CN103665758A - Modified epoxy resin system for carbon fiber boards for pultrusion structure reinforcement - Google Patents
Modified epoxy resin system for carbon fiber boards for pultrusion structure reinforcement Download PDFInfo
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- CN103665758A CN103665758A CN201210359092.3A CN201210359092A CN103665758A CN 103665758 A CN103665758 A CN 103665758A CN 201210359092 A CN201210359092 A CN 201210359092A CN 103665758 A CN103665758 A CN 103665758A
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Abstract
The invention discloses a modified epoxy resin system for carbon fiber boards for pultrusion structure reinforcement, which comprises the following components in parts by mass: 100 parts of epoxy resin, 60-90 parts of acid anhydride curing agent, 0-20 parts of epoxy group micromolecule compound, 0.5-10 parts of flaky organized montmorillonite or silica and 0.5-5 parts of curing accelerator. The organized montmorillonite is dispersed in the epoxy resin matrix in an interlayer stripping or intercalation mode by high-speed mechanical stirring, ultrasonic dispersion, vacuumizing and the like; and the mixture is further mixed with other assistants for carbon fiber pultrusion, thereby preparing the carbon fiber board for structure reinforcement, which has the advantages of high durability and high mechanical properties. The modified epoxy resin system has low viscosity and can easily implement pultrusion; and meanwhile, the cured molded board has the advantages of high strength, high modulus, high toughness, low water absorption and diffusion coefficient, and excellent durability in severe service environments.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of modified resin system of using carbon fiber sheet for pultrusion high performance structure reinforcement.
Background technology
As novel civil engineering material, the civil engineering material (as steel, concrete etc.) of carbon fiber pultrusion sheet material simultaneous interpretation system is compared, there is high-strength light, corrosion-resistant, fatigue performance is excellent, designability is strong, the easy advantage such as construction, is considered to realize civil engineering structure long lifetime, the most potential structured material of high-performance.In recent years, be applied to the repair and retrofit of civil engineering structure, to extend the work-ing life of Infrastructure, building, improve the properties such as its antidetonation, carrying, improve the safety performance of Infrastructure and engineering structure, as carbon fiber pultrusion sheet material is applied to Bending Reinforcement for Bridge, Shear Strengthening, harbour reinforcing reparation etc.Because civil engineering work Service Environment is severe, the carbon fiber pultrusion sheet material that is applied to structural strengthening is met to various hygrothermal environments, caustic soln, various sound loads etc.; What the service life of civil engineering structure also will be grown compared with traditional carbon fibres matrix material Application Areas (as aerospace) requirement simultaneously was many, as 50～100 years.In above-mentioned severe civil engineering work environment and long-term military service process, the performance degradation of carbon fiber pultrusion sheet material has determined the scope of security, economy and the application thereof of its structural strengthening.
For pultrusion structural strengthening, with the resin system of carbon fiber sheet, be mainly epoxy resin, in its military service process (as outer subsides Carbon Fiber Sheet-Reinforced, surperficial embedding inlay technique are reinforced).Because epoxy resin-base has stronger polarity, in civil engineering work military service process, it is inner that water molecules and various corrosive ion are inevitably penetrated into carbon fiber pultrusion sheet material, not only can cause plasticizing, the hydrolysis of resin matrix, and can cause the degeneration of fiber and resin matrix interface performance; Particularly, under stress coupling effect, the interface deterioration velocity of resin matrix, resin-fiber increases substantially.Therefore, the over-all properties (mechanical property, thermal characteristics) of structural strengthening carbon fiber pultrusion sheet material is along with the prolongation of active time, occur deteriorated, complete failure even, the performance that has a strong impact on ruggedized construction with use safety.Improving the endurance quality of fibre composite under complicated building environment, and predict its service life, is the important directions of modern civil engineering matrix material research.
