CN114133829A - Antibacterial waterproof epoxy floor paint and preparation method thereof - Google Patents
Antibacterial waterproof epoxy floor paint and preparation method thereof Download PDFInfo
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- CN114133829A CN114133829A CN202111569210.9A CN202111569210A CN114133829A CN 114133829 A CN114133829 A CN 114133829A CN 202111569210 A CN202111569210 A CN 202111569210A CN 114133829 A CN114133829 A CN 114133829A
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- epoxy resin
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- floor paint
- itaconic acid
- epoxy
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- 239000004593 Epoxy Substances 0.000 title claims abstract description 58
- 239000003973 paint Substances 0.000 title claims abstract description 49
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000003822 epoxy resin Substances 0.000 claims abstract description 77
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 77
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims abstract description 67
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000002156 mixing Methods 0.000 claims abstract description 35
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 31
- 239000000945 filler Substances 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002216 antistatic agent Substances 0.000 claims abstract description 15
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 15
- 239000002562 thickening agent Substances 0.000 claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 48
- 238000010438 heat treatment Methods 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 30
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 30
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 28
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 21
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- 238000010992 reflux Methods 0.000 claims description 19
- XFNJYAKDBJUJAJ-UHFFFAOYSA-N 1,2-dibromopropane Chemical compound CC(Br)CBr XFNJYAKDBJUJAJ-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000005639 Lauric acid Substances 0.000 claims description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 15
- -1 tetradecyl tertiary amine Chemical class 0.000 claims description 15
- NHQDETIJWKXCTC-UHFFFAOYSA-N 3-chloroperbenzoic acid Chemical compound OOC(=O)C1=CC=CC(Cl)=C1 NHQDETIJWKXCTC-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 11
- 239000006004 Quartz sand Substances 0.000 claims description 8
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 7
- BHELZAPQIKSEDF-UHFFFAOYSA-N allyl bromide Chemical compound BrCC=C BHELZAPQIKSEDF-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000003242 anti bacterial agent Substances 0.000 claims 1
- 230000003115 biocidal effect Effects 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 2
- 238000004332 deodorization Methods 0.000 abstract description 2
- 229920006334 epoxy coating Polymers 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract description 2
- 230000008023 solidification Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 229910000042 hydrogen bromide Inorganic materials 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- XSVQKTDPCLNSPD-UHFFFAOYSA-N C=CC.[Br] Chemical compound C=CC.[Br] XSVQKTDPCLNSPD-UHFFFAOYSA-N 0.000 description 2
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000012360 testing method 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
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Plant Pathology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses an antibacterial waterproof epoxy floor paint and a preparation method thereof, wherein the floor paint is prepared by mixing a component A and a component B according to the mass part ratio of 1-1.5:3, the component A comprises 50-60 parts of epoxy resin, 20-25 parts of modified epoxy resin, 0.2-0.4 part of antistatic agent, 1-1.5 parts of filler and 0.5-1 part of emulsifier according to the following parts by weight, and the component B comprises 40-50 parts of epoxy curing agent, 1-3 parts of curing accelerator, 0.2-0.3 part of thickening agent and 0.5-1 part of defoaming agent according to the following parts by weight. Itaconic acid has been added to this application, and itaconic acid has good adhesive force to certain deodorization nature has, because its self has two active carboxyls and double bond, makes its chemical property active, consequently this application uses bisphenol A type epoxy diglycidyl ether to react rather than, generates the epoxy that contains the bio-based, the coating that obtains after the solidification is for the better effect of traditional epoxy coating performance.
Description
Technical Field
The invention relates to the technical field of floor paint preparation, in particular to an antibacterial waterproof epoxy floor paint and a preparation method thereof.
Background
The epoxy floor paint has the advantages that the epoxy floor paint has strong acid and strong alkali resistance, wear resistance and skid resistance, so that the epoxy floor paint has wide application range, and the epoxy floor paint has the advantages that the main component is epoxy resin, the epoxy resin reacts with a curing agent, and the epoxy floor paint is crosslinked into macromolecules with a net structure, so that various excellent performances can be displayed.
