CN103408902B - A kind of preparation method of composition epoxy resin and utilize it to prepare the method for M race carbon fiber/matrix resin matrix material - Google Patents
A kind of preparation method of composition epoxy resin and utilize it to prepare the method for M race carbon fiber/matrix resin matrix material Download PDFInfo
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Abstract
A kind of preparation method of composition epoxy resin and utilize it to prepare the method for M race carbon fiber/matrix resin matrix material.It relates to the preparation method of a kind of composition epoxy resin preparation method and a kind of M race carbon fiber/matrix resin matrix material.The present invention in order to the epoxy resin that solves prior art and prepare for preparing M race carbon fiber/matrix resin matrix material time Presence of an interface intensity low problem, and a kind of preparation method of composition epoxy resin is provided and utilizes it to prepare the method for M race carbon fiber/matrix resin matrix material.The present invention is by adding polyacrylic acid in the epoxy and urethane obtains composition epoxy resin.Mix with substrate resin solution after making Epoxy resin composition solution, by infiltrating carbon fiber, drying, mold pressing, solidification, obtained M race carbon fiber/matrix resin matrix material.The present invention is for the preparation of the M race carbon fiber/matrix resin matrix material of high interfacial strength.
Description
Technical field
The present invention relates to the preparation method of a kind of composition epoxy resin preparation method and a kind of M race carbon fiber/matrix resin matrix material.
Background technology
The raising of interfacial shear strength, relies on fiber surface performance to a great extent.Fiber surface-processing method has a lot, and wherein coating is the most simple and practical, and this kind of surface treatment agent is mainly organo-silicon coupling agent, titanic acid ester, complex compound etc., is coated in fiber surface under certain condition, for improving the interface shear strength of matrix material.But after using these treatment agents, some the fiber interface intensity for high-modulus improves little, does not even have effect.Although common epoxy resin has good bonding strength to metallic substance, but bonding non-metallic material intensity is low, particularly to fiber, the problem that when therefore the epoxy resin prepared of prior art is for preparing M race carbon fiber/matrix resin matrix material, Presence of an interface intensity is low and utilize present stage M race carbon fiber/matrix resin interfacial shear strength of preparing of technology low.
Summary of the invention
Object of the present invention will solve epoxy resin prepared by existing preparation method for the preparation of the problem of the M race carbon fiber/matrix resin matrix material of high interfacial strength and cannot utilize the present stage problem that M race carbon fiber/matrix resin interfacial shear strength is low prepared of technology, and provides a kind of preparation method of composition epoxy resin and utilize it to prepare the method for the M race carbon fiber/matrix resin matrix material of high interfacial strength.
A preparation method for composition epoxy resin, specifically carries out according to following steps:
Step one: weigh: the catalyzer taking the epoxy resin of 70 ~ 100 parts, the polyacrylic acid of 1 ~ 10 part, the urethane of 1 ~ 10 part and 0.01 ~ 0.1 part by weight;
Step 2: the epoxy resin of 70 ~ 100 parts that step one are taken is heated to 140 DEG C ~ 160 DEG C, then the polyacrylic acid of 1 ~ 10 part that step one takes and the urethane of 1 ~ 10 part is added, add the catalyzer of 0.01 ~ 0.1 part that step one takes again, be react 1.2h ~ 1.8h under the condition of 140 ~ 160 DEG C in temperature, obtain composition epoxy resin.
Utilize above-mentioned composition epoxy resin to prepare a method for M race carbon fiber/matrix resin matrix material, specifically carry out according to following steps:
Step one: add thinner I when composition epoxy resin being cooled to 40 DEG C ~ 60 DEG C, make Epoxy resin composition solution, the massfraction of solution in ethylene resin combination is 40 ~ 60%.
Step 2: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 40 ~ 60%;
Step 3: by substrate resin solution and Epoxy resin composition solution according to parts by weight proportioning substrate resin solution: Epoxy resin composition solution 100:(5 ~ 25), and mix at ambient temperature, until mix, obtain mixed resin solution;
Step 4: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 40 ~ 60 circles on fixed leg, be carry out drying under the condition of 65 DEG C ~ 75 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 0..8h ~ 1.2h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 5: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material;
Matrix resin described in step 2 is 4211 matrix resins, and the M race carbon fiber described in step 4 is M55J carbon fiber, and carbon fiber K number is 3K ~ 80K.
