CN106867202A - A kind of composition epoxy resin - Google Patents
A kind of composition epoxy resin Download PDFInfo
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- CN106867202A CN106867202A CN201710195322.XA CN201710195322A CN106867202A CN 106867202 A CN106867202 A CN 106867202A CN 201710195322 A CN201710195322 A CN 201710195322A CN 106867202 A CN106867202 A CN 106867202A
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- epoxy resin
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- tio
- composition epoxy
- toughener
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/22—Di-epoxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/05—Polymer mixtures characterised by other features containing polymer components which can react with one another
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a kind of composition epoxy resin, the composition epoxy resin in parts by weight, including following component：100 parts of epoxy resin, 10 ~ 80 parts of curing agent, 2 ~ 40 parts of toughener, 0 ~ 20 part of accelerator, 0 ~ 25 part of diluent, 1 ~ 15 part of coupling agent, nano-TiO21 ~ 3 part.Reactive diluent that the present invention is used is so that composition epoxy resin just has a certain fluidity at normal temperatures, and there is diluent epoxy construction can participate in reaction, and compared to addition non-activated thinner, the performance of resin cured matter is more preferably；The toughener and epoxy resin that the present invention is used have reactivity, solidfied material is had more excellent mechanical performance；The coupling agent that the present invention is used has epoxide group, can increase the adhesive property of epoxy resin and pbo fiber, and the crosslink density of solidfied material can be increased again.Composition epoxy resin of the invention has preferable wellability to pbo fiber, good with pbo fiber associativity.
Description
Technical field
The invention belongs to technical field of polymer materials, it is related to a kind of composition epoxy resin.
Background technology
Composite prepared by high-modulus pbo fiber and epoxy resin has been used as structural material, be applied to spacecraft and
In space probe.Pbo fiber there is also the shortcoming of itself while a series of excellent properties are possessed.The surface of pbo fiber
Unusual light, in chemical inertness, is difficult to be infiltrated with resin matrix, causes the interface bond strength of composite relatively low, it is impossible to fill
The effect of the existing reinforcement of split.Therefore the wellability and interfacial bonding property for improving epoxy resin with pbo fiber are necessary.
In order to change wellability of the epoxy resin to pbo fiber, two aspects are generally divided into：One is that pbo fiber is carried out
Surface is modified, and two is that epoxy resin-base is modified, wherein：Directly carrying out that surface is modified to pbo fiber unavoidably can be to fibre
The performance of dimension itself causes destruction in varying degrees, the performance of material is influenceed, so carrying out thing by epoxy resin-base
Reason and chemical modification just seem particularly critical.
The content of the invention
It is an object of the invention to provide a kind of composition epoxy resin, it with pbo fiber when for preparing composite
With good wellability and interfacial combined function.
The purpose of the present invention is achieved through the following technical solutions：
A kind of composition epoxy resin, in parts by weight, including following component：100 parts of epoxy resin, 10 ~ 80 parts of curing agent, increasing
Tough dose 2 ~ 40 parts, 0 ~ 20 part of accelerator, 0 ~ 25 part of diluent, 1 ~ 15 part of coupling agent, nano-TiO21 ~ 3 part.
In the present invention, the epoxy resin is bisphenol A epoxide resin, and epoxide number is 0.48 ~ 0.54；Viscosity is at 25 DEG C
11000~14000mPa.s；Curing agent is 3,3 '-diethyl -4,4 '-MDA（H-256）Or low-molecular-weight polyamides
Amine；Accelerator is 2,4,6- tri-（Dimethylamino methyl）Phenol（DMP-30）；Toughener is polyamide or end carboxyl nitrile (HTBN)
Rubber；Diluent is 1,4- butanediol diglycidyl ethers；Coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane
（KH-560）Or gamma-aminopropyl-triethoxy-silane（KH-550）；Nano-TiO2It is the modified nano-TiO in surface2, modifying agent
It is KH-560, specific method of modifying is as follows：Nano-TiO is added in ethanol2And the consumption of KH-560, KH-560 is TiO2Quality
2 ~ 6%, using ultrasonic disintegrator ultrasound 2 hours, ultrasonic power be 500 ~ 1000W.
