CN103113712A - Preparation method and application of modified nano-silicon dioxide toughened epoxy resin - Google Patents
Preparation method and application of modified nano-silicon dioxide toughened epoxy resin Download PDFInfo
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- CN103113712A CN103113712A CN2013100431192A CN201310043119A CN103113712A CN 103113712 A CN103113712 A CN 103113712A CN 2013100431192 A CN2013100431192 A CN 2013100431192A CN 201310043119 A CN201310043119 A CN 201310043119A CN 103113712 A CN103113712 A CN 103113712A
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Abstract
The invention relates to a preparation method of modified nano-silicon dioxide toughened epoxy resin; the preparation method comprises the following steps of: (1), adding 1-2g of amino silane coupling agent into 48-50g of absolute ethyl alcohol firstly, adding glacial acetic acid to adjust the pH (potential of hydrogen) value to be 3-4, shaking by ultrasonic wave in order to fully dissolve the amino silane coupling agent into the absolute ethyl alcohol; (2), putting 5-6g of nano-SiO2 into a flask, pouring 20-30g of the solution obtained in step (1), dispersing by ultrasonic wave for 30min, stirring for 3-5 hours at the constant temperature of 75 DEG C at the stirring speed of 450rpm, cooling, centrifugally separating, and drying for 24 hours at 140 DEG C, so as to obtain modified nano-silicon dioxide; and (3), adding 50-150g of liquid epoxy resin into a reaction container, heating to 60 DEG C, slowly adding 0.1-1% by weight of liquid epoxy resin of modified nano-silicon dioxide prepared by step (2) while stirring, after adding, stirring uniformly, dispersing by high-speed shearing, heating to 90 DEG C within 1 hour, and then reacting for 3-5 hours at a constant temperature, cooling, finally the product is obtained. The resin prepared by the preparation method is stable in property, and the property of the prepared coating is greatly improved.
Description
Technical field
The present invention relates to a kind of preparation method of epoxy resin, the preparation method who specifically relates to the epoxy resin toughened and environment-friendly type protective coating of a kind of modified manometer silicon dioxide chemistry, the environment-friendly type coating that prepare production by this method can be widely used in the anticorrosive coating of steel construction.
Background technology
Epoxy resin has excellent performance, and is strong such as cohesive force, processibility good and shrinking percentage is little etc., is one of maximum thermosetting resin of application at present.But epoxy resin, the low low-molecular-weight epoxy resin of viscosity particularly, there is a large amount of epoxide groups in molecule, during curing, cross-linking density is very large, property is very crisp, fatigue strength and impelling strength poorer, and thermotolerance, stripping strength are especially poor, have influence on sticking power and the antiseptic property of epoxy coat, are difficult to satisfy the demand for development of modern industrial technology.Therefore, need to carry out toughening modifying to epoxy resin and improve its excellent performance, but when improving epoxy resin toughness, tend to reduce the mechanical modulus of cured article and thermotolerance etc.
Along with the development of nanotechnology, nano material has obtained studying widely and using, and its application in coating is also more and more.Small-size effect, surface-interface effect, quantum size effect and macro quanta tunnel effect and its special light electrical characteristic, high Magnetoresistance Phenomena, the non-linear resistance phenomenon that nano material does not possess with its unique physics, chemical property and conventional material and at high temperature still have the characteristics such as high-strength, high-ductility, excellent stability, increase substantially the coatingsurface toughness of coating products and hardness, water-wash resistance, sticking power, smooth finish, resistance to deterioration, also had wear resistance and excellent resistance to chemical corrosion.Nano particle as toughner, is a kind of novel method that nanocomposite applications is expanded.Improve the epoxy-resin systems internal structure by the modification to the nano material functionalization, and then the method for lifting coating overall performance has also obtained approval widely.
