CN117844344A - Hydrogenated epoxy floor paint and preparation method thereof - Google Patents
Hydrogenated epoxy floor paint and preparation method thereof Download PDFInfo
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- CN117844344A CN117844344A CN202410088435.XA CN202410088435A CN117844344A CN 117844344 A CN117844344 A CN 117844344A CN 202410088435 A CN202410088435 A CN 202410088435A CN 117844344 A CN117844344 A CN 117844344A
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- floor paint
- epoxy resin
- propylene glycol
- hydrogenated epoxy
- hydrogenated
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- 239000004593 Epoxy Substances 0.000 title claims abstract description 100
- 239000003973 paint Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003822 epoxy resin Substances 0.000 claims abstract description 57
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 57
- 239000000463 material Substances 0.000 claims abstract description 56
- 150000001412 amines Chemical class 0.000 claims abstract description 47
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 24
- 239000000080 wetting agent Substances 0.000 claims abstract description 22
- 229920001451 polypropylene glycol Polymers 0.000 claims abstract description 18
- -1 poly (dimethylsiloxane) -diglycidyl Polymers 0.000 claims abstract description 17
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 13
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims abstract description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 6
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 41
- 239000003795 chemical substances by application Substances 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000002270 dispersing agent Substances 0.000 claims description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000000839 emulsion Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- MECNWXGGNCJFQJ-UHFFFAOYSA-N 3-piperidin-1-ylpropane-1,2-diol Chemical compound OCC(O)CN1CCCCC1 MECNWXGGNCJFQJ-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000004408 titanium dioxide Substances 0.000 claims description 10
- 230000004224 protection Effects 0.000 claims description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 5
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 5
- 239000013530 defoamer Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000000903 blocking effect Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 230000001804 emulsifying effect Effects 0.000 abstract description 9
- 239000004848 polyfunctional curative Substances 0.000 abstract description 8
- 239000000945 filler Substances 0.000 abstract description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000001038 titanium pigment Substances 0.000 abstract description 2
- LHENQXAPVKABON-UHFFFAOYSA-N 1-methoxypropan-1-ol Chemical compound CCC(O)OC LHENQXAPVKABON-UHFFFAOYSA-N 0.000 abstract 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- 239000011248 coating agent Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000011161 development Methods 0.000 description 5
- 230000018109 developmental process Effects 0.000 description 5
- 229920006334 epoxy coating Polymers 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 239000004568 cement Substances 0.000 description 4
- 239000003995 emulsifying agent Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 239000005058 Isophorone diisocyanate Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000006750 UV protection Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000008786 sensory perception of smell Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
- C08G59/4085—Curing agents not provided for by the groups C08G59/42 - C08G59/66 silicon containing compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The application relates to the technical field of floor paint, and particularly discloses hydrogenated epoxy floor paint and a preparation method thereof. A hydrogenated epoxy floor paint is prepared from hydrogenated epoxy resin as basic material, triglycidyl ether of trimethylolpropane, modified amine epoxy hardener prepared from diethylenetriamine, poly (dimethylsiloxane) -diglycidyl ether end-capped, E-51 epoxy resin, poly (propylene glycol) -tolyl-2, 4-diisocyanate and poly (ethylene glycol) methacrylate, titanium pigment and barium sulfate as filler, and propanediol methyl ether, disperser, defoaming agent and wetting agent as assistant through emulsifying the hydrogenated epoxy resin to obtain small particle size, and high solidifying power. The hydrogenated epoxy floor paint prepared by the method has the advantages of good emulsifying property and curing property, low viscosity, long service life and excellent mechanical property.
Description
Technical Field
The application relates to the technical field of floor paint, in particular to hydrogenated epoxy floor paint and a preparation method thereof.
Background
With the continuous development of epoxy technology, the original industrial floor materials such as cement and plastic can not meet the requirements of modernization on the floor materials, and then the epoxy floor paint is produced. Due to the advantages of the epoxy system paint, the epoxy system paint is widely applied to the field of industrial floor paint, and accounts for about 70% of the market share of the floor paint. Therefore, the development and research of the epoxy system paint in the field of industrial floor paint are also receiving more and more attention, and the application and development of the epoxy floor paint are greatly promoted. Along with the improvement and development of an epoxy system, the epoxy floor paint is developed from the traditional solvent-type solvent-free epoxy floor paint to the current water-based epoxy floor paint. Compared with the water-based epoxy floor paint, the comprehensive performance of the water-based epoxy floor paint is still a certain difference from that of the solvent-based epoxy floor paint, and the solvent-based epoxy floor paint still occupies most of the market at present, but the market share of the water-based epoxy floor paint is larger and larger along with the continuous improvement and development of the water-based epoxy paint technology and formula.
The water-based epoxy paint on the market can be divided into two types according to the composition: (1) a two-component epoxy coating; (2) one-component epoxy coating. Compared with the single-component epoxy coating, the double-component epoxy coating has more excellent performance, more convenient use and wider application field. Thus, the current market is dominated by two-component waterborne epoxy coating products. The product mainly comprises two formula components: (1) A aqueous curing agent formulation components; (2) B epoxy resin formulation components.
Curing agents are of great interest as important base components for waterborne epoxy floor paint systems. However, most of the domestic aqueous curing agent market is occupied by foreign products. The domestic floor paint product is still immature and has poor emulsifying property. The aqueous curing agent can stabilize the emulsified epoxy resin in water only with excellent emulsifying property, and the two components can be fully contacted and completely cured in the mixing curing process.
Disclosure of Invention
In order to further improve the emulsification and solidification performance of the waterborne epoxy floor paint, the application provides a hydrogenated epoxy floor paint and a preparation method thereof.
In a first aspect, the present application provides a hydrogenated epoxy floor paint, which adopts the following technical scheme:
a hydrogenated epoxy floor paint comprises a material A and a material B; the material A comprises the following components in parts by weight: 90-95 parts of hydrogenated epoxy resin and 5-10 parts of trimethylolpropane triglycidyl ether; the material B comprises the following components in parts by weight: 30-40 parts of modified amine epoxy curing agent, 18-20 parts of titanium dioxide, 15-20 parts of barium sulfate, 0.5-1 part of propylene glycol methyl ether, 0.8-1.2 parts of dispersing agent, 0.1-0.5 part of defoamer, 0.1-0.5 part of wetting agent and 25-30 parts of deionized water; the weight ratio of the material A to the material B is (1-2) to (4-7); the preparation method of the modified amine epoxy curing agent comprises the following steps: s1, mixing E-51 epoxy resin, propylene glycol monomethyl ether and poly (propylene glycol) -tolyl-2, 4-diisocyanate in a blocking manner, reacting for 30-40min at 50-70 ℃, and then adding poly (ethylene glycol) methacrylate for continuous reaction for 15-20min to obtain an emulsion; s2, uniformly mixing the poly (dimethylsiloxane) -diglycidyl ether end-capped and propylene glycol monomethyl ether under the protection of nitrogen, then dropwise adding the mixture into diethylenetriamine, and reacting for 30-40min at 40-60 ℃ to obtain a modified amine solution; s3, uniformly stirring the emulsion, the E-51 epoxy resin and the propylene glycol monomethyl ether, slowly adding the mixture into a modified amine solution, reacting for 2-3 hours at 70-80 ℃, and adding deionized water to dilute the mixture after the reaction is finished to obtain the modified amine epoxy curing agent.
According to the technical scheme, hydrogenated epoxy resin is used as a base material, the viscosity of the hydrogenated epoxy resin is reduced by adding trimethylolpropane triglycidyl ether serving as an active diluent, the crosslinking density of a hydrogenated epoxy resin cured product is improved, and then modified amine epoxy curing agents with excellent emulsifying performance, which are prepared from diethylenetriamine, poly (dimethylsiloxane) -diglycidyl ether end-capped, E-51 epoxy resin, poly (propylene glycol) -tolyl-2, 4-diisocyanate and poly (ethylene glycol) methacrylate serving as raw materials, are mixed, and titanium pigment and barium sulfate filler, propylene glycol methyl ether, a dispersing agent, a defoaming agent and a wetting agent serving as auxiliary agents are used for emulsifying the hydrogenated epoxy resin into small particle size, so that the curing capacity of the hydrogenated epoxy resin cured product is improved, and the hydrogenated epoxy floor paint with excellent performance is obtained.
Preferably, the hydrogenated epoxy resin is a TaiLuck-ST3000 hydrogenated bisphenol A epoxy resin.
By adopting the technical scheme, the hydrogenated epoxy resin has low viscosity, high transparency, long-term non-discoloration, ultraviolet resistance and aging resistance, and is suitable for being used as an epoxy resin component in floor paint.
Preferably, the dispersing agent is one or two of a DISPUPER S27 dispersing agent and a DISPUPER S19 dispersing agent.
By adopting the technical scheme, the dispersing agent can enable the filler titanium dioxide and barium sulfate to be better dispersed in the epoxy system of the application, and improve the mechanical property of the hydrogenated epoxy floor paint.
Preferably, the wetting agent is a ZY-8131 organosilicon wetting agent.
By adopting the technical scheme, the wetting agent is favorable for reducing the dynamic surface tension of the hydrogenated epoxy floor paint, has good wettability and permeability, can be quickly leveled, and has low foam stability.
Preferably, the mass volume ratio of the E-51 epoxy resin, propylene glycol monomethyl ether, poly (propylene glycol) -tolyl-2, 4-diisocyanate end-capped mixture and the poly (ethylene glycol) methacrylate in the S1 is as follows: (10-20) g (2-3) mL (22-30) g (4-6) g.
By adopting the technical scheme, the emulsifier with excellent emulsifying property is obtained by introducing poly (propylene glycol) -tolyl-2, 4-diisocyanate and poly (ethylene glycol) methacrylate into the short chain of the E-51 epoxy resin.
Preferably, the mass volume ratio of the poly (dimethylsiloxane) -diglycidyl ether end-capped, propylene glycol monomethyl ether and diethylenetriamine in the S2 is: (7-16) g (5-8) mL (1-1.5) g.
By adopting the technical scheme, diethylenetriamine is used as basic amine, and poly (dimethylsiloxane) -diglycidyl ether is introduced for end-capping modification, so that the modified amine epoxy curing agent has good compatibility with hydrogenated epoxy resin.
Preferably, the volume ratio of the emulsion, the E-51 epoxy resin, the propylene glycol monomethyl ether, the modified amine solution and the deionized water in the S3 is as follows: (8-15) mL, (3-5) g, (4-6) mL, (12-16) mL and (20-40) mL.
By adopting the technical scheme, the emulsifier is added to the modified diethylenetriamine, and the compatibility of the modified amine epoxy curing agent and the hydrogenated epoxy resin is further adjusted, so that the curing capacity of the modified amine epoxy curing agent is improved, and the modified amine epoxy curing agent is fully crosslinked and cured.
In a second aspect, the present application provides a method for preparing a hydrogenated epoxy floor paint, comprising the steps of: (1) Adding trimethylolpropane triglycidyl ether while stirring by taking hydrogenated epoxy resin as a base material, stirring at 650rpm for 15min, and uniformly mixing to obtain a material A; (2) Adding deionized water while stirring by taking a modified amine epoxy curing agent as a base material, stirring at 600rpm for 20min, sequentially adding propylene glycol methyl ether, a defoaming agent, a wetting agent and a dispersing agent, uniformly stirring, and finally adding titanium dioxide and barium sulfate, wherein the stirring speed is increased to 1600rpm, and the stirring time is not less than 1h, so as to obtain a material B; (3) The material A and the material B are uniformly mixed according to a proportion, and the mixture can be used.
In summary, the present application has the following beneficial effects:
1. the hydrogenated epoxy resin is taken as a base material, the viscosity of the hydrogenated epoxy resin is reduced by adding the trimethylolpropane triglycidyl ether serving as an active diluent, the crosslinking density of a cured product of the hydrogenated epoxy resin is improved, then a self-made modified amine epoxy curing agent with excellent emulsifying property is matched, titanium dioxide and barium sulfate filler, propylene glycol methyl ether, a dispersing agent, a defoaming agent and a wetting agent are taken as auxiliary agents, the hydrogenated epoxy resin is emulsified into small particle size, the curing capacity of the hydrogenated epoxy resin is improved, and the hydrogenated epoxy floor paint with excellent performance is obtained by fully curing the hydrogenated epoxy resin.
