CN115717029A - Low-temperature curing epoxy floor paint and preparation method thereof - Google Patents
Low-temperature curing epoxy floor paint and preparation method thereof Download PDFInfo
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- CN115717029A CN115717029A CN202211567919.XA CN202211567919A CN115717029A CN 115717029 A CN115717029 A CN 115717029A CN 202211567919 A CN202211567919 A CN 202211567919A CN 115717029 A CN115717029 A CN 115717029A
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Abstract
The application relates to the technical field of coatings, in particular to low-temperature curing epoxy floor paint and a preparation method thereof. A low-temperature curing epoxy floor paint comprises a component A and a component B; the component A comprises modified epoxy resin, filler, pigment, a defoaming agent and water; the component B comprises an isocyanate curing agent and a reactive diluent; the preparation method comprises the following steps: adding the pigment and the filler into the mixed solution of water and the defoaming agent, stirring and mixing, then adding the modified epoxy resin, and stirring and mixing to obtain a component A; mixing an isocyanate curing agent and an active diluent to obtain a component B; and stirring and mixing the component A and the component B to obtain the low-temperature curing epoxy floor paint. In the low-temperature curing epoxy floor paint, the modified epoxy resin contains a large amount of hydroxyl and can react with the isocyanate curing agent to be cured into a film, so that the low-temperature curing efficiency of the floor paint is improved.
Description
Technical Field
The application relates to the technical field of coatings, in particular to low-temperature curing epoxy floor paint and a preparation method thereof.
Background
The epoxy floor paint is a high-strength, wear-resistant and beautiful floor decoration material. Because the epoxy floor paint also has the advantages of seamless integrity, dust prevention, moisture prevention, impact resistance, easy cleaning and the like, the epoxy floor paint is widely applied to places such as factories, hospitals, schools, offices, airports and the like.
The main components of the epoxy floor paint comprise epoxy resin and a curing agent, and under the action of the curing agent, the liquid epoxy resin is cured to form a high polymer material with a three-dimensional network structure.
However, although many room temperature curable epoxy floor finishes are currently available on the market. However, in cold regions, when the environmental temperature is lower than 10 ℃, the epoxy floor paint is slowly cured after low-temperature construction in winter, and the problem of inconvenient construction in winter is solved.
Disclosure of Invention
In order to improve the curing rate of the epoxy floor paint at a low temperature, the application provides the low-temperature curing epoxy floor paint and the preparation method thereof.
In a first aspect, the application provides a low-temperature curing epoxy floor paint, which adopts the following technical scheme:
a low-temperature curing epoxy floor paint comprises a component A and a component B;
the component A comprises the following components in parts by weight:
20-40 parts of modified epoxy resin;
15-30 parts of a filler;
10-15 parts of a pigment;
0.2-0.5 part of defoaming agent;
10-20 parts of water;
the component B comprises the following components in parts by weight:
15-30 parts of an isocyanate curing agent;
3-6 parts of a reactive diluent;
the modified epoxy resin comprises the following modification steps: mixing epoxy resin, epoxy silane and an organic solvent, adding N, N-di (aminopropyl) ethylenediamine, stirring and mixing at 60-75 ℃ for 1-2h to obtain the modified epoxy resin.
By adopting the technical scheme, the epoxy resin is modified by adopting the N, N-di (aminopropyl) ethylenediamine, the epoxy groups in the epoxy resin and the epoxy silane are converted into secondary amine by the active groups in the N, N-di (aminopropyl) ethylenediamine, and a large amount of hydroxyl and siloxane are introduced into the obtained modified epoxy resin. Therefore, when the obtained modified epoxy resin is cured, the isocyanic acid radical in the isocyanate curing agent can directly react with secondary amine and hydroxyl for curing, and the epoxy resin does not need to be subjected to a ring-opening reaction, so that the curing efficiency of a floor paint system is improved. Meanwhile, siloxane groups with flexible chain segments are introduced into the modified epoxy resin, so that the flexibility of the finally obtained floor paint after curing can be improved, the surface energy of the floor paint can be reduced, and the hydrophobic performance of the floor paint is improved.
Preferably, the epoxysilane includes 3- (2, 3 glycidoxy) propyltrimethoxysilane, 3- (2, 3 glycidoxy) propylmethyldiethoxysilane, or 3- (2, 3 glycidoxy) propylmethyldimethoxysilane.