Chinese patent CN 102190858 A disclose a kind of by toughness reinforcing epoxide resin material of nano silicon and preparation method thereof.The method is with dendritic macromole Grafted Nano-scale silicon-dioxide, then take epoxy resin as base-material, nano silicon toughner and solidifying agent is added to wherein, and then obtains nanometer toughening-modifiedepoxy resin material.The prepared epoxide resin material toughness of this invention has obtained certain raising.But described in invention and dendritic macromole (Changchun should change produce) be special, can not buy from the market.So, in the present invention, will adopt the amino silane coupler modified nano silicon of band, so Toughening Modification of Epoxy, add reactive thinner, defoamer and solidifying agent, make the environment-friendly type solvent-free epoxy coating, be used for the toughness reinforcing anticorrosion of steel construction.The solvent-free environment-protection epoxy coating that utilizes the present invention to make with greatly improving the impact of coating on environment, reaches the VOC zero release, improves the performance of the each side of filming.
Summary of the invention
For the shortcoming and deficiency that overcomes prior art, the objective of the invention is nano material technology is combined with the epoxy resin roughening technology, adopt a kind of new modified method, at first modified manometer silicon dioxide, and then carry out chemical bonding with nano material and the low-molecular-weight liquid epoxies of modification.In existing Toughening Epoxy Resin, toughness strengthens and the technical barrier of the excellent properties reduction of epoxy resin own thereby overcome.
For achieving the above object, the technical solution used in the present invention step is as follows:
(1) at first get 1g～2g amino silicane coupling agent and join 48g～50g dehydrated alcohol, then add between Glacial acetic acid adjusting pH value to 3～4, ultrasonic oscillation 10min～20 min make it be dissolved in dehydrated alcohol fully;
(2) take 5g～6g nanometer SiO
2Put into there-necked flask, pour scattered ethanol solution in 20g～30g step (1) into, ultra-sonic dispersion 30min, then put into thermostat water bath, under the stirring velocity of 450r/min, 75 ℃ of stirrings of constant temperature 3～5 hours, cooling afterwards, centrifugation, 140 ℃ of dry 24h obtain the modified manometer silicon dioxide powder;
(3) 50g～150g liquid epoxies is joined in reaction vessel, load onto the electrodynamictype homogenizer, be heated to 60 ℃, slowly add the modified manometer silicon dioxide that is made by step (2) that is equivalent to liquid epoxies weight 0.1%～1% under whipped state, after adding, stir, under the high speed shear dispersion condition, be heated to 90 ℃ in 1 hour, then isothermal reaction 3～5 hours.After remove heating installation, stir cooling after, products therefrom is exactly the toughness reinforcing epoxy resin product of modified manometer silicon dioxide.
As further measure of the present invention, preparation solvent-free environment-protection epoxy coating comprises the following steps:
By mass percentage, the improved silica that makes is epoxy resin toughened: the polypropylene glycol diglycidyl ether reactive thinner: defoamer=50～60%:15～20%:0.1～0.6% mixes under the middling speed agitation condition, and is standby.Add the epoxy hardener of mass percent 25～28% before brushing, after the short mix slaking, brush immediately at pretreated steel structure surface in above-mentioned material, controlling the sealing bottom coating layer thickness is (30 ± 5) μ m.
By the enforcement of technique scheme, made the solvent-free environment-protection epoxypaint, make the snappiness of epoxy resin be greatly improved, and other performances of epoxy resin are well kept.
Compared with prior art, in the present invention, the reaction through silane coupling agent and nano silicon makes silane coupling agent by chemical bond and nano silicon grafting, obtains modified manometer silicon dioxide.End is amino owing to containing in silane coupling agent, and then can reach the purpose with the epoxy resin ring-opening reaction, prepares the toughness reinforcing epoxy resin of modified manometer silicon dioxide.This resin property is stable, and the coating property of preparing is greatly improved.
Embodiment
The present invention is further detailed explanation below in conjunction with embodiment, but the present invention never is limited to these embodiment.
Embodiment 1
(1) preparation of modified manometer silicon dioxide
At first get 1gKH-550 and join the 48g dehydrated alcohol, then adding Glacial acetic acid, to regulate the pH value be 3.5, ultrasonic oscillation 10min is dissolved in dehydrated alcohol it fully.