2. The application takes diethylenetriamine as basic amine preferentially, and leads the modified amine epoxy hardener to have good compatibility with hydrogenated epoxy resin by introducing poly (dimethylsiloxane) -diglycidyl ether for end capping modification, and then leads poly (propylene glycol) -tolyl-2, 4-diisocyanate and poly (ethylene glycol) methacrylate to be used as emulsifying agents on E-51 epoxy resin short chain, and then adds the emulsifying agents to the modified diethylenetriamine, thereby further adjusting the compatibility of the modified amine epoxy hardener with the hydrogenated epoxy resin and further improving the curing capability of the modified amine epoxy hardener.
3. The hydrogenated epoxy resin floor paint prepared by the preparation method has the advantages of good emulsifying and curing properties, low viscosity, long pot life, excellent mechanical property, high tensile bonding strength with cement base materials, smooth and crack-free appearance of a coating film, and good storage stability and thermal stability of the prepared curing agent, and meets the use requirements of the actual market.
Detailed Description
The present application is described in further detail below with reference to examples.
The raw materials of the examples and comparative examples herein are commercially available in general unless otherwise specified.
The poly (propylene glycol) -tolyl-2, 4-diisocyanate end-capped number average molecular weight Mn is 2300.
The poly (dimethylsiloxane) diglycidyl ether capped number average molecular weight Mn was 800.
Examples
Example 1
A hydrogenated epoxy floor paint comprises a material A and a material B; the material A comprises the following components in parts by weight: 90g of hydrogenated epoxy resin and 5g of trimethylolpropane triglycidyl ether; the material B comprises the following components in parts by weight: 30g of modified amine epoxy curing agent, 18g of titanium dioxide, 15g of barium sulfate, 0.5g of propylene glycol methyl ether, 0.8g of dispersing agent, 0.1g of defoamer, 0.1g of wetting agent and 25g of deionized water; the weight ratio of the material A to the material B is 1:4.
The model of the hydrogenated epoxy resin is TaiLuck-ST3000 hydrogenated bisphenol A epoxy resin.
The dispersing agent is DISPUPER S27 dispersing agent.
The wetting agent is ZY-8131 organic silicon wetting agent.
The preparation method of the modified amine epoxy curing agent comprises the following steps: s1, mixing 10g of E-51 epoxy resin, 2mL of propylene glycol monomethyl ether and 22g of poly (propylene glycol) -tolyl-2, 4-diisocyanate end cap, reacting for 30min at 50 ℃, then adding 4g of poly (ethylene glycol) methacrylate, and continuing to react for 15min to obtain emulsion; s2, uniformly mixing 7g of poly (dimethylsiloxane) -diglycidyl ether end-capped with 5mL of propylene glycol monomethyl ether under the protection of nitrogen, then dropwise adding into 1g of diethylenetriamine, and reacting for 30min at 40 ℃ to obtain a modified amine solution; s3, 8mL of emulsion, 3g of E-51 epoxy resin and 4mL of propylene glycol monomethyl ether are stirred uniformly, then the mixture is slowly added into 12mL of modified amine solution, the mixture is reacted for 2h at 70 ℃, and 20mL of deionized water is added for dilution after the reaction is completed, so that the modified amine epoxy curing agent is obtained.
Example 2
A hydrogenated epoxy floor paint comprises a material A and a material B; the material A comprises the following components in parts by weight: 93g of hydrogenated epoxy resin and 8g of trimethylolpropane triglycidyl ether; the material B comprises the following components in parts by weight: 35g of modified amine epoxy hardener, 19g of titanium dioxide, 18g of barium sulfate, 0.8g of propylene glycol methyl ether, 1g of dispersant, 0.3g of defoamer, 0.3g of wetting agent and 28g of deionized water; the weight ratio of the material A to the material B is 2:6.
The model of the hydrogenated epoxy resin is TaiLuck-ST3000 hydrogenated bisphenol A epoxy resin.
The dispersing agent is DISPERS 19 dispersing agent.
The wetting agent is ZY-8131 organic silicon wetting agent.