The endurance quality of carbon fiber pultrusion sheet material under severe civil engineering work environment, depend primarily on water molecules absorption and the rate of diffusion of portion within it, reduce specific absorption and the rate of diffusion of water molecules in carbon fiber pultrusion sheet material, can increase substantially the endurance quality of carbon fiber pultrusion sheet material.Polynite has sheet silicate structure, and after organising, by certain preparation technology, its sheet silicate structure can be dispersed in resin matrix and (peel off dispersion), or resin matrix is inserted in sheet silicate structure (intercalation).Because silicate lamella has two-dirnentional structure, the sub the evolving path in epoxy resin inside that can moisturize, reduces the rate of diffusion of water molecules, thereby improves the endurance quality of resin matrix and corresponding carbon fiber pultrusion sheet material.Meanwhile, because the montmorillonite layer of good distribution (peeling off or intercalation) has nanostructure (its thickness is about 1 nanometer), can improve intensity, the modulus of resin and pultrusion sheet material thereof.How by the effective technique of simple economy, realize the high dispersing of epoxy-resin systems for polynite and pultrusion, guarantee that modified epoxy is applicable to the pultrude process of carbon fiber sheet simultaneously, moulding has the civil engineering structure reinforcing of high obstructing performance and uses pultrusion sheet material, yet there are no relevant report.
Summary of the invention
The object of this invention is to provide a kind of pultrusion structural strengthening with the modified epoxy resin system of pultrusion carbon fiber sheet and, modified epoxy resin system not only has good pultrusion performance, can improve the mechanical properties such as intensity, modulus of carbon fiber pultrusion sheet material simultaneously, and there is low water absorption and spread coefficient, possess the excellent durability energy under severe civil engineering work Service Environment.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of modified epoxy resin system of using carbon fiber sheet for pultrusion structural strengthening, it is characterized in that, count by weight, comprise following composition: 100 parts of epoxy resin, 60～90 parts of acid anhydride type curing agents, 0～20 part of the micromolecular compound that contains epoxide group, 0.5～10 part of sheet organic montmorillonoid, 0.5～5 part of curing catalyst.Described epoxy resin is selected from one or more of glycidyl ether based epoxy resin, Racemic glycidol amine epoxy resin, glycidyl ester based epoxy resin, phenolic epoxy resin, alicyclic ring based epoxy resin.
Described anhydride curing agent is selected from one or more of methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyl carbic anhydride, dodecenylsuccinic anhydride etc.
The described micromolecular compound with epoxide group is selected from propylene oxide, 2,3-propylene oxide methyl ether, phenyl glycidyl ether, butylglycidyl ether, glycidyl allyl ether, cresylglycidylether, ethylene glycol diglycidylether, butanediol diglycidyl ether, neopentylglycol diglycidyl ether, hexanediol diglycidyl ether, resorcinol diglycidyl ether, diglycidylaniline, trihydroxymethylpropanyltri diglycidyl ether, C
12-14one or more in alkyl glycidyl ether.
Described curing catalyst is one or more of imidazoles, phenols.
Described imidazoles curing catalyst, comprises, 2-ethyl-4-methylimidazole, benzyl-glyoxal ethyline, cyanoethyl-2-ethyl-4-methylimidazole, glyoxal ethyline.Described phenol curing catalyst is for example 2,4,6-three (dimethylamino methyl) phenol.
Described sheet organic montmorillonoid is the polynite through organic cation intercalation processing.
Another object of the present invention is to provide the preparation method of described modified epoxy resin system, and the method comprises the steps:
A) first by 100 parts of epoxy resin and 0～20 part of micromolecular compound that contains epoxide group in proportion by low speed (being less than 500 revs/min) mechanical stirring or mix with hand;
B), under stirring at low speed, 0.5～10 part of organo montmorillonite powder of treated cation is slowly joined to steps A) in the liquid prepared;
C) utilize high-shear stirring rake, at the high-speed stirring step B that surpasses 5000 revs/min) mixed solution prepared 0.5～2 hour;
D) by step C) mixed solution prepared is through ultrasonication 0.1～1 hour;
E) by step D) mixed solution prepared vacuumizes 0.1～1 hour;
F) pass through step e) in the mixed solution prepared, by adding in proper order 60～90 parts of anhydride curing agents and 0.5～5 part of curing catalyst, after stirring, for civil structure, reinforce and use sheet material pultrusion.
The inventor studies discovery: by preparation method of the present invention, can effectively positively charged ion organic montmorillonoid be scattered in epoxy resin-base, the dispersion state of organo montmorillonite in resin matrix is to peel off with intercalation to coexist, good stability; The micromolecular compound with epoxide group can effectively reduce the viscosity of organo montmorillonite and epoxy resin-base, is conducive on the one hand the dispersion of organo montmorillonite, is conducive to the infiltration of modified resin matrix and carbon fiber simultaneously, contributes to pultrude process; Carbon fiber strengthens the pultrusion sheet material of organic imvite modified resin system, the mechanical property such as tensile strength, modulus not only with improvement, and can significantly reduce the rate of diffusion of water molecules, thereby improved the endurance quality of carbon fiber pultrusion sheet material under severe civil engineering work environment.
Compare with carbon fiber pultrusion sheet material with existing civil engineering work, the present invention adopts the resin system of simple preparation technology, economy, has prepared the high-performance organic imvite modified epoxyresin system that is applicable to carbon fiber sheet pultrusion.
With unmodified epoxy resin, compare, the tensile strength of the organic imvite modified epoxyresin system of preparing by above-mentioned technique can improve more than 10%, and tensile modulus improves more than 20%, and elongation at break remains unchanged substantially; Meanwhile, water molecules also can significantly reduce more than 25% in the rate of diffusion of organic imvite modified epoxyresin system, thereby improves the water resistance of resin system.
Embodiment
Embodiment 1
By 500g bisphenol A-type glycidyl ether based epoxy resin E-51(Wuxi Resin Factory of Blue Star New Chemical Material Co., Ltd., oxirane value is 0.48～0.54) and 50g C
12-14alkyl glycidyl ether (AGE, Guangzhou Ku Te Chemical Co., Ltd.) low speed (stirring velocity is less than 200 revs/min) mixes; Then, slowly add 15g organic montmorillonoid (Zhejiang Feng Hong clay Chemical Co., Ltd.); After adding completely, improve rotating speed (high-shear stirring rake) to 5000～6000 revs/min, continuously stirring 60 minutes, in whipping process, barrel needs recirculated water cooling, keeps barrel temperature lower than 120
oc; After high-speed stirring, mixture contains a large amount of bubbles, becomes oyster white, with ultrasonic wave separating apparatus (Shanghai Bi Lang Instrument Ltd.), processes 30 minutes, and it is transparent that mixed solution becomes; Barrel is put into vacuum drying oven, vacuumizes 30 minutes; Under stirring at low speed, 400g methylhexahydrophthalic anhydride, 10g curing catalyst 2-ethyl-4-methylimidazole are blended in the mixture after vacuumizing, stir for pultrusion.Pultrusion molding process is hopper temperature 50
oc, die temperature (three sections) 160
oc, 170
oC, 180
oC, after fixing temperature 200
oc, pultrusion speed is 25mm/min; Pultrusion carbon fiber forming board dimension is wide 25mm, thick 1.4mm.According to pultrusion sheet material stretching intensity, modulus and the elongation at break of standard GB/T/T1447-2005 test index, test repeats 5 times, and the intensity that records this pultrusion sheet material is 2.4GPa, modulus 140GPa, and elongation at break is 1.5%.60
oin C deionized water, soak 3 months, its water-intake rate is less than 1%, and modulus declines and is less than 5%, and strength degradation is less than 10%.
Embodiment 2
By 250g bisphenol A-type glycidyl ether based epoxy resin E-51(Wuxi Resin Factory of Blue Star New Chemical Material Co., Ltd., oxirane value is 0.48～0.54), 250g Bisphenol F type tetraglycidel ether epoxy resin (Guangzhou Xin Ye trade Co., Ltd, model: YDF170) with 50g C
12-14alkyl glycidyl ether (AGE, Guangzhou Ku Te Chemical Co., Ltd.) low speed (stirring velocity is less than 200 revs/min) mixes; Then, slowly add 10g organic montmorillonoid (Zhejiang Feng Hong clay Chemical Co., Ltd.); After adding completely, improve rotating speed (high-shear stirring rake) to 5000～6000 revs/min, continuously stirring 60 minutes, in whipping process, barrel needs recirculated water cooling, keeps barrel temperature lower than 80
oc; After high-speed stirring, mixture contains a large amount of bubbles, becomes oyster white, with ultrasonic wave separating apparatus (Shanghai Bi Lang Instrument Ltd.), processes 30 minutes, and it is transparent that mixed solution becomes; Barrel is put into vacuum drying oven, vacuumizes 30 minutes; Under stirring at low speed, 400g methylhexahydrophthalic anhydride, 10g curing catalyst 2-ethyl-4-methylimidazole are blended in the mixture after vacuumizing, stir for pultrusion.Pultrusion molding process is hopper temperature 50
oc, die temperature (three sections) 160
oc, 170
oc, 180
oc, after fixing temperature 200
oc, pultrusion speed is 25mm/min; Pultrusion carbon fiber forming board dimension is wide 25mm, thick 1.4mm.According to standard GB/T/T
1447-2005tensile strength, modulus and the elongation at break of test pultrusion sheet material, test repeats 5 times, and the intensity that records this pultrusion sheet material is 2.5GPa, modulus 140GPa, elongation at break is 1.6%.60
oin C deionized water, soak 3 months, its water-intake rate is less than 0.8%, and modulus declines and is less than 6%, and strength degradation is less than 12%.
Embodiment 3
By 100 parts of bisphenol A-type glycidyl ether based epoxy resin E-51(Wuxi Resin Factory of Blue Star New Chemical Material Co., Ltd., oxirane value is 0.48～0.54) and 10 parts of C
12-14alkyl glycidyl ether (AGE, Guangzhou Ku Te Chemical Co., Ltd.) low speed (stirring velocity is less than 200 revs/min) mixes; Then, slowly add 10g organic montmorillonoid (Zhejiang Feng Hong clay Chemical Co., Ltd.); After adding completely, improve rotating speed (high-shear stirring rake) to 5000～6000 revs/min, continuously stirring 60 minutes, in whipping process, barrel needs recirculated water cooling, keeps barrel temperature lower than 120
oc; After high-speed stirring, mixture contains a large amount of bubbles, becomes oyster white, with ultrasonic wave separating apparatus (Shanghai Bi Lang Instrument Ltd.), processes 30 minutes, and it is transparent that mixed solution becomes; Barrel is put into vacuum drying oven, vacuumizes 30 minutes; Under stirring at low speed, 60 parts of methylhexahydrophthalic anhydrides, 2g curing catalyst 2-ethyl-4-methylimidazole are blended in the mixture after vacuumizing, stir for pultrusion.Pultrusion molding process is hopper temperature 50
oc, die temperature (three sections) 160
oc, 170
oC, 180
oC, after fixing temperature 200
oc, pultrusion speed is 25mm/min; Pultrusion carbon fiber forming board dimension is wide 25mm, thick 1.4mm.According to pultrusion sheet material stretching intensity, modulus and the elongation at break of standard GB/T/T1447-2005 test index, test repeats 5 times, and the intensity that records this pultrusion sheet material is 2.4GPa, modulus 140GPa, and elongation at break is 1.5%.60
oin C deionized water, soak 3 months, its water-intake rate is less than 1%, and modulus declines and is less than 5%, and strength degradation is less than 8%.
Embodiment 4
By 100 parts of bisphenol A-type glycidyl ether based epoxy resin E-51(Wuxi Resin Factory of Blue Star New Chemical Material Co., Ltd., oxirane value is 0.48～0.54) and 10 parts of C
12-14alkyl glycidyl ether (AGE, Guangzhou Ku Te Chemical Co., Ltd.) low speed (stirring velocity is less than 200 revs/min) mixes; Then, slowly add 10g organic montmorillonoid (Zhejiang Feng Hong clay Chemical Co., Ltd.); After adding completely, improve rotating speed (high-shear stirring rake) to 5000～6000 revs/min, continuously stirring 60 minutes, in whipping process, barrel needs recirculated water cooling, keeps barrel temperature lower than 120
oc; After high-speed stirring, mixture contains a large amount of bubbles, becomes oyster white, with ultrasonic wave separating apparatus (Shanghai Bi Lang Instrument Ltd.), processes 30 minutes, and it is transparent that mixed solution becomes; Barrel is put into vacuum drying oven, vacuumizes 30 minutes; Under stirring at low speed, 90 parts of methylhexahydrophthalic anhydrides, 2g curing catalyst 2-ethyl-4-methylimidazole are blended in the mixture after vacuumizing, stir for pultrusion.Pultrusion molding process is hopper temperature 50
oc, die temperature (three sections) 160
oc, 170
oC, 180
oC, after fixing temperature 200
oc, pultrusion speed is 25mm/min; Pultrusion carbon fiber forming board dimension is wide 25mm, thick 1.4mm.According to pultrusion sheet material stretching intensity, modulus and the elongation at break of standard GB/T/T1447-2005 test index, test repeats 5 times, and the intensity that records this pultrusion sheet material is 2.35GPa, modulus 140GPa, and elongation at break is 1.5%.60
oin C deionized water, soak 3 months, its water-intake rate is less than 1.2%, and modulus declines and is less than 8%, and strength degradation is less than 10%.
Comparing embodiment
By 100 parts of bisphenol A-type glycidyl ether based epoxy resin E-51(Wuxi Resin Factory of Blue Star New Chemical Material Co., Ltd., oxirane value is 0.48～0.54) and 10 parts of C
12-14alkyl glycidyl ether (AGE, Guangzhou Ku Te Chemical Co., Ltd.) low speed (stirring velocity is less than 200 revs/min) mixes; Then, add 80 parts of methylhexahydrophthalic anhydrides, 2 parts of curing catalyst 2-ethyl-4-methylimidazoles to be blended in the mixture after vacuumizing, stir for pultrusion.Pultrusion molding process is hopper temperature 50
oc, die temperature (three sections) 160
oc, 170
oC, 180
oC, after fixing temperature 200
oc, pultrusion speed is 25mm/min; Pultrusion carbon fiber forming board dimension is wide 25mm, thick 1.4mm.According to pultrusion sheet material stretching intensity, modulus and the elongation at break of standard GB/T/T1447-2005 test index, test repeats 5 times, and the intensity that records this pultrusion sheet material is 2.2GPa, modulus 130GPa, and elongation at break is 1.5%.60
oin C deionized water, soak 3 months, its water-intake rate is about 2.5%, and modulus declines approximately 12%, strength degradation approximately 20%.
Compare with the carbon fiber pultrusion sheet material of unmodified epoxy resin in comparing embodiment, carbon fiber of the present invention strengthens the pultrusion sheet material of organic imvite modified resin system, the mechanical property such as tensile strength, modulus not only with improvement, and can significantly reduce the rate of diffusion of water molecules, thereby improved the endurance quality of carbon fiber pultrusion sheet material under severe civil engineering work environment.
Claims (6)
1. one kind for the modified epoxy resin system of carbon fiber sheet for pultrusion structural strengthening, it is characterized in that, count by weight, comprise following composition: 100 parts of epoxy resin, 60～90 parts of acid anhydride type curing agents, 0～20 part of the micromolecular compound that contains epoxide group, 0.5～10 part of sheet organic montmorillonoid, 0.5～5 part of curing catalyst.
2. modified epoxy resin system according to claim 1, it is characterized in that, wherein said epoxy resin is selected from: one or more of glycidyl ether based epoxy resin, Racemic glycidol amine epoxy resin, glycidyl ester based epoxy resin, phenolic epoxy resin, alicyclic ring based epoxy resin.
3. modified epoxy resin system according to claim 1, it is characterized in that, wherein said acid anhydride type curing agent is selected from: one or more of methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyl carbic anhydride, dodecenylsuccinic anhydride.