With the advancement of science and technology, the bio-based epoxy resin gradually enters the sight of people, and belongs to renewable energy sources, so that the consumption of petrochemical products can be reduced, the harm to the environment can be reduced, the practical value and the utilization space are high, byproducts are inevitably generated in the preparation process, the overall quality of the product is influenced by the generation of the byproducts, and the invention is particularly important in order to improve the product quality and endow the product with certain antibacterial performance.
Disclosure of Invention
The invention aims to provide an antibacterial waterproof epoxy floor paint and a preparation method thereof, and aims to solve the problems in the background art.
In order to solve the technical problems, the invention provides the following technical scheme: an antibacterial waterproof epoxy floor paint is prepared by mixing a component A and a component B according to the mass part ratio of 1-1.5: 3;
the component A comprises the following raw materials, by weight, 50-60 parts of epoxy resin, 20-25 parts of modified epoxy resin, 0.2-0.4 part of antistatic agent, 1-1.5 parts of filler and 0.5-1 part of emulsifier;
the component B comprises the following raw materials, by weight, 40-50 parts of an epoxy curing agent, 1-3 parts of a curing accelerator, 0.2-0.3 part of a thickening agent and 0.5-1 part of a defoaming agent.
Further, the modified epoxy resin is prepared from bisphenol A type epoxy resin diglycidyl ether and modified itaconic acid.
Further, the modified itaconic acid is prepared from propylene bromide, itaconic acid, N-dimethylformamide and m-chloroperoxybenzoic acid, wherein the mass ratio of the propylene bromide to the itaconic acid is 1.4-1.5: 1.
Further, the epoxy curing agent is a mixture of ethylenediamine and diethylenetriamine.
Further, the defoaming agent is one of a high alcohol defoaming agent and an organic silicon dioxide defoaming agent.
Furthermore, the filler is quartz sand, titanium dioxide and talcum powder.
A preparation method of antibacterial waterproof epoxy floor paint comprises the following steps,
(1) preparation of modified epoxy resin:
adding a solvent into bisphenol A type epoxy resin diglycidyl ether, stirring, adding N, N-dimethylformamide, allyl bromide and potassium hydroxide, stirring for 15-18min, heating at 60-63 ℃, and refluxing for 10-12h to obtain modified itaconic acid;
adding dichloromethane and m-chloroperoxybenzoic acid into the obtained modified itaconic acid, heating at 40-45 ℃ for 4-5 days to obtain modified epoxy resin, and condensing and recovering evaporated gas;
when itaconic acid and bromine allyl are reacted at 60-63 ℃, hydrogen bromide is removed, and hydrogen bromide is generated.
(2) And (3) recovery treatment:
mixing lauric acid and sulfuric acid, stirring and adding the obtained recovered liquid, heating at 90-95 ℃, refluxing for 8-9h, cooling, preserving heat at 30-32 ℃ for 8-8.5h, layering, adding alkali liquor, and adjusting pH to obtain a mixture A;
secondly, adding thiourea and ethanol into the mixture A, heating under reflux, adding sodium hydroxide and deionized water, reacting for 2-2.5h, separating and taking an oil phase, and heating to 165-168 ℃ to obtain a mixture B;
according to the preparation method, lauric acid and sulfuric acid are added to react with hydrogen bromide, thiourea and ethanol are added to react after the reaction is finished, a dodecyl mercaptan compound can be obtained, the antibacterial performance of the product coating can be improved due to the addition of the dodecyl mercaptan compound, and the dodecyl mercaptan compound can be added into the preparation process of modified epoxy resin in the continuous production process, so that the polymerization degree of the obtained modified epoxy resin is controlled, and the phenomena that the cross-linking of functional groups is excessive, the molecular weight is too large, and the quality of the product is reduced are avoided.