The preparation method of the modified amine epoxy curing agent comprises the following steps: s1, mixing 15g of E-51 epoxy resin, 2.5mL of propylene glycol monomethyl ether and 28g of poly (propylene glycol) -tolyl-2, 4-diisocyanate end-capped, reacting for 35min at 60 ℃, then adding 5g of poly (ethylene glycol) methacrylate, and continuously reacting for 18min to obtain an emulsion; s2, uniformly mixing 12g of poly (dimethylsiloxane) -diglycidyl ether end-capped with 6mL of propylene glycol monomethyl ether under the protection of nitrogen, then dropwise adding into 1.3g of diethylenetriamine, and reacting for 35min at 50 ℃ to obtain a modified amine solution; s3, uniformly stirring 12mL of emulsion, 4g of E-51 epoxy resin and 5mL of propylene glycol monomethyl ether, slowly adding the mixture into 14mL of modified amine solution, reacting at 75 ℃ for 2.5h, and adding 30mL of deionized water for dilution after the reaction is completed to obtain the modified amine epoxy curing agent.
Example 3
A hydrogenated epoxy floor paint comprises a material A and a material B; the material A comprises the following components in parts by weight: 95g of hydrogenated epoxy resin and 10g of trimethylolpropane triglycidyl ether; the material B comprises the following components in parts by weight: 40g of modified amine epoxy hardener, 20g of titanium dioxide, 20g of barium sulfate, 1g of propylene glycol methyl ether, 1.2g of dispersant, 0.5g of defoamer, 0.5g of wetting agent and 30g of deionized water; the weight ratio of the material A to the material B is 2:7.
The model of the hydrogenated epoxy resin is TaiLuck-ST3000 hydrogenated bisphenol A epoxy resin.
The dispersing agent is a DISPUPER S27 dispersing agent and a DISPUPER S19 dispersing agent, which are uniformly mixed according to the mass ratio of 1:1.
The wetting agent is ZY-8131 organic silicon wetting agent.
The preparation method of the modified amine epoxy curing agent comprises the following steps: s1, mixing 20g of E-51 epoxy resin, 3mL of propylene glycol monomethyl ether and 30g of poly (propylene glycol) -tolyl-2, 4-diisocyanate end-capped, reacting at 70 ℃ for 40min, and then adding 6g of poly (ethylene glycol) methacrylate for continuous reaction for 20min to obtain an emulsion; s2, uniformly mixing 16g of poly (dimethylsiloxane) -diglycidyl ether end-capped with 8mL of propylene glycol monomethyl ether under the protection of nitrogen, then dropwise adding into 1.5g of diethylenetriamine, and reacting for 40min at 60 ℃ to obtain a modified amine solution; s3, 15mL of emulsion, 5g of E-51 epoxy resin and 6mL of propylene glycol monomethyl ether are stirred uniformly, then the mixture is slowly added into 16mL of modified amine solution, the mixture is reacted for 3 hours at 80 ℃, and 40mL of deionized water is added for dilution after the reaction is completed, so that the modified amine epoxy curing agent is obtained.
The preparation method of the hydrogenated epoxy floor paint comprises the following steps: (1) Adding trimethylolpropane triglycidyl ether while stirring by taking hydrogenated epoxy resin as a base material, stirring at 650rpm for 15min, and uniformly mixing to obtain a material A; (2) Adding deionized water while stirring by taking a modified amine epoxy curing agent as a base material, stirring at 600rpm for 20min, sequentially adding propylene glycol methyl ether, a defoaming agent, a wetting agent and a dispersing agent, uniformly stirring, and finally adding titanium dioxide and barium sulfate, wherein the stirring speed is increased to 1600rpm, and the stirring time is 1.5h, so that a material B is obtained; and (3) uniformly mixing the material A and the material B according to a proportion.
Comparative example
Comparative example 1
The same as in example 1, except that "poly (propylene glycol) -tolyl-2, 4-diisocyanate end-capping" was replaced with an equimolar amount of "isophorone diisocyanate".
Comparative example 2
The same as in example 1, except that the "poly (dimethylsiloxane) -diglycidyl ether cap" was replaced with an equal mass of "polypropylene glycol diglycidyl ether".
Comparative example 3
The same as in example 1, except that the "emulsion" in S3 was removed.
Performance test
The hydrogenated epoxy floor paints prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to the following performance tests.
1. Odor measurement of hydrogenated epoxy floor paint:
the odor test of the hydrogenated epoxy floor paint adopts a direct olfaction test method, the prepared hydrogenated epoxy floor paint is placed in a glass bottle for sealing, the glass bottle is placed in a constant temperature box at 55 ℃, after the glass bottle is placed for 1h, the sealing cover is opened, and the hydrogenated epoxy floor paint is close to a nose for judging whether the odor exists.
