CN110330852A - Preparation method of waterproof coating for ceramic tiles - Google Patents
Preparation method of waterproof coating for ceramic tiles Download PDFInfo
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- CN110330852A CN110330852A CN201910633888.5A CN201910633888A CN110330852A CN 110330852 A CN110330852 A CN 110330852A CN 201910633888 A CN201910633888 A CN 201910633888A CN 110330852 A CN110330852 A CN 110330852A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/01—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to unsaturated polyesters
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
- C08F283/105—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule on to unsaturated polymers containing more than one epoxy radical per molecule
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/122—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to saturated polysiloxanes containing hydrolysable groups, e.g. alkoxy-, thio-, hydroxy-
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- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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- 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
- C09D7/65—Additives macromolecular
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention provides a preparation method of a waterproof coating for a ceramic tile. The waterproof coating for the ceramic tile is composed of acrylate resin, a waterproof agent, an adhesion promoter, water and ammonium persulfate, wherein the acrylate resin is prepared by reacting styrene, butyl acrylate, methyl methacrylate, isooctyl acrylate, glycidyl methacrylate, vinyl acetate, an SE-10 emulsifier, nano-cellulose, hydroxyethyl methacrylate and azodiisobutyronitrile, the waterproof agent is prepared by reacting hydroxyl-terminated fluorine-containing polysiloxane, methacrylic acid, an SE-10 emulsifier, acrylonitrile, octane and aluminum trichloride, and the adhesion promoter is prepared by reacting 2-acrylamide-2-methylpropanesulfonic acid, acrylic acid, bisphenol A epoxy acrylate, fumed silica and low-viscosity tetrafunctional polyester acrylate FS96 9601Y. The waterproof coating for the ceramic tile prepared by the method has excellent waterproofness and bonding strength.
Description
Technical field
The present invention relates to technical field of coatings, particularly, are related to a kind of preparation method of ceramic tile water-repellent paint.
Background technique
With economical fast development and continuous improvement of people's living standards, waterproof performance and environmental protection of the people to coating
Performance requirement is continuously improved.But currently, the status of China's aqueous waterproofing paint exists, vacation is aqueous, waterproofness is poor, and environment-friendly type is poor
The problems such as.In recent years, with the increasing of national policy dynamics, people recognize environmental protection coating material and require constantly to be promoted, people
Primary requirement for water paint is environmental protection, secondly therefore only really meets the green ring of customer requirement for waterproofness
Guarantor, high waterproofness, high-adhesion water paint are just able to satisfy the high target requirement of existing customer.
Currently, water-repellent paint mainly uses styrene-acrylic emulsion system, such as the China that Authorization Notice No. is 101486868 B of CN
Patent discloses a kind of water-repellent paint, by pure-acrylic emulsion, dispersing agent, water, defoaming agent, pigments and fillers, hydroxyethyl cellulose, inorganic touching
Become thickener, surfactant, mould inhibitor, coalescing agent, plasticizer, ammonium hydroxide composition.The present invention is due to using pure-acrylic emulsion to make
Based on resin material, the resin material itself has certain waterproofness, can improve the waterproof performance of water-proof emulsion.
In addition to above-mentioned water-proof emulsion, there are also largely using styrene-butadiene emulsion, propyl benzene lotion as the porcelain of main material currently on the market
Brick water-repellent paint, principle be main waterproof resin using matrix resin, addition waterproofing agent as auxiliary waterproof agent, thus
Reach waterproof effect.
But the waterproof effect that above-mentioned ceramic tile is played with water-repellent paint is limited, and water-proof emulsion there are the feature of environmental protection poor, bonding
Waterproof period short defect after intensity is low and coating film forming.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of ceramic tile water-repellent paint, are used with solving ceramic tile in the prior art
Water-repellent paint waterproof period short technical problem.
To achieve the above object, the present invention provides a kind of preparation methods of ceramic tile water-repellent paint, comprising the following steps:
(1), by 2- acrylamide-2-methyl propane sulfonic, acrylic acid, bisphenol A epoxy acrylate and low viscosity tetrafunctional
Base polyester acrylate FS9601Y is that 12:8~15:6~20:0.01~0.6 is added in reaction kettle according to mass parts ratio,
Mixing speed is 90r/min, and maintenance system reaction temperature stirs 30min under the conditions of being 30~50 DEG C, by mass parts ratio be 3~
9 fumed silica is added in reaction kettle according to 0.2 mass parts/min adding rate, maintain under above-mentioned reaction condition after
Continuous stirring 30min, obtains adhesion promoter；
(2), by terminal hydroxy group fluorinated polysiloxane, methacrylic acid, SE-10 emulsifier, acrylonitrile, octane and alchlor
It is that 23:12~20:2~7:1~5:53~70:0.1~0.6 is added in reaction kettle according to mass fraction ratio, mixing speed is
85r/min, maintenance system reaction temperature is 87~140 DEG C, reduced-pressure backflow reacts 1.5~6h under the conditions of -0.05~0.1MPa, is produced
Object is evaporated under reduced pressure 1~3h through 100~120 DEG C, -0.06~0.09MPa, product through water washing 3 times, ethanol washing 3 times, dry,
Obtain waterproofing agent；
(3), styrene, butyl acrylate, methyl methacrylate, Isooctyl acrylate monomer, Glycidyl methacrylate is sweet
Grease, vinylacetate, SE-10 emulsifier, nano-cellulose, hydroxyethyl methacrylate and azodiisobutyronitrile are according to quality
Score ratio is that 1:18~21:1~2:11~19:6~9:13~17:2~5:3~6:5~11:0.03~0.07 is added to reaction
In kettle, mixing speed 100r/min, maintenance system reaction temperature reacts 0.5~1h under the conditions of being 50~63 DEG C, by reaction kettle
Temperature is warming up to 70~83 DEG C of 15~40min of reaction to get acrylate is arrived；
(4), it is 46:2~5 according to mass fraction ratio by acrylate, adhesion promoter, water and ammonium persulfate:
65~77:0.04~0.15 is added in reaction kettle, mixing speed 95r/min, under the conditions of 67~72 DEG C of maintenance system temperature
40min is reacted, the waterproofing agent that mass parts ratio is 3~8 is added to reaction kettle according to 0.01 mass parts/min adding rate
In, to waterproofing agent addition after, the 20min that maintains under above-mentioned reaction condition that the reaction was continued, temperature of reaction kettle is warming up to 75~
86 DEG C of 0.5~4h of reaction are to get to ceramic tile water-repellent paint.
In the inventive solutions, it is not changed to adopt using traditional styrene-acrylic resin or pure C resin as basic resin
To styrene, butyl acrylate, methyl methacrylate, Isooctyl acrylate monomer, glycidyl methacrylate, acetic acid second
Acrylate after enester, SE-10 emulsifier, nano-cellulose, hydroxyethyl methacrylate pre-polymerization is main base tree
Rouge.Compared with styrene-acrylic resin or pure C resin, acrylate prepared by the application is because it contains rigid unitary particle conduct
Reinforcing agent, lower glass transition temperature, hydrophilic radical, lipophilic group and response type surfactant active and assign its have compared with
High adhesion strength, lower temperature resistance, amphipathic property and compatibility；It is designed simultaneously in acrylate macromolecular structure hydrophilic
The purpose of group and lipophilic group, this design makes to reduce reactive emulsifier SE-10 usage amount, reduce reactive emulsifier
With cost, improve it between compatibility unclassified stores, because having the hydrophilic parent of surfactant-like in acrylate structure
Oil base group and the function of assigning surfactant, can improve the dispersion stabilization of water-repellent paint each component, so as to be obviously improved
The compatibility and dispersibility of waterproofing agent and adhesion promoter in acrylate.But traditional pure C resin and phenylpropyl alcohol
Resin, due to, by addition non-reactive emulsifier and non-reactive waterproofing agent, waterproof being caused to apply in base resin lotion
Mixed stability between material each component is in the metastable condition of physical layer, and long-time storage will appear lamination, waterproof
Each component still belongs to discrete state in microcosmic point after coating film forming, soaks in water in terms of showing macro property for long-time
It steeps oneself-meeting and coating film surface occurs and whiten or even fall off, therefore, coating cannot maintain waterproofness for a long time, seriously affected reality and answered
With.
Waterproofing agent of the invention modifies terminal hydroxy group fluorinated polysiloxane with methacrylic acid, hence it is evident that it is fluorine-containing to improve terminal hydroxy group
While the chemical reactivity of polysiloxanes, because methacrylic acid have excellent chemical activity, polymerizability and with it is more
Kind acrylate monomer has excellent compatibility, assigns the polymerizable reactivity of terminal hydroxy group fluorinated polysiloxane and improves end
Fluorinated hydroxy polysiloxanes and acrylate monomer consistency problem；Terminal hydroxy group fluorinated polysiloxane after methacrylic acid modification
It after aggregated, is grafted in acrylate structure, is on a microscopic level same macromolecular structure with acrylate,
With excellent chemical stability, long-term waterproof performance can be played.Traditional waterproofing agent generally use addition type waterproof material or
A-171 silane coupling agent or A-151 silane coupling agent, but addition type waterproofing agent exist with matrix resin or other monomers and its
The incompatible problem of his material, and the presence of the reactive waterproofing agents such as A-171 silane coupling agent or A-151 silane coupling agent is easy to water
The defects of solution, poor storage stability, high production operation technical requirements, eventually leading to the water-proof emulsion produced, there are stability to have
The defect of difference.Therefore, using methacrylic acid as the bridge between cohesive end fluorinated hydroxy polysiloxanes and acrylate
Terminal hydroxy group fluorinated polysiloxane can be stably secured in acrylate macromolecular structure by beam, and because of acrylate
Dispersion performance be evenly distributed in acrylate molecular structure, to play excellent waterproof performance.
Adhesion promoter of the invention, with 2- acrylamide-2-methyl propane sulfonic, acrylic acid, bisphenol-A epoxy acrylic acid
Ester is raw material, the acidity and corrosivity of 2- acrylamide-2-methyl propane sulfonic and acrylic acid is made full use of, first to base to be bonded
Material surface carries out microcorrosion, improves the surface and interface performance and roughness of substrate surface, secondly the ring in bisphenol A epoxy acrylate
Oxygen groups have excellent adhesion property to the substrate after the micro- modification in surface, thus, by 2- acrylamide-2-methyl propane sulfonic
After the surface preparation of acrylic acid, the epoxy group in bisphenol A epoxy acrylate structure is to through 2- acrylamide -2- methyl
Substrate surface after propane sulfonic acid and acrylic surface modification, which is infiltrated and bonds to be obviously improved, treats bonding substrates surface
Adhesion property, meanwhile, 2- acrylamide-2-methyl propane sulfonic, acrylic acid, the double bond energy in bisphenol A epoxy acrylate structure
Polymerization reaction is participated in acrylate, so as to by 2- acrylamide-2-methyl propane sulfonic, acrylic acid, bisphenol-A epoxy third
Olefin(e) acid polyisocyanate polyaddition improves 2- acrylamide-2-methyl propane sulfonic, acrylic acid and bis-phenol into acrylate macromolecular structure
Dispersibility of the A epoxy acrylate in acrylate, storage stability and to have ensured that adhesion promoter improves anti-
Adhesion property of the aqueous emulsion to substrate.Traditional adhesion promoter is generally acrylate phosphate, although its have can be anti-
Activity is answered, energy graft polymerization is into polyacrylate resin macromolecular structure, but such adhesion promoter can not be treated
Surface modification or wetting action are played in bonding substrates surface, therefore, waterproof coating and substrate surface to be bonded be unable to reach compared with
Therefore good bonding interface layer promotes the adhesion strength of water-repellent paint limited.
The invention has the following advantages:
The ceramic tile water-repellent paint of the method for the present invention preparation, belongs to water soluble green environmental protection coating material, and synthesis technology is simple, tool
There are excellent storage stability, waterproofness and adhesion strength, is able to solve ceramic tile water-repellent paint waterproof performance in the prior art
With the technical problem of adhesion strength difference.
Other than objects, features and advantages described above, there are also other objects, features and advantages by the present invention.
The present invention is further detailed explanation below.
Specific embodiment
A specific embodiment of the invention is described below with reference to embodiment, to better understand the present invention.This
It is a little that examples are only for illustrating the present invention and not for limiting the scope of the present invention.Actual conditions are not specified in lower example embodiment
Experimental method, usually according to this field normal condition or the condition suggested according to manufacturer；Used raw material, reagent etc.,
It unless otherwise specified, is the raw materials and reagents that can be obtained from commercial sources such as conventional markets.Those skilled in the art is at this
The variation and replacement of any unsubstantiality done on the basis of invention belong to scope of the present invention.
Embodiment 1
A kind of preparation method of ceramic tile water-repellent paint, comprising the following steps:
(1), 12 parts of 2- acrylamide-2-methyl propane sulfonics, 12.3 parts of acrylic acid, 10.6 parts of bisphenol-A epoxy propylene are weighed
Acid esters and 0.03 part of low viscosity tetrafunctional base polyester acrylate FS9601Y are added in reaction kettle, mixing speed 90r/
Min, maintenance system reaction temperature stirs 30min under the conditions of being 39 DEG C, by 4.1 parts of fumed silicas according to 0.2 part/min's
Adding rate is added in reaction kettle, is maintained to continue to stir 30min under above-mentioned reaction condition, is obtained adhesion promoter；
(2), 23 parts of terminal hydroxy group fluorinated polysiloxanes, 17.6 parts of methacrylic acids, 2.7 parts of SE-10 emulsifiers, 2.2 are weighed
Part acrylonitrile, 62 parts of octanes and 0.2 part of alchlor are added in reaction kettle, mixing speed 85r/min, maintenance system reaction
Temperature is 121 DEG C, reduced-pressure backflow reacts 4.5h under the conditions of -0.08MPa, and product is evaporated under reduced pressure 2.5h through 107 DEG C, -0.08MPa,
Product obtains waterproofing agent through water washing 3 times, ethanol washing 3 times, dry；
(3), it is different that 1 part of styrene, 19.6 parts of butyl acrylates, 1.2 parts of methyl methacrylates, 15.2 parts of acrylic acid are weighed
Monooctyl ester, 7.7 parts of glycidyl methacrylate, 15.1 parts of vinylacetates, 2.5 parts of SE-10 emulsifiers, 4.6 parts of Nanowires
Dimension element, 7.8 parts of hydroxyethyl methacrylates and 0.04 part of azodiisobutyronitrile are added in reaction kettle, mixing speed 100r/
Min, maintenance system reaction temperature be 56 DEG C under the conditions of react 0.8h, by temperature of reaction kettle be warming up to 81 DEG C of reaction 30min to get
To acrylate；
(4), 46 parts of acrylates, 3.2 parts of adhesion promoters, 70 parts of water and 0.06 part of ammonium persulfate is weighed to be added
Into reaction kettle, mixing speed 95r/min reacts 40min under the conditions of 69 DEG C of maintenance system temperature, 5.6 parts of waterproofing agents is pressed
Be added in reaction kettle according to the adding rate of 0.01 part/min, to waterproofing agent addition after, maintain under above-mentioned reaction condition after
Temperature of reaction kettle is warming up to 78 DEG C of reaction 1.5h to get to ceramic tile water-repellent paint by continuous reaction 20min.
Embodiment 2
A kind of preparation method of ceramic tile water-repellent paint, comprising the following steps:
(1), weigh 12 parts of 2- acrylamide-2-methyl propane sulfonics, 8 parts of acrylic acid, 6 parts of bisphenol A epoxy acrylates and
0.01 part of low viscosity tetrafunctional base polyester acrylate FS9601Y is added in reaction kettle, mixing speed 90r/min, is maintained
System reaction temperature stirs 30min under the conditions of being 30 DEG C, and 3 parts of fumed silicas are added according to the adding rate of 0.2 part/min
It adds in reaction kettle, maintains to continue to stir 30min under above-mentioned reaction condition, obtain adhesion promoter；
(2), 23 parts of terminal hydroxy group fluorinated polysiloxanes, 12 parts of methacrylic acids, 2 parts of SE-10 emulsifiers, 1 part of propylene are weighed
Nitrile, 53 parts of octanes and 0.1 part of alchlor are added in reaction kettle, mixing speed 85r/min, and maintenance system reaction temperature is
87 DEG C, reduced-pressure backflow reacts 6h under the conditions of -0.05MPa, product is evaporated under reduced pressure 3h through 100 DEG C, -0.06MPa, and product is through water washing
3 times, it is ethanol washing 3 times, dry, obtain waterproofing agent；
(3), 1 part of styrene, 18 parts of butyl acrylates, 1 part of methyl methacrylate, 11 parts of Isooctyl acrylate monomers, 6 are weighed
Part glycidyl methacrylate, 13 parts of vinylacetates, 2 parts of SE-10 emulsifiers, 3 parts of nano-celluloses, 5 parts of methyl-props
Olefin(e) acid hydroxyl ethyl ester and 0.03 part of azodiisobutyronitrile are added in reaction kettle, mixing speed 100r/min, maintenance system reaction
Temperature reacts 1h under the conditions of being 50 DEG C, and temperature of reaction kettle is warming up to 70 DEG C of reaction 40min to get acrylate is arrived；
(4), 46 parts of acrylates, 2 parts of adhesion promoters, 65 parts of water and 0.045 part of ammonium persulfate is weighed to be added
Into reaction kettle, mixing speed 95r/min reacts 40min under the conditions of 67 DEG C of maintenance system temperature, by 3 parts of waterproofing agents according to
The adding rate of 0.01 part/min is added in reaction kettle, after adding to waterproofing agent, maintains to continue under above-mentioned reaction condition
20min is reacted, temperature of reaction kettle is warming up to 75 DEG C of reaction 4h to get to ceramic tile water-repellent paint.
Embodiment 3
A kind of preparation method of ceramic tile water-repellent paint, comprising the following steps:
(1), 12 parts of 2- acrylamide-2-methyl propane sulfonics, 15 parts of acrylic acid, 20 parts of bisphenol A epoxy acrylates are weighed
It is added in reaction kettle, mixing speed 90r/min, maintains with 0.6 part of low viscosity tetrafunctional base polyester acrylate FS9601Y
System reaction temperature stirs 30min under the conditions of being 50 DEG C, and 9 parts of fumed silicas are added according to the adding rate of 0.2 part/min
It adds in reaction kettle, maintains to continue to stir 30min under above-mentioned reaction condition, obtain adhesion promoter；
(2), 23 parts of terminal hydroxy group fluorinated polysiloxanes, 20 parts of methacrylic acids, 7 parts of SE-10 emulsifiers, 5 parts of propylene are weighed
Nitrile, 70 parts of octanes and 0.6 part of alchlor are added in reaction kettle, mixing speed 85r/min, and maintenance system reaction temperature is
140 DEG C, reduced-pressure backflow reacts 1.5h under the conditions of -0.1MPa, product is evaporated under reduced pressure 1h through 120 DEG C, -0.09MPa, and product is through washing
Wash 3 times, it is ethanol washing 3 times, dry, obtain waterproofing agent；
(3), 1 part of styrene, 21 parts of butyl acrylates, 2 parts of methyl methacrylates, 19 parts of Isooctyl acrylate monomers, 9 are weighed
Part glycidyl methacrylate, 17 parts of vinylacetates, 5 parts of SE-10 emulsifiers, 6 parts of nano-celluloses, 11 parts of methyl-props
Olefin(e) acid hydroxyl ethyl ester and 0.07 part of azodiisobutyronitrile are added in reaction kettle, mixing speed 100r/min, maintenance system reaction
Temperature reacts 0.5h under the conditions of being 63 DEG C, and temperature of reaction kettle is warming up to 83 DEG C of reaction 15min to get acrylate is arrived；
(4), 46 parts of acrylates, 5 parts of adhesion promoters, 77 parts of water and 0.15 part of ammonium persulfate is weighed to be added to
In reaction kettle, mixing speed 95r/min reacts 40min under the conditions of 72 DEG C of maintenance system temperature, by 8 parts of waterproofing agents according to
The adding rate of 0.01 part/min is added in reaction kettle, after adding to waterproofing agent, maintains to continue under above-mentioned reaction condition
20min is reacted, temperature of reaction kettle is warming up to 86 DEG C of reaction 0.5h to get to ceramic tile water-repellent paint.
Embodiment 4
A kind of preparation method of ceramic tile water-repellent paint, comprising the following steps:
(1), weigh 12 parts of 2- acrylamide-2-methyl propane sulfonics, 9 parts of acrylic acid, 8 parts of bisphenol A epoxy acrylates and
0.06 part of low viscosity tetrafunctional base polyester acrylate FS9601Y is added in reaction kettle, mixing speed 90r/min, is maintained
System reaction temperature stirs 30min under the conditions of being 33 DEG C, and 5 parts of fumed silicas are added according to the adding rate of 0.2 part/min
It adds in reaction kettle, maintains to continue to stir 30min under above-mentioned reaction condition, obtain adhesion promoter；
(2), 23 parts of terminal hydroxy group fluorinated polysiloxanes, 14 parts of methacrylic acids, 3 parts of SE-10 emulsifiers, 2 parts of propylene are weighed
Nitrile, 56 parts of octanes and 0.2 part of alchlor are added in reaction kettle, mixing speed 85r/min, and maintenance system reaction temperature is
92 DEG C, reduced-pressure backflow reacts 1.9h under the conditions of -0.06MPa, product is evaporated under reduced pressure 1.3h through 105 DEG C, -0.07MPa, and product is through water
It is washing 3 times, ethanol washing 3 times, dry, obtain waterproofing agent；
(3), it is different pungent that 1 part of styrene, 19 parts of butyl acrylates, 1.5 parts of methyl methacrylates, 13 parts of acrylic acid are weighed
Ester, 6.8 parts of glycidyl methacrylate, 14 parts of vinylacetates, 2.6 parts of SE-10 emulsifiers, 4.3 parts of nano-celluloses,
6.5 parts of hydroxyethyl methacrylates and 0.04 part of azodiisobutyronitrile are added in reaction kettle, mixing speed 100r/min, dimension
It holds under the conditions of system reaction temperature is 55 DEG C and reacts 0.7h, temperature of reaction kettle is warming up to 73 DEG C of reaction 19min to get propylene is arrived
Acid ester resin；
(4), 46 parts of acrylates, 2.5 parts of adhesion promoters, 69 parts of water and 0.07 part of ammonium persulfate is weighed to be added
Into reaction kettle, mixing speed 95r/min reacts 40min under the conditions of maintenance system temperature 70 C, 4.5 parts of waterproofing agents is pressed
Be added in reaction kettle according to the adding rate of 0.01 part/min, to waterproofing agent addition after, maintain under above-mentioned reaction condition after
Temperature of reaction kettle is warming up to 78 DEG C of reaction 1h to get to ceramic tile water-repellent paint by continuous reaction 20min.
Embodiment 5
A kind of preparation method of ceramic tile water-repellent paint, comprising the following steps:
(1), 12 parts of 2- acrylamide-2-methyl propane sulfonics, 10 parts of acrylic acid, 15 parts of bisphenol A epoxy acrylates are weighed
It is added in reaction kettle, mixing speed 90r/min, maintains with 0.1 part of low viscosity tetrafunctional base polyester acrylate FS9601Y
System reaction temperature stirs 30min under the conditions of being 40 DEG C, and 5 parts of fumed silicas are added according to the adding rate of 0.2 part/min
It adds in reaction kettle, maintains to continue to stir 30min under above-mentioned reaction condition, obtain adhesion promoter；
(2), 23 parts of terminal hydroxy group fluorinated polysiloxanes, 15 parts of methacrylic acids, 4 parts of SE-10 emulsifiers, 3 parts of propylene are weighed
Nitrile, 60 parts of octanes and 0.3 part of alchlor are added in reaction kettle, mