CN103571300A - Epoxy resin-organic bentonite-metal oxide composite material and preparation method thereof - Google Patents
Epoxy resin-organic bentonite-metal oxide composite material and preparation method thereof Download PDFInfo
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- CN103571300A CN103571300A CN201310440025.9A CN201310440025A CN103571300A CN 103571300 A CN103571300 A CN 103571300A CN 201310440025 A CN201310440025 A CN 201310440025A CN 103571300 A CN103571300 A CN 103571300A
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Abstract
The invention discloses an epoxy resin-organic bentonite-metal oxide composite material. The epoxy resin-organic bentonite-metal oxide composite material is formed by dispersing and compounding nano particles formed by mixing organic bentonite and ZnO-ZrO2 metal oxides in an epoxy resin matrix material; the preparation method of the composite material comprises the following steps of: uniformly dispersing nano particles of organic bentonite and ZnO-ZrO2 metal oxides into epoxy resin liquid by a mechanical mixing method; finally obtaining a novel epoxy resin-organic bentonite-ZnO-Zr2O2 metal oxide composite material by a series of stirring, adding and processing. In a preparation process, a leveling agent and a defoaming agent are not used, and therefore, preparation cost of the material is further lowered. An anti-corrosive coating material disclosed by the invention has good corrosion resistance and can be applied in marine engineering architectures and structural steel or a reinforcing steel bar in a relatively special industrial production condition; the preparation method of the composite material is simple in process, does not need a special device, and can realize large-scale production and application.
Description
Technical field
The present invention relates to a kind of epoxy coat material and preparation method thereof, especially relate to a kind of high-performance epoxy coat material based on nano material doping vario-property and preparation method thereof, be applied to technical field of composite materials.
Background technology
In building field, Steel Concrete is to concern the safety of whole engineering and the important materials in life-span.And the corrosion condition of reinforcing bar to be skeleton construction be damaged and the major cause of early failure, particularly under oceanographic engineering building and special industrial production condition.Therefore to the key position protection of skeleton construction, be, a kind of important means of strengthening its structural safety.In existing various concrete materials, the reinforcing bar in its structure often produces passivation because of alkaline pore water at present.But in actual applications, all can to cause surface to have the passive film of protectiveness destroyed for the factors such as infiltration of carbonation, chlorion and other ion.So studying that more suitable method protects reinforcing bar in skeleton construction, avoids burn into increase its work-ing life is a urgent requirement.Up to the present, the coated materials such as epoxy coat, zinc-plated, glass fiber reinforced polymer, solid stainless steel, stainless steel composite muscle all can be used to increase the solidity to corrosion of reinforcing bar, particularly improve the ability of its opposing chlorion induction corrosion.In these materials, consider the problems such as initial cost, construction and solidity to corrosion thereof, epoxy coat is extremely potential as the material of a kind of physical barriers, protection rebar surface.And the protective value of epoxy coat often depends on quality and the integrity of coating, so improve quality and the integrity of epoxy coat material, become technical problem urgently to be resolved hurrily.
Summary of the invention
In order to solve prior art problem, the object of the invention is to overcome the defect that prior art exists, provide a kind of epoxy resin-organobentonite-metal oxide composite and preparation method thereof, by adding two kinds of metal oxide ZnO-ZrO
2form the erosion shield material of epoxy resin/organobentonite/nano-complex, its Application Areas can be used on structural steel or the reinforcing bar in oceanographic engineering building and more special industrial production condition.It is simple that erosion shield material provided by the invention and preparation method thereof has technique, without specific installation, therefore do not use levelling agent and defoamer composition, greatly reduce cost prepared by material and there is good corrosion resistance nature, can realize large-scale production application.
For reaching foregoing invention, create object, the present invention adopts following technical proposals:
-organobentonite-metal oxide composite, is disperseed in epoxy resin-base material by organobentonite, metal oxide nanoparticles to be compounded to form, and is specially:
(1) matrix material constituents comprises epoxy resin, solidifying agent and silane coupling agent, wherein epoxide resin material is the epoxy resin of bisphenol A-type GCC135, be ethylene glycol bisthioglycolate propylene oxide ether, the outward appearance of epoxy resin is transparent liquid shape, machinery-free foreign material, oxirane value is 0.54-0.6 eq/100g, and viscosity is 700-1100 mPas, and density is 1.13-1.17 g/cm
3; Wherein solidifying agent is isophorone-low viscosity liquid solidifying agent of modification, the outward appearance of solidifying agent is colourless to flaxen liquid, amine value is 550-600mg KOH/g, and viscosity is 10-100 mPas, and epoxy resin mixes with the ratio of weight ratio 10:3 with solidifying agent; Wherein alkane coupling agent is 3-aminopropyl triethoxysilane, i.e. KH550;
(2) component of nano-complex comprises organobentonite and metal oxide nanoparticles, and wherein bentonite concentration is 1～3.5 phr; Wherein metal oxide component material is ZnO-ZrO
2the nano particle being mixed to form of two kinds of metal oxides, wherein ZnO nano granule density is 0.5～1.75phr, and the concentration of ZrO2 nano particle is 0.5～1.75 phr, and wherein phr is the per-cent of component to the gross weight of epoxy resin and solidifying agent.
