CN103525007A - Method for preparing rectorite-modified epoxy resin/glass fiber composite material - Google Patents
Method for preparing rectorite-modified epoxy resin/glass fiber composite material Download PDFInfo
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- CN103525007A CN103525007A CN201310408241.5A CN201310408241A CN103525007A CN 103525007 A CN103525007 A CN 103525007A CN 201310408241 A CN201310408241 A CN 201310408241A CN 103525007 A CN103525007 A CN 103525007A
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- rectorite
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Abstract
The invention relates to a method for preparing a rectorite-modified epoxy resin/glass fiber composite material. The method comprises the following steps: uniformly mixing and stirring rectorite and distilled water to obtain a rectorite suspension A; uniformly mixing and stirring organic amine and distilled water, and dripping an acid to obtain an ammonium salt B; slowly adding the obtained ammonium salt B into the rectorite suspension A, fully stirring, filtering and drying to obtain organic rectorite; trimming a glass fiber, cleaning and fully drying for later use; adding an epoxy resin curing agent into epoxy resin for uniformly mixing, adding the organic rectorite, and uniformly mixing to obtain a mixture C; putting the mixture C and the prepared glass fiber into a mold for curing to obtain the rectorite-modified epoxy resin/glass fiber composite material. The preparation method is simple in preparation process and low in cost, and the glass fiber/epoxy resin composite material with excellent mechanical property can be obtained.
Description
Technical field
The present invention relates to field of compound material, relate in particular to a kind of preparation method of rectorite modified epoxy/glass fiber compound material.
Background technology
Polymer matrix composite is the strongthener of one or more tiny shapes, be scattered in the matrix material forming in polymeric matrix, there is high specific strength, high specific stiffness, corrosion-resistant, the good performances such as antifatigue, easy machine-shaping, be the indispensable base mateiral of modern industry and hi-tech, become the main body of matrix material industry.Wherein glass fiber compound material is the matrix material that current production rate is maximum, purposes is the widest, has formed the main body of matrix material.How further to improve the problem that its mechanical property becomes people's extensive concern.
Nanoparticle is the brand-new material of Recent study and exploitation, because its size is little, specific surface area large, high, active high, the good dispersity of surface energy, and the toughening effect that can obtain.So-called nano composite material refers to that inorganic filler forms Organic/Inorganic Composite Nanomaterials with nano-size dispersion in organic polymer matrix.In nano composite material, the size of disperse phase at least at one-dimensional square to being less than 100nm.Stronger interfacial interaction between the nano effect bringing due to nanoparticle and nanoparticle and matrix, polymer nanocomposites has the performance such as mechanics, calorifics that is better than same composition conventional polymer matrix material.Nano composite material also has the not available excellent properties of general plastics.
Rectorite is a kind of have special construction, comparatively rare clay of laminar silicate mineral, is a kind of natural nano lamellar material.Unmodified rectorite has strong wetting ability, poor with the consistency of polymkeric substance, while therefore preparing polymkeric substance/rectorite nano composite material, must first to it, carry out organic modification.The ultimate principle of modification is: organic quaternary ammonium salt positively charged ion and rectorite the exchangeable cationic type between layer generation ion exchange reaction, and make organic group be covered in rectorite surface, change its surface property, from original wetting ability, become lipophilicity.Rectorite after modification has good affinity with a lot of organic solvents and polymer.These rectorites that organised are dispersed in polymkeric substance with nano level, form inorganic and matrix material organic hybrid, and its over-all properties will obviously improve.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of rectorite modified epoxy/glass fiber compound material.
The technical scheme that the present invention realizes above-mentioned purpose is as follows: a kind of preparation method of rectorite modified epoxy/glass fiber compound material, comprises the steps:
Rectorite and distilled water mixing and stirring are obtained to rectorite suspension liquid A;
By organic amine and distilled water mixing and stirring, drip acid and obtain ammonium salt B;
The ammonium salt B obtaining is slowly joined in rectorite suspension liquid A, after fully stirring, filter, drying, obtain the rectorite that organises;
After glass fibre is pruned, standby after cleaning, being fully dried;
To in epoxy resin, add epoxy curing agent, after mixing, add the rectorite that organises, stir and obtain mixture C;
Mixture C is put into mould together with ready glass fibre and solidify, obtain rectorite modified epoxy/glass fiber compound material.
