CN101368059A - Process for producing solvent-free epoxy matte paint for gravity flow flat ground - Google Patents

Process for producing solvent-free epoxy matte paint for gravity flow flat ground Download PDF

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CN101368059A
CN101368059A CNA2008101247985A CN200810124798A CN101368059A CN 101368059 A CN101368059 A CN 101368059A CN A2008101247985 A CNA2008101247985 A CN A2008101247985A CN 200810124798 A CN200810124798 A CN 200810124798A CN 101368059 A CN101368059 A CN 101368059A
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preparation
epoxy
drop
small molecules
component
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CN101368059B (en
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许彩奎
钱旭锋
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WUXI NANYA CHEMICALS CO Ltd
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WUXI NANYA CHEMICALS CO Ltd
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Abstract

The invention discloses a method for preparing solventless epoxy matt self-leveling floor paint, which comprises preparation of epoxy component and preparation of curing agent component. The method combines a physical photoextinction method with a chemical method. The physical photoextinction method is to eliminate light by adding photoextinction wax; the chemical method adopts three epoxy curing agents to manufacture single-phase curing agent through a series of complicated reactions; when the single-phase curing agent is combined with the epoxide resin, the matt effect can be reproduced well. In addition, the luster can be reproduced well through simulated construction at a series of different temperatures in different humid environments.

Description

A kind of preparation method of solvent-free epoxy matte paint for gravity flow flat ground
Technical field
The present invention relates to a kind of preparation method of coating, belong to and decorate the protection field of coating, specifically is a kind of preparation method of solvent-free epoxy matte paint for gravity flow flat ground.
Background technology
Modern industrialization is produced, and requires that the mill floor cleaning is dustless, protection against corrosion, abrasion performance.The terrace paint that is used for industrial plant at present; general epoxies commonly used and polyurethanes coating; and solvent-free epoxy self-leveling coating becomes the first-selection of industrial plant terrace paint gradually owing to have characteristics such as excellent application property, one-pass film-forming are thick, levelling property, snappiness, shock-resistance, resistant to chemical media corrosion; and progressively raising along with environmental consciousness and labour protection consciousness; the range of application of non-solvent epoxy terrace is constantly expanded, and is increasingly extensive in manufacturing shop applications such as medicine, health, food, tobacco, electronics, locomotive, biologies.
After the solvent-free epoxy self-leveling coating application film forming, generally have higher gloss, planeness, paint film fullness ratio height.At present domestic non-solvent epoxy terrace is all with light or Gao Guangwei master, and this just causes in terrace uses, all the problem that has light pollution in various degree; And if adopt mute light ground, can make then integrally that face and space present soft simple and elegant atmosphere, greatly reduce because light stimulates staff's the eye strain degree in this environment that causes.In recent years, the mute light type solvent-free epoxy self-leveling coating of exploitation becomes industry focus gradually, requirement reduces surface luster under the physical and chemical performance prerequisite that keeps light type coating, become the direction of all kinds of terrace paint manufacturer research and development of products to reach reduction " light pollution ".But because non-solvent epoxy terrace paint one-pass film-forming is at 200-300um, the unit surface consumption is about 0.8-1.0kg, its surface drying is slow, paint film is thicker, levelling requires high, and the surface is difficult to form mute light effect, so how to reduce gloss, making light pollution be reduced to eyesight can acceptance level, becomes the non-solvent epoxy terrace and studies new problem.
Summary of the invention
The objective of the invention is provides a kind of low production cost in order to overcome above-mentioned technical problem, and reproducibility is good, and can realize the preparation method of the solvent-free epoxy matte paint for gravity flow flat ground of industrialization.
The preparation method of solvent-free epoxy matte paint for gravity flow flat ground of the present invention comprises the preparation of epoxy component and preparation two portions of solidifying agent component, and preparation process is as follows: (following content is weight ratio)
1) preparation of epoxy component: the small molecules bisphenol A epoxide resin, the reactive thinner of 5.7-8.0% and 1.1-1.6% the surperficial auxiliary agent that in Scattered Kettle, drop into 35-45%, begin to stir evenly, starting input 2.5-22.7% pigment under the stirring state, the delustring wax powder of 0-2% reaches 10.0-17.5% process white and 21.7-29.2% silicon powder as filler; Behind the high speed dispersion 45min, call in three-roller and be ground to fineness≤30um to call in the paint still standby;
2) preparation of solidifying agent component: in having the porous reaction still of vacuum apparatus and condensing equipment, drop into 16.3% polymeric amide, slowly be warming up to 80 ℃, drop into 65% aliphatic cyclic amine, behind the insulation 15min, add 9.9% small molecules aliphatic amide, behind the insulation 15-20min, drop into the small molecules bisphenol A epoxide resin of formula ratio 7.6%, drip 0.7% catalyzer, Whitfield's ointment and 0.5% Virahol isothermal reaction 4-4.5 hour, open vacuum and detach excessive small molecules aliphatic amide, sampling and measuring ammonia value, ammonia value scope is 350 ± 10, be cooled to 40 ℃ after qualified, filter and package.
During construction, press the epoxy component: solidifying agent component=100: formula rate (21.0-25.5), epoxy component and curing agent component are stirred, leave standstill after froth breaking 5-10 minute and get final product application.
Above-mentioned steps 1) reactive thinner is a glycidyl allyl ether.The surface auxiliary agent comprises the dispersion agent of 0.3-0.5%, the defoamer of 0.35-0.5%, the flow agent of 0.45-0.6%.
The composition of solvent-free epoxy matte paint for gravity flow flat ground and analysis:
1.1 main film forming substance
At present, what extensively adopt is the bisphenol A type epoxy resin of low viscosity small molecular weight, bisphenol f type epoxy resin, aliphatic epoxy resin, the addition-crosslinked curing of bisphenol A type epoxy resin and solidifying agent back coating hydroxyl is few, and effectively cross-linking density is big, non-corrosibility medium osmosis ability is strong, water-fast and chemical proofing is excellent, after through the performance screening, this product is selected small molecules bisphenol-A epoxy SM828 (three wooden companies) product for use.
1.2 selecting for use of amine hardener
Amine hardener kind commonly used at present is more, as aliphatic amide, and aliphatic cyclic amine, polymeric amide and affixture thereof, aliphatic cyclic amine and affixture thereof etc., aliphatic cyclic amine and addition thereof are looked for shallow, good leveling property, the gloss height does not whiten, and does not need inductive phase, but its second-order transition temperature is higher, paint film fragility is big, and polymeric amide and epoxy intermiscibility are bad, and slaking is insufficient before the construction a fuel-displaced phenomenon of turning white.Optimized the compatibility of polymeric amide and epoxy and combined aliphatic cyclic amine and the excellent specific property of small molecules aliphatic amide, after composite, can form evenly smooth mute lac varnish film with the epoxy component.
2, reactive thinner
Thinner can dissolving resin solvent, main effect is to reduce resin liquid viscosity, and reactive thinner has epoxy group(ing), and is non-volatile, can participate in the curing reaction of Resins, epoxy, it is reactive thinner that the present invention has selected low viscous product glycidyl allyl ether (AGE) for use.
3.1 the selection of color stuffing
The viscosity of solvent-free terrace coating directly influences workability, because solid part is high, the requirement of color stuffing is also pointed.The pigment choice criteria, low oil absorption ferric, high covering power, unreactiveness and pH value neutrality, according to the singularity of this type of coating, the pigment that the present invention selects for use mainly is mineral dye, as Rutile type Titanium Dioxide, chromoxide green, filler is selected process white and silicon powder for use.
3.2 selecting for use of delustring wax powder
What the wax powder was selected for use is that a kind of special modified Poly Propylene Wax powder that outstanding chemical industry provides is encircled in Shanghai, and it has low oil number, and high extinction effect in order to the adjusting gloss of film, and has the anti-heavy effect that improves wear resistance that reaches.
4, auxiliary agent selects for use
Solvent-free epoxy matte paint for gravity flow flat ground is had relatively high expectations to the levelling property of filming, in case particularly under the situation that film forming is thicker, should make the abundant levelling before surface drying of filming, require in the wet film bubble to discharge rapidly again and the surface does not stay defective, therefore auxiliary agents such as levelling, froth breaking select for use and consumption control is The key factor very, various pigment, filler must pass through dispersion grinding in the coating, are the assurance fineness, improve dispersion efficiency, also will add dispersion agent.The adding of all auxiliary agents all is with the application property that improves epoxy matte paint for gravity flow flat ground and to improve film performance be purpose.
4.1 dispersion agent
The ideal dispersion agent should have wetting viscosity reduction, dispersion, anti-loose colour, anti-effect such as grow dim, and can also promote levelling to prevent effects such as filler precipitation, and through the contrast screening, the present invention has selected for use the BYK-161 of German BYK company as dispersion agent.
4.2 flow agent
Because solvent-free matte paint for gravity flow flat ground does not contain volatile solvent, dope viscosity is higher, and surface tension is big, and levelling property is not good, film and be prone to withered skin, brush mark, wrinkle, contract and also also wait surface imperfection with pin, through experiment screening, it is leveling auxiliary agent that the present invention selects BYK-354 for use.
4.3 defoamer
Solvent-free epoxy matte paint for gravity flow flat ground contains the multiple surface-active material that has, and is easy to generate bubble in producing, constructing, and there are a lot of holes in the cement based surface, and air is cemented out by coating in the space, thereby produces bubble.Through experiment screening, proper defoamer is selected BYK-A530 for use.
The present invention combines physical method delustring means and chemical process, and wherein physical method promptly reaches extinction effect by adding delustring wax; Chemical process then is to have adopted three kinds of dissimilar epoxy hardeners, behind the process chemical reaction of a series of complexity, make a kind of single-phase solidifying agent, in composite with Resins, epoxy, mute light effect circulation ratio is splendid, and by a series of differing tempss, the construction simulation under the humidity environment, the gloss circulation ratio is good.
Performance index of the present invention are:
1, paint outward appearance: thick liquid of all kinds
2, pot-life: 〉=1h
3, surface drying≤4h
Do solid work≤24h
4, hardness 〉=2H
5, ultimate compression strength 〉=80MPa
6, cohesive strength 〉=2MPa
7, anti-3%H 2SO 472h passes through
3%NaOH is the same
3%NaCl is the same
8, anti-gasoline, machine oil 168h pass through
9, wear resistance 250g/1000r≤10mg
10, gloss (60 ° of angles)≤500 °
Description of drawings
Fig. 1 is the preparation flow figure of epoxy component;
Fig. 2 is the preparation flow figure of solidifying agent component;
Embodiment:
(following content is weight ratio)
Embodiment 1:
1) preparation of epoxy component: as Fig. 1, in Scattered Kettle, drop into 35% small molecules bisphenol A epoxide resin (SM828), 7.0% reactive thinner glycidyl allyl ether (AGE), 0.3% dispersant B YK-161,0.35% defoamer BYK-A530 and 0.45% flow agent BYK-354, begin to stir evenly, starting input pigment and filler under the stirring state, the composition of pigment is 5.0% titanium dioxide R-706 and 10% chromoxide green, 0.3% delustring wax powder; The composition of filler is the silicon powder of 15% process white and 26.6%; Behind the high speed dispersion 45min, call in three-roller and be ground to fineness≤30um, it is standby to call in the paint still at last.
2) preparation of solidifying agent component: as Fig. 2, in having the porous reaction still of vacuum apparatus and condensing equipment, drop into 16.3% polymeric amide, slowly be warming up to 80 ℃, drop into 65% aliphatic cyclic amine, behind the insulation 15min, add 9.9% small molecules aliphatic amide, behind the insulation 15-20min, drop into the small molecules bisphenol A epoxide resin of formula ratio 7.6%, the Whitfield's ointment of dropping 0.7% and 0.5% Virahol isothermal reaction 4-4.5 hour, open vacuum and detach excessive small molecules aliphatic amide, sampling and measuring ammonia value, ammonia value scope is 350 ± 10, be cooled to 40 ℃ after qualified, filter and package.
During construction, by the epoxy component: the formula rate of solidifying agent component=100: 21 stirs two kinds of components, leaves standstill after froth breaking 5-10 minute and gets final product application.