4. modified epoxy resin system according to claim 1, it is characterized in that, the micromolecular compound that wherein contains epoxide group is selected from: propylene oxide, 2,3-propylene oxide methyl ether, phenyl glycidyl ether, butylglycidyl ether, glycidyl allyl ether, cresylglycidylether, ethylene glycol diglycidylether, butanediol diglycidyl ether, neopentylglycol diglycidyl ether, hexanediol diglycidyl ether, resorcinol diglycidyl ether, diglycidylaniline, trihydroxymethylpropanyltri diglycidyl ether, C
12-14one or more in alkyl glycidyl ether.
5. modified epoxy resin system according to claim 1, is characterized in that, wherein sheet organic montmorillonoid, is the polynite through organic cation intercalation processing.
6. modified epoxy resin system according to claim 1, it is characterized in that, curing catalyst is wherein one or more of following compound: imidazoles curing catalyst, comprise 2-ethyl-4-methylimidazole, benzyl-glyoxal ethyline, cyanoethyl-2-ethyl-4-methylimidazole, glyoxal ethyline; Phenol curing catalyst, as 2,4,6-three (dimethylamino methyl) phenol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210359092.3A CN103665758A (en) | 2012-09-25 | 2012-09-25 | Modified epoxy resin system for carbon fiber boards for pultrusion structure reinforcement |
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|---|---|---|---|
| CN201210359092.3A CN103665758A (en) | 2012-09-25 | 2012-09-25 | Modified epoxy resin system for carbon fiber boards for pultrusion structure reinforcement |
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| CN103665758A true CN103665758A (en) | 2014-03-26 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104060533A (en) * | 2014-06-03 | 2014-09-24 | 武汉二航路桥特种工程有限责任公司 | Novel compound deck repairing layer for concrete beam bridge |
| CN105111693A (en) * | 2015-08-27 | 2015-12-02 | 江苏易成电力器材有限公司 | Carbon nano composite fiber material and preparation method thereof |
| CN106432691A (en) * | 2016-07-21 | 2017-02-22 | 嘉兴市正大化工有限公司 | Curing agent special for pultrusion, and application thereof |
| CN107686632A (en) * | 2017-09-27 | 2018-02-13 | 卡本复合材料（天津）有限公司 | A kind of epoxy-resin systems of pultrusion carbon fiber sheet |
| CN111534260A (en) * | 2020-04-24 | 2020-08-14 | 北京康美特科技股份有限公司 | Epoxy resin packaging adhesive and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354198A (en) * | 2001-12-26 | 2002-06-19 | 河北工业大学 | Epoxy resin/montmorillonoid nano-compoiste-material and its preparation method |
-
2012
- 2012-09-25 CN CN201210359092.3A patent/CN103665758A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354198A (en) * | 2001-12-26 | 2002-06-19 | 河北工业大学 | Epoxy resin/montmorillonoid nano-compoiste-material and its preparation method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104060533A (en) * | 2014-06-03 | 2014-09-24 | 武汉二航路桥特种工程有限责任公司 | Novel compound deck repairing layer for concrete beam bridge |
| CN105111693A (en) * | 2015-08-27 | 2015-12-02 | 江苏易成电力器材有限公司 | Carbon nano composite fiber material and preparation method thereof |
| CN106432691A (en) * | 2016-07-21 | 2017-02-22 | 嘉兴市正大化工有限公司 | Curing agent special for pultrusion, and application thereof |
| CN107686632A (en) * | 2017-09-27 | 2018-02-13 | 卡本复合材料（天津）有限公司 | A kind of epoxy-resin systems of pultrusion carbon fiber sheet |
| CN111534260A (en) * | 2020-04-24 | 2020-08-14 | 北京康美特科技股份有限公司 | Epoxy resin packaging adhesive and preparation method and application thereof |
| CN111534260B (en) * | 2020-04-24 | 2021-12-14 | 北京康美特科技股份有限公司 | Epoxy resin packaging adhesive and preparation method and application thereof |
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Application publication date: 20140326 |