(3) Preparing floor paint:
adding absolute ethyl alcohol into the obtained modified epoxy resin, adding tetradecyl tertiary amine in an inert atmosphere for 2-3h, heating to 50 ℃ after the reaction is finished, and preserving heat for 24-25 h;
according to the method, for the purpose of fully utilizing itaconic acid, the amount of added propylene bromide is limited, the mass ratio of the added propylene bromide to the itaconic acid is 1.4-1.5:1, the full utilization of the itaconic acid can be guaranteed, but partial propylene bromide is generated to be remained.
Secondly, mixing and stirring the epoxy resin, the mixture B and the modified epoxy resin, adding an emulsifier, an antistatic agent and a filler, and uniformly stirring to obtain a component A;
mixing the epoxy curing agent, the curing accelerator and the thickening agent, stirring, adding the defoaming agent, and uniformly stirring to obtain a component B;
and fourthly, mixing the component A and the component B, coating the mixture on the surface of a carrier, and curing to obtain the floor paint.
Further, in the step (1), the solvent added is acetone.
Further, in the step (2), the mass ratio of the added lauric acid, thiourea and itaconic acid is 1.53-1.54: 0.58: 1.
this application can produce the hydrogen bromide accessory substance through the add volume of control lauric acid and thiourea and react, can also reduce the residual quantity of lauric acid and thiourea to minimum, and then guaranteed the quality of product.
Further, in the step (3), the mass ratio of the tetradecyl tertiary amine to the itaconic acid is 0.9-0.92: 1.
The method controls the adding amount of the tetradecylamine, ensures that the mass ratio of the adding amount to the itaconic acid is 0.9-0.92:1, further can ensure that the residual propylene bromine after the preparation of the modified epoxy resin is finished can be completely converted into the quaternary ammonium salt, and can also ensure that the residual amount of the tetradecylamine in the product is the lowest.
Compared with the prior art, the invention has the following beneficial effects: itaconic acid has been added to this application, and itaconic acid has good adhesive force to certain deodorization nature has, because its self has two active carboxyls and double bond, makes its chemical property active, consequently this application uses bisphenol A type epoxy diglycidyl ether to react rather than, generates the epoxy that contains the bio-based, and the coating that obtains after the solidification is better for traditional epoxy coating performance.
The filler is added, the filler is composed of quartz sand, titanium dioxide and talcum powder, and the waterproof and anti-skid performance of the product coating can be improved after the filler is added.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An antibacterial waterproof epoxy floor paint is prepared by mixing a component A and a component B according to the mass part ratio of 1: 3;
the component A comprises the following raw materials, by weight, 50 parts of epoxy resin, 20 parts of modified epoxy resin, 0.2 part of antistatic agent, 1 part of filler and 0.5 part of emulsifier;
the component B comprises the following raw materials, by weight, 40 parts of an epoxy curing agent, 1 part of a curing accelerator, 0.2 part of a thickening agent and 0.5 part of a defoaming agent.
The modified epoxy resin is prepared from bisphenol A type epoxy resin diglycidyl ether and modified itaconic acid.
The modified itaconic acid is prepared from propylene bromide, itaconic acid, N-dimethylformamide and m-chloroperoxybenzoic acid, wherein the mass ratio of the propylene bromide to the itaconic acid is 1.4: 1.
The epoxy curing agent is a mixture of ethylenediamine and diethylenetriamine.
The defoaming agent is a high-carbon alcohol defoaming agent.
The filler is quartz sand, titanium dioxide and talcum powder.