The preparation method of epoxy resin-organobentonite-metal oxide composite of the present invention, organobentonite, ZnO-ZrO
2nano-particle material is dispersed in epoxy resin liquid uniformly by mechanically mixing method, and add stiffening agent in preparation process before, mixture carries out from degassed at least 6 hours under more than 45 degrees Celsius temperature condition.
The preparation method of above-mentioned epoxy resin-organobentonite-metal oxide composite, comprises the steps:
A. according to two kinds of metal oxide part by weight, be 1:1 making ZnO-ZrO
2nano metal oxide powder;
B. GCC135 type reacting epoxy resin is heated to the low viscosity epoxy resin that obtains of 45 ℃;
C. the organobentonite that by concentration is 1～3.5 phr is added in the low viscosity epoxy resin of preparing in above-mentioned b step, is stirred to whole organobentonites and is immersed in epoxy resin-base material, forms epoxy resin-organobentonite mixture;
D. epoxy-organobentonite mixture of gained in above-mentioned c step is stirred;
E. epoxy resin-organobentonite the mixture after stirring in above-mentioned d step is carried out from degassed 6 hours under 45 degrees celsius;
F. according to part by weight, be the ZnO-ZrO that 1:2 takes respectively acetone and prepares in above-mentioned a
2nano metal oxide powder, by ZnO-ZrO
2nano metal oxide powder is added to acetone, carries out ultrasonic dispersion, the dispersion liquid of the nano metal oxide powder of formation, ZnO nano granule density and ZrO in dispersion liquid
2concentrations of nanoparticles is all 0.5～1.75phr, and wherein phr is ZnO nano grain fraction or ZrO
2the per-cent of nano particle component to the gross weight of epoxy resin and solidifying agent;
G. the low viscosity epoxy resin of preparing in above-mentioned b step is poured in the dispersion liquid of the nano metal oxide powder of preparing in above-mentioned f step and mixed, and stir, obtain by epoxy resin, organobentonite and ZnO-ZrO
2the matrix material mixture that nano-metal-oxide forms;
H. the matrix material mixture of preparing in above-mentioned g step is carried out from degassed in water-bath, autospasy temperature degree is controlled at 45 ℃, from the degassed time, keep 6 hours, then be placed in the vacuum environment lower than 0.1MPa, and place 2 hours under 45 ℃ of temperature condition;
I. solidifying agent is joined through in above-mentioned h step through from degassed and place after matrix material mixture in, be cooled to 25 ℃, solidify 72 hours, obtain epoxy resin-organobentonite-ZnO-ZrO
2metal oxide composite.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. to have technique simple for the preparation method of epoxy resin-organobentonite-metal oxide composite of the present invention, without specific installation, do not use levelling agent and defoamer composition, therefore greatly reduce cost prepared by material and there is good corrosion resistance nature, can realize large-scale production application;
2. preparation condition of the present invention is gentle, and reproducible, the epoxy coat material of preparing can be used for building material field.
Embodiment
Details are as follows for the preferred embodiments of the present invention:
embodiment mono-:
In the present embodiment, a kind of epoxy resin-organobentonite-metal oxide composite, is disperseed in epoxy resin-base material by organobentonite, metal oxide nanoparticles to be compounded to form, and is specially:
(1) matrix material constituents comprises epoxy resin, solidifying agent and silane coupling agent, wherein epoxide resin material is the epoxy resin of bisphenol A-type GCC135, be ethylene glycol bisthioglycolate propylene oxide ether, the outward appearance of epoxy resin is transparent liquid shape, machinery-free foreign material, oxirane value is 0.6 eq/100g, and viscosity is 1000 mPas, and density is 1.17 g/cm
3; Wherein solidifying agent is isophorone-low viscosity liquid solidifying agent of modification, and the outward appearance of solidifying agent is colourless extremely flaxen liquid, and amine value is 600mg KOH/g, and viscosity is 80 mPas, and epoxy resin mixes with the ratio of weight ratio 10:3 with solidifying agent; Wherein alkane coupling agent is 3-aminopropyl triethoxysilane, i.e. KH550;
(2) component of nano-complex comprises organobentonite and metal oxide nanoparticles, and wherein bentonite concentration is 1.5 phr; Wherein metal oxide component material is ZnO-ZrO
2the nano particle being mixed to form of two kinds of metal oxides, wherein ZnO nano granule density is 0.75phr, and the concentration of ZrO2 nano particle is 0.75 phr, and wherein phr is the per-cent of component to the gross weight of epoxy resin and solidifying agent.
