CN108192289A - A kind of high-toughness epoxy resin composite material and its preparation method and application - Google Patents
A kind of high-toughness epoxy resin composite material and its preparation method and application Download PDFInfo
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- CN108192289A CN108192289A CN201711472178.6A CN201711472178A CN108192289A CN 108192289 A CN108192289 A CN 108192289A CN 201711472178 A CN201711472178 A CN 201711472178A CN 108192289 A CN108192289 A CN 108192289A
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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
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention discloses a kind of high-toughness epoxy resin composite materials, include the component of following parts by weight：120 200 parts of epoxy resin, 16 25 parts of di-n-butyl phosphite, 14 18 parts of Ultra Tex 2,10 15 parts of 2 methyl cyclopentyl-dialkyl-tricarbon manganium, 15 parts of pyridoxine, 26 parts of acetylene carbon black, 15 parts of curing agent.The epoxy resin composite material of the present invention has preferable impact strength, and toughness is high；And tensile strength, bending strength are high, flame retardant effect, heat-resisting effect are good；Preparation method is simple, can preferably be used for power domain, and market popularization value is high.
Description
Technical field
The present invention relates to a kind of composite material, specifically a kind of high-toughness epoxy resin composite material and preparation method thereof and
Using.
Background technology
Epoxy resin composite material is with its high specific strength, high ratio modulus, high temperature resistant, numerous excellent properties such as corrosion-resistant and it is wide
It is general to be applied on space flight, automobile, electronics, sports goods and medical instrument.It is well known that one kind is obtained after epoxy resin cure
Three-dimensional is insoluble not to melt reticular structure, and this structure shows as the characteristics of matter is crisp, holds when the micro-crack of load or defect generation
It easily spreads rapidly and makes material failure, so as to influence its use scope.Therefore epoxy resin composite material need to be carried out at toughening
It manages to improve its impact strength.At present, the method for toughening of epoxy resin composite material mainly has rubber toughened, thermoplastic elastomer (TPE)
Toughening, Rigid Particles Toughened.These methods can undoubtedly improve the impact flexibility of composite material to a certain extent.But due to
The compatibility of epoxy resin is not good enough, is usually associated with the reduction of other mechanical properties.Therefore, the present invention provides a kind of high tenacity ring
Epoxy resin composite material and its preparation method and application.
Invention content
The purpose of the present invention is to provide a kind of high-toughness epoxy resin composite material and its preparation method and application, with solution
Certainly the problems mentioned above in the background art.
To achieve the above object, the present invention provides following technical solution：
A kind of high-toughness epoxy resin composite material includes the component of following parts by weight：120-200 parts of epoxy resin,
16-25 parts of di-n-butyl phosphite, 14-18 parts of Ultra Tex 2,2- methyl cyclopentyl-dialkyl-tricarbon manganiums 10-15
Part, 1-5 parts of pyridoxine, 2-6 parts of acetylene carbon black, 1-5 parts of curing agent.
As further embodiment of the present invention：Include the component of following parts by weight：160-180 parts of epoxy resin, phosphorous
Sour di-n-butyl 18-21 parts, 15-17 parts of Ultra Tex 2,11-14 parts of 2- methyl cyclopentyl-dialkyl-tricarbon manganiums, pyrrole
It trembles 2-4 parts plain, 3-5 parts of acetylene carbon black, 2-4 parts of curing agent.
As further embodiment of the present invention：Include the component of following parts by weight：172 parts of epoxy resin, phosphorous acid two
19 parts of N-butyl, 16 parts of Ultra Tex 2,12 parts of 2- methyl cyclopentyl-dialkyl-tricarbon manganiums, 3 parts of pyridoxine, acetylene carbon
Black 4 parts, 3 parts of curing agent.
A kind of preparation method of high-toughness epoxy resin composite material, includes the following steps：(1) by epoxy resin and phosphorous
Sour di-n-butyl, pyridoxine, acetylene carbon black mixing, are passed through protective gas protection, 15-20min are mixed at 75-85 DEG C；(2) to
Ultra Tex 2 and 2- methyl cyclopentyl-dialkyl-tricarbon manganiums are added in upper step gains, is passed through protective gas protection,
10-20min is mixed at 112-125 DEG C；(3) curing agent is added in step gains upwards, is passed through protective gas protection, 140-155
40-55min is mixed at DEG C；(4) by upper step gains by extruder squeeze out to get.
As further embodiment of the present invention：The protective gas uses helium.
A kind of high-toughness epoxy resin composite material is in the application of power domain.