A preparation method of antibacterial waterproof epoxy floor paint comprises the following steps,
(1) preparation of modified epoxy resin:
adding acetone into bisphenol A type epoxy resin diglycidyl ether, stirring, adding N, N-dimethylformamide, allyl bromide and potassium hydroxide, stirring for 15min, heating at 60 ℃, and refluxing for 10h to obtain modified itaconic acid;
adding dichloromethane and m-chloroperoxybenzoic acid into the obtained modified itaconic acid, heating at 40 ℃ for 4 days to obtain modified epoxy resin, and condensing and recovering evaporated gas;
(2) and (3) recovery treatment:
mixing lauric acid and sulfuric acid, wherein the mass ratio of the added lauric acid to the added itaconic acid is 1.53: 1, stirring and adding the obtained recovered liquid, heating at 90 ℃, refluxing for 8 hours, cooling, preserving heat at 30 ℃ for 8 hours, layering, adding alkali liquor, and adjusting pH to obtain a mixture A;
adding thiourea and ethanol into the mixture A, wherein the mass ratio of the thiourea to the itaconic acid is 0.58: 1, heating under reflux, adding sodium hydroxide and deionized water, reacting for 2 hours, separating to obtain an oil phase, and heating to 165 ℃ to obtain a mixture B;
(3) preparing floor paint:
adding absolute ethyl alcohol into the obtained modified epoxy resin, adding tetradecyl tertiary amine in an inert atmosphere, wherein the mass ratio of the tetradecyl tertiary amine to the itaconic acid is 0.9:1, the reaction time is 2 hours, heating to 50 ℃ after the reaction is finished, and keeping the temperature for 24 hours;
secondly, mixing and stirring the epoxy resin, the mixture B and the modified epoxy resin, adding an emulsifier, an antistatic agent and a filler, and uniformly stirring to obtain a component A;
mixing the epoxy curing agent, the curing accelerator and the thickening agent, stirring, adding the defoaming agent, and uniformly stirring to obtain a component B;
and fourthly, mixing the component A and the component B, coating the mixture on the surface of a carrier, and curing to obtain the floor paint.
Example 2
An antibacterial waterproof epoxy floor paint is prepared by mixing a component A and a component B according to the mass part ratio of 1.2: 3;
the component A comprises the following raw materials, by weight, 55 parts of epoxy resin, 23 parts of modified epoxy resin, 0.3 part of antistatic agent, 1.2 parts of filler and 0.8 part of emulsifier;
the component B comprises the following raw materials, by weight, 45 parts of an epoxy curing agent, 2 parts of a curing accelerator, 0.3 part of a thickening agent and 0.8 part of a defoaming agent.
The modified epoxy resin is prepared from bisphenol A type epoxy resin diglycidyl ether and modified itaconic acid.
The modified itaconic acid is prepared from propylene bromide, itaconic acid, N-dimethylformamide and m-chloroperoxybenzoic acid, wherein the mass ratio of the propylene bromide to the itaconic acid is 1.45: 1.
The epoxy curing agent is a mixture of ethylenediamine and diethylenetriamine.
The defoaming agent is an organic silicon dioxide defoaming agent.
The filler is quartz sand, titanium dioxide and talcum powder.
A preparation method of antibacterial waterproof epoxy floor paint comprises the following steps,
(1) preparation of modified epoxy resin:
adding acetone into bisphenol A type epoxy resin diglycidyl ether, stirring, adding N, N-dimethylformamide, allyl bromide and potassium hydroxide, stirring for 17min, heating at 62 ℃, and refluxing for 11h to obtain modified itaconic acid;
adding dichloromethane and m-chloroperoxybenzoic acid into the obtained modified itaconic acid, heating at 43 ℃ for 5 days to obtain modified epoxy resin, and condensing and recovering evaporated gas;
(2) and (3) recovery treatment:
mixing lauric acid and sulfuric acid, wherein the mass ratio of the added lauric acid to the added itaconic acid is 1.54: 1, stirring and adding the obtained recovered liquid, heating at 93 ℃, refluxing for 8 hours, cooling, preserving heat at 31 ℃ for 8-8.5 hours, layering, adding alkali liquor, and adjusting pH to obtain a mixture A;
adding thiourea and ethanol into the mixture A, wherein the mass ratio of the thiourea to the itaconic acid is 0.58: 1, heating under reflux, adding sodium hydroxide and deionized water, reacting for 2.5h, separating to obtain an oil phase, and heating to 167 ℃ to obtain a mixture B;
(3) preparing floor paint:
adding absolute ethyl alcohol into the obtained modified epoxy resin, adding tetradecyl tertiary amine in an inert atmosphere, wherein the mass ratio of the tetradecyl tertiary amine to the itaconic acid is 0.91:1, the reaction time is 2.5h, heating to 50 ℃ after the reaction is finished, and keeping the temperature for 25 h;
secondly, mixing and stirring the epoxy resin, the mixture B and the modified epoxy resin, adding an emulsifier, an antistatic agent and a filler, and uniformly stirring to obtain a component A;
mixing the epoxy curing agent, the curing accelerator and the thickening agent, stirring, adding the defoaming agent, and uniformly stirring to obtain a component B;
and fourthly, mixing the component A and the component B, coating the mixture on the surface of a carrier, and curing to obtain the floor paint.