Take 5g nanometer SiO
2, put into there-necked flask, pour the ethanol solution of the scattered KH-550 of 20g into, ultra-sonic dispersion 30min, then put into thermostat water bath, and under the stirring velocity of 450r/min, 75 ℃ of stirrings of constant temperature 3.5 hours.Cooling afterwards, centrifugation, 140 ℃ of dry 24h obtain the modified manometer silicon dioxide powder.
(2) the epoxy resin toughened preparation of modified manometer silicon dioxide
The 100g liquid epoxies is joined in reaction vessel, load onto the electrodynamictype homogenizer, be heated to 60 ℃, the modified manometer silicon dioxide that adds 0.1g under whipped state will slowly add, after adding, stir, under the high speed shear dispersion condition, be heated to 90 ℃ in 1 hour, then isothermal reaction 4 hours.After remove heating installation, stir cooling after, products therefrom is exactly the toughness reinforcing epoxy resin product of modified manometer silicon dioxide.
With 56.8g modified epoxy, 16.1g polypropylene glycol diglycidyl ether and 0.3g defoamer (BYK-141, the production of Germany BYK company) mix under the middling speed agitation condition, after a while with 26.8g solidifying agent (NX-2007, U.S. Ka Delai company produces) add and the short mix slaking after, brush immediately at pretreated steel structure surface, filming of making has following performance:
Shock resistance/cm:50
Snappiness/mm:1
Coating hardness: H
Sticking power/Mpa: 〉=12A/B
Salt fog resistance/h: 〉=800.
Embodiment 2
(1) preparation of modified manometer silicon dioxide
At first get 1.5gKH-550 and join the 49g dehydrated alcohol, then adding Glacial acetic acid, to regulate the pH value be 4, ultrasonic oscillation 15min is dissolved in dehydrated alcohol it fully.
Take 5.5g nanometer SiO
2, put into there-necked flask, pour the ethanol solution of the scattered KH-550 of 25g into, ultra-sonic dispersion 30min, then put into thermostat water bath, and under the stirring velocity of 450r/min, 75 ℃ of stirrings of constant temperature 4 hours.Cooling afterwards, centrifugation, 140 ℃ of dry 24h obtain the modified manometer silicon dioxide powder.
(2) the epoxy resin toughened preparation of modified manometer silicon dioxide
The 100g liquid epoxies is joined in reaction vessel, load onto the electrodynamictype homogenizer, be heated to 60 ℃, add 0.5g(by the amount of epoxy resin under whipped state) modified manometer silicon dioxide, slowly add, after adding, stir, under the high speed shear dispersion condition, be heated to 90 ℃ in 1 hour, then isothermal reaction 4 hours.After remove heating installation, stir cooling after, products therefrom is exactly the toughness reinforcing epoxy resin product of modified manometer silicon dioxide.
With 55.8g modified epoxy, 17.2g polypropylene glycol diglycidyl ether and 0.4g defoamer (BYK-141, the production of Germany BYK company) mix under the middling speed agitation condition, after a while with 26.6g solidifying agent (NX-2007, U.S. Ka Delai company produces) add and the short mix slaking after, brush immediately at pretreated steel structure surface, filming of making has following performance:
Shock resistance/cm:50
Snappiness/mm:1
Coating hardness: H
Sticking power/Mpa: 〉=12A/B
Salt fog resistance/h: 〉=800
Embodiment 3
(1) preparation of modified manometer silicon dioxide
At first get 2gKH-550 and join the 50g dehydrated alcohol, then adding Glacial acetic acid, to regulate the pH value be 3.6, ultrasonic oscillation 20 min are dissolved in dehydrated alcohol it fully.
Take 6g nanometer SiO
2, put into there-necked flask, pour the ethanol solution of the scattered KH-550 of 30g into, ultra-sonic dispersion 30min, then put into thermostat water bath, and under the stirring velocity of 450r/min, 75 ℃ of stirrings of constant temperature 4.5 hours.Cooling afterwards, centrifugation, 140 ℃ of dry 24h obtain the modified manometer silicon dioxide powder.