By adopting the technical scheme, the modified epoxy silane prepared by mixing the three epoxy silanes, the epoxy resin and the N, N-di (aminopropyl) ethylenediamine has small viscosity change, is beneficial to improving the dispersibility and compatibility of the modified epoxy resin in raw material components of the floor paint, and further improves the curing rate of the floor paint at low temperature and the water resistance and flexibility of the cured paint film.
Preferably, the organic solvent is one or more of absolute ethyl alcohol, isopropyl alcohol and n-propyl alcohol.
By adopting the technical scheme, the organic solvent can better dissolve the epoxy resin, the epoxy silane and the N, N-di (aminopropyl) ethylenediamine, and is beneficial to improving various properties of the obtained modified epoxy resin. Meanwhile, the organic solvent has good solubility in water, and is favorable for improving the compatibility and the dispersibility of the obtained modified epoxy resin in a floor paint system.
Preferably, the epoxy resin is an aliphatic epoxy resin or an aliphatic epoxy resin.
By adopting the technical scheme, the two types of epoxy resin are modified, and the obtained floor paint can be quickly cured at the ambient temperature of-25-0 ℃, so that the curing rate of the floor paint at a low temperature is greatly improved.
Preferably, the aliphatic epoxy resin has a viscosity of 700 to 1100 mPas at25 ℃.
By adopting the technical scheme, the epoxy resin with the viscosity is modified, the obtained modified epoxy resin has good dispersibility and compatibility in raw material components of the floor paint, the time of curing the floor paint at a low temperature is further shortened, and meanwhile, the water resistance and the flexibility of the cured paint film are also improved.
Preferably, the epoxy resin is one or two of bisphenol A type epoxy resin and bisphenol F type epoxy resin.
By adopting the technical scheme, the epoxy resin of the type is modified, and the obtained modified resin can improve the curing rate of the obtained paint film at low temperature and can also improve the water resistance of the obtained paint film.
Preferably, in the step of modifying the modified epoxy resin, the mass ratio of the epoxy group in the epoxy resin, the epoxy group in the epoxysilane and the primary amine group in the N, N-bis (aminopropyl) ethylenediamine is 1 (0.2-0.6) to (0.7-1.1).
Preferably, in the step of modifying the modified epoxy resin, the mass ratio of the epoxy group in the epoxy resin, the epoxy group in the epoxysilane and the primary amine group in the N, N-bis (aminopropyl) ethylenediamine is 1.
By adopting the technical scheme, on one hand, the epoxy resin, the epoxy silane and the N, N-bis (aminopropyl) ethylenediamine are fed according to the proportion, the three raw materials have good reaction degree and more groups for isocyanate reaction, the reaction rate of the raw materials and the isocyanate is promoted, and the curing time of the obtained floor paint is shortened. On the other hand, the three raw materials are fed according to the proportion, and the adsorption of the paint film on the surface of the base material is promoted by controlling the quantity of generated hydroxyl in the modified epoxy resin, so that the paint film obtained after the raw material components of the floor paint are quickly cured has good flexibility. Meanwhile, the viscosity of the modified epoxy resin obtained under the conditions is moderate, so that the modified epoxy resin has good dispersibility and compatibility in raw material components for preparing the floor paint, is favorable for being cured into a compact paint film, and improves the water resistance of the obtained floor paint film.
In a second aspect, the application provides a preparation method of low-temperature curing epoxy floor paint, which adopts the following technical scheme:
a preparation method of low-temperature curing epoxy floor paint comprises the following preparation steps:
s1: adding the pigment and the filler into the mixed liquid of the water and the defoamer, stirring and mixing, then adding the modified epoxy resin, and stirring and mixing to obtain a component A;
s2: mixing an isocyanate curing agent and an active diluent, and stirring and mixing to obtain a component B;
s3: and stirring and mixing the component A and the component B to obtain the low-temperature curing epoxy floor paint.
By adopting the technical scheme, the raw material components are added step by step, so that the dispersibility of the raw materials can be improved, a floor paint system can be favorably and quickly formed into a compact paint film, and the water resistance and the flexibility of the paint film are improved.