Example 3
An antibacterial waterproof epoxy floor paint is prepared by mixing a component A and a component B according to the mass part ratio of 1.5: 3;
the component A comprises the following raw materials, by weight, 60 parts of epoxy resin, 25 parts of modified epoxy resin, 0.4 part of antistatic agent, 1.5 parts of filler and 1 part of emulsifier;
the component B comprises 50 parts of epoxy curing agent, 1-3 parts of curing accelerator, 0.3 part of thickening agent and 1 part of defoaming agent by weight.
The modified epoxy resin is prepared from bisphenol A type epoxy resin diglycidyl ether and modified itaconic acid.
The modified itaconic acid is prepared from propylene bromide, itaconic acid, N-dimethylformamide and m-chloroperoxybenzoic acid, wherein the mass ratio of the propylene bromide to the itaconic acid is 1.5: 1.
The epoxy curing agent is a mixture of ethylenediamine and diethylenetriamine.
The defoaming agent is a high-carbon alcohol defoaming agent.
The filler is quartz sand, titanium dioxide and talcum powder.
A preparation method of antibacterial waterproof epoxy floor paint comprises the following steps,
(1) preparation of modified epoxy resin:
adding acetone into bisphenol A type epoxy resin diglycidyl ether, stirring, adding N, N-dimethylformamide, allyl bromide and potassium hydroxide, stirring for 18min, heating at 63 ℃, and refluxing for 12h to obtain modified itaconic acid;
adding dichloromethane and m-chloroperoxybenzoic acid into the obtained modified itaconic acid, heating at 45 ℃ for 5 days to obtain modified epoxy resin, and condensing and recovering evaporated gas;
(2) and (3) recovery treatment:
mixing lauric acid and sulfuric acid, wherein the mass ratio of the added lauric acid to the added itaconic acid is 1.54: 1, stirring and adding the obtained recovered liquid, heating at 95 ℃, refluxing for 9 hours, cooling, preserving heat at 32 ℃, preserving heat for 8.5 hours, layering, adding alkali liquor, and adjusting pH to obtain a mixture A;
adding thiourea and ethanol into the mixture A, wherein the mass ratio of the thiourea to the itaconic acid is 0.58: 1, heating under reflux, adding sodium hydroxide and deionized water, reacting for 2.5h, separating to obtain an oil phase, and heating to 168 ℃ to obtain a mixture B;
(3) preparing floor paint:
adding absolute ethyl alcohol into the obtained modified epoxy resin, adding tetradecyl tertiary amine in an inert atmosphere, wherein the mass ratio of the tetradecyl tertiary amine to the itaconic acid is 0.92:1, the reaction time is 3 hours, heating to 50 ℃ after the reaction is finished, and keeping the temperature for 25 hours;
secondly, mixing and stirring the epoxy resin, the mixture B and the modified epoxy resin, adding an emulsifier, an antistatic agent and a filler, and uniformly stirring to obtain a component A;
mixing the epoxy curing agent, the curing accelerator and the thickening agent, stirring, adding the defoaming agent, and uniformly stirring to obtain a component B;
and fourthly, mixing the component A and the component B, coating the mixture on the surface of a carrier, and curing to obtain the floor paint.
