CN107573649A - A kind of fast curing prepreg epoxy-resin systems and preparation method thereof - Google Patents
A kind of fast curing prepreg epoxy-resin systems and preparation method thereof Download PDFInfo
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- CN107573649A CN107573649A CN201710265971.2A CN201710265971A CN107573649A CN 107573649 A CN107573649 A CN 107573649A CN 201710265971 A CN201710265971 A CN 201710265971A CN 107573649 A CN107573649 A CN 107573649A
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Abstract
The present invention relates to a kind of fast curing prepreg epoxy-resin systems and preparation method thereof, the matrix resin of epoxy-resin systems is the composition of bisphenol A epoxide resin, multiple functional radical novolac epoxy resin, halogenated epoxy resin and multiple functional radical epihydric alcohol amine resin, latent curing agent, accelerator and catalyst are added in the matrix resin of the epoxy-resin systems, produces epoxy-resin systems.The present invention makes hardening time shorten within 30 minutes, can substantially reduce the cost of composite material process planning by adding catalyst and increase multiple functional radical resin ratio；Due to fully applying the cooperative effect of a variety of epoxy resin characteristics, make system that there is excellent wellability to fiber, can be used as the making of the multiple fiber prepreg such as carbon fiber, glass fibre, aramid fiber.
Description
Technical field
The present invention relates to resin preparation field in a kind of high polymer material, and in particular to a kind of fast curing prepreg ring
Epoxy resin system and preparation method thereof.
Background technology
Fiber-resin composite is with the premium properties such as its high temperature resistant, rub resistance, corrosion-resistant, Gao Biqiang, Gao Bimo
It is widely used in the field such as Aeronautics and Astronautics and naval vessel.Prepreg is the intermediate for preparing composite, and its performance is again
Depend primarily on resin system.Therefore, the research and development of prepreg resin system turn into the focus of field of compound material concern.As
The representative of thermosetting resin, epoxy resin have good physical and chemical performance, and its solidfied material dielectric properties is good, shrinkage factor
Small, dimensionally stable, hardness is high, good toughness, to alkali and most of solvent-stable.The particularly good adhesive property of epoxy resin
With excellent fiber wetness energy, have the function that its is irreplaceable for manufacture prepreg.But current prepreg asphalt mixtures modified by epoxy resin
Resin system hardening time is grown, typically at 180 minutes or so.
The content of the invention
It is an object of the invention to provide a kind of fast curing prepreg epoxy-resin systems.
The present invention also aims to provide the preparation method of above-mentioned fast curing prepreg epoxy-resin systems.
The purpose of the present invention is to be achieved through the following technical solutions:A kind of fast curing prepreg epoxy-resin systems
Preparation method, the preparation method comprises the following steps：1. the preparation of epoxy-resin systems matrix resin:By bisphenol-A epoxy
Resin, multiple functional radical novolac epoxy resin, halogenated epoxy resin and multiple functional radical epihydric alcohol amine resin are progressively added by proportional quantity
Enter into the equipment heated with oil bath, after being sufficiently stirred, being sufficiently mixed at 110 DEG C, be cooled to 70~75 DEG C, obtain matrix resin；
2. after latent curing agent, accelerator and catalyst are mixed by proportioning, ground and mixed is carried out on three-roll grinder,
Until levigate and uniform curing agent composition；
3. 2. curing agent composition that step is obtained be added step-wise to 70~75 DEG C and the lower step of stirring 1. obtained by base
In body resin, make latent curing agent, accelerator and catalyst dispersed；Discharging, produces fast curing prepreg epoxy
Resin system；
The step 1. described in bisphenol A epoxide resin, multiple functional radical novolac epoxy resin, halogenated epoxy resin and multiple functional radical
The weight proportion of epihydric alcohol amine resin is bisphenol A epoxide resin:Polyfunctionality novolac epoxy resin：Halogenated epoxy resin：It is more
Functional group epihydric alcohol amine resin=20~40：20~30：20~30：5~20；
The weight proportion of the step 3. matrix resin, latent curing agent, accelerator and catalyst is：Matrix resin：It is latent
Curing agent：Accelerator：Catalyst=100：4~7：1.5~3.0：0.05~0.15.
Halogenated epoxy resin of the present invention is fluorinated epoxy resin, one kind in brominated epoxy resin or combination.
Multiple functional radical phenolic resin of the present invention is multiple functional radical phenol linear phenolic epoxy resin, multiple functional radical neighbour's first
One kind or combination in phenol linear phenolic epoxy resin.
Multiple functional radical epihydric alcohol amine resin of the present invention is triglycidyl group isocyanuric acid ester, four glycidols
Base dimethylphenylene diamine, one kind in four glycidyl group diaminourea dimethylene benzene or combination.
Further, step 1. described in bisphenol A epoxide resin be liquid or solid, its amount changes according to season.
Step of the present invention 2. in latent curing agent be dicyandiamide.
Step of the present invention 2. in accelerator for benzyl dimethyl urea, 3-（3,4 dichlorophenyls）One in -1,1- dimethyl urea
Kind or combination.