In summary, the present application has the following beneficial effects:
according to the preparation method, the epoxy resin is modified by adopting N, N-di (aminopropyl) ethylenediamine and epoxy silane, so that an epoxy group in the epoxy resin is promoted to open a ring in advance, the reaction rate of the obtained modified epoxy resin and an isocyanate curing agent can be effectively improved, and the low-temperature curing efficiency of a floor paint system is improved; meanwhile, the N, N-di (aminopropyl) ethylenediamine and epoxy silane contained in the modified epoxy resin improve the dispersibility and compatibility of the modified epoxy resin, and are beneficial to forming a compact paint film in a floor paint system, so that the hydrophobicity and the flexibility of the floor paint are improved.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example of modified epoxy resin
Preparation example 1
The components and the weight of the modified epoxy resin are shown in the following table.
The modified epoxy resin is prepared by the following preparation steps:
mixing epoxy resin, epoxy silane and an organic solvent, adding N, N-di (aminopropyl) ethylenediamine, stirring and mixing for 1.5 hours at 65 ℃ to obtain the modified epoxy resin.
In the examples of the present application, the epoxy resin having a DER 353 designation was a mixed resin composed of a bisphenol A type epoxy resin and a bisphenol F type epoxy resin, and was purchased from Kyonghin chemical Co., ltd, shanghai, having an epoxy value of 0.53eq./100g and a viscosity of 800-1000 (mPa. Multidot.s, AT25 ℃ C.).
3- (2,3 glycidoxy) propyltrimethoxysilane, with a molecular weight of 236.3376, and the amount of 3- (2,3 glycidoxy) propyltrimethoxysilane used is calculated as the molecular weight of 236 in the examples of this application.
N, N-di (aminopropyl) ethylenediamine with a molecular weight of 174.29, was used in the present examples in an amount calculated as molecular weight of 174.
The mass ratio of epoxy groups in the epoxy resin, epoxy groups in the epoxysilane, and primary amine groups in the N, N-di (aminopropyl) ethylenediamine was 1.
Preparation examples 2 to 5
A modified epoxy resin was different from preparation example 1 in that the components and their weights are shown in the following table.
Preparation example 6
A modified epoxy resin was different from preparation example 1 in that epoxy resin NPEL-128E was used in weight in place of epoxy resin DER 353.
In the preparation examples of the present application, the epoxy resin NPEL-128E was bisphenol A type epoxy resin, having an epoxy value of 0.53eq./100g and a viscosity of 12000-15000 (mPa. Multidot.s, AT25 ℃ C.), and was purchased from Kaiyn chemical Co., ltd.
Preparation example 7
A modified epoxy resin was different from preparation example 1 in that an epoxy resin NPEF-176 of an equal weight was used in place of the epoxy resin DER 353.
In the preparation examples, the epoxy resin NPEF-176 is bisphenol F type epoxy resin, the epoxy value is 0.53eq./100g, the viscosity is 3000-5000 (mPa. Multidot.s, AT25 ℃), and the epoxy resin is purchased from Guangzhou Wei Rina chemical Co., ltd.
Preparation example 8
A modified epoxy resin is different from the modified epoxy resin prepared in preparation example 1 in that epoxy resin DER 353 is replaced by epoxy resin EPolead PB3600 with the same weight.
In the preparation examples of the present application, the epoxy resin EPolead PB3600 is an aliphatic epoxy resin, and has an epoxy value of 0.53eq./100g and a viscosity of 28000 (mPa · s AT25 ℃).
Preparation example 9
A modified epoxy resin is different from the preparation example 1 in that an epoxy resin of equal mass, namely EPIKOTE 240, is used for replacing an epoxy resin DER 353.
In the preparation examples of the present application, the epoxy resin EPIKOTE 240 is a mixture of a bisphenol A type epoxy resin and a bisphenol F type epoxy resin, and has an epoxy value of 0.53 eq/100 g, a viscosity of 700-1100 (mPa. Multidot.s, AT25 ℃ C.), and is purchased from Kyowa Kay chemical Co., ltd.
Preparation example 10
A modified epoxy resin was different from preparation example 1 in that 3- (2, 3-glycidoxy) propyltriethoxysilane, in which 3- (2, 3-glycidoxy) propyltriethoxysilane had a molecular weight of 278.4173, was used in an amount equal to the amount of epoxy group species, calculated as the molecular weight of 3- (2, 3-glycidoxy) propyltriethoxysilane in preparation example 278.