Comparative example 1
An antibacterial waterproof epoxy floor paint is prepared by mixing a component A and a component B according to the mass part ratio of 1.5: 3;
the component A comprises the following raw materials, by weight, 60 parts of epoxy resin, 25 parts of modified epoxy resin, 0.4 part of antistatic agent, 1.5 parts of filler and 1 part of emulsifier;
the component B comprises 50 parts of epoxy curing agent, 1-3 parts of curing accelerator, 0.3 part of thickening agent and 1 part of defoaming agent by weight.
The modified epoxy resin is prepared from bisphenol A type epoxy resin diglycidyl ether and modified itaconic acid.
The modified itaconic acid is prepared from propylene bromide, itaconic acid, N-dimethylformamide and m-chloroperoxybenzoic acid, wherein the mass ratio of the propylene bromide to the itaconic acid is 1.5: 1.
The epoxy curing agent is a mixture of ethylenediamine and diethylenetriamine.
The defoaming agent is a high-carbon alcohol defoaming agent.
The filler is quartz sand, titanium dioxide and talcum powder.
A preparation method of antibacterial waterproof epoxy floor paint comprises the following steps,
(1) preparation of modified epoxy resin:
adding acetone into bisphenol A type epoxy resin diglycidyl ether, stirring, adding N, N-dimethylformamide, allyl bromide and potassium hydroxide, stirring for 18min, heating at 63 ℃, and refluxing for 12h to obtain modified itaconic acid;
adding dichloromethane and m-chloroperoxybenzoic acid into the obtained modified itaconic acid, heating at 45 ℃ and reacting for 5 days to obtain modified epoxy resin;
(2) preparing floor paint:
adding absolute ethyl alcohol into the obtained modified epoxy resin, adding tetradecyl tertiary amine in an inert atmosphere, wherein the mass ratio of the tetradecyl tertiary amine to the itaconic acid is 0.92:1, the reaction time is 3 hours, heating to 50 ℃ after the reaction is finished, and keeping the temperature for 25 hours;
secondly, mixing and stirring the epoxy resin and the modified epoxy resin, adding the emulsifier, the antistatic agent and the filler, and uniformly stirring to obtain a component A;
mixing the epoxy curing agent, the curing accelerator and the thickening agent, stirring, adding the defoaming agent, and uniformly stirring to obtain a component B;
and fourthly, mixing the component A and the component B, coating the mixture on the surface of a carrier, and curing to obtain the floor paint.
Comparative example 2
An antibacterial waterproof epoxy floor paint is prepared by mixing a component A and a component B according to the mass part ratio of 1.5: 3;
the component A comprises the following raw materials, by weight, 60 parts of epoxy resin, 25 parts of modified epoxy resin, 0.4 part of antistatic agent, 1.5 parts of filler and 1 part of emulsifier;
the component B comprises 50 parts of epoxy curing agent, 1-3 parts of curing accelerator, 0.3 part of thickening agent and 1 part of defoaming agent by weight.
The modified epoxy resin is prepared from bisphenol A type epoxy resin diglycidyl ether and modified itaconic acid.
The modified itaconic acid is prepared from propylene bromide, itaconic acid, N-dimethylformamide and m-chloroperoxybenzoic acid, wherein the mass ratio of the propylene bromide to the itaconic acid is 1.5: 1.
The epoxy curing agent is a mixture of ethylenediamine and diethylenetriamine.
The defoaming agent is a high-carbon alcohol defoaming agent.
The filler is quartz sand, titanium dioxide and talcum powder.
