium-foil paper, puts into the stainless steel specimen mounting, intercepts heat transmission in the aluminium foil bottom with asbestos.Caloradiance is 35kW/m on the horizontal sample vertical direction
2, electric arc is lighted.The every 5s automatic data collection of computer 1 time adopts Excel to carry out data and processes.
Fig. 4 is that the epoxy resin composite material sample is at caloradiance 35kW/m
2Under HRR HRR curve, Fig. 5 and Fig. 6 are respectively living cigarette rate curve and the accumulation smoke release curves of epoxy resin composite material.Wherein A represents the epoxy resin composite material without flame treatment, and B represents the epoxy resin composite material through the fire retardant processing, and C represents to process the epoxy resin composite material that the while top layer is covered with aluminium foil through fire retardant.
As shown in Figure 4, appear at the 140s front and back without flame treatment epoxy resin composite material HRR peak of curve, peak value is 270.70 kW/m
2, in 300s, emit net quantity of heat; The epoxy resin composite material HRR peak of curve of processing through fire retardant appears at the 205s front and back, and peak value is 172.56 kW/m
2, net quantity of heat releases in 510s; The HRR curve of the composite that fire retardant was processed is lower than undressed composite HRR curve, shows that fire retardant has suppressed the burning exothermic effects of epoxy resin composite material.Do not light through 30min under this radiation intensity and process the epoxy resin composite material that top layer simultaneously is covered with aluminium foil through fire retardant, its HRR is zero, and decomposition combustion does not occur this explanation inner loop epoxy resins under the protection of aluminium foil.
By Fig. 5 and Fig. 6 as can be known, the SPR curve of the epoxy resin composite material that fire retardant was processed and TSR curve all are lower than the curve without the flame treatment epoxy resin composite material, and the introducing of this explanation fire retardant has not only been played fire-retardant effect but also pressed down the cigarette effect obvious.And behind the Surface mulch aluminium foil, it is almost nil that epoxy resin composite material is given birth to cigarette speed, and the living cigarette amount of accumulation is very little.
Final conclusion: selecting APP and boric acid 1:1 composite flame-retardant agent addition is 25% processing epoxy resin, the Surface mulch aluminium foil, its fire-retardant fire resistance of the high-performance fire-retarding epoxy resin composite material of making increases substantially, limited oxygen index surpasses 40, resisting the acetylene flame calcination did not burn through more than 10 minutes, heat discharges and cigarette release ratio ordinary epoxy resin hangs down more than 100 times, drips without melting, and heat discharges and the flue gas release performance can satisfy aircraft and ship manufacturing needs.
The comparative example:
Proportioning according to material in the table 2, according to the method among the embodiment 1, we have studied three kinds of dissimilar composites and have carried out the fire resistance contrast, can find out that by the data in the table 2 fire retardant and aluminium foil veneer that we prepare all can obviously increase flame retardant effect, fire-retarding epoxy resin composite material of the present invention has better performance.
Table 2 epoxy resin composite material sample prescription and performance
| Weight portion prescription and performance | Epoxy resin | Epoxy resin composite material | Fire-retarding epoxy resin composite material |
| Epoxy |
100 | 100 | 100 |
| Dicyandiamide+glyoxal ethyline | 10.2 | 10.2 | 10.2 |
| |
0 | 150 | 150 |
| Fire retardant | 0 | 0 | 25 |
| The aluminium foil veneer | Nothing | Nothing | Have |
| LOI（%）（GB/T2406） | 19.8 | 20.1 | ﹥40 |
| Burning grade (UL-94) | Burning | Burning | V-0 |
| Hot strength (MPa) (GB/T1447) | 310 | 335 | 300 |
| Total heat release (MJ/m 2）（GB/T16172-2007） | 61.247 | 33.980 | 0.187 |
| Smoke release (k m 2/m 2）（GB/T16172-2007） | 7435.7 | 3383.2 | 67.2 |
| Anti-flame is grilled thoroughly (HB/Z277-1995) | 0.4 min | 2.3 min | ﹥10min |
Claims (4)
1. high-performance fire-retarding epoxy resin composite material, it is characterized in that structure is divided into two parts: (1) is the top layer up and down, and (2) are the main body between the top layer up and down; The top layer is aluminium foil up and down, and main body is comprised of following raw material: glass fabric 50-70 weight portion, and epoxy resin 20-40 weight portion accounts for the curing agent of epoxy resin 8%-12% weight portion, the promoter that accounts for epoxy resin 0.1%-1% weight portion; Fire retardant, described fire retardant be APP and boric acid in mass ratio 1:1 form, amount of flame-retardant agent is 25% weight portion of epoxy resin.
2. a kind of high-performance fire-retarding epoxy resin composite material according to claim 1, it is characterized in that: described glass fabric kind is one or both in twill, the plain.
3. a kind of high-performance fire-retarding epoxy resin composite material according to claim 1, it is characterized in that: described curing agent is dicyandiamide, consumption is 10% weight portion of epoxy resin.
4. a kind of high-performance fire-retarding epoxy resin composite material according to claim 1, it is characterized in that: described promoter is glyoxal ethyline, consumption is 0.2% weight portion of epoxy resin.
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| WO2013113455A1 (en) | 2012-01-30 | 2013-08-08 | Valsem Industries Sas | Thermal insulation material with improved fire resistance |
| CN102785445A (en) * | 2012-08-06 | 2012-11-21 | 衡阳星鑫绝缘材料有限公司 | High-temperature heat-insulation electromagnetic shielding fabric and production method thereof |
| CN103979098B (en) * | 2014-05-22 | 2016-03-30 | 航天材料及工艺研究所 | A kind of flame-proof composite material floor and preparation method thereof |
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| CN106994803A (en) * | 2017-04-06 | 2017-08-01 | 湖南大学 | fibre metal laminate preparation method and fibre metal laminate |
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| CN116330807A (en) * | 2023-02-20 | 2023-06-27 | 江苏奇安特节能科技有限公司 | High-flame-retardance reinforced aluminum foil veneer and preparation method thereof |
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| JP4470578B2 (en) * | 2004-05-17 | 2010-06-02 | 日東紡績株式会社 | Reinforcing materials for cryogenic material containers |
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