Compared with prior art, the beneficial effects of the invention are as follows：
The epoxy resin composite material of the present invention has preferable impact strength, and toughness is high；And tensile strength, bending strength
Height, flame retardant effect, heat-resisting effect are good；Preparation method is simple, can preferably be used for power domain, and market popularization value is high.
Specific embodiment
The technical solution of this patent is described in more detail With reference to embodiment.
Embodiment 1
A kind of high-toughness epoxy resin composite material includes the component of following parts by weight：120 parts of epoxy resin, phosphorous
Sour 16 parts of di-n-butyl, 14 parts of Ultra Tex 2,10 parts of 2- methyl cyclopentyl-dialkyl-tricarbon manganiums, 1 part of pyridoxine, second
2 parts of alkynes carbon black, 1 part of curing agent.
A kind of preparation method of high-toughness epoxy resin composite material, includes the following steps：(1) by epoxy resin and phosphorous
Sour di-n-butyl, pyridoxine, acetylene carbon black mixing, are passed through helium protection, 15min are mixed at 75 DEG C；(2) gains are walked upwards
Middle addition Ultra Tex 2 and 2- methyl cyclopentyl-dialkyl-tricarbon manganiums are passed through helium protection, are mixed at 112 DEG C
10min；(3) curing agent is added in step gains upwards, is passed through helium protection, 40min is mixed at 140 DEG C；It (4) will be obtained by upper step
Object by extruder squeeze out to get.
Embodiment 2
A kind of high-toughness epoxy resin composite material includes the component of following parts by weight：200 parts of epoxy resin, phosphorous
Sour 25 parts of di-n-butyl, 18 parts of Ultra Tex 2,15 parts of 2- methyl cyclopentyl-dialkyl-tricarbon manganiums, 5 parts of pyridoxine, second
6 parts of alkynes carbon black, 5 parts of curing agent.
A kind of preparation method of high-toughness epoxy resin composite material, includes the following steps：(1) by epoxy resin and phosphorous
Sour di-n-butyl, pyridoxine, acetylene carbon black mixing, are passed through helium protection, 20min are mixed at 85 DEG C；(2) gains are walked upwards
Middle addition Ultra Tex 2 and 2- methyl cyclopentyl-dialkyl-tricarbon manganiums are passed through helium protection, are mixed at 125 DEG C
20min；(3) curing agent is added in step gains upwards, is passed through helium protection, 55min is mixed at 155 DEG C；It (4) will be obtained by upper step
Object by extruder squeeze out to get.
Embodiment 3
A kind of high-toughness epoxy resin composite material includes the component of following parts by weight：172 parts of epoxy resin, phosphorous
Sour 19 parts of di-n-butyl, 16 parts of Ultra Tex 2,12 parts of 2- methyl cyclopentyl-dialkyl-tricarbon manganiums, 3 parts of pyridoxine, second
4 parts of alkynes carbon black, 3 parts of curing agent.
A kind of preparation method of high-toughness epoxy resin composite material, includes the following steps：(1) by epoxy resin and phosphorous
Sour di-n-butyl, pyridoxine, acetylene carbon black mixing, are passed through helium protection, 18min are mixed at 80 DEG C；(2) gains are walked upwards
Middle addition Ultra Tex 2 and 2- methyl cyclopentyl-dialkyl-tricarbon manganiums are passed through helium protection, are mixed at 118 DEG C
15min；(3) curing agent is added in step gains upwards, is passed through helium protection, 48min is mixed at 150 DEG C；It (4) will be obtained by upper step
Object by extruder squeeze out to get.
Embodiment 4
A kind of high-toughness epoxy resin composite material includes the component of following parts by weight：160 parts of epoxy resin, phosphorous
Sour 18 parts of di-n-butyl, 15 parts of Ultra Tex 2,11 parts of 2- methyl cyclopentyl-dialkyl-tricarbon manganiums, 2 parts of pyridoxine, second
3 parts of alkynes carbon black, 2 parts of curing agent.
A kind of preparation method of high-toughness epoxy resin composite material, includes the following steps：(1) by epoxy resin and phosphorous
Sour di-n-butyl, pyridoxine, acetylene carbon black mixing, are passed through helium protection, 18min are mixed at 78 DEG C；(2) gains are walked upwards
Middle addition Ultra Tex 2 and 2- methyl cyclopentyl-dialkyl-tricarbon manganiums are passed through helium protection, are mixed at 115 DEG C
12min；(3) curing agent is added in step gains upwards, is passed through helium protection, 45min is mixed at 145 DEG C；It (4) will be obtained by upper step
Object by extruder squeeze out to get.
Embodiment 5
A kind of high-toughness epoxy resin composite material includes the component of following parts by weight：180 parts of epoxy resin, phosphorous
Sour 21 parts of di-n-butyl, 17 parts of Ultra Tex 2,14 parts of 2- methyl cyclopentyl-dialkyl-tricarbon manganiums, 4 parts of pyridoxine, second
5 parts of alkynes carbon black, 4 parts of curing agent.
A kind of preparation method of high-toughness epoxy resin composite material, includes the following steps：(1) by epoxy resin and phosphorous
Sour di-n-butyl, pyridoxine, acetylene carbon black mixing, are passed through helium protection, 19min are mixed at 82 DEG C；(2) gains are walked upwards
Middle addition Ultra Tex 2 and 2- methyl cyclopentyl-dialkyl-tricarbon manganiums are passed through helium protection, are mixed at 121 DEG C
18min；(3) curing agent is added in step gains upwards, is passed through helium protection, 50min is mixed at 152 DEG C；It (4) will be obtained by upper step
Object by extruder squeeze out to get.
Comparative example 1
A kind of high-toughness epoxy resin composite material includes the component of following parts by weight：180 parts of epoxy resin, acetyl
Change 17 parts of PASELLI EASYGEL, 14 parts of 2- methyl cyclopentyl-dialkyl-tricarbon manganiums, 4 parts of pyridoxine, 5 parts of acetylene carbon black, curing agent 4
Part.
A kind of preparation method of high-toughness epoxy resin composite material, includes the following steps：(1) epoxy resin and pyrrole are trembled
Element, acetylene carbon black mixing, are passed through helium protection, 19min are mixed at 82 DEG C；(2) acetylation two is added in step gains upwards
Starch phosphate and 2- methyl cyclopentyl-dialkyl-tricarbon manganiums are passed through helium protection, 18min are mixed at 121 DEG C；(3) institute is walked upwards
It obtains in object and adds in curing agent, be passed through helium protection, 50min is mixed at 152 DEG C；(4) upper step gains are squeezed out by extruder,
To obtain the final product.
Comparative example 2
A kind of high-toughness epoxy resin composite material includes the component of following parts by weight：180 parts of epoxy resin, phosphorous
Sour 21 parts of di-n-butyl, 17 parts of Ultra Tex 2,4 parts of pyridoxine, 5 parts of acetylene carbon black, 4 parts of curing agent.
A kind of preparation method of high-toughness epoxy resin composite material, includes the following steps：(1) by epoxy resin and phosphorous
Sour di-n-butyl, pyridoxine, acetylene carbon black mixing, are passed through helium protection, 19min are mixed at 82 DEG C；(2) gains are walked upwards
Middle addition Ultra Tex 2 is passed through helium protection, 18min is mixed at 121 DEG C；(3) it is added in step gains upwards
Curing agent is passed through helium protection, 50min is mixed at 152 DEG C；(4) by upper step gains by extruder squeeze out to get.
Comparative example 3
A kind of high-toughness epoxy resin composite material includes the component of following parts by weight：180 parts of epoxy resin, acetyl
Change 17 parts of PASELLI EASYGEL, 4 parts of pyridoxine, 5 parts of acetylene carbon black, 4 parts of curing agent.
A kind of preparation method of high-toughness epoxy resin composite material, includes the following steps：(1) epoxy resin and pyrrole are trembled
Element, acetylene carbon black mixing, are passed through helium protection, 19min are mixed at 82 DEG C；(2) acetylation two is added in step gains upwards
Starch phosphate is passed through helium protection, 18min is mixed at 121 DEG C；(3) curing agent is added in step gains upwards, is passed through helium
It protects, 50min is mixed at 152 DEG C；(4) by upper step gains by extruder squeeze out to get.
Experimental example
Above-described embodiment 5 and comparative example the 1-3 epoxy resin composite material prepared are subjected to following test：1. by ASTM
D2863-97 standards carry out limit oxygen index test.2. being heated 10 hours at 230 DEG C, its physical property is tested.3. according to
" GBT1451-2005 fibre reinforced plastics freely-supported beam type impact ductility tests method " measures its impact strength.4. it is strong to measure impact
Degree, disruptive field intensity, volume resistivity and dielectric constant.
As a result it is as shown in table 1 below.