A preparation method of antibacterial waterproof epoxy floor paint comprises the following steps,
(1) preparation of modified epoxy resin:
adding acetone into bisphenol A type epoxy resin diglycidyl ether, stirring, adding N, N-dimethylformamide, allyl bromide and potassium hydroxide, stirring for 18min, heating at 63 ℃, and refluxing for 12h to obtain modified itaconic acid;
adding dichloromethane and m-chloroperoxybenzoic acid into the obtained modified itaconic acid, heating at 45 ℃ for 5 days to obtain modified epoxy resin, and condensing and recovering evaporated gas;
(2) and (3) recovery treatment:
mixing lauric acid and sulfuric acid, wherein the mass ratio of the added lauric acid to the added itaconic acid is 1.54: 1, stirring and adding the obtained recovered liquid, heating at 95 ℃, refluxing for 9 hours, cooling, preserving heat at 32 ℃, preserving heat for 8.5 hours, layering, adding alkali liquor, and adjusting pH to obtain a mixture A;
adding thiourea and ethanol into the mixture A, wherein the mass ratio of the thiourea to the itaconic acid is 0.58: 1, heating under reflux, adding sodium hydroxide and deionized water, reacting for 2.5h, separating to obtain an oil phase, and heating to 168 ℃ to obtain a mixture B;
(3) preparing floor paint:
firstly, mixing and stirring the epoxy resin, the mixture B and the modified epoxy resin, adding an emulsifier, an antistatic agent and a filler, and uniformly stirring to obtain a component A;
mixing the epoxy curing agent, the curing accelerator and the thickening agent, stirring, adding the defoaming agent, and uniformly stirring to obtain a component B;
and thirdly, mixing the component A and the component B, coating the mixture on the surface of a carrier, and curing to obtain the floor paint.
Experiment of
And (3) setting comparative example 1 and comparative example 2 to carry out a control experiment by taking the example 3 as a control, wherein the comparative example 1 does not carry out recovery treatment on the hydrogen bromide, and the comparative example 2 does not carry out treatment on residual propylene bromine to carry out the control experiment.
The antibacterial performance tests of example 1, example 2, example 3, comparative example 1 and comparative example 2 are carried out according to GB/T-21866-2008, the test results are as follows,
watch 1
In comparative example 1, hydrogen bromide is not recovered, so that the inhibition rate is lower than that of example 1, example 2 and example 3.
In comparative example 2, the residual propylene bromide was not treated, so that the bacteriostatic rate was low compared to example 1, example 2, and example 3.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides an antibiotic waterproof epoxy floor paint which characterized in that: the floor paint is formed by mixing a component A and a component B according to the mass part ratio of 1-1.5: 3;
the component A comprises the following raw materials, by weight, 50-60 parts of epoxy resin, 20-25 parts of modified epoxy resin, 0.2-0.4 part of antistatic agent, 1-1.5 parts of filler and 0.5-1 part of emulsifier;
the component B comprises the following raw materials, by weight, 40-50 parts of an epoxy curing agent, 1-3 parts of a curing accelerator, 0.2-0.3 part of a thickening agent and 0.5-1 part of a defoaming agent.
2. The antibacterial waterproof epoxy floor paint according to claim 1, characterized in that: the modified epoxy resin is prepared from bisphenol A type epoxy resin diglycidyl ether and modified itaconic acid.
3. The antibacterial waterproof epoxy floor paint according to claim 2, characterized in that: the modified itaconic acid is prepared from propylene bromide, itaconic acid, N-dimethylformamide and m-chloroperoxybenzoic acid, wherein the mass ratio of the propylene bromide to the itaconic acid is 1.4-1.5: 1.
4. The antibacterial waterproof epoxy floor paint according to claim 1, characterized in that: the epoxy curing agent is a mixture of ethylenediamine and diethylenetriamine.
5. The antibacterial waterproof epoxy floor paint according to claim 1, characterized in that: the defoaming agent is one of a high alcohol defoaming agent and an organic silicon dioxide defoaming agent.
6. The antibacterial waterproof epoxy floor paint according to claim 1, characterized in that: the filler is quartz sand, titanium dioxide and talcum powder.