Advantage of the present invention:
The invention provides a kind of preparation method of composition epoxy resin, the composition epoxy resin that the method is prepared can prepare the M race carbon fiber/matrix resin matrix material of high interfacial strength, simultaneously by the advantage having boundary strength high of M race carbon fiber/matrix resin matrix material prepared by the epoxy resin that utilizes method of the present invention to prepare.When above-mentioned composition epoxy resin add-on is 5 parts, (be 100 part calculating by matrix resin weight fraction proportioning) is compared the M race carbon fiber/matrix resin composite material interface shearing resistance adding merely epoxy resin and prepare and is improved 10.1%, compares the M race carbon fiber/matrix resin composite material interface shearing resistance not adding epoxy resin or composition epoxy resin and improves 3.1%.Add-on is that the M race carbon fiber/matrix resin composite material interface shearing resistance of 5 ~ 25 parts reaches 43.3MPa ~ 47.6MPa.
Embodiment
Embodiment one: in present embodiment, a kind of preparation method of composition epoxy resin carries out according to following steps:
Step one: weigh: the catalyzer taking the epoxy resin of 70 ~ 100 parts, the polyacrylic acid of 1 ~ 10 part, the urethane of 1 ~ 10 part and 0.01 ~ 0.1 part by weight;
Step 2: the epoxy resin of 70 ~ 100 parts that step one are taken is heated to 140 DEG C ~ 160 DEG C, then the polyacrylic acid of 1 ~ 10 part that step one takes and the urethane of 1 ~ 10 part is added, add the catalyzer of 0.01 ~ 0.1 part that step one takes again, be react 1.2h ~ 1.8h under the condition of 140 ~ 160 DEG C in temperature, obtain composition epoxy resin.
Embodiment two: the difference of present embodiment and embodiment one is: weigh in step one epoxy resin be 90 parts, polyacrylic ester is 5 parts, urethane 5 parts, and catalyzer is 0.05 part, and other are identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment one or two is: the catalyzer described in step one is benzyldimethylamine, and other are identical with embodiment one or two.
Embodiment four: in present embodiment, a kind of method utilizing composition epoxy resin that described in embodiment one prepared by method to prepare a kind of M race carbon fiber/matrix resin matrix material is carried out according to following steps:
Step one: add thinner I when composition epoxy resin being cooled to 40 DEG C ~ 60 DEG C, make Epoxy resin composition solution, the massfraction of solution in ethylene resin combination is 40 ~ 60%.
Step 2: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 40 ~ 60%;
Step 3: by substrate resin solution and Epoxy resin composition solution according to parts by weight proportioning substrate resin solution solute: Epoxy resin composition solution solute 100:(5 ~ 25), and mix at ambient temperature, until mix, obtain mixed resin solution;
Step 4: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 40 ~ 60 circles on fixed leg, be carry out drying under the condition of 65 DEG C ~ 75 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 0..8h ~ 1.2h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 5: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material;
Matrix resin described in step 2 is 4211 matrix resins, and the M race carbon fiber described in step 4 is M55J carbon fiber, and carbon fiber K number is 3K ~ 80K.
Embodiment five: the difference of present embodiment and embodiment four is: the Thinner Ⅰ described in step 2 is acetone, and other are identical with embodiment four.
Embodiment six: the difference of present embodiment and embodiment four is: the thinner II described in step 2 is acetone, and other are identical with embodiment four or five.
Embodiment seven: the difference of present embodiment and embodiment four to six is: the solidification described in step 5 is carried out according to following curing cycle: keep 60min under temperature is 90 DEG C of conditions, then under temperature is 130 DEG C of conditions, 60min is kept, finally under temperature is 180 DEG C of conditions, keep 4h, other are identical with embodiment four to six.
By following verification experimental verification effect of the present invention:
Test one:
Step one: weigh: the catalyzer taking the epoxy resin of 90 parts, the polyacrylic acid of 5 parts, the urethane of 5 parts and 0.05 part by weight;
Step 2: the epoxy resin of 90 parts that step one are taken is heated to 150 DEG C, then the polyacrylic acid of 5 parts that step one takes and the urethane of 5 parts is added, add the catalyzer of 0.05 part that step one takes again, be react 1.5h under the condition of 150 DEG C in temperature, obtain composition epoxy resin.