The material mixture ratio of the present embodiment epoxy resin-organobentonite-metal oxide composite is as follows:
Epoxy resin, solidifying agent, 1.5 phr organobentonites, 0.75 phr ZnO nano particle and 0.75 phr ZrO
2nano particle.
The present embodiment epoxy resin-organobentonite-metal oxide composite preparation method comprise the steps:
The first step: respectively by 20g ZnO nano metal oxide powder and ZrO
2nano metal oxide powder was 120 ℃ of vacuum-dryings 12 hours;
Second step: dried powder is added in the mixing liquid of 80 ml dehydrated alcohols and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:1, and mechanical stirring is even, and stirring velocity is that 300 revs/min of times are 1 hour, then ultrasonic 30 minutes, obtain mixed solution;
The 3rd: after taking weight and be the 20wt% silane coupling agent of 4g and being added drop-wise in the mixing liquid of preparing at second step, continue to stir 12 hours;
The 4th: the mixing liquid after stirring in the 3rd step is carried out centrifugal, centrifugal speed I 8000 revs/min, 10 minutes time; Then the powder after using deionized water and dehydrated alcohol cleaning centrifugal, repeats 3 times.By powder 80 ℃ of vacuum-dryings 24 hours;
The 5th step: GCC135 type reacting epoxy resin is heated to 45 ℃ and obtains low viscosity epoxy resin;
The 6th step: the organobentonite that is 1.5phr by concentration is added in the low viscosity epoxy resin of preparing in the 5th step, is stirred to whole organobentonites and is immersed in epoxy resin-base material, forms epoxy resin-organobentonite mixture; Phr be organobentonite as component the per-cent to the gross weight of epoxy resin and solidifying agent;
The 7th step: epoxy-organobentonite mixture of gained in the 6th step is stirred, condition is followed successively by: mixing speed is 600 revs/min for the first time, churning time is 15 minutes for the first time, mixing speed is 1200 revs/min for the second time, churning time is 15 minutes for the second time, mixing speed is 2600 revs/min for the third time, churning time is 60 minutes for the third time, and the 4th mixing speed is that 300 revs/min, the 4th time churning time is 30 minutes;
The 8th step: the epoxy resin-organobentonite mixture after stirring in the 7th step is carried out from degassed under 45 ℃ of conditions, and the time is 6 hours;
The 9th step: be the ZnO-ZrO that 1:2 takes respectively acetone and prepares in above-mentioned a according to part by weight
2nano metal oxide powder, by ZnO-ZrO
2nano metal oxide powder is added to acetone, carries out ultrasonic dispersion, the dispersion liquid of the nano metal oxide powder of formation, ZnO nano granule density and ZrO in dispersion liquid
2concentrations of nanoparticles is all 0.75phr, and wherein phr is ZnO nano grain fraction or ZrO
2the per-cent of nano particle component to the gross weight of epoxy resin and solidifying agent;
The tenth step: the low viscosity epoxy resin of preparing in the 5th step is poured in the dispersion liquid of the nano metal oxide powder of preparing in the 9th step and mixed, and stir, obtain by epoxy resin, organobentonite and ZnO-ZrO
2the matrix material mixture that nano-metal-oxide forms, agitation condition is followed successively by: mixing speed is 900 revs/min for the first time, churning time keeps 15 minutes for the first time, mixing speed is 2000 revs/min for the second time, churning time keeps 60 minutes for the second time, and mixing speed is 300 revs/min for the third time, churning time keeps 30 minutes for the third time;
The 11 step: the matrix material mixture of preparing in the tenth step is carried out from degassed in water-bath, autospasy temperature degree is controlled at 45 ℃, from the degassed time, keep 6 hours, then be placed in the vacuum environment lower than 0.1MPa, and place 2 hours under 45 ℃ of temperature condition;
The 12 step: by W83 type solidifying agent join through in the 11 step through from degassed and place after matrix material mixture in, be cooled to 25 ℃, solidify 72 hours, obtain epoxy resin-organobentonite-ZnO-ZrO
2metal oxide composite.