2. middle catalyst is cobalt naphthenate, chromium naphthenate, cobaltous octadecanate, one kind or group in cobalt octoate to step of the present invention
Close.
The product of the present invention, its technical indicator are as follows：
The present invention by add catalyst and increase multiple functional radical resin ratio, hardening time is shortened within 30 minutes, can
Reduce the cost of composite material process planning；Due to fully applying the cooperative effect of a variety of epoxy resin characteristics, make system pair
Fiber has good wellability, can be used as the making of the multiple fiber prepreg such as carbon fiber, glass fibre and aramid fiber.This
Invent make carbon fiber prepreg, glass fibre prepreg and aramid fiber prepreg, be successfully applied to aviation mask case,
Aircarrier aircraft and high-speed train chair and helicopter ducting assembly, the production of aircrew helmet.
Embodiment
Embodiment 1
By 10.8 kilograms of dicyandiamide, 2.7 kilograms of phenyl dimethylurea and cobalt naphthenate, chromium naphthenate, cobaltous octadecanate mixture
After 0.12 kilogram of mixing, ground and mixed is carried out on three-roll grinder, curing agent composition is made；In 300 heated with oil bath
20 kilograms of liquid bisphenol A epoxy resin, slowly heating, progressively solid bisphenol A rings under stirring are gradually added in the reactor of liter
32 kilograms of oxygen tree fat, 64 kilograms of multiple functional radical orthoresol linear phenolic epoxy resin, 54 kilograms of brominated epoxy resin and four shrinks
10 kilograms of glyceryl dimethylphenylene diamine, is warming up to 110 DEG C, after being thoroughly mixed, and is cooled to 70~75 DEG C, is gradually added above-mentioned
Curing agent composition, and be dispersed with stirring in this temperature range（If discharging is cooled to the milky that room temperature produces about 193 kilograms
Stored under semi-solid products, room temperature or low temperature stand-by）, then glue spreader is sent to by measuring pump, regulation applies rubber-surfaced roll spacing
With release liners transfer rate, glued membrane is made；Carbon fiber/epoxy resin prepreg, prepreg is made with K12 monofilament carbon fibers in glued membrane
Solidify 30 minutes at 130 DEG C, completion of cure.
Embodiment 2
By 10.0 kilograms of dicyandiamide, benzyl dimethyl urea and 3-（3,4 dichlorophenyls）3.0 kilograms of the mixture of -1,1- dimethyl urea
After 0.1 kilogram of mixing of cobalt naphthenate, ground and mixed is carried out on three-roll grinder, curing agent composition is made；In band oil
Bathe and 35 kilograms of liquid bisphenol A epoxy resin, slowly heating, progressively solid under stirring are added in the reactor of 300 liters of heating
20 kilograms of bisphenol A epoxide resin, 60 kilograms of polyfunctionality phenol linear phenolic epoxy resin, 50 kilograms of brominated epoxy resin and four
15 kilograms of glycidyl dimethylphenylene diamine, is warming up to 110 DEG C, after being thoroughly mixed, and is cooled to 70~75 DEG C, is gradually added
Curing agent composition, and be dispersed with stirring in this temperature range（If discharging is cooled to the milky half that room temperature produces about 194 kilograms
Stored under solid product, room temperature or low temperature stand-by）, then glue spreader is sent to by measuring pump, regulation apply rubber-surfaced roll spacing and
Release liners transfer rate, is made glued membrane；Glass fibre/epoxy prepreg is made in glued membrane and eight satin weave glass cloth dimension, presoaks
Material solidifies 30 minutes at 130 DEG C, completion of cure.
Claims (8)
1. a kind of preparation method of fast curing prepreg epoxy-resin systems, it is characterised in that comprise the following steps：1. ring
The preparation of epoxy resin system matrix resin:By bisphenol A epoxide resin, multiple functional radical novolac epoxy resin, halogenated epoxy resin and
Multiple functional radical epihydric alcohol amine resin is added step-wise to by proportional quantity in the equipment of oil bath heating, to be sufficiently stirred, fill at 110 DEG C
After dividing mixing, 70~75 DEG C are cooled to, obtains matrix resin；
2. after latent curing agent, accelerator and catalyst are mixed by proportioning, ground and mixed is carried out on three-roll grinder,
Until levigate and uniform curing agent composition；
3. 2. curing agent composition that step is obtained be added step-wise to 70~75 DEG C and the lower step of stirring 1. obtained by base
In body resin, make latent curing agent, accelerator and catalyst dispersed；Discharging, produces fast curing prepreg epoxy
Resin system；
The step 1. described in bisphenol A epoxide resin, multiple functional radical novolac epoxy resin, halogenated epoxy resin and multiple functional radical
The weight proportion of epihydric alcohol amine resin is bisphenol A epoxide resin:Polyfunctionality novolac epoxy resin：Halogenated epoxy resin：It is more
Functional group epihydric alcohol amine resin=20~40：20~30：20~30：5~20；
The weight proportion of the step 3. matrix resin, latent curing agent, accelerator and catalyst is：Matrix resin：It is latent
Curing agent：Accelerator：Catalyst=100：4~7：1.5~3.0：0.05~0.15.
