CN103965585A - Preparation method of hollow glass bead-modified epoxy resin composite material - Google Patents
Preparation method of hollow glass bead-modified epoxy resin composite material Download PDFInfo
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- CN103965585A CN103965585A CN201410208172.8A CN201410208172A CN103965585A CN 103965585 A CN103965585 A CN 103965585A CN 201410208172 A CN201410208172 A CN 201410208172A CN 103965585 A CN103965585 A CN 103965585A
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Abstract
The invention discloses a preparation method of a hollow glass bead-modified epoxy resin composite material. The hollow glass bead-modified epoxy resin composite material is prepared by a method of adding organic montmorillonite, casting and curing in steps at a varying temperature. The method disclosed by the invention can effectively prevent separation of low-density filler, solves a phase separation problem of the composite material and realizes uniform dispersion of the hollow glass beads in a basal body. The method disclosed by the invention can eliminate air bubbles which are produced in a preparation process of the epoxy resin composite material, and can reduce internal defects of the composite material.
Description
Technical field
The invention belongs to field of compound material, relate to a kind of preparation method of Filled With Hollow Bead epoxy resin composite material, specifically a kind of nothing be separated, the preparation method of hollow glass micropearl filler finely dispersed epoxy resin composite material in matrix.
Background technology
Epoxy resin is because of its good electrical isolation, machinery, adhesiveproperties, and the characteristic such as resistance to chemical attack is widely used in the matrix of matrix material.It more and more comes into one's own in fields such as steamer, automobile, aerospace as advanced composite material.Hollow glass micropearl is that a kind of density is at 0.125～0.6g/cm
3between, the inorganic silicic acid salt material of micron order particle diameter, hollow structure, have that quality is light, particle diameter and an advantage such as wall thickness is controlled.And its ultimate compression strength, fusing point and resistivity are high, and thermal conductivity coefficient and Thermal Contraction Coefficient are little etc., and feature makes it have broad application prospects in fields such as petroleum industry, aerospace, Novel high-speed train, automobile steamer, thermal insulating coatings.Adopt hollow glass micropearl to fill and can effectively reduce the density of epoxy resin, and give its damping drag reduction, sound insulation, the characteristic such as heat insulation.
Because the density difference of epoxy resin and hollow glass micropearl is large, the two surface tissue significant difference and interact a little less than, prepare in the process of Filled With Hollow Bead epoxy resin composite material at conventional means, hollow glass micropearl and epoxy resin-base present significantly and are separated, and cause final matrix material to occur that the excellent specific property of demixing phenomenon, matrix material cannot fully demonstrate.The viscosity of raising system can alleviate the demixing phenomenon of matrix material.But in molding process, viscosity increase usually causes mass transfer and the difficulty of conducting heat, and causes the non-homogeneous dispersion of filler.
Summary of the invention
The invention provides a kind of preparation method of Filled With Hollow Bead epoxy resin composite material, object is by taking organo montmorillonite as thixotropic agent, and carry out the viscosity in hollow regulating glass microballon modified epoxy resin system molding process in conjunction with alternating temperature segmentation curing process, realize dispersed, the lamination problem that effectively solve matrix material of hollow glass micropearl in epoxy resin-base.
The invention reside in the preparation method that a kind of Filled With Hollow Bead epoxy resin composite material is provided, concrete steps are as follows:
1) under high speed shear stirs, organo montmorillonite is dispersed in and in epoxy resin, makes polynite pre-gelled; Wherein the consumption of epoxy resin accounts for 10～50wt% of epoxy resin total amount in hollow glass micropearl modified epoxy resin composite;
2) hollow glass micropearl is distributed in the silane coupling agent aqueous solution, makes coupling agent modified hollow glass micropearl;
3) fully dried coupling agent modified hollow glass micropearl, remaining epoxy resin, polynite pre-gelled, solidifying agent mix rear shear agitation, make finely dispersed Filled With Hollow Bead epoxy resin composite dispersion liquid;
4) Filled With Hollow Bead epoxy resin composite dispersion liquid is vacuumized after removing bubble and add curing catalyst, and be uniformly mixed;
5) by step 4) gained adds after the epoxy resin of curing catalyst and the casting of hollow glass micropearl composite dispersion liquid, is cured respectively at low temperature, middle gentle high temperature, makes epoxy resin and hollow glass micropearl matrix material.
In aforesaid method,
High speed shear stirs and typically refers to speed more than 300rpm.
Step 1) and 3) any in described epoxy resin be bisphenol A-type E-51, E-44, E-54, E-42 epoxy resin; Described organo montmorillonite is quaternary ammonium salt organo montmorillonite, 0.5～5.0wt% that the addition of organo montmorillonite is epoxy resin.
Described hollow glass micropearl granularity is micron order, and density is 125～600kg/m
3; The addition of hollow glass micropearl is 2～20wt% of epoxy resin.
Step 2) described silane coupling agent is 3-aminopropyl triethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicon, γ-thin propyl-triethoxysilicane, the one in γ-(quadrol base) propyl trimethoxy silicane; Its concentration of aqueous solution is 0.1～10wt%.
Step 3) described solidifying agent is hexahydrophthalic anhydride, Tetra Hydro Phthalic Anhydride, methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, Tetra hydro Phthalic anhydride, any one in methyl carbic anhydride; The addition of solidifying agent is 40～100wt% of epoxy resin.
Step 4) described curing catalyst is trolamine, benzyldimethylamine, 2-ethyl-4 Methylimidazole, dimethylaminomethylphenol, 2,4, a kind of in 6-tri-(dimethylamino methyl) phenol or two kinds; The addition of curing catalyst is 0.5～2wt% of epoxy resin.
Step 4) described low-temperature curing temperature is 50～80 DEG C, be 1～5 hour set time; Described intermediate temperature setting temperature is 100～120 DEG C, and be 1～5 hour set time; Described hot setting temperature is 150～180 DEG C, and be 3～10 hours set time.
The preparation method who the invention provides a kind of Filled With Hollow Bead epoxy resin composite material that solves problem of phase separation, this preparation method can eliminate the bubble producing in epoxy resin composite material preparation process simultaneously, reduces the subsurface defect of matrix material.
Brief description of the drawings
Fig. 1 is the low range stereoscan photograph on the embodiment 1 Filled With Hollow Bead epoxy resin composite material brittle failure surface of preparing.
Fig. 2 is the high magnification stereoscan photograph on the embodiment 1 Filled With Hollow Bead epoxy resin composite material brittle failure surface of preparing.
Embodiment
The present invention can make aathermoset resin system under high shear forces, present low-viscosity to be beneficial to the even mixing of component by adding thixotropic agent; After shearing action stops, thixotroping system becomes three-dimensional net structure and effectively prevents the appearance being separated.Organo montmorillonite is not only the efficient thixotropic agent that the industry such as application, oil is used, and because its natural nanometer laminated structure becomes the desirable reinforcing filler of polymkeric substance.
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further.It should be noted that at this, be used for helping to understand the present invention for the explanation of these embodiments, but do not form limitation of the invention.In addition,, in each embodiment of described the present invention, involved technical characterictic just can combine mutually as long as do not form each other conflict.
Embodiment 1:
1.2 grams of Cloisite30B type organo montmorillonites are distributed to the high speed shear stirring with 500rpm in 10 grams of E-51 type epoxy resin and within 0.5 hour, make polynite pre-gelled.
Be 150kg/m by 6 grams of density
3hollow glass micropearl be distributed in the 3-aminopropyl triethoxysilane coupling agent aqueous solution that concentration is 1wt%, dispersed with stirring is fully dry after 3 hours, makes dry coupling agent modified hollow glass micropearl.
By polynite pre-gelled, dry coupling agent modified hollow glass micropearl, fully mix under high speed shear stirs with 50 grams of E-51 type epoxy resin, 45 grams of Tetra Hydro Phthalic Anhydride solidifying agent, make finely dispersed Filled With Hollow Bead epoxy resin composite dispersion liquid.
By after Filled With Hollow Bead epoxy resin composite dispersion liquid vacuumize degassing bubble, add 0.6 gram of dimethylaminomethylphenol curing catalyst, and stirring at low speed mix after cast molding at 80 DEG C.Then, at 80 DEG C, 100 DEG C, 150 DEG C, solidify 3 hours, 3 hours, 8 hours respectively, make Filled With Hollow Bead epoxy resin composite material.
The Filled With Hollow Bead epoxy resin composite material making is adopted to liquid nitrogen brittle failure, after section metal spraying, observe by scanning electron microscope (SEM).Can find out that from low multiple SEM photo (Fig. 1) hollow glass micropearl is dispersed in epoxy resin-base; Can find out that from high multiple SEM photo (Fig. 2) hollow glass micropearl and epoxy resin have good interface to cohere.
Embodiment 2:
1.2 grams of Cloisite30B organo montmorillonites are distributed to the high speed shear stirring with 500rpm in 6 grams of E-44 type epoxy resin and within 0.5 hour, make polynite pre-gelled.
Be 200kg/m by 6 grams of density
3hollow glass micropearl be distributed in the γ that concentration is 1.0wt%-(2,3-epoxy the third oxygen) propyl trimethoxy silicane coupling agent aqueous solution, dispersed with stirring is fully dry after 3 hours, makes dry coupling agent modified hollow glass micropearl.
By polynite pre-gelled, dry coupling agent modified hollow glass micropearl, fully mix under high speed shear stirs with 54 grams of E-44 type epoxy resin, 40 grams of hexahydrophthalic anhydride solidifying agent, make finely dispersed Filled With Hollow Bead epoxy resin composite dispersion liquid.
By after Filled With Hollow Bead epoxy resin composite dispersion liquid vacuumize degassing bubble, add 0.6 gram of 2-ethyl-4-methylimidazole curing catalyst, and stirring at low speed mix after cast molding at 80 DEG C.Then, at 80 DEG C, 100 DEG C, 150 DEG C, solidify 3 hours, 5 hours, 10 hours respectively, make Filled With Hollow Bead epoxy resin composite material.
Embodiment 3:
0.6 gram of Cloisite30B organo montmorillonite is distributed to the high speed shear stirring with 300rpm in 10 grams of E-51 type epoxy resin and within 0.5 hour, makes polynite pre-gelled.
Be 125kg/m by 6 grams of density
3hollow glass micropearl be distributed in the γ that concentration is 2.0wt%-(methacryloxypropyl) propyl trimethoxy silicane coupling agent aqueous solution, dispersed with stirring is fully dry after 3 hours, makes dry coupling agent modified hollow glass micropearl.
By polynite pre-gelled, dry coupling agent modified hollow glass micropearl, fully mix under high speed shear stirs with 50 grams of E-51 type epoxy resin, 48 grams of hexahydrophthalic anhydride solidifying agent, make finely dispersed Filled With Hollow Bead epoxy resin composite dispersion liquid.
By after Filled With Hollow Bead epoxy resin composite dispersion liquid vacuumize degassing bubble, add 0.9 gram of benzyldimethylamine curing catalyst, and stirring at low speed mix after cast molding at 80 DEG C.Then, at 50 DEG C, 120 DEG C, 150 DEG C, solidify 5 hours, 1 hour, 5 hours respectively, make Filled With Hollow Bead epoxy resin composite material.
Embodiment 4:
0.6 gram of Cloisite30B organo montmorillonite is distributed to the high speed shear stirring with 300rpm in 12 grams of E-44 type epoxy resin and within 0.5 hour, makes polynite pre-gelled.
Be 600kg/m by 3 grams of density
3hollow glass micropearl be distributed to the γ that concentration is 3.0wt%-dredge in propyl-triethoxysilicane coupling agent aqueous solution, dispersed with stirring is fully dry after 3 hours, makes dry coupling agent modified hollow glass micropearl.
By polynite pre-gelled, dry coupling agent modified hollow glass micropearl, fully mix under high speed shear stirs with 48 grams of E-44 type epoxy resin, 44 grams of methyl tetrahydrophthalic anhydride solidifying agent, make finely dispersed Filled With Hollow Bead epoxy resin composite dispersion liquid.
By after Filled With Hollow Bead epoxy resin composite dispersion liquid vacuumize degassing bubble, add 0.3 gram 2,4,6-tri-(dimethylamino methyl) phenol, 0.6 gram of trolamine curing catalyst, and stirring at low speed mix after cast molding at 80 DEG C.Then, at 80 DEG C, 100 DEG C, 180 DEG C, solidify 3 hours, 5 hours, 3 hours respectively, make Filled With Hollow Bead epoxy resin composite material.
Embodiment 5:
0.3 gram of BP-188 organo montmorillonite is distributed to the high speed shear stirring with 600rpm in 18 grams of E-54 type epoxy resin and within 0.5 hour, makes polynite pre-gelled.
Be 150kg/m by 1.2 grams of density
3hollow glass micropearl be distributed in the γ that concentration is 0.5wt%-(2,3-epoxy the third oxygen) propyl trimethoxy silicane coupling agent aqueous solution, dispersed with stirring is fully dry after 5 hours, makes dry coupling agent modified hollow glass micropearl.
By polynite pre-gelled, dry coupling agent modified hollow glass micropearl, fully mix under high speed shear stirs with 42 grams of E-54 type epoxy resin, 54 grams of methyl tetrahydrophthalic anhydride solidifying agent, make finely dispersed Filled With Hollow Bead epoxy resin composite dispersion liquid.
By after Filled With Hollow Bead epoxy resin composite dispersion liquid vacuumize degassing bubble, add 0.3 gram of 2-ethyl-4-methylimidazole curing catalyst, and stirring at low speed mix after cast molding at 80 DEG C.Then, at 80 DEG C, 120 DEG C, 180 DEG C, solidify 1 hour, 1 hour, 8 hours respectively, make Filled With Hollow Bead epoxy resin composite material.
Embodiment 6:
1.8 grams of BP-188 organo montmorillonites are distributed to the high speed shear stirring with 600rpm in 18 grams of E-54 type epoxy resin and within 0.5 hour, make polynite pre-gelled.
Be 600kg/m by 9 grams of density
3hollow glass micropearl be distributed in the γ that concentration is 4.0wt%-(quadrol base) propyl trimethoxy silicane coupling agent aqueous solution, dispersed with stirring is fully dry after 3 hours, makes dry coupling agent modified hollow glass micropearl.
By polynite pre-gelled, dry coupling agent modified hollow glass micropearl, fully mix under high speed shear stirs with 42 grams of E-54 type epoxy resin, 60 grams of methyl carbic anhydride solidifying agent, make finely dispersed Filled With Hollow Bead epoxy resin composite dispersion liquid.
By after Filled With Hollow Bead epoxy resin composite dispersion liquid vacuumize degassing bubble, add 1.2 grams of 2-ethyl-4-methylimidazole curing catalysts, and stirring at low speed mix after cast molding at 80 DEG C.Then, at 80 DEG C, 100 DEG C, 150 DEG C, solidify 3 hours, 3 hours, 10 hours respectively, make Filled With Hollow Bead epoxy resin composite material.
Embodiment 7:
3 grams of BP-188 organo montmorillonites are distributed to the high speed shear stirring with 500rpm in 30 grams of E-42 type epoxy resin and within 0.5 hour, make polynite pre-gelled.
Be 600kg/m by 12 grams of density
3hollow glass micropearl be distributed in the 3-aminopropyl triethoxysilane coupling agent aqueous solution that concentration is 5.0wt%, dispersed with stirring is fully dry after 3 hours, makes dry coupling agent modified hollow glass micropearl.
By polynite pre-gelled, dry coupling agent modified hollow glass micropearl, fully mix under high speed shear stirs with 30 grams of E-42 type epoxy resin, 24 grams of phthalic acid anhydride curing agents, make finely dispersed Filled With Hollow Bead epoxy resin composite dispersion liquid.
By after Filled With Hollow Bead epoxy resin composite dispersion liquid vacuumize degassing bubble, add 0.3 gram of 2-ethyl-4-methylimidazole curing catalyst, and stirring at low speed mix after cast molding at 80 DEG C.Then, at 80 DEG C, 100 DEG C, 150 DEG C, solidify 3 hours, 3 hours, 8 hours respectively, make Filled With Hollow Bead epoxy resin composite material.
Table 1 embodiment 1-7 material addition and proportionlity thereof
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment and accompanying drawing.Do not depart from the equivalence or the amendment that under spirit disclosed in this invention, complete so every, all fall into the scope of protection of the invention.
Claims (8)
1. a preparation method for Filled With Hollow Bead epoxy resin composite material, concrete steps are as follows:
1) under high speed shear stirs, organo montmorillonite is dispersed in and in epoxy resin, makes polynite pre-gelled; Wherein the consumption of epoxy resin accounts for 10～50wt% of epoxy resin total amount in hollow glass micropearl modified epoxy resin composite;
2) hollow glass micropearl is distributed in the silane coupling agent aqueous solution, makes coupling agent modified hollow glass micropearl;
3) fully dried coupling agent modified hollow glass micropearl, remaining epoxy resin, polynite pre-gelled, solidifying agent mix rear high speed shear stirring, make finely dispersed Filled With Hollow Bead epoxy resin composite dispersion liquid;
4) Filled With Hollow Bead epoxy resin composite dispersion liquid is vacuumized after removing bubble and add curing catalyst, and stirring at low speed is mixed;
5) by step 4) gained adds after the Filled With Hollow Bead epoxy resin composite dispersion liquid casting of curing catalyst, is cured respectively at low temperature, middle gentle high temperature, makes Filled With Hollow Bead epoxy resin composite material.
2. according to the preparation method of Filled With Hollow Bead epoxy resin composite material claimed in claim 1, it is characterized in that: in E-51, E-44 that described epoxy resin is bisphenol A-type, E-54, E-42 any.
3. according to the preparation method of Filled With Hollow Bead epoxy resin composite material claimed in claim 1, it is characterized in that: described hollow glass micropearl granularity is micron order, density is 125～600kg/m
3; The addition of hollow glass micropearl is 2～20wt% of epoxy resin.
4. according to the preparation method of Filled With Hollow Bead epoxy resin composite material claimed in claim 1, it is characterized in that: described organo montmorillonite is quaternary ammonium salt organo montmorillonite; The addition of organo montmorillonite is 0.5～5.0wt% of epoxy resin.
5. according to the preparation method of Filled With Hollow Bead epoxy resin composite material claimed in claim 1, it is characterized in that described silane coupling agent is 3-aminopropyl triethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicon, γ-thin propyl-triethoxysilicane, the one in γ-(quadrol base) propyl trimethoxy silicane; Its concentration of aqueous solution is 0.1～10wt%.
6. according to the preparation method of Filled With Hollow Bead epoxy resin composite material claimed in claim 1, it is characterized in that: described solidifying agent is hexahydrophthalic anhydride, Tetra Hydro Phthalic Anhydride, methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, Tetra hydro Phthalic anhydride, any one in methyl carbic anhydride; The addition of solidifying agent is 40～100wt% of epoxy resin.
7. according to the preparation method of Filled With Hollow Bead epoxy resin composite material claimed in claim 1, it is characterized in that: described curing catalyst is trolamine, benzyldimethylamine, 2-ethyl-4 Methylimidazole, dimethylaminomethylphenol, 2, a kind of in 4,6-tri-(dimethylamino methyl) phenol or two kinds; The addition of curing catalyst is 0.5～2wt% of epoxy resin.
8. according to the preparation method of Filled With Hollow Bead epoxy resin composite material claimed in claim 1, it is characterized in that: described low-temperature curing temperature is 50～80 DEG C, be 1～5 hour set time; Described intermediate temperature setting temperature is 100～120 DEG C, and be 1～5 hour set time; Described hot setting temperature is 150～180 DEG C, and be 3～10 hours set time.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106084277A (en) * | 2016-06-17 | 2016-11-09 | 江苏科技大学 | A kind of porous material of split-phase synthesis and preparation method thereof |
| CN108642921A (en) * | 2018-05-29 | 2018-10-12 | 郭震 | One kind is ventilative, wear-resisting compound-type fabric and preparation method thereof |
| CN109074902A (en) * | 2016-03-15 | 2018-12-21 | 亨斯迈先进化工材料许可(瑞士)有限公司 | Preparation is used for the method for the insulation system of electrical engineering, thus obtained product and application thereof |
| CN111118643A (en) * | 2020-02-28 | 2020-05-08 | 山东锦程地毯有限公司 | Peculiar smell removal type carpet and preparation method thereof |
| CN111154230A (en) * | 2020-01-19 | 2020-05-15 | 吴娟 | Sound insulation composite material and preparation method thereof |
| CN111326298A (en) * | 2020-04-07 | 2020-06-23 | 华北电力大学（保定） | Inner-filling light extra-high voltage composite insulating cross arm |
| CN114891316A (en) * | 2022-05-16 | 2022-08-12 | 江苏理工学院 | Novel light epoxy electronic packaging material |
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| CN102277117A (en) * | 2011-08-02 | 2011-12-14 | 达森(天津)材料科技有限公司 | Carbon nano tube reinforced epoxy structural glue used for megawatt-level wind power generating blades and preparation method thereof |
| CN103555149A (en) * | 2013-10-28 | 2014-02-05 | 安徽明都电气有限公司 | Powder coating for radiator shell |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102277117A (en) * | 2011-08-02 | 2011-12-14 | 达森(天津)材料科技有限公司 | Carbon nano tube reinforced epoxy structural glue used for megawatt-level wind power generating blades and preparation method thereof |
| CN103555149A (en) * | 2013-10-28 | 2014-02-05 | 安徽明都电气有限公司 | Powder coating for radiator shell |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109074902A (en) * | 2016-03-15 | 2018-12-21 | 亨斯迈先进化工材料许可(瑞士)有限公司 | Preparation is used for the method for the insulation system of electrical engineering, thus obtained product and application thereof |
| CN106084277A (en) * | 2016-06-17 | 2016-11-09 | 江苏科技大学 | A kind of porous material of split-phase synthesis and preparation method thereof |
| CN108642921A (en) * | 2018-05-29 | 2018-10-12 | 郭震 | One kind is ventilative, wear-resisting compound-type fabric and preparation method thereof |
| CN111154230A (en) * | 2020-01-19 | 2020-05-15 | 吴娟 | Sound insulation composite material and preparation method thereof |
| CN111118643A (en) * | 2020-02-28 | 2020-05-08 | 山东锦程地毯有限公司 | Peculiar smell removal type carpet and preparation method thereof |
| CN111118643B (en) * | 2020-02-28 | 2022-05-06 | 山东锦程地毯有限公司 | Peculiar smell removal type carpet and preparation method thereof |
| CN111326298A (en) * | 2020-04-07 | 2020-06-23 | 华北电力大学（保定） | Inner-filling light extra-high voltage composite insulating cross arm |
| CN114891316A (en) * | 2022-05-16 | 2022-08-12 | 江苏理工学院 | Novel light epoxy electronic packaging material |
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