One kind prepares epoxy-resin systems/pbo fiber composite using above-mentioned composition epoxy resin and pbo fiber
Method, comprises the following steps：
First, epoxy resin modification：
When toughener is carboxyl end of the liquid acrylonitrile-butadiene rubber, toughener, coupling agent are charged first in epoxy resin first, heated
And mechanical agitation, reacted 3 ~ 4 hours at a temperature of 90 ~ 120 DEG C, obtain modified epoxy prepolymer；Then changing
Property after epoxy prepolymer in add curing agent, accelerator, diluent and nano-TiO2, obtain it is chemical with it is filler modified after
Epoxy resin.
When toughener is polyamide, coupling agent is charged first in epoxy resin first, heated and mechanical agitation, 90
Reacted 3 ~ 4 hours at a temperature of ~ 120 DEG C, obtain modified epoxy prepolymer；Then epoxy resin prepolymer after modification
Toughener, curing agent, accelerator, diluent and nano-TiO are added in polymers2, obtain it is chemical with it is filler modified after asphalt mixtures modified by epoxy resin
Fat.
2nd, epoxy-resin systems/pbo fiber composite is prepared：
By chemistry with it is filler modified after epoxy resin stir after vacuum defoamation, then will wind pbo fiber infiltration
To wherein, immersion is transferred in the metal die having been warmed up after 10 ~ 20 minutes, is solidified according to corresponding curing cycle,
Obtain composite.
The invention has the advantages that：
1st, the reactive diluent that the present invention is used is so that composition epoxy resin is with regard to having certain fluidity and dilute at normal temperatures
Release agent have epoxy construction can participate in reaction, compared to addition non-activated thinner, the performance of resin cured matter is more preferably；
2nd, the toughener and epoxy resin that the present invention is used have reactivity, solidfied material is had more excellent mechanical performance；
3rd, the coupling agent that the present invention is used has epoxide group, can increase the adhesive property of epoxy resin and pbo fiber, and energy
Increase the crosslink density of solidfied material；
4th, composition epoxy resin of the invention has preferable wellability to pbo fiber, good with pbo fiber associativity.
Specific embodiment
Technical scheme is further described with reference to embodiment, but is not limited thereto, it is every right
Technical solution of the present invention is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should be contained
Cover in protection scope of the present invention.
Embodiment 1：
In parts by weight, the composition epoxy resin in the present embodiment is made up of following component：100 parts of epoxy resin, curing agent
32 parts, 20 parts of toughener, 1 part of accelerator, 25 parts of diluent, 3 parts of coupling agent, nano-TiO21 part.
In the present embodiment, the epoxy resin is liquid bisphenol A epoxy resin, epoxide number 0.48 ~ 0.54, model E-51.
In the present embodiment, the curing agent is H-256, Jiangsu Hui Feng.
In the present embodiment, the toughener is polyamide, model 651.
In the present embodiment, the diluent is BDDE, Aladdin product；
In the present embodiment, the coupling agent is KH-550.
In the present embodiment, the nano-TiO2：60 ~ 100nm, Aladdin product；
In the present embodiment, the accelerator is DMP-30.
In the present embodiment, above-mentioned composition epoxy resin can be used to prepare E-51+H-256 epoxy-resin systems/pbo fiber
Composite, specific preparation process is as follows：
100 parts of E-51 epoxy resin and 3 parts of KH-550 are mixed, 90 DEG C is heated under mechanical stirring and is reacted 4 hours；Then plus
Enter 25 parts of 1,4- butanediol diglycidyl ethers, 1 part of modified nano-TiO2, ultrasonic disperse 1 hour is eventually adding 32 parts of H-
256th, 1 part of DMP-30 and 20 part of polyamide 6 51, vacuum defoamation after being well mixed；Then prepared using mould with pbo fiber compound
Material, curing cycle is 90 DEG C and is incubated 2 hours, and 120 DEG C are incubated 2 hours, and 150 DEG C are incubated 2 hours.
After being modified to epoxy resin according to the method described above, the interlaminar shear strength ILSS of composite is from unmodified
31.2Mpa increases to modified 41.1MPa, and single fiber pull-out test intensity I FSS increases 27.9MPa from unmodified 20.4MPa.
Embodiment 2：
As different from Example 1, the coupling agent is KH-560 to the present embodiment.
Embodiment 3：
From unlike embodiment 1 or 2, the composition epoxy resin is made up of the present embodiment following component：Epoxy resin 100
Part, 32 parts of curing agent, 20 parts of toughener, 25 parts of diluent, 3 parts of coupling agent, nano-TiO21 part.