Preparation example 11
A modified epoxy resin, which is different from preparation example 1 in that 3- (2, 3-glycidoxy) propylmethyldimethoxysilane having a molecular weight of 220.3382 is used in place of 3- (2, 3-glycidoxy) propyltriethoxysilane in an amount of equal amount of epoxy group material, and preparation example herein calculates the amount of 3- (2, 3-glycidoxy) propylmethyldimethoxysilane having a molecular weight of 220.
Preparation example 12
A modified epoxy resin was distinguished from preparation example 1 in that 2- (3, 4 epoxycyclohexyl) ethyltrimethoxysilane, which had a molecular weight of 246.3755, was used in an amount equal to the amount of epoxy group species in place of 3- (2, 3 epoxypropoxy) propyltriethoxysilane, preparation example being calculated from 2- (3, 4 epoxycyclohexyl) ethyltrimethoxysilane, which had a molecular weight of 246.
Preparation example 13
A modified epoxy resin which differs from example 1 in that it is prepared by the following preparation steps:
mixing epoxy resin, epoxy silane and an organic solvent, adding N, N-di (aminopropyl) ethylenediamine, stirring and mixing for 2 hours at the temperature of 60 ℃ to obtain the modified epoxy resin.
Preparation example 14
A modified epoxy resin, which is different from example 1 in that it is prepared by the following preparation steps:
mixing epoxy resin, epoxy silane and an organic solvent, adding N, N-di (aminopropyl) ethylenediamine, stirring and mixing at 75 ℃ for 1h to obtain the modified epoxy resin.
Preparation example 15
A modified epoxy resin is different from preparation example 1 in that 3-aminopropyltriethoxysilane having a molecular weight of 221.31 is used in an amount equal to the amount of primary amine group substance in place of N, N-bis (aminopropyl) ethylenediamine, and preparation example herein calculates the amount of 3-aminopropyltriethoxysilane having a molecular weight of 221.
Preparation example 16
A modified epoxy resin was different from preparation example 1 in that 3- (2, 3-glycidoxy) propyltrimethoxysilane was replaced with the epoxy resin DER 353 in an amount equal to the amount of the epoxy group species.
Preparation example 17
A modified epoxy resin which is different from preparation example 1 in that it is prepared by the following preparation steps:
epoxy resin, epoxy silane, an organic solvent and N, N-di (aminopropyl) ethylenediamine are stirred and mixed for 1.5 hours at the temperature of 65 ℃ to obtain the modified epoxy resin.
To the epoxy floor paint that low temperature curing epoxy floor paint that this application embodiment obtained and comparative example obtained, carry out drying time, water proofness, pliability and adhesive force and detect, detection standard as follows:
and (3) detecting the drying time: reference GB/T1728-2020;
and (3) detecting water resistance: reference is made to GB/T5209-1985;
and (3) flexibility detection: reference GB/T1731-1993;
and (3) adhesive force detection: refer to GB/T9286-2021.
Examples
Example 1
The low-temperature curing epoxy floor paint comprises the following components in parts by weight
The preparation method of the low-temperature curing epoxy floor paint comprises the following preparation steps:
s1: adding titanium dioxide, calcined kaolin and talcum powder into a mixed solution of water, a defoaming agent, a dispersing agent, a wetting agent and a film-forming additive, stirring and mixing at 1500r/min for 30min, then adding modified epoxy resin, and stirring and mixing for 30min to obtain a component A;
in the embodiment of the application, the pigment is titanium dioxide with the model of R706, which is purchased from new color materials, inc. of Anhui Jing.
The filler is filled withThe core glass micro-beads and the silicon micro-powder are mixed, wherein the hollow glass micro-beads are white powder with the fineness of 20 mu m, the porosity of 0.03 and the density of 0.12g/cm 3 The compression strength is 1.5MPa (240 PSI) -123MPa (27600 PSI), and the Mohs hardness is 7H;
silicon micropowder, white powder, 6000 meshes, 7 hardness and 2.6 density.
Defoamer, model EZ8825, purchased from shanghai cast industries ltd.
The dispersant is JN-2085, and is purchased from Shandong energy-gathering chemical Co.
Wetting agent, model SS-940, purchased from Tianjin Sheng Cheng scientific development Limited.
In the examples of the present application, the modified epoxy resin prepared in preparation example 1 was used.
S2: mixing a curing agent and an active diluent, and stirring and mixing at 800r/min for 5min to obtain a component B; isocyanate curing agent of the type
HT-600 was purchased from Jinan Kogyo GmbH.
The reactive diluent, model AGE-A, was purchased from Jinan quanxin New materials, inc.