2. And (3) measuring the viscosity of a hydrogenated epoxy floor paint mixed system:
the test was performed using a rotational viscometer: and (3) placing the hydrogenated epoxy floor paint in a sample bottle, drying for 1h at 25 ℃, estimating the size according to the viscosity, selecting a proper rotor and rotating speed, vertically pouring the rotor into the hydrogenated epoxy floor paint until the liquid level of the hydrogenated epoxy floor paint is flush with the surface of the liquid level of the rotor, measuring the viscosity value of the hydrogenated epoxy floor paint at 25 ℃, measuring three times in parallel, and taking a viscosity average value.
3. Determination of pot life of hydrogenated epoxy floor paint:
the pot life was determined according to GB5206.5-91 by measuring the change in the mixed viscosity of the hydrogenated epoxy floor paint over time.
4. Thermal storage stability test of curing agent:
storage stability test method: storing the modified amine epoxy curing agent in a closed glass bottle, measuring the appearance change of the curing agent every one month at a dark and dull place, and recording the time of layering phenomenon.
The heat stability test method of the curing agent comprises the following steps: adding water into the prepared modified amine epoxy hardener according to the mass ratio of 1:1, stirring and dissolving the mixture into a uniform solution, then gradually raising the temperature, and recording the temperature when layering phenomenon occurs in the hardener.
5. Coating appearance test:
and (3) curing the prepared hydrogenated epoxy floor paint film for 7 days and 28 days at room temperature by adopting a visual inspection method, and observing whether pinholes, shrinkage, cracking and the like appear on the surface of the film.
6. And (3) testing tensile bonding strength of the hydrogenated epoxy floor paint coating:
the tensile bond strength test method adopts a manual drawing type adhesive force instrument for testing (measurement principle: through drawing type adhesive force instrument)
The adhesive force meter separates the unit area of the coating film from the whole coating film, the hydrogenated epoxy floor paint is coated on a cement board, and the test is carried out after curing for 7 days at normal temperature. The hydrogenated epoxy floor paint coating material requires that the tensile bonding strength of the cured coating film is more than or equal to 2MPa and can reach the application standard.
The above test results are shown in Table 1:
TABLE 1 hydrogenated epoxy floor paint Performance test results
As can be seen from Table 1, the viscosity of the hydrogenated epoxy floor paint prepared in examples 1-3 is 2557-2607 mPa.S, the pot life is up to 110min, the application performance is met, the mechanical property is excellent, the tensile bonding strength with a cement base material is up to 4.83MPa, the application performance of the epoxy floor paint is met, the appearance of a coating film is smooth and has no crack, the storage stability of the prepared curing agent is up to 7 months, the thermal stability can be up to 78 ℃, and the use requirement of the actual market is met. It can be seen from the combination of comparative examples 1 to 3 that the addition of poly (propylene glycol) -tolyl-2, 4-diisocyanate was slightly increased in viscosity, but longer in pot life, and better in storage stability and thermal stability, compared to isophorone diisocyanate, probably because the poly (propylene glycol) -tolyl-2, 4-diisocyanate was blocked with more ether bonds, the oxygen atoms of which were hydrogen bonded with the hydrogen atoms in water, improving the water solubility of the curing agent and making it more stable. Compared with polypropylene glycol diglycidyl ether, the hydrogenated epoxy floor paint has the advantages that the added poly (dimethylsiloxane) -diglycidyl ether is blocked, the appearance of the coating film of the hydrogenated epoxy floor paint is smooth and smooth, and the cracking is less, probably because the added poly (dimethylsiloxane) -diglycidyl ether is blocked, compared with the structure of the polypropylene glycol diglycidyl ether, more methyl groups are added, the hydrophilicity is slightly reduced, the compatibility with epoxy resin is better, the internal stress of the epoxy resin is reduced, and the problem that the hydrogenated epoxy resin is brittle and easy to crack is solved. Compared with the traditional amine solution curing agent, the hydrogenated epoxy floor paint prepared by using the modified amine epoxy curing agent of the emulsion has better performance, and probably because the modified amine epoxy curing agent has good self-emulsifying performance after the emulsion is added, better compatibility with the hydrogenated epoxy resin in aqueous dispersion and more complete curing and crosslinking reaction, the prepared cured coating has better performance, strong tensile bonding strength, relatively lower viscosity and better construction performance.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, insofar as they are protected by the patent laws within the scope of protection of the present application.