7. A preparation method of antibacterial waterproof epoxy floor paint is characterized by comprising the following steps: the steps are as follows,
(1) preparation of modified epoxy resin:
adding a solvent into bisphenol A type epoxy resin diglycidyl ether, stirring, adding N, N-dimethylformamide, allyl bromide and potassium hydroxide, stirring for 15-18min, heating at 60-63 ℃, and refluxing for 10-12h to obtain modified itaconic acid;
adding dichloromethane and m-chloroperoxybenzoic acid into the obtained modified itaconic acid, heating at 40-45 ℃ for 4-5 days to obtain modified epoxy resin, and condensing and recovering evaporated gas;
(2) and (3) recovery treatment:
mixing lauric acid and sulfuric acid, stirring and adding the obtained recovered liquid, heating at 90-95 ℃, refluxing for 8-9h, cooling, preserving heat at 30-32 ℃ for 8-8.5h, layering, adding alkali liquor, and adjusting pH to obtain a mixture A;
secondly, adding thiourea and ethanol into the mixture A, heating under reflux, adding sodium hydroxide and deionized water, reacting for 2-2.5h, separating and taking an oil phase, and heating to 165-168 ℃ to obtain a mixture B;
(3) preparing floor paint:
adding absolute ethyl alcohol into the obtained modified epoxy resin, adding tetradecyl tertiary amine in an inert atmosphere for 2-3h, heating to 50 ℃ after the reaction is finished, and preserving heat for 24-25 h;
secondly, mixing and stirring the epoxy resin, the mixture B and the modified epoxy resin, adding an emulsifier, an antistatic agent and a filler, and uniformly stirring to obtain a component A;
mixing the epoxy curing agent, the curing accelerator and the thickening agent, stirring, adding the defoaming agent, and uniformly stirring to obtain a component B;
and fourthly, mixing the component A and the component B, coating the mixture on the surface of a carrier, and curing to obtain the floor paint.
8. The preparation method of the antibacterial waterproof epoxy floor paint according to claim 7, characterized in that: in the step (1), the added solvent is acetone.
9. The preparation method of the antibacterial waterproof epoxy floor paint according to claim 7, characterized in that: in the step (2), the mass ratio of the added lauric acid to thiourea to the added itaconic acid is 1.53-1.54: 0.58: 1.
10. the preparation method of the antibacterial waterproof epoxy floor paint according to claim 7, characterized in that: in the step (3), the mass ratio of the tetradecyl tertiary amine to the itaconic acid is 0.9-0.92: 1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718945A (en) * | 2012-06-12 | 2012-10-10 | 中国科学院宁波材料技术与工程研究所 | Itaconic acid-based epoxy resin composition and method for preparing cured substance |
| CN102775884A (en) * | 2012-08-22 | 2012-11-14 | 山西省交通科学研究院 | Solvent-free colored floor coating |
| CN109517341A (en) * | 2018-11-22 | 2019-03-26 | 金华市源成新材料有限公司 | Biology base citric acid composition epoxy resin and its curing method and application |
| CN113072868A (en) * | 2021-04-02 | 2021-07-06 | 游燕英 | Wear-resistant and water-skid-resistant floor paint for civil air defense and preparation method thereof |
-
2021
- 2021-12-21 CN CN202111569210.9A patent/CN114133829A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718945A (en) * | 2012-06-12 | 2012-10-10 | 中国科学院宁波材料技术与工程研究所 | Itaconic acid-based epoxy resin composition and method for preparing cured substance |
| CN102775884A (en) * | 2012-08-22 | 2012-11-14 | 山西省交通科学研究院 | Solvent-free colored floor coating |
| CN109517341A (en) * | 2018-11-22 | 2019-03-26 | 金华市源成新材料有限公司 | Biology base citric acid composition epoxy resin and its curing method and application |
| CN113072868A (en) * | 2021-04-02 | 2021-07-06 | 游燕英 | Wear-resistant and water-skid-resistant floor paint for civil air defense and preparation method thereof |
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Application publication date: 20220304 |