S3: and stirring and mixing the component A and the component B to obtain the low-temperature curing epoxy floor paint.
Examples 2 to 3
A low-temperature curing epoxy floor paint, which is different from the example 1 in that the components and the weight thereof are shown in the following table.
The low-temperature curing epoxy floor paint obtained in the examples 1 to 3 of the present application was subjected to drying time, water resistance and flexibility tests, and the test results are shown in the following table.
Data analysis on the above table shows that the low-temperature curing epoxy floor paint obtained in the embodiments 1 to 3 has a surface drying time of less than 0.9h at 0 ℃ and a solid drying time of less than 1.4 h; the surface drying time is as low as below 1.1h at minus 10 ℃, and the actual drying time is as low as below 15 h; the surface drying time at the temperature of minus 25 ℃ is as low as below 5h, and the actual drying time is as low as below 29 h; the paint film does not blister and rust after 720 hours, and the 1mm paint film is bent, and the phenomena of cracks, reticulate patterns, peeling and the like do not occur on the surface of the paint film. Therefore, the low-temperature curing epoxy floor paint obtained in the embodiments 1 to 3 can be rapidly cured at the temperature of-25 to 0 ℃, and has good water resistance and flexibility.
Examples 4 to 7
The difference between the low-temperature curing epoxy floor paint and the example 1 is that in the total raw materials for preparing the modified epoxy resin, the quantity ratio of substances of an epoxy group in the epoxy resin, an epoxy group in epoxy silane and a primary amine group in N, N-di (aminopropyl) ethylenediamine is different.
That is, in examples 4 to 7 of the present application, the modified epoxy resins prepared in preparation examples 2 to 5 were used as the modified epoxy resins. Meanwhile, in the total raw materials for the preparation of the modified epoxy resins used in examples 4 to 7, the amounts of the substances of the epoxy groups in the epoxy resins were the same.
In examples 4 to 7 of the present application, the components and their weights, and the preparation of the modified epoxy resin are shown in the following tables.
The low-temperature curing epoxy floor paints obtained in examples 4 to 7 of the present application were subjected to drying time, water resistance, flexibility and adhesion detection, and the detection results are shown in the following table.
Data analysis on the above table shows that the low-temperature curing epoxy floor paint obtained in the embodiments 4-7 of the present application has a surface drying time of less than 1.2h at 0 ℃ and a full drying time of less than 1.7 h; the surface drying time is reduced to below 1.2h at the temperature of minus 10 ℃, and the actual drying time is reduced to below 13.4 h; the surface drying time at minus 25 ℃ is as low as below 3.2h, and the actual drying time is as low as below 25.4 h. Therefore, the low-temperature curing epoxy floor paint obtained in the embodiments 4 to 7 can be rapidly cured at the temperature of-25 to 0 ℃, and has good water resistance and flexibility.
As can be seen from comparison of the low-temperature-cured epoxy floor paints obtained in examples 1, 4 and 5 with the low-temperature-cured epoxy floor paints obtained in examples 6 and 7, the surface drying time and the actual drying time of the low-temperature-cured epoxy floor paints obtained in examples 1, 4 and 5 at-25-0 ℃ are both smaller than those of the low-temperature-cured epoxy floor paints obtained in examples 6 and 7, and the water resistance and the flexibility of the paint film are better. Therefore, in the total raw materials for preparing the low-temperature curing epoxy floor paint, the amount ratio of substances of the epoxy group in the epoxy resin, the epoxy group in the epoxy silane and the primary amine group in the N, N-bis (aminopropyl) ethylenediamine in the adopted modified epoxy resin is 1 (0.2-0.6) to (0.7-1.1), which is beneficial to improving the flexibility of the paint film of the obtained floor paint and shortening the curing time of the floor paint at the temperature of-25-0 ℃.
Example 8
A low-temperature curing epoxy floor paint is different from that of example 1 in that in the total raw material for preparing the modified epoxy resin, epoxy resin NPEL-128E with equal weight is adopted to replace epoxy resin DER 353.
That is, in the examples of the present application, the modified epoxy resin prepared in preparation example 6 was used.
Example 9
The difference between the low-temperature curing epoxy floor paint and the embodiment 1 is that in the total raw materials for preparing the modified epoxy resin, epoxy resin NPEF-176 with equal weight is adopted to replace epoxy resin DER 353.