The present embodiment provides a kind of cheap, high quality and integrity, has had a wide range of applications the preparation method of the epoxy coat of potentiality, wherein organobentonite, ZnO-ZrO2 nano-particle material are dispersed in epoxy resin liquid uniformly by mechanically mixing method, pass through again a series of stirring, interpolation and processing, finally obtain a kind of novel epoxy coat material, i.e. epoxy resin-organobentonite-ZnO-ZrO
2metal oxide composite.In preparation process, do not use levelling agent and defoamer, therefore further reduce cost prepared by material.
embodiment bis-:
The present embodiment and embodiment mono-are basic identical, and special feature is:
In the present embodiment, the material mixture ratio of epoxy resin-organobentonite-metal oxide composite is as follows:
Epoxy resin, solidifying agent, 2.5 phr organobentonites, 1.25 phr ZnO nano particles and 1.25 phr ZrO
2nano particle.
The present embodiment epoxy resin-organobentonite-metal oxide composite preparation method comprise the steps:
The first step: identical with embodiment mono-;
Second step: identical with embodiment mono-;
The 3rd: identical with embodiment mono-;
The 4th: identical with embodiment mono-;
The 5th step: identical with embodiment mono-;
The 6th step: the organobentonite that is 2.5phr by concentration is added in the low viscosity epoxy resin of preparing in the 5th step, is stirred to whole organobentonites and is immersed in epoxy resin-base material, forms epoxy resin-organobentonite mixture; Phr be organobentonite as component the per-cent to the gross weight of epoxy resin and solidifying agent;
The 7th step: identical with embodiment mono-;
The 8th step: identical with embodiment mono-;
The 9th step: be the ZnO-ZrO that 1:2 takes respectively acetone and prepares in above-mentioned a according to part by weight
2nano metal oxide powder, by ZnO-ZrO
2nano metal oxide powder is added to acetone, carries out ultrasonic dispersion, the dispersion liquid of the nano metal oxide powder of formation, ZnO nano granule density and ZrO in dispersion liquid
2concentrations of nanoparticles is all 1.25phr, and wherein phr is ZnO nano grain fraction or ZrO
2the per-cent of nano particle component to the gross weight of epoxy resin and solidifying agent;
The tenth step: identical with embodiment mono-;
The 11 step: identical with embodiment mono-;
The 12 step: identical with embodiment mono-.
testing of materials:
Testing of materials result to the epoxy resin-organobentonite-metal oxide composite of the embodiment of the present invention one and embodiment bis-preparations is as follows:
The physics of nano composite material prepared by table 1 the present invention, mechanical experimental results
| Physicals | Embodiment mono- | Embodiment bis- |
| Density (g/cm 3) | 1.16~1.18 | 1.17~1.19 |
| Rate of weight loss is in drying process 80 0C/24 hour (%) | 0.21 | 0.17 |
| In artificial seawater, soak rate of weight loss (%) after 28 days | 0.88 | 0.85 |
| HV | 149 | 168 |
| Sticking power grade (GB/T9286-98) | 0 | 0 |
The corrosive nature test result of nano composite material prepared by table 2 the present invention
| Corrosive nature (soaking in artificial seawater after 91 days) | Embodiment mono- | Embodiment bis- |
| Corrosion potential (V) | -0.628 | -0.619 |
| Corrosion electric current density (A/cm 2） | 4.007x10 -9 | 3.734x10 -9 |
| Corrosion speed (gr/h) | 4.175 x10 -9 | 3.945 x10 -9 |
By the above-mentioned testing of materials result to the epoxy resin-organobentonite-metal oxide composite of the embodiment of the present invention one and embodiment bis-preparations, prove, the nano composite material of utilizing the technology of the present invention to prepare, there is very high hardness and specific tenacity, and raw materials cost is cheap, is applicable to marine traffic engineering and produces and apply.
The invention is not restricted to above-described embodiment; can also make multiple variation according to the object of innovation and creation of the present invention; the change of making under all spirit according to technical solution of the present invention and principle, modification, substitute, combination, simplify; all should be equivalent substitute mode; as long as goal of the invention according to the invention; only otherwise deviate from know-why and the inventive concept of epoxy resin-organobentonite-metal oxide composite of the present invention and preparation method thereof, all belong to protection scope of the present invention.
Claims (3)
1. epoxy resin-organobentonite-metal oxide composite, is characterized in that, is disperseed to be compounded to form by organobentonite, metal oxide nanoparticles in epoxy resin-base material, is specially:
(1) matrix material constituents comprises epoxy resin, solidifying agent and silane coupling agent, wherein epoxide resin material is the epoxy resin of bisphenol A-type GCC135, be ethylene glycol bisthioglycolate propylene oxide ether, the outward appearance of epoxy resin is transparent liquid shape, machinery-free foreign material, oxirane value is 0.54-0.6 eq/100g, and viscosity is 700-1100 mPas, and density is 1.13-1.17 g/cm
3; Wherein solidifying agent is isophorone-low viscosity liquid solidifying agent of modification, the outward appearance of solidifying agent is colourless to flaxen liquid, amine value is 550-600mg KOH/g, and viscosity is 10-100 mPas, and epoxy resin mixes with the ratio of weight ratio 10:3 with solidifying agent; Wherein alkane coupling agent is 3-aminopropyl triethoxysilane, i.e. KH550;
(2) component of nano-complex comprises organobentonite and metal oxide nanoparticles, and wherein bentonite concentration is 1～3.5 phr; Wherein metal oxide component material is ZnO-ZrO
2the nano particle being mixed to form of two kinds of metal oxides, wherein ZnO nano granule density is 0.5～1.75phr, and the concentration of ZrO2 nano particle is 0.5～1.75 phr, and wherein phr is the per-cent of component to the gross weight of epoxy resin and solidifying agent.
2. a preparation method for epoxy resin-organobentonite-metal oxide composite claimed in claim 1, is characterized in that: organobentonite, ZnO-ZrO
2nano-particle material is dispersed in epoxy resin liquid uniformly by mechanically mixing method, and add stiffening agent in preparation process before, mixture carries out from degassed at least 6 hours under more than 45 degrees Celsius temperature condition.
3. the preparation method of epoxy resin-organobentonite-metal oxide composite according to claim 2, is characterized in that, comprises the steps:
A. according to two kinds of metal oxide part by weight, be 1:1 making ZnO-ZrO
2nano metal oxide powder;
B. GCC135 type reacting epoxy resin is heated to 45 ℃ and obtains low viscosity epoxy resin;
C. the organobentonite that by concentration is 1～3.5 phr is added in the low viscosity epoxy resin of preparing in above-mentioned b step, is stirred to whole organobentonites and is immersed in epoxy resin-base material, forms epoxy resin-organobentonite mixture;
D. epoxy-organobentonite mixture of gained in above-mentioned c step is stirred;
E. epoxy resin-organobentonite the mixture after stirring in above-mentioned d step is carried out from degassed 6 hours under 45 ℃ of conditions;
F. according to part by weight, be the ZnO-ZrO that 1:2 takes respectively acetone and prepares in above-mentioned a
2nano metal oxide powder, by ZnO-ZrO
2nano metal oxide powder is added to acetone, carries out ultrasonic dispersion, the dispersion liquid of the nano metal oxide powder of formation, ZnO nano granule density and ZrO in dispersion liquid
2concentrations of nanoparticles is all 0.5～1.75phr, and wherein phr is ZnO nano grain fraction or ZrO
2the per-cent of nano particle component to the gross weight of epoxy resin and solidifying agent;
G. the low viscosity epoxy resin of preparing in above-mentioned b step is poured in the dispersion liquid of the nano metal oxide powder of preparing in above-mentioned f step and mixed, and stir, obtain by epoxy resin, organobentonite and ZnO-ZrO
2the matrix material mixture that nano-metal-oxide forms;
H. the matrix material mixture of preparing in above-mentioned g step is carried out from degassed in water-bath, autospasy temperature degree is controlled at 45 ℃, from the degassed time, keep 6 hours, then be placed in the vacuum environment lower than 0.1MPa, and place 2 hours under 45 ℃ of temperature condition;
I. solidifying agent is joined through in above-mentioned h step through from degassed and place after matrix material mixture in, be cooled to 25 ℃, solidify 72 hours, obtain epoxy resin-organobentonite-ZnO-ZrO
2metal oxide composite.
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| JP2007186682A (en) * | 2005-12-12 | 2007-07-26 | Dainippon Ink & Chem Inc | Water-based coating composition, organic-inorganic composite coating film and method for producing the same |
| CN101805554A (en) * | 2009-02-16 | 2010-08-18 | 中国科学院金属研究所 | Boron phenolics-titanium nano composite temperature and pressure resistant heavy anti-corrosive coating and preparation method thereof |
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