Test two:
Step one: take 90 parts of epoxy resin when being heated to 50 DEG C, add Thinner Ⅰ, make epoxy resin solution;
Step 2: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 50%;
Step 3: substrate resin solution and epoxy resin solution are added 5 parts of epoxy resin solutions according to the every 100 parts of substrate resin solutions of parts by weight proportioning, and mixes at ambient temperature, until mix, obtain mixed resin solution;
Step 4: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 50 circles on fixed leg, be carry out drying under the condition of 70 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 1h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 5: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material;
Matrix resin described in step 2 is 4211 matrix resins, and the M race carbon fiber described in step 4 is M55J carbon fiber.
Test three:
Step one: add thinner I when composition epoxy resin being cooled to 50 DEG C, make Epoxy resin composition solution, the massfraction of solution in ethylene resin combination is 50%.
Step 2: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 50%;
Step 3: substrate resin solution and Epoxy resin composition solution are added 5 parts of Epoxy resin composition solution according to the every 100 parts of substrate resin solutions of parts by weight proportioning, and mixes at ambient temperature, until mix, obtain mixed resin solution;
Step 4: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 50 circles on fixed leg, be carry out drying under the condition of 70 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 1h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 5: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material;
Matrix resin described in step 2 is 4211 matrix resins, and the M race carbon fiber described in step 4 is M55J carbon fiber.
Test four:
Step one: add thinner I when composition epoxy resin being cooled to 50 DEG C, make Epoxy resin composition solution, the massfraction of solution in ethylene resin combination is 50%.
Step 2: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 50%;
Step 3: substrate resin solution and Epoxy resin composition solution are added 10 parts of Epoxy resin composition solution according to the every 100 parts of substrate resin solutions of parts by weight proportioning, and mixes at ambient temperature, until mix, obtain mixed resin solution;
Step 4: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 50 circles on fixed leg, be carry out drying under the condition of 70 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 1h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 5: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material;
Matrix resin described in step 2 is 4211 matrix resins, and the M race carbon fiber described in step 4 is M55J carbon fiber.
Test five:
Step one: add thinner I when composition epoxy resin being cooled to 50 DEG C, make Epoxy resin composition solution, the massfraction of solution in ethylene resin combination is 50%.
Step 2: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 50%;
Step 3: substrate resin solution and Epoxy resin composition solution are added 15 parts of Epoxy resin composition solution according to the every 100 parts of substrate resin solutions of parts by weight proportioning, and mixes at ambient temperature, until mix, obtain mixed resin solution;
Step 4: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 50 circles on fixed leg, be carry out drying under the condition of 70 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 1h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 5: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material;
Matrix resin described in step 2 is 4211 matrix resins, and the M race carbon fiber described in step 4 is M55J carbon fiber.
Test six:
Step one: add thinner I when composition epoxy resin being cooled to 50 DEG C, make Epoxy resin composition solution, the massfraction of solution in ethylene resin combination is 50%.
Step 2: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 50%;
Step 3: substrate resin solution and Epoxy resin composition solution are added 20 parts of Epoxy resin composition solution according to the every 100 parts of substrate resin solutions of parts by weight proportioning, and mixes at ambient temperature, until mix, obtain mixed resin solution;
Step 4: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 50 circles on fixed leg, be carry out drying under the condition of 70 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 1h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 5: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material;
Matrix resin described in step 2 is 4211 matrix resins, and the M race carbon fiber described in step 4 is M55J carbon fiber.
Test seven:
Step one: add thinner I when composition epoxy resin being cooled to 50 DEG C, make Epoxy resin composition solution, the massfraction of solution in ethylene resin combination is 50%.
Step 2: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 50%;
Step 3: substrate resin solution and Epoxy resin composition solution are added 25 parts of Epoxy resin composition solution according to the every 100 parts of substrate resin solutions of parts by weight proportioning, and mixes at ambient temperature, until mix, obtain mixed resin solution;
Step 4: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 50 circles on fixed leg, be carry out drying under the condition of 70 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 1h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 5: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material;
Matrix resin described in step 2 is 4211 matrix resins, and the M race carbon fiber described in step 4 is M55J carbon fiber.
Test eight:
Step one: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 50%;
Step 2: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 50 circles on fixed leg, be carry out drying under the condition of 70 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 1h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 3: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material.
Test nine:
M race carbon fiber/matrix resin matrix material test two to test eight obtained is cut into specification and is: long 30mm ± 1mm, wide 6.0mm, thick 2.5mm ± 0.1mm sample, across according to than being greater than 5:1.Three-point bending pressure head radius is 2mm, and loading velocity is that 2mm is minimum, and interlaminar shear strength is tested by GB GB3357-82.
Testing method is three-point bending, and the calculation formula of test data adopts
In formula, τ---interlaminar shear strength, units MPa;
F---pressure head ultimate load, unit N;
B---sample thickness, unit mm;
H---sample thickness, unit mm.
Then, the Mechanical Data of test is converted into interlaminar shear strength.
Table 1 composition epoxy resin or epoxy resin add-on will be obtained on the impact of M race carbon fiber/matrix resin matrix material interlayer shearing resistance after interpretation.
Table 1
As seen from the above table, when composition epoxy resin add-on is 5 parts, (be 100 part calculating by matrix resin weight fraction proportioning) is compared the M race carbon fiber/matrix resin composite material interface shearing resistance adding merely epoxy resin and prepare and is improved 10.1%, compares the M race carbon fiber/matrix resin composite material interface shearing resistance not adding epoxy resin or composition epoxy resin and improves 3.1%.Add-on is that the M race carbon fiber/matrix resin composite material interface shearing resistance of 5 ~ 25 parts reaches 43.3MPa ~ 47.6MPa.
Claims (4)
1. utilize composition epoxy resin to prepare a method for M race carbon fiber/matrix resin matrix material, it is characterized in that a kind of method utilizing composition epoxy resin to prepare M race carbon fiber/matrix resin matrix material is carried out according to following steps:
Step one: add thinner I when composition epoxy resin being cooled to 40 DEG C ~ 60 DEG C, make Epoxy resin composition solution, the massfraction of solution in ethylene resin combination is 40 ~ 60%;
Step 2: matrix resin is dissolved in thinner II and makes substrate resin solution, in solution, the massfraction of matrix resin is 40 ~ 60%;
Step 3: by substrate resin solution and Epoxy resin composition solution according to parts by weight proportioning substrate resin solution solute: Epoxy resin composition solution solute 100:(5 ~ 25), and mix at ambient temperature, until mix, obtain mixed resin solution;
Step 4: adopt continuous impregnating method, drawn by Extruded roller, mixed resin solution is utilized to infiltrate Dan Shu M race carbon fiber in glue groove, M race carbon fiber winding 40 ~ 60 circles on fixed leg, be carry out drying under the condition of 65 DEG C ~ 75 DEG C in temperature by the M race carbon fiber be wrapped on fixed leg, time of drying is 0.8h ~ 1.2h, namely obtains the blank material of M race carbon fiber/matrix resin matrix material;
Step 5: the blank material of M race carbon fiber/matrix resin matrix material is placed in mould, then vulcanizing press XLB-D0.5MN is utilized to carry out compression molding under pressure is for 0.7MPa ~ 0.8MPa condition, finally by solidification treatment, obtain M race carbon fiber/matrix resin matrix material;
Matrix resin described in step 2 is 4211 matrix resins, and the M race carbon fiber described in step 4 is M55J carbon fiber, and carbon fiber K number is 3K ~ 80K;
Wherein, a kind of preparation method of composition epoxy resin carries out according to following steps:
Step one: weigh: the catalyzer taking the epoxy resin of 70 ~ 100 parts, the polyacrylic acid of 1 ~ 10 part, the urethane of 1 ~ 10 part and 0.01 ~ 0.1 part by weight;
Step 2: the epoxy resin of 70 ~ 100 parts that step one are taken is heated to 140 DEG C ~ 160 DEG C, then the polyacrylic acid of 1 ~ 10 part that step one takes and the urethane of 1 ~ 10 part is added, add the catalyzer of 0.01 ~ 0.1 part that step one takes again, be react 1.2h ~ 1.8h under the condition of 140 ~ 160 DEG C in temperature, obtain composition epoxy resin; Wherein, described catalyzer is benzyldimethylamine.
2., according to a kind of method utilizing composition epoxy resin to prepare M race carbon fiber/matrix resin matrix material described in claim 1, it is characterized in that the thinner I described in step one prepared in the method for M race carbon fiber/matrix resin matrix material is acetone.
3., according to a kind of method utilizing composition epoxy resin to prepare M race carbon fiber/matrix resin matrix material described in claim 1, it is characterized in that the thinner II described in step 2 prepared in the method for M race carbon fiber/matrix resin matrix material is acetone.
4. according to a kind of method utilizing composition epoxy resin to prepare M race carbon fiber/matrix resin matrix material described in claim 1, it is characterized in that the solidification treatment described in step 5 is carried out according to following curing cycle: under temperature is 90 DEG C of conditions, keep 60min, then under temperature is 130 DEG C of conditions, keep 60min, finally under temperature is 180 DEG C of conditions, keep 4h.
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