That is, in the examples of the present application, the modified epoxy resin prepared in preparation example 7 was used.
Example 10
The difference between the low-temperature curing epoxy floor paint and the embodiment 1 is that epoxy resin DER 353 is replaced by epoxy resin EPolead PB3600 with equal weight in the total raw materials for preparing the modified epoxy resin.
That is, in the examples of the present application, the modified epoxy resin prepared in preparation example 8 was used.
Example 11
The difference between the low-temperature curing epoxy floor paint and the embodiment 1 is that in the total raw materials for preparing the modified epoxy resin, epoxy resin DER 353 is replaced by epoxy resin EPIKOTE 240 with equal weight.
That is, in the examples of the present application, the modified epoxy resin prepared in preparation example 9 was used.
The low-temperature curing epoxy floor paint obtained in the examples 8 to 11 of the present application was tested for drying time, water resistance and flexibility, and the test results are shown in the following table.
Data analysis on the above table shows that the low-temperature curing epoxy floor paint obtained in the embodiments 8 to 11 of the present application has a surface drying time of less than 1.4h at 0 ℃ and a solid drying time of less than 1.9 h; the surface drying time is reduced to below 1.5h at the temperature of minus 10 ℃, and the actual drying time is reduced to below 13.8 h; the surface drying time at the temperature of minus 25 ℃ is as low as below 4.7h, and the actual drying time is as low as below 28.2 h; the water resistance is up to 672h, and a paint film with the thickness of 1mm is bent, so that the phenomena of cracks, reticulate patterns, peeling and the like do not occur on the surface of the paint film. Therefore, the low-temperature curing epoxy floor paint obtained in the examples 8 to 11 can be cured at the temperature of-25 to 0 ℃, and has good water resistance and flexibility.
Comparing the low-temperature cured epoxy floor paints obtained in examples 1, 8 and 9 with the low-temperature cured epoxy floor paint obtained in example 10, it can be seen that the surface drying time and the actual drying time of the low-temperature cured epoxy floor paints obtained in examples 1, 8 and 9 at-25-0 ℃ are less than those of the low-temperature cured epoxy floor paint obtained in example 10. Therefore, the modified epoxy resin adopted in the low-temperature curing epoxy floor paint is aliphatic epoxy resin which is one or two of bisphenol A epoxy resin and bisphenol F epoxy resin in the total raw materials, and is favorable for reducing the curing time at minus 25-0 ℃.
Meanwhile, as can be seen from comparison between the low-temperature cured epoxy floor paints obtained in examples 1 and 11 and the low-temperature cured epoxy floor paints obtained in examples 8 and 9, the surface drying time and the actual drying time of the low-temperature cured epoxy floor paints obtained in examples 1 and 11 at-25 to 0 ℃ are both shorter than those of the low-temperature cured epoxy floor paints obtained in examples 8 and 9, and the water resistance time is longer. Therefore, the preparation method shows that in the total raw materials for preparing the low-temperature curing epoxy floor paint, the viscosity of the aliphatic epoxy resin at25 ℃ is 700-1100mPa & s in the modified epoxy resin, so that the curing time of the floor paint at-25-0 ℃ can be shortened, and the water resistance is improved.
Examples 12 to 14
The difference between the low-temperature curing epoxy floor paint and the embodiment 1 is that in the total raw materials for preparing the modified epoxy resin, the type of epoxy silane is different.
That is, in examples 12 to 14 of the present application, the modified epoxy resins prepared in preparation examples 10 to 12 were used as the modified epoxy resins. Meanwhile, the modified epoxy resins used in examples 12 to 14 were prepared in the same amount of the substance of the epoxy group in the epoxysilane as the total raw material.
In examples 12 to 14 of the present application, the components and their weights, and the preparation of the modified epoxy resin are shown in the following tables.
The low-temperature curing epoxy floor paints obtained in examples 13-15 of the present application were tested for drying time, water resistance and flexibility, and the test results are shown in the following table.
Data analysis on the above table shows that the low-temperature curing epoxy floor paint obtained in the embodiments 1, 12, 13 and 14 has a surface drying time of less than 1.0h at 0 ℃ and a solid drying time of less than 1.8 h; the surface drying time at minus 10 ℃ is reduced to below 1.5h, and the actual drying time is reduced to below 13.5 h; surface drying time is as low as below 3.2h at minus 25 ℃, and actual drying time is as low as below 26 h; the paint film does not blister and rust after 720 hours, and the 1mm paint film is bent, and the phenomena of cracks, reticulate patterns, peeling and the like do not occur on the surface of the paint film. Therefore, the low-temperature curing epoxy floor paint obtained in the examples 1, 12, 13 and 14 can be cured at the temperature of-25-0 ℃, and has good water resistance and flexibility.