Embodiment 2
1) preparation of epoxy component: as Fig. 1, in Scattered Kettle, drop into 40% small molecules bisphenol A epoxide resin (SM828), 8.0% reactive thinner glycidyl allyl ether (AGE), 0.4% dispersant B YK-161,0.45% defoamer BYK-A530 and 0.5% flow agent BYK-354, begin to stir evenly, drop into pigment and filler starting under the stirring state, the composition of pigment is 10.0% titanium dioxide R-706 and 0.1% high-carbon black pigment; The composition of filler is the silicon powder of 12.5% process white and 28.05%; Behind the high speed dispersion 45min, calling in three-roller, to be ground to fineness≤30um standby;
2) preparation of solidifying agent component: as Fig. 2, in having the porous reaction still of vacuum apparatus and condensing equipment, drop into 16.3% polymeric amide, slowly be warming up to 80 ℃, drop into 65% aliphatic cyclic amine, behind the insulation 15min, add 9.9% small molecules aliphatic amide, behind the insulation 15-20min, drop into the small molecules bisphenol A epoxide resin of formula ratio 7.6%, drip 0.7% catalyzer, Whitfield's ointment and 0.5% Virahol isothermal reaction 4-4.5 hour are opened vacuum and are detached excessive small molecules aliphatic amide, sampling and measuring ammonia value, ammonia value scope is 350 ± 10, is cooled to 40 ℃ after qualified, filters and packages.
During construction, by the epoxy component: the formula rate of solidifying agent component=100: 24 stirs two kinds of components, leaves standstill after froth breaking 5-10 minute and gets final product application.
Embodiment 3
1) preparation of epoxy component: as Fig. 1, in Scattered Kettle, drop into 38% small molecules bisphenol A epoxide resin (SM828), 5.7% reactive thinner glycidyl allyl ether (AGE), 0.45% dispersant B YK-161,0.4% defoamer BYK-A530 and 0.55% flow agent BYK-354, begin to stir evenly, starting input pigment and filler under the stirring state, the composition of pigment is 7.5% titanium dioxide R-706 and 0.2% high-carbon black pigment, 0.5% delustring wax powder; The composition of filler is the silicon powder of 17.5% process white and 29.2%; Behind the high speed dispersion 45min, calling in three-roller, to be ground to fineness≤30um standby;
2) preparation of solidifying agent component: as Fig. 2, in having the porous reaction still of vacuum apparatus and condensing equipment, drop into 16.3% polymeric amide, slowly be warming up to 80 ℃, drop into 65% aliphatic cyclic amine, behind the insulation 15min, add 9.9% small molecules aliphatic amide, behind the insulation 15-20min, drop into the small molecules bisphenol A epoxide resin of formula ratio 7.6%, drip 0.7% catalyzer, Whitfield's ointment and 0.5% Virahol isothermal reaction 4-4.5 hour are opened vacuum and are detached excessive small molecules aliphatic amide, sampling and measuring ammonia value, ammonia value scope is 350 ± 10, is cooled to 40 ℃ after qualified, filters and packages.
During construction, by the epoxy component: the formula rate of solidifying agent component=100: 21.5 stirs two kinds of components, leaves standstill after froth breaking 5-10 minute and gets final product application.
Embodiment 4
1) preparation of epoxy component: as Fig. 1, in Scattered Kettle, drop into 45% small molecules bisphenol A epoxide resin (SM828), 6.5% reactive thinner glycidyl allyl ether (AGE), 0.5% dispersant B YK-161,0.5% defoamer BYK-A530 and 0.6% flow agent BYK-354, begin to stir evenly, starting input pigment and filler under the stirring state, the composition of pigment is 2.5% titanium dioxide R-706 and 12.5% chromoxide green, 0.2% delustring wax powder; The composition of filler is the silicon powder of 10% process white and 21.7%; Behind the high speed dispersion 45min, calling in three-roller, to be ground to fineness≤30um standby;
2) preparation of solidifying agent component: as Fig. 2, in having the porous reaction still of vacuum apparatus and condensing equipment, drop into 16.3% polymeric amide, slowly be warming up to 80 ℃, drop into 65% aliphatic cyclic amine, behind the insulation 15min, add 9.9% small molecules aliphatic amide, behind the insulation 15-20min, drop into the small molecules bisphenol A epoxide resin of formula ratio 7.6%, drip 0.7% catalyzer, Whitfield's ointment and 0.5% Virahol isothermal reaction 4-4.5 hour are opened vacuum and are detached excessive small molecules aliphatic amide, sampling and measuring ammonia value, ammonia value scope is 350 ± 10, is cooled to 40 ℃ after qualified, filters and packages.