On the basis of technique scheme, the present invention can also do following improvement.
It is further, described that rectorite and distilled water mixing and stirring are obtained to the concrete steps of rectorite suspension liquid A is as follows:
By rectorite, distilled water, according to mass ratio, be that 1:2～1:8 mixes and stirs and obtains rectorite suspension liquid A.
Further, described by organic amine and distilled water mixing and stirring, the concrete steps that dropping acid obtains ammonium salt B are as follows:
By organic amine, distilled water, according to mass ratio, be that 1:10～1:20 mixes and stirs, then drip hydrochloric acid or nitric acid obtains ammonium salt B until pH is less than 7.
Further, described the ammonium salt B obtaining is slowly joined in rectorite suspension liquid A, the concrete steps of the rectorite that obtains organising after fully stirring, filter, drying are as follows:
Ammonium salt B is slowly joined in rectorite suspension liquid A, after fully stirring, filter, drying, obtain the rectorite that organises, wherein the mass ratio of organic ammonium and rectorite is 1:2～1:10.
Further, described by after glass fibre pruning, concrete steps standby after cleaning, being fully dried are as follows:
By content be 1～1.2 times of liquid-state epoxy resin quality glass fibre prune after, clean, standby after fully dry.
Further, describedly will in epoxy resin, add epoxy curing agent, after mixing, add the rectorite that organises, stirring, it is as follows to obtain the concrete steps of mixture C:
At E-44(6101) or E-54(616) in any one liquid-state epoxy resin, by liquid-state epoxy resin, be that 100g:0.50～10g adds the rectorite that organises with the rectorite mass ratio that organises, by liquid-state epoxy resin and reactive thinner mass ratio, be that 100g:0～0.50g adds any one reactive thinner in 050 reactive thinner or n-butyl glycidyl ether, be heated to 80～90 ℃, vacuumize and stir 1～1.5h;
By liquid-state epoxy resin and liquid-state epoxy resin solidifying agent mass ratio, be that 100g:8～100g adds any one liquid-state epoxy resin solidifying agent in 650 polymeric amide, poly-nonane diacid acid anhydride, Triethylenetetramine (TETA) again, and stir and obtain mixture C.
Further, describedly mixture C is put into mould together with ready glass fibre solidify, the concrete steps that obtain rectorite modified epoxy/glass fiber compound material are as follows:
Mixture C is put into mould together with ready glass fibre, at 60～160 ℃ of temperature, solidify 1～1.5h;
Obtain the compound rectorite modified epoxy/glass fiber compound material compound with glass fibre again of rectorite and epoxy resin substrate, wherein rectorite content is 0.17%～4.4% with respect to whole matrix material.
The invention has the beneficial effects as follows:
1. preparation process is simple and easy, with low cost;
2, the present invention adopts organic quaternary ammonium salt positively charged ion and rectorite the exchangeable cationic type between layer generation ion exchange reaction, makes its surface property, from original wetting ability, becomes lipophilicity.Make itself and epoxide resin polymer have very high consistency;
3, rectorite has natural nano-lamellar structure, and the system that is introduced into is middle can form pillared intercalation configuration, makes glass fiber/epoxy composite material have more outstanding mechanical property.
Accompanying drawing explanation
Fig. 1 is preparation method's schema of rectorite modified epoxy/glass fiber compound material of the present invention;
Embodiment
Below in conjunction with accompanying drawing, principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
As shown in Figure 1, a kind of preparation method of rectorite modified epoxy/glass fiber compound material, comprises the steps:
Rectorite and distilled water mixing and stirring are obtained to rectorite suspension liquid A;
By organic amine and distilled water mixing and stirring, drip acid and obtain ammonium salt B;
The ammonium salt B obtaining is slowly joined in rectorite suspension liquid A, after fully stirring, filter, drying, obtain the rectorite that organises;
After glass fibre is pruned, standby after cleaning, being fully dried;
To in epoxy resin, add epoxy curing agent, after mixing, add the rectorite that organises, stir and obtain mixture C;
Mixture C is put into mould together with ready glass fibre and solidify, obtain rectorite modified epoxy/glass fiber compound material.