Comparing the low-temperature-cured epoxy floor paints obtained in examples 1, 12 and 13 with the low-temperature-cured epoxy floor paint obtained in example 14, it can be seen that the surface drying time and the actual drying time of the low-temperature-cured epoxy floor paints obtained in examples 1, 12 and 13 are both smaller than those of the low-temperature-cured epoxy floor paint obtained in example 14 at-25 to 0 ℃. Therefore, in the total raw materials for preparing the low-temperature curing epoxy floor paint, the epoxy silane in the adopted modified epoxy resin is 3- (2, 3-glycidoxy) propyl trimethoxy silane, 3- (2, 3-glycidoxy) propyl triethoxy silane or 3- (2, 3-glycidoxy) propyl methyl dimethoxy silane, so that the curing time of the floor paint at the temperature of-25-0 ℃ is favorably shortened.
Example 15
The difference between the low-temperature curing epoxy floor paint and the embodiment 1 is that the preparation steps of the modified epoxy resin are different.
That is, in the examples of the present application, the modified epoxy resin was prepared by preparation example 13, and in preparation example 13, the modified epoxy resin was prepared by the following preparation steps:
mixing epoxy resin, epoxy silane and an organic solvent, adding N, N-di (aminopropyl) ethylenediamine, stirring and mixing for 2 hours at the temperature of 60 ℃ to obtain the modified epoxy resin.
Example 16
The difference between the low-temperature curing epoxy floor paint and the embodiment 1 is that the preparation steps of the modified epoxy resin are different.
That is, in the examples of the present application, the modified epoxy resin was prepared by preparation example 14, and in preparation example 14, the modified epoxy resin was prepared by the following preparation steps:
mixing epoxy resin, epoxy silane and an organic solvent, adding N, N-di (aminopropyl) ethylenediamine, stirring and mixing for 1h at 75 ℃ to obtain the modified epoxy resin.
The low-temperature curing epoxy floor paints obtained in examples 15 to 16 of the present application were tested for drying time, water resistance and flexibility, and the test results are shown in the following table.
Data analysis on the above table shows that the low-temperature curing epoxy floor paint obtained in the embodiments 1, 15 and 16 has a surface drying time of less than 1.0h at 0 ℃ and a solid drying time of less than 1.5 h; the surface drying time is reduced to below 1.0h at the temperature of minus 10 ℃, and the actual drying time is reduced to below 12.5 h; the surface drying time at minus 25 ℃ is as low as below 2.3h, and the actual drying time is as low as below 24.5 h; the paint film does not bubble and rust within 720h, and the 1mm paint film is bent, and the phenomena of cracks, reticulate patterns, peeling and the like do not occur on the surface of the paint film. Therefore, the low-temperature curing epoxy floor paint prepared from the modified epoxy resin prepared by the preparation method can be cured at the temperature of-25-0 ℃, and has good water resistance and flexibility.
Comparative example
Comparative example 1
An epoxy floor paint is different from that of example 1 in that 3-aminopropyltriethoxysilane with the same amount of primary amine group substances is used to replace N, N-di (aminopropyl) ethylenediamine in the total raw materials for preparing the modified epoxy resin.
That is, in the comparative example of the present application, a modified epoxy resin was prepared from preparation example 15.
Comparative example 2
An epoxy floor paint is different from example 1 in that 3- (2, 3-glycidoxy) propyl trimethoxy silane is replaced by epoxy resin DER 353 with the same amount of epoxy group substances in the total raw materials for preparing the modified epoxy resin.
That is, in the comparative example of the present application, a modified epoxy resin was prepared from preparation example 16.
In comparative examples 1 to 2 of the present application, the components and their weights, and the preparation of the modified epoxy resin are shown in the following tables.
Comparative example 3
An epoxy floor paint, which is different from the epoxy floor paint in example 1 in that the modified epoxy resin is prepared by the following preparation steps:
epoxy resin, epoxy silane, an organic solvent and N, N-di (aminopropyl) ethylenediamine are stirred and mixed for 1.5 hours at the temperature of 65 ℃ to obtain the modified epoxy resin.