During construction, by the epoxy component: the formula rate of solidifying agent component=100: 25.5 stirs two kinds of components, leaves standstill after froth breaking 5-10 minute and gets final product application.
The invention provides the preparation method's of solvent-free epoxy matte paint for gravity flow flat ground thinking; should be understood that; for those skilled in the art; under the prerequisite that does not break away from the principle of the invention; can also make some improvement and variation, these improvement and variation also should be considered as protection scope of the present invention.

Claims (3)

1. the preparation method of a solvent-free epoxy matte paint for gravity flow flat ground comprises the preparation of epoxy component and preparation two portions of solidifying agent component, it is characterized in that preparation process is as follows: (following content is weight ratio)
1) preparation of epoxy component: the small molecules bisphenol A epoxide resin, the reactive thinner of 5.7-8.0% and 1.1-1.6% the surperficial auxiliary agent that in Scattered Kettle, drop into 35-45%, begin to stir evenly, starting input 2.5-22.7% pigment under the stirring state, 0-2% is that optional component is because the different delustring wax powder of glossy requirement reaches 10.0-17.5% process white and 21.7-29.2% silicon powder as filler; Behind the high speed dispersion 45min, call in three-roller and be ground to fineness≤30um, it is standby to call in the paint still again;
2) preparation of solidifying agent component: in having the porous reaction still of vacuum apparatus and condensing equipment, drop into 16.3% polymeric amide, slowly be warming up to 80 ℃, drop into 65% aliphatic cyclic amine, behind the insulation 15min, add 9.9% small molecules aliphatic amide, behind the insulation 15-20min, drop into the small molecules bisphenol A epoxide resin of formula ratio 7.6%, 0.7% dropping catalyzer Whitfield's ointment and 0.5% Virahol, isothermal reaction 4-4.5 hour, open vacuum and detach free small molecules aliphatic amide and Virahol, sampling and measuring ammonia value, ammonia value scope is 350 ± 10, be cooled to 40 ℃ after qualified, filter and package.
2. the preparation method of solvent-free epoxy matte paint for gravity flow flat ground according to claim 1, the reactive thinner that it is characterized in that step 1) is a glycidyl allyl ether.
3. the preparation method of solvent-free epoxy matte paint for gravity flow flat ground according to claim 1 and 2 is characterized in that the surperficial auxiliary agent of step 1) comprises the dispersion agent of 0.3-0.5%, the defoamer of 0.35-0.5%, the flow agent of 0.45-0.6%.
CN2008101247985A 2008-09-04 2008-09-04 Process for producing solvent-free epoxy matte paint for gravity flow flat ground Expired - Fee Related CN101368059B (en)

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914339A (en) * 2010-07-30 2010-12-15 张侃 Kieselguhr self leveling epoxy flooring coating
CN102442800A (en) * 2010-10-09 2012-05-09 苏州工业园区鑫丰林塑料科技有限公司 Solvent-free epoxy self-leveling floor coating process
CN102816499A (en) * 2012-08-21 2012-12-12 中山蓝海洋水性涂料有限公司 Quick-drying type environmental protection water epoxy floor paint and preparation method thereof
CN102838917A (en) * 2012-09-13 2012-12-26 上海阳森精细化工有限公司 Formula and manufacturing process of flexible self-leveling epoxy materials
CN102876198A (en) * 2012-09-16 2013-01-16 广州秀珀化工股份有限公司 Solvent-free high-elasticity epoxy self-leveling coating and preparation method thereof
CN103554438A (en) * 2013-10-12 2014-02-05 瑞奇化工(松滋)有限公司 Preparation method of modified epoxy hardener for reducing bleaching
CN105778711A (en) * 2016-03-17 2016-07-20 成都虹润制漆有限公司 Water-based epoxy floor paint and production method thereof