2. the preparation method of fast curing prepreg epoxy-resin systems according to claim 1, it is characterised in that：Institute
It is fluorinated epoxy resin, one kind in brominated epoxy resin or combination to state halogenated epoxy resin.
3. the preparation method of fast curing prepreg epoxy-resin systems according to claim 1, it is characterised in that：Institute
Multiple functional radical phenolic resin is stated as multiple functional radical phenol linear phenolic epoxy resin, multiple functional radical orthoresol novolac epoxy tree
One kind or combination in fat.
4. the preparation method of fast curing prepreg epoxy-resin systems according to claim 1, it is characterised in that：Institute
Multiple functional radical epihydric alcohol amine resin is stated as triglycidyl group isocyanuric acid ester, four glycidyl group dimethylphenylene diamine, four
One kind or combination in glycidyl diaminourea dimethylene benzene.
5. the preparation method of fast curing prepreg epoxy-resin systems according to claim 1, it is characterised in that：Step
Suddenly 2. in latent curing agent be dicyandiamide.
6. the preparation method of fast curing prepreg epoxy-resin systems according to claim 1, it is characterised in that：Step
Suddenly 2. in accelerator for benzyl dimethyl urea, 3-（3,4 dichlorophenyls）One kind or combination in -1,1- dimethyl urea.
7. the preparation method of fast curing prepreg epoxy-resin systems according to claim 1, it is characterised in that：Step
Rapid 2. middle catalyst is cobalt naphthenate, chromium naphthenate, cobaltous octadecanate, one kind in cobalt octoate or combination.
It is 8. fast prepared by a kind of preparation method of the fast curing prepreg epoxy-resin systems described in claim 1 to 7
Speed solidification epoxy resin for prepreg system.
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| CN201710265971.2A CN107573649A (en) | 2017-04-21 | 2017-04-21 | A kind of fast curing prepreg epoxy-resin systems and preparation method thereof |
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| CN201710265971.2A CN107573649A (en) | 2017-04-21 | 2017-04-21 | A kind of fast curing prepreg epoxy-resin systems and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111100423A (en) * | 2019-12-27 | 2020-05-05 | 惠柏新材料科技（上海）股份有限公司 | Single-liquid epoxy resin composition and fiber-reinforced composite material |
| CN111139660A (en) * | 2019-12-24 | 2020-05-12 | 深圳昌茂粘胶新材料有限公司 | Graphene modified anticorrosion composite adhesive tape and preparation method thereof |
| CN113480766A (en) * | 2021-06-17 | 2021-10-08 | 牧世复合材料科技(苏州)有限公司 | Preparation method of rapid curing fiber prepreg with incubation period |
| CN115044172A (en) * | 2022-06-09 | 2022-09-13 | 台州市黄岩区武汉理工高性能复合材料技术研究院 | Single-component epoxy resin composition for prepreg and preparation method thereof |
Citations (2)
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|---|---|---|---|---|
| CN103694455A (en) * | 2012-09-28 | 2014-04-02 | 中国石油天然气股份有限公司 | Blending method of epoxy resin applicable to preparing carbon fiber preimpregnated material by medium-temperature heat melting method |
| CN106046680A (en) * | 2016-05-30 | 2016-10-26 | 中航复合材料有限责任公司 | Flame-retardant and heat-resistant epoxy resin for self-adhesive prepreg |
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2017
- 2017-04-21 CN CN201710265971.2A patent/CN107573649A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694455A (en) * | 2012-09-28 | 2014-04-02 | 中国石油天然气股份有限公司 | Blending method of epoxy resin applicable to preparing carbon fiber preimpregnated material by medium-temperature heat melting method |
| CN106046680A (en) * | 2016-05-30 | 2016-10-26 | 中航复合材料有限责任公司 | Flame-retardant and heat-resistant epoxy resin for self-adhesive prepreg |
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| 徐小兵: "《油气长输管道工程施工技术手册》", 31 May 2011, 石油工业出版社 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111139660A (en) * | 2019-12-24 | 2020-05-12 | 深圳昌茂粘胶新材料有限公司 | Graphene modified anticorrosion composite adhesive tape and preparation method thereof |
| CN111100423A (en) * | 2019-12-27 | 2020-05-05 | 惠柏新材料科技（上海）股份有限公司 | Single-liquid epoxy resin composition and fiber-reinforced composite material |
| CN113480766A (en) * | 2021-06-17 | 2021-10-08 | 牧世复合材料科技(苏州)有限公司 | Preparation method of rapid curing fiber prepreg with incubation period |
| CN115044172A (en) * | 2022-06-09 | 2022-09-13 | 台州市黄岩区武汉理工高性能复合材料技术研究院 | Single-component epoxy resin composition for prepreg and preparation method thereof |
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