That is, in the comparative example of the present application, a modified epoxy resin was prepared from preparation example 18.
The epoxy floor paint obtained in the comparative examples 1 to 3 of the application is subjected to drying time, water resistance, flexibility and adhesion detection, and the detection results are shown in the following table.
Data analysis on the above table shows that, compared with the epoxy floor paint obtained in comparative examples 1 and 2, the low-temperature curing epoxy floor paint obtained in example 1 has shorter surface drying time and actual drying time at-25-0 ℃, longer water resistance time and thinner paint film detected by flexibility. The modified epoxy resin prepared from the epoxy resin, the epoxy silane, the organic solvent and the N, N-di (aminopropyl) ethylenediamine can improve the water resistance and the flexibility of the obtained floor paint and can obviously shorten the curing time of the floor paint at the temperature of-25-0 ℃.
Compared with the epoxy floor paint obtained in the comparative example 3, the low-temperature curing epoxy floor paint obtained in the example 1 has shorter surface drying time and actual drying time at-25-0 ℃, longer water resistance time and thinner paint film detected by flexibility. Therefore, the modified epoxy resin prepared by the preparation method is beneficial to improving the water resistance and the flexibility of the obtained floor paint, and can obviously shorten the curing time of the floor paint at the temperature of-25-0 ℃.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. The low-temperature curing epoxy floor paint is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
20-40 parts of modified epoxy resin;
15-30 parts of a filler;
10-15 parts of pigment;
0.2-0.5 part of defoaming agent;
10-20 parts of water;
the component B comprises the following components in parts by weight:
15-30 parts of an isocyanate curing agent;
3-6 parts of a reactive diluent;
the modified epoxy resin comprises the following modification steps: mixing epoxy resin, epoxy silane and an organic solvent, adding N, N-di (aminopropyl) ethylenediamine, stirring and mixing at 60-75 ℃ for 1-2h to obtain the modified epoxy resin.
2. The low-temperature curing epoxy floor paint according to claim 1, characterized in that: the epoxysilane includes 3- (2, 3-glycidoxy) propyltrimethoxysilane, 3- (2, 3-glycidoxy) propylmethyldiethoxysilane or 3- (2, 3-glycidoxy) propylmethyldimethoxysilane.
3. The low-temperature curing epoxy floor paint according to claim 1, characterized in that: the organic solvent is one or more of absolute ethyl alcohol, isopropanol and n-propanol.
4. The low-temperature curing epoxy floor paint according to claim 1, characterized in that: the epoxy resin is aliphatic epoxy resin or aliphatic epoxy resin.
5. The low-temperature curing epoxy floor paint according to claim 4, characterized in that: the viscosity of the aliphatic epoxy resin at25 ℃ is 700-1100mPa.s.
6. The low-temperature curing epoxy floor paint according to claim 4, characterized in that: the epoxy resin is one or two of bisphenol A type epoxy resin and bisphenol F type epoxy resin.
7. The low-temperature curing epoxy floor paint according to claim 1, characterized in that: in the step of modifying the modified epoxy resin, the mass ratio of the epoxy group in the epoxy resin, the epoxy group in the epoxy silane and the primary amine group in the N, N-di (aminopropyl) ethylenediamine is 1 (0.2-0.6) to (0.7-1.1).
8. The low-temperature curing epoxy floor paint according to claim 7, characterized in that: in the step of modifying the modified epoxy resin, the mass ratio of the epoxy group in the epoxy resin, the epoxy group in the epoxysilane and the primary amine group in the N, N-di (aminopropyl) ethylenediamine is 1.
9. The preparation method of the low-temperature curing epoxy floor paint as claimed in any one of claims 1 to 8, which is characterized by comprising the following preparation steps:
s1: adding the pigment and the filler into the mixed solution of water and the defoaming agent, stirring and mixing, then adding the modified epoxy resin, and stirring and mixing to obtain a component A;
s2: mixing an isocyanate curing agent and an active diluent, and stirring and mixing to obtain a component B;
s3: and stirring and mixing the component A and the component B to obtain the low-temperature curing epoxy floor paint.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116478600A (en) * | 2023-04-30 | 2023-07-25 | 千浪化研新材料(上海)有限公司 | Water-based bi-component corrosion-resistant paint and preparation method thereof |
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| CN115717029B (en) | 2023-07-25 |
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