Embodiment 1:
10g rectorite is joined in 20g distilled water, mix and stir obtaining rectorite suspension liquid A; 5g organic amine is joined in 50g distilled water, mix and stir, then drip hydrochloric acid and obtain ammonium salt B until pH is less than 7; The ammonium salt B that is 5g by organic amine content slowly joins in the rectorite suspension liquid A that rectorite content is 10g, after fully stirring, filter, drying, obtains the rectorite that organises; By quality, be after 1 times of liquid-state epoxy resin quality is the glass fibre pruning of 100g, standby after cleaning, being fully dried; At 100gE-44(6101) in liquid-state epoxy resin, add the 0.50g rectorite that organises, add 0.30g050 reactive thinner, be heated to 80 ℃, vacuumize and stir 1h; Then add again 100g650 polymeric amide liquid-state epoxy resin solidifying agent, and stir and obtain mixture C; Mixture C is put into mould together with ready glass fibre, at 60 ℃ of temperature, solidify 1h; Obtain the compound rectorite modified epoxy/glass fiber compound material compound with glass fibre again of rectorite and epoxy resin substrate, wherein through composition detection analysis, show that rectorite content is 0.17% with respect to whole matrix material.
Embodiment 2
25g rectorite is joined in 150g distilled water, mix and stir obtaining rectorite suspension liquid A; 5g organic amine is joined in 75g distilled water, mix and stir, then drip nitric acid and obtain ammonium salt B until pH is less than 7; The ammonium salt B that is 5g by organic amine content slowly joins in the rectorite suspension liquid A that rectorite content is 25g, after fully stirring, filter, drying, obtains the rectorite that organises; By quality, be after 1.1 times of liquid-state epoxy resin quality are the glass fibre pruning of 110g, standby after cleaning, being fully dried; At 100g E-54(616) in liquid-state epoxy resin, add the 10g rectorite that organises, be heated to 90 ℃, vacuumize and stir 1h; Add again 8g to gather nonane diacid acid anhydride liquid-state epoxy resin solidifying agent, and stir and obtain mixture C; Mixture C is put into mould together with ready glass fibre, at 130 ℃ of temperature, solidify 1.5h; Obtain the compound rectorite modified epoxy/glass fiber compound material compound with glass fibre again of rectorite and epoxy resin substrate, wherein through composition detection analysis, show that rectorite content is 4.4% with respect to whole matrix material.
Embodiment 3:
50g rectorite is joined in 400g distilled water, mix and stir obtaining rectorite suspension liquid A; 5g organic amine is joined in 100g distilled water, mix and stir, then drip hydrochloric acid and obtain ammonium salt B until pH is less than 7; The ammonium salt B that is 5g by organic amine content slowly joins in the rectorite suspension liquid A that rectorite content is 50g, after fully stirring, filter, drying, obtains the rectorite that organises; By quality, be after 1.2 times of liquid-state epoxy resin quality are the glass fibre pruning of 120g, standby after cleaning, being fully dried; At 100g E-54(616) in liquid-state epoxy resin, add the 1.0g rectorite that organises, add 0.50g n-butyl glycidyl ether reactive thinner, be heated to 80 ℃, vacuumize and stir 1.5h; Add again 14g Triethylenetetramine (TETA) liquid-state epoxy resin solidifying agent, and stir and obtain mixture C; Mixture C is put into mould together with ready glass fibre, at 100 ℃ of temperature, solidify 1.5h; Obtain the compound rectorite modified epoxy/glass fiber compound material compound with glass fibre again of rectorite and epoxy resin substrate, wherein through composition detection analysis, show that rectorite content is 0.43% with respect to whole matrix material.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a preparation method for rectorite modified epoxy/glass fiber compound material, comprises the steps:
Rectorite and distilled water mixing and stirring are obtained to rectorite suspension liquid A;
By organic amine and distilled water mixing and stirring, drip acid and obtain ammonium salt B;
The ammonium salt B obtaining is slowly joined in rectorite suspension liquid A, after fully stirring, filter, drying, obtain the rectorite that organises;
After glass fibre is pruned, standby after cleaning, being fully dried;
To in epoxy resin, add epoxy curing agent, after mixing, add the rectorite that organises, stir and obtain mixture C;
Mixture C is put into mould together with ready glass fibre and solidify, obtain rectorite modified epoxy/glass fiber compound material.