(2) the epoxy resin toughened preparation of modified manometer silicon dioxide
The 100g liquid epoxies is joined in reaction vessel, load onto the electrodynamictype homogenizer, be heated to 60 ℃, add 1g(by the amount of epoxy resin under whipped state) modified manometer silicon dioxide, slowly add, after adding, stir, under the high speed shear dispersion condition, be heated to 90 ℃ in 1 hour, then isothermal reaction 5 hours.After remove heating installation, stir cooling after, products therefrom is exactly the toughness reinforcing epoxy resin product of modified manometer silicon dioxide.
With 54.8g modified epoxy, 19.1g polypropylene glycol diglycidyl ether and 0.5g defoamer (BYK-141, the production of Germany BYK company) mix under the middling speed agitation condition, after a while with 25.6g solidifying agent (NX-2007, U.S. Ka Delai company produces) add and the short mix slaking after, brush immediately at pretreated steel structure surface, filming of making has following performance:
Shock resistance/cm:50
Snappiness/mm:1
Coating hardness: H
Sticking power/Mpa: 〉=12A/B
Salt fog resistance/h: 〉=800.
The examples of implementation of the above only are the present invention's preferred embodiment, are not to limit practical range of the present invention with this, therefore the variation that all shapes according to the present invention, principle are done all should be encompassed in protection scope of the present invention.
Claims (2)
1. preparation method that modified manometer silicon dioxide is epoxy resin toughened, it is characterized in that: concrete steps are
(1) at first get 1g～2g amino silicane coupling agent and join 48g～50g dehydrated alcohol, then add between Glacial acetic acid adjusting pH value to 3～4, ultrasonic oscillation 10min～20 min make it be dissolved in dehydrated alcohol fully;
(2) take 5g～6g nanometer SiO
2Put into there-necked flask, pour scattered ethanol solution in 20g～30g step (1) into, ultra-sonic dispersion 30min, then put into thermostat water bath, under the stirring velocity of 450r/min, 75 ℃ of stirrings of constant temperature 3～5 hours, cooling afterwards, centrifugation, 140 ℃ of dry 24h obtain the modified manometer silicon dioxide powder;
(3) 50g～150g liquid epoxies is joined in reaction vessel, load onto the electrodynamictype homogenizer, be heated to 60 ℃, slowly add the modified manometer silicon dioxide that is made by step (2) that is equivalent to liquid epoxies weight 0.1%～1% under whipped state, after adding, stir, under the high speed shear dispersion condition, be heated to 90 ℃ in 1 hour, isothermal reaction is 3～5 hours again, after remove heating installation, stir cooling after, products therefrom is exactly the toughness reinforcing epoxy resin product of modified manometer silicon dioxide.
2. the application of the epoxy resin that makes of a method according to claim 1, it is characterized in that: with its preparation solvent-free environment-protection epoxy coating, comprise the following steps: by mass percentage, the improved silica that makes is epoxy resin toughened: the polypropylene glycol diglycidyl ether reactive thinner: defoamer=50～60%:15～20%:0.1～0.6% mixes under the middling speed agitation condition, and is standby; Add the epoxy hardener of mass percent 25～28% before brushing, after the short mix slaking, brush immediately at pretreated steel structure surface in above-mentioned material, controlling the sealing bottom coating layer thickness is 30 ± 5 μ m.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530647A (en) * | 2014-12-25 | 2015-04-22 | 太原理工大学 | Method for preparing epoxy resin/nanometer silicon oxide composite material by centrifugation-assisted method |
| CN105400475A (en) * | 2015-12-21 | 2016-03-16 | 广东工业大学 | Preparation method of leak repairing filling glue and house leak repairing method by using the filling glue |