Embodiment 4：
From unlike embodiment 1 or 2, the composition epoxy resin is made up of the present embodiment following component：Epoxy resin 100
Part, 32 parts of curing agent, 20 parts of toughener, 3 parts of coupling agent, nano-TiO21 part.
Embodiment 5：
In parts by weight, the composition epoxy resin in the present embodiment is made up of following component：100 parts of epoxy resin, curing agent
30 parts, 30 parts of toughener, 1 part of accelerator, 25 parts of diluent, 3 parts of coupling agent, nano-TiO21 part.
In the present embodiment, the epoxy resin is liquid bisphenol A epoxy resin, epoxide number 0.48 ~ 0.54, model E-51.
In the present embodiment, the curing agent is polyamide, model 651.
In the present embodiment, the toughener is poly- carboxyl end of the liquid acrylonitrile-butadiene rubber, model TL910.
In the present embodiment, the diluent is BDDE, Aladdin product；
In the present embodiment, the coupling agent is KH-550.
In the present embodiment, the nano-TiO2：60 ~ 100nm, Aladdin product；
In the present embodiment, the accelerator is DMP-30.
In the present embodiment, above-mentioned composition epoxy resin can be used to prepare 51 epoxy-resin systems of E-51+ polyamide 6s/PBO
Fibrous composite, specific preparation process is as follows：
100 parts of E-51 epoxy resin, 30 parts of TL910,3 parts of KH-550 are mixed, 120 DEG C of reactions 3 are heated under mechanical stirring
Hour；It is subsequently adding 25 parts of 1,4- butanediol diglycidyl ethers, 1 part of modified nano-TiO2, ultrasonic disperse 1 hour；Again plus
Enter 30 parts of polyamide 6s, 51,1 part of DMP-30, vacuum defoamation after being well mixed；Then composite wood is prepared using mould with pbo fiber
Material, curing cycle is 40 DEG C and is incubated 2 hours, and 80 DEG C are incubated 2 hours.
Embodiment 6：
As different from Example 5, the coupling agent is KH-560 to the present embodiment.
Embodiment 7：
As different from Example 6, the composition epoxy resin is made up of the present embodiment following component：100 parts of epoxy resin,
30 parts of curing agent, 30 parts of toughener, 1 part of accelerator, 3 parts of coupling agent, nano-TiO21 part.
Claims (10)
1. a kind of composition epoxy resin, it is characterised in that the composition epoxy resin in parts by weight, by following component group
Into：100 parts of epoxy resin, 10 ~ 80 parts of curing agent, 2 ~ 40 parts of toughener, 0 ~ 20 part of accelerator, 0 ~ 25 part of diluent, coupling agent 1
~ 15 parts, nano-TiO21 ~ 3 part.
2. composition epoxy resin according to claim 1, it is characterised in that the epoxy resin is bisphenol-A epoxy tree
Fat, epoxide number is 0.48 ~ 0.54；Viscosity is 11000 ~ 14000mPa.s at 25 DEG C.
3. composition epoxy resin according to claim 1, it is characterised in that the curing agent is 3,3 '-diethyl -4,
4 '-MDA or low molecular polyamides.
4. composition epoxy resin according to claim 1, it is characterised in that the accelerator is 2,4,6- tri-（Dimethylamine
Ylmethyl）Phenol.
5. composition epoxy resin according to claim 1, it is characterised in that the toughener is polyamide or end carboxyl
LNBR.
6. composition epoxy resin according to claim 1, it is characterised in that the diluent contracts for BDO two
Water glycerin ether.
7. composition epoxy resin according to claim 1, it is characterised in that the coupling agent is γ-glycidyl ether oxygen
Propyl trimethoxy silicane or gamma-aminopropyl-triethoxy-silane.
8. composition epoxy resin according to claim 1, it is characterised in that the nano-TiO2Received for surface is modified
Rice TiO2。
9. composition epoxy resin according to claim 8, it is characterised in that the nano-TiO2Method of modifying it is as follows：
Nano-TiO is added in ethanol2And KH-560, KH-560 consumption are TiO2The 2 ~ 6% of quality, it is small using ultrasonic disintegrator ultrasound 2
When, ultrasonic power is 500 ~ 1000W.