2. a kind of preparation method of rectorite modified epoxy/glass fiber compound material according to claim 1, is characterized in that, described that rectorite and distilled water mixing and stirring are obtained to the concrete steps of rectorite suspension liquid A is as follows:
By rectorite, distilled water, according to mass ratio, be that 1:2～1:8 mixes and stirs and obtains rectorite suspension liquid A.
3. a kind of preparation method of rectorite modified epoxy/glass fiber compound material according to claim 1, is characterized in that, described by organic amine and distilled water mixing and stirring, and dripping acid, to obtain the concrete steps of ammonium salt B as follows:
By organic amine, distilled water, according to mass ratio, be that 1:10～1:20 mixes and stirs, then drip hydrochloric acid or nitric acid obtains ammonium salt B until pH is less than 7.
4. according to claim a kind of preparation method of rectorite modified epoxy/glass fiber compound material according to claim 1, it is characterized in that, described the ammonium salt B obtaining is slowly joined in rectorite suspension liquid A, the concrete steps of the rectorite that obtains organising after fully stirring, filter, drying are as follows:
Ammonium salt B is slowly joined in rectorite suspension liquid A, after fully stirring, filter, drying, obtain the rectorite that organises, wherein the mass ratio of organic ammonium and rectorite is 1:2～1:10.
5. according to claim a kind of preparation method of rectorite modified epoxy/glass fiber compound material according to claim 1, it is characterized in that, described glass fibre is pruned after, clean, concrete steps standby after fully dry are as follows:
Standby after after the glass fibre that is 1～1.2 times of liquid-state epoxy resin quality by content is pruned, cleaning, being fully dried.
6. according to claim a kind of preparation method of rectorite modified epoxy/glass fiber compound material according to claim 1, it is characterized in that, describedly epoxy curing agent will be added in epoxy resin, after mixing, add the rectorite that organises, stirring, it is as follows to obtain the concrete steps of mixture C:
At E-44(6101) or E-54(616) in any one liquid-state epoxy resin, by liquid-state epoxy resin, be that 100g:0.50～10g adds the rectorite that organises with the rectorite mass ratio that organises, by liquid-state epoxy resin and reactive thinner mass ratio, be that 100g:0～0.50g adds any one reactive thinner in 050 reactive thinner or n-butyl glycidyl ether, be heated to 80～90 ℃, vacuumize and stir 1～1.5h;
By liquid-state epoxy resin and liquid-state epoxy resin solidifying agent mass ratio, be that 100g:8～100g adds any one liquid-state epoxy resin solidifying agent in 650 polymeric amide, poly-nonane diacid acid anhydride, Triethylenetetramine (TETA) again, and stir and obtain mixture C.
7. according to claim a kind of preparation method of rectorite modified epoxy/glass fiber compound material according to claim 1, it is characterized in that, describedly mixture C is put into mould together with ready glass fibre solidify, the concrete steps that obtain rectorite modified epoxy/glass fiber compound material are as follows:
Mixture C is put into mould together with ready glass fibre, at 60～160 ℃ of temperature, solidify 1～1.5h;
Obtain the compound rectorite modified epoxy/glass fiber compound material compound with glass fibre again of rectorite and epoxy resin substrate, wherein rectorite content is 0.17%～4.4% with respect to whole matrix material.
8. rectorite modified epoxy/glass fiber compound material of preparing according to any method of claim 1 to 7.
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| CN201310408241.5A CN103525007A (en) | 2013-09-09 | 2013-09-09 | Method for preparing rectorite-modified epoxy resin/glass fiber composite material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385470A (en) * | 2002-04-25 | 2002-12-18 | 武汉大学 | Organic composite rectorite and preparation process thereof |
| CN1462768A (en) * | 2003-06-11 | 2003-12-24 | 武汉大学 | Nano composite material of epoxy resin and its preparing method |
| CN101492572A (en) * | 2008-12-24 | 2009-07-29 | 暨南大学 | Antimicrobial macromolecule material and method for preparing the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385470A (en) * | 2002-04-25 | 2002-12-18 | 武汉大学 | Organic composite rectorite and preparation process thereof |
| CN1462768A (en) * | 2003-06-11 | 2003-12-24 | 武汉大学 | Nano composite material of epoxy resin and its preparing method |
| CN101492572A (en) * | 2008-12-24 | 2009-07-29 | 暨南大学 | Antimicrobial macromolecule material and method for preparing the same |
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Application publication date: 20140122 |
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