| CN107722792A (en) * | 2017-11-13 | 2018-02-23 | 吉林大学 | A kind of preparation method with high anticorrosive property energy epoxy coating |
| CN108300111A (en) * | 2016-08-16 | 2018-07-20 | 洛阳尖端技术研究院 | A kind of water paint and preparation method thereof |
| CN109274027A (en) * | 2018-09-30 | 2019-01-25 | 浙江奔月电气科技有限公司 | A kind of switchgear sliding rail and its production technology |
| CN109439170A (en) * | 2018-11-26 | 2019-03-08 | 蚌埠星烁新材料科技有限公司 | A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable- |
| CN109825036A (en) * | 2019-02-15 | 2019-05-31 | 安庆市虹泰新材料有限责任公司 | A kind of modified epoxy and preparation method thereof |
| CN110227349A (en) * | 2019-06-12 | 2019-09-13 | 常州大学 | Based on the nano-silicon dioxide modified blended ultrafiltration membrane and preparation method thereof of functionalization sodium base bentonite and amination |
| CN110845937A (en) * | 2019-11-25 | 2020-02-28 | 成都普瑞斯特新材料有限公司 | Solvent-free pipeline inner wall anticorrosion hydrophobic coating and preparation method thereof |
| CN113045940A (en) * | 2021-03-24 | 2021-06-29 | 天津德普威涂料有限公司 | Emulsion paint for external wall and preparation method thereof |
| CN113387352A (en) * | 2021-07-02 | 2021-09-14 | 西安交通大学 | Easily-dispersible modified graphene oxide and preparation method thereof |
| CN115536601A (en) * | 2022-10-14 | 2022-12-30 | 重庆交通大学 | Curing agent capable of resisting flame, strengthening and toughening epoxy resin, epoxy resin material and application |
| CN116178744A (en) * | 2023-03-09 | 2023-05-30 | 广州豫顺新材料有限公司 | Preparation process of functionalized silica toughening agent applied to epoxy resin |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104530647A (en) * | 2014-12-25 | 2015-04-22 | 太原理工大学 | Method for preparing epoxy resin/nanometer silicon oxide composite material by centrifugation-assisted method |
| CN105400475A (en) * | 2015-12-21 | 2016-03-16 | 广东工业大学 | Preparation method of leak repairing filling glue and house leak repairing method by using the filling glue |
| CN105400475B (en) * | 2015-12-21 | 2019-05-24 | 广东工业大学 | The method that leak repairing fills the preparation method of glue and carries out house leak repairing using it |
| CN108300111A (en) * | 2016-08-16 | 2018-07-20 | 洛阳尖端技术研究院 | A kind of water paint and preparation method thereof |
| CN107722792A (en) * | 2017-11-13 | 2018-02-23 | 吉林大学 | A kind of preparation method with high anticorrosive property energy epoxy coating |
| CN109274027A (en) * | 2018-09-30 | 2019-01-25 | 浙江奔月电气科技有限公司 | A kind of switchgear sliding rail and its production technology |
| CN109439170A (en) * | 2018-11-26 | 2019-03-08 | 蚌埠星烁新材料科技有限公司 | A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable- |
| CN109825036A (en) * | 2019-02-15 | 2019-05-31 | 安庆市虹泰新材料有限责任公司 | A kind of modified epoxy and preparation method thereof |
| CN110227349A (en) * | 2019-06-12 | 2019-09-13 | 常州大学 | Based on the nano-silicon dioxide modified blended ultrafiltration membrane and preparation method thereof of functionalization sodium base bentonite and amination |
| CN110845937A (en) * | 2019-11-25 | 2020-02-28 | 成都普瑞斯特新材料有限公司 | Solvent-free pipeline inner wall anticorrosion hydrophobic coating and preparation method thereof |
| CN113045940A (en) * | 2021-03-24 | 2021-06-29 | 天津德普威涂料有限公司 | Emulsion paint for external wall and preparation method thereof |
| CN113045940B (en) * | 2021-03-24 | 2022-04-08 | 天津德普威涂料有限公司 | Emulsion paint for external wall and preparation method thereof |
| CN113387352A (en) * | 2021-07-02 | 2021-09-14 | 西安交通大学 | Easily-dispersible modified graphene oxide and preparation method thereof |
| CN113387352B (en) * | 2021-07-02 | 2022-07-12 | 西安交通大学 | Easily-dispersible modified graphene oxide and preparation method thereof |
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| CN116178744B (en) * | 2023-03-09 | 2023-09-15 | 广州豫顺新材料有限公司 | Preparation process of functionalized silica toughening agent applied to epoxy resin |
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