Table 1
| Project | Embodiment 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Tensile strength (MPa) | 69 | 28 | 24 | 20 |
| 10 hours post-tensioning intensity (MPa) is heated at 230 DEG C | 64 | 24 | 18 | 15 |
| Bending strength (MPa) | 112 | 60 | 58 | 52 |
| Bending strength (MPa) after being heated 10 hours at 230 DEG C | 98 | 53 | 50 | 46 |
| Limit oxygen index (%) | 31 | 24 | 25 | 18 |
| Impact strength kJ/m2 | 30 | 21 | 16 | 14 |
| Disruptive field intensity kV/mm | 61 | 55 | 52 | 49 |
| Volume resistivity Ω cm | 7.5E16 | 6.6E16 | 6.8E16 | 6.1E16 |
| Dielectric constant | 4.13 | 4.14 | 4.17 | 4.18 |
The better embodiment of this patent is explained in detail above, but this patent is not limited to above-mentioned embodiment party
Formula, can also be under the premise of this patent objective not be departed from the knowledge that one skilled in the relevant art has
It makes a variety of changes.
Claims (6)
1. a kind of high-toughness epoxy resin composite material, which is characterized in that include the component of following parts by weight：Epoxy resin
120-200 parts, 16-25 parts of di-n-butyl phosphite, 14-18 parts of Ultra Tex 2, three carbonyl of 2- methyl cyclopentadienes
10-15 parts of base manganese, 1-5 parts of pyridoxine, 2-6 parts of acetylene carbon black, 1-5 parts of curing agent.
2. high-toughness epoxy resin composite material according to claim 1, which is characterized in that including following parts by weight
Component：160-180 parts of epoxy resin, 18-21 parts of di-n-butyl phosphite, 15-17 parts of Ultra Tex 2,2- methyl
11-14 parts of cyclopentadiene tricarbonyl manganese, 2-4 parts of pyridoxine, 3-5 parts of acetylene carbon black, 2-4 parts of curing agent.
3. high-toughness epoxy resin composite material according to claim 1, which is characterized in that including following parts by weight
Component：172 parts of epoxy resin, 19 parts of di-n-butyl phosphite, 16 parts of Ultra Tex 2,2- methyl cyclopentadienes three
12 parts of manganese carbonyl, 3 parts of pyridoxine, 4 parts of acetylene carbon black, 3 parts of curing agent.
4. a kind of preparation method of high-toughness epoxy resin composite material as described in any one of claims 1-3, which is characterized in that
Include the following steps：（1）Epoxy resin with di-n-butyl phosphite, pyridoxine, acetylene carbon black is mixed, is passed through protective gas guarantor
Shield, 15-20min is mixed at 75-85 DEG C；（2）Upwards Ultra Tex 2 and 2- methyl rings are added in step gains
Pentadiene manganese tricarbonyl is passed through protective gas protection, 10-20min is mixed at 112-125 DEG C；（3）It is added in step gains upwards
Curing agent is passed through protective gas protection, 40-55min is mixed at 140-155 DEG C；（4）Upper step gains are squeezed by extruder
Go out to get.
5. the preparation method of high-toughness epoxy resin composite material according to claim 4, which is characterized in that the protection
Gas uses helium.
6. a kind of high-toughness epoxy resin composite material as described in any one of claims 1-3 is in the application of power domain.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694637A (en) * | 2013-12-17 | 2014-04-02 | 新誉集团有限公司 | High-tenacity vacuum slow epoxy resin for wind power blade and preparation method thereof |
| CN104559063A (en) * | 2015-01-19 | 2015-04-29 | 深圳市沃尔核材股份有限公司 | High-toughness low-shrinkage epoxy resin composition, insulating part and preparation method |
| CN104559064A (en) * | 2015-01-28 | 2015-04-29 | 江苏恒神纤维材料有限公司 | High-toughness high-Tg-value epoxy resin and preparation method |
| CN106188512A (en) * | 2016-07-22 | 2016-12-07 | 哈尔滨理工大学 | A kind of low dielectric, the preparation method of high-toughness epoxy resin solidfied material |
-
2017
- 2017-12-29 CN CN201711472178.6A patent/CN108192289A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694637A (en) * | 2013-12-17 | 2014-04-02 | 新誉集团有限公司 | High-tenacity vacuum slow epoxy resin for wind power blade and preparation method thereof |
| CN104559063A (en) * | 2015-01-19 | 2015-04-29 | 深圳市沃尔核材股份有限公司 | High-toughness low-shrinkage epoxy resin composition, insulating part and preparation method |
| CN104559064A (en) * | 2015-01-28 | 2015-04-29 | 江苏恒神纤维材料有限公司 | High-toughness high-Tg-value epoxy resin and preparation method |
| CN106188512A (en) * | 2016-07-22 | 2016-12-07 | 哈尔滨理工大学 | A kind of low dielectric, the preparation method of high-toughness epoxy resin solidfied material |
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Application publication date: 20180622 |