10. it is a kind of to prepare epoxy resin using composition epoxy resin described in claim 1-9 any claims and pbo fiber
The method of system/pbo fiber composite, it is characterised in that methods described step is as follows：
First, epoxy resin modification：
When toughener is carboxyl end of the liquid acrylonitrile-butadiene rubber, toughener, coupling agent are charged first in epoxy resin first, heated
And mechanical agitation, reacted 3 ~ 4 hours at a temperature of 90 ~ 120 DEG C, obtain modified epoxy prepolymer；Then changing
Property after epoxy prepolymer in add curing agent, accelerator, diluent and nano-TiO2, obtain it is chemical with it is filler modified after
Epoxy resin；
When toughener is polyamide, coupling agent is charged first in epoxy resin first, heated and mechanical agitation, 90 ~ 120
Reacted 3 ~ 4 hours at a temperature of DEG C, obtain modified epoxy prepolymer；Then epoxy prepolymer after modification
Middle addition toughener, curing agent, accelerator, diluent and nano-TiO2, obtain it is chemical with it is filler modified after epoxy resin；
2nd, epoxy-resin systems/pbo fiber composite is prepared：
By chemistry with it is filler modified after epoxy resin stir after vacuum defoamation, then will wind pbo fiber infiltration
To wherein, immersion is transferred in the metal die having been warmed up after 10 ~ 20 minutes, is solidified according to corresponding curing cycle,
Obtain composite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710195322.XA CN106867202A (en) | 2017-03-29 | 2017-03-29 | A kind of composition epoxy resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710195322.XA CN106867202A (en) | 2017-03-29 | 2017-03-29 | A kind of composition epoxy resin |
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| CN106867202A true CN106867202A (en) | 2017-06-20 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107385919A (en) * | 2017-07-06 | 2017-11-24 | 国网湖南省电力公司带电作业中心 | The coating material being modified for pbo fiber surface；Surface is modified pbo fiber, preparation and its application |
| CN107501866A (en) * | 2017-09-07 | 2017-12-22 | 苏州浩焱精密模具有限公司 | A kind of metal-resin composite die material and preparation method thereof |
| CN110484222A (en) * | 2019-07-31 | 2019-11-22 | 中国石油集团工程技术研究院有限公司 | A kind of epoxy resin-matrix cementing fluid and preparation method thereof |
| WO2023206651A1 (en) * | 2022-04-25 | 2023-11-02 | 叶金蕊 | Ultrahigh-voltage-resistant insulating resin suitable for vacuum resin absorbable molding, and preparation method therefor |
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| CN101575419A (en) * | 2008-05-09 | 2009-11-11 | 中国石油天然气股份有限公司 | Method for preparing repair prepreg for pipelines with defects |
| CN102212330A (en) * | 2010-04-07 | 2011-10-12 | 深圳市诚德来实业有限公司 | Epoxy resin adhesive for hollow fiber membrane end sealing as well as preparation and application methods thereof |
| CN105348729A (en) * | 2015-10-30 | 2016-02-24 | 陕西科技大学 | Preparation method of organic fiber reinforced carbon cloth/resin composite material |
-
2017
- 2017-03-29 CN CN201710195322.XA patent/CN106867202A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575419A (en) * | 2008-05-09 | 2009-11-11 | 中国石油天然气股份有限公司 | Method for preparing repair prepreg for pipelines with defects |
| CN102212330A (en) * | 2010-04-07 | 2011-10-12 | 深圳市诚德来实业有限公司 | Epoxy resin adhesive for hollow fiber membrane end sealing as well as preparation and application methods thereof |
| CN105348729A (en) * | 2015-10-30 | 2016-02-24 | 陕西科技大学 | Preparation method of organic fiber reinforced carbon cloth/resin composite material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107385919A (en) * | 2017-07-06 | 2017-11-24 | 国网湖南省电力公司带电作业中心 | The coating material being modified for pbo fiber surface；Surface is modified pbo fiber, preparation and its application |
| CN107501866A (en) * | 2017-09-07 | 2017-12-22 | 苏州浩焱精密模具有限公司 | A kind of metal-resin composite die material and preparation method thereof |
| CN110484222A (en) * | 2019-07-31 | 2019-11-22 | 中国石油集团工程技术研究院有限公司 | A kind of epoxy resin-matrix cementing fluid and preparation method thereof |
| WO2023206651A1 (en) * | 2022-04-25 | 2023-11-02 | 叶金蕊 | Ultrahigh-voltage-resistant insulating resin suitable for vacuum resin absorbable molding, and preparation method therefor |
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