Claims (8)
1. The hydrogenated epoxy floor paint is characterized by comprising a material A and a material B; the material A comprises the following components in parts by weight: 90-95 parts of hydrogenated epoxy resin and 5-10 parts of trimethylolpropane triglycidyl ether; the material B comprises the following components in parts by weight: 30-40 parts of modified amine epoxy curing agent, 18-20 parts of titanium dioxide, 15-20 parts of barium sulfate, 0.5-1 part of propylene glycol methyl ether, 0.8-1.2 parts of dispersing agent, 0.1-0.5 part of defoamer, 0.1-0.5 part of wetting agent and 25-30 parts of deionized water; the weight ratio of the material A to the material B is (1-2) to (4-7); the preparation method of the modified amine epoxy curing agent comprises the following steps: s1, mixing E-51 epoxy resin, propylene glycol monomethyl ether and poly (propylene glycol) -tolyl-2, 4-diisocyanate in a blocking manner, reacting for 30-40min at 50-70 ℃, and then adding poly (ethylene glycol) methacrylate for continuous reaction for 15-20min to obtain an emulsion; s2, uniformly mixing the poly (dimethylsiloxane) -diglycidyl ether end-capped and propylene glycol monomethyl ether under the protection of nitrogen, then dropwise adding the mixture into diethylenetriamine, and reacting for 30-40min at 40-60 ℃ to obtain a modified amine solution; s3, uniformly stirring the emulsion, the E-51 epoxy resin and the propylene glycol monomethyl ether, slowly adding the mixture into a modified amine solution, reacting for 2-3 hours at 70-80 ℃, and adding deionized water to dilute the mixture after the reaction is finished to obtain the modified amine epoxy curing agent.
2. The hydrogenated epoxy floor paint of claim 1, wherein the hydrogenated epoxy resin is a TaiLuck-ST3000 hydrogenated bisphenol a epoxy resin.
3. The hydrogenated epoxy floor paint according to claim 2, wherein the dispersant is one or both of a dispeuper S27 dispersant and a dispeupers 19 dispersant.
4. A hydrogenated epoxy floor paint according to claim 3, wherein the wetting agent is ZY-8131 silicone wetting agent.
5. The hydrogenated epoxy floor paint according to claim 4, wherein the mass-volume ratio of the E-51 epoxy resin, propylene glycol monomethyl ether, poly (propylene glycol) -tolyl-2, 4-diisocyanate end-capped mixed poly (ethylene glycol) methacrylate in S1 is: (10-20) g (2-3) mL (22-30) g (4-6) g.
6. The hydrogenated epoxy floor paint according to claim 5, wherein the mass-to-volume ratio of poly (dimethylsiloxane) -diglycidyl ether terminated, propylene glycol monomethyl ether, diethylenetriamine in S2 is: (7-16) g (5-8) mL (1-1.5) g.
7. The hydrogenated epoxy floor paint according to claim 6, wherein the volume ratio of the emulsion, the E-51 epoxy resin, the propylene glycol monomethyl ether, the modified amine solution and the deionized water in the S3 is: (8-15) mL, (3-5) g, (4-6) mL, (12-16) mL and (20-40) mL.
8. A process for the preparation of a hydrogenated epoxy floor paint, characterized in that it is based on any one of claims 1 to 7, comprising the following steps: (1) Adding trimethylolpropane triglycidyl ether while stirring by taking hydrogenated epoxy resin as a base material, stirring at 650rpm for 15min, and uniformly mixing to obtain a material A; (2) Adding deionized water while stirring by taking a modified amine epoxy curing agent as a base material, stirring at 600rpm for 20min, sequentially adding propylene glycol methyl ether, a defoaming agent, a wetting agent and a dispersing agent, uniformly stirring, and finally adding titanium dioxide and barium sulfate, wherein the stirring speed is increased to 1600rpm, and the stirring time is not less than 1h, so as to obtain a material B; (3) The material A and the material B are uniformly mixed according to a proportion, and the mixture can be used.
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