CN105802497A (en) * 2016-05-30 2016-07-27 珠海市澜诺新材料科技有限公司 Antislip sound attenuation floor coating
CN106118357A (en) * 2016-06-27 2016-11-16 济南大禹环保科技有限公司 No-solvent type epoxy flooring coating and preparation method thereof
CN106833117A (en) * 2017-03-06 2017-06-13 宁波瑞联特油墨有限公司 A kind of non-solvent epoxy ink and its preparation technology
CN107163776A (en) * 2017-05-08 2017-09-15 南京长江涂料有限公司 A kind of garnet modified solvent free epoxy flooring coating and preparation method thereof
CN107586504A (en) * 2016-07-07 2018-01-16 株洲飞鹿高新材料技术股份有限公司 Color sand self-leveling floor coating of one kind floating and preparation method thereof
CN107760166A (en) * 2017-11-22 2018-03-06 江门市水星涂料科技有限公司 A kind of double-component aqueous epoxide terrace paint of high-performance and preparation method thereof
CN108250907A (en) * 2018-01-25 2018-07-06 河北晨阳工贸集团有限公司 A kind of dumb light solvent-free epoxy self-leveling coating and preparation method thereof
CN109096866A (en) * 2018-06-13 2018-12-28 河北晨阳工贸集团有限公司 A kind of water-base epoxy dumb light floor coatings and preparation method thereof

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914339A (en) * 2010-07-30 2010-12-15 张侃 Kieselguhr self leveling epoxy flooring coating
CN102442800A (en) * 2010-10-09 2012-05-09 苏州工业园区鑫丰林塑料科技有限公司 Solvent-free epoxy self-leveling floor coating process
CN102816499A (en) * 2012-08-21 2012-12-12 中山蓝海洋水性涂料有限公司 Quick-drying type environmental protection water epoxy floor paint and preparation method thereof
CN102816499B (en) * 2012-08-21 2014-10-08 中山蓝海洋水性涂料有限公司 Quick-drying type environmental protection water epoxy floor paint and preparation method thereof
CN102838917A (en) * 2012-09-13 2012-12-26 上海阳森精细化工有限公司 Formula and manufacturing process of flexible self-leveling epoxy materials
CN102876198A (en) * 2012-09-16 2013-01-16 广州秀珀化工股份有限公司 Solvent-free high-elasticity epoxy self-leveling coating and preparation method thereof
CN102876198B (en) * 2012-09-16 2015-11-18 广州秀珀化工涂料有限公司 A kind of Solvent-free high-elasticity epoxy self-leveling coating and preparation method thereof
CN103554438A (en) * 2013-10-12 2014-02-05 瑞奇化工(松滋)有限公司 Preparation method of modified epoxy hardener for reducing bleaching
CN105778711A (en) * 2016-03-17 2016-07-20 成都虹润制漆有限公司 Water-based epoxy floor paint and production method thereof
CN105802497A (en) * 2016-05-30 2016-07-27 珠海市澜诺新材料科技有限公司 Antislip sound attenuation floor coating
CN106118357A (en) * 2016-06-27 2016-11-16 济南大禹环保科技有限公司 No-solvent type epoxy flooring coating and preparation method thereof
CN107586504A (en) * 2016-07-07 2018-01-16 株洲飞鹿高新材料技术股份有限公司 Color sand self-leveling floor coating of one kind floating and preparation method thereof
CN107586504B (en) * 2016-07-07 2020-07-17 株洲飞鹿高新材料技术股份有限公司 Floating color sand self-leveling floor coating and preparation method thereof
CN106833117A (en) * 2017-03-06 2017-06-13 宁波瑞联特油墨有限公司 A kind of non-solvent epoxy ink and its preparation technology
CN107163776A (en) * 2017-05-08 2017-09-15 南京长江涂料有限公司 A kind of garnet modified solvent free epoxy flooring coating and preparation method thereof
CN107163776B (en) * 2017-05-08 2019-12-06 南京长江涂料有限公司 garnet modified solvent-free epoxy floor coating and preparation method thereof
CN107760166A (en) * 2017-11-22 2018-03-06 江门市水星涂料科技有限公司 A kind of double-component aqueous epoxide terrace paint of high-performance and preparation method thereof
CN108250907A (en) * 2018-01-25 2018-07-06 河北晨阳工贸集团有限公司 A kind of dumb light solvent-free epoxy self-leveling coating and preparation method thereof
CN109096866A (en) * 2018-06-13 2018-12-28 河北晨阳工贸集团有限公司 A kind of water-base epoxy dumb light floor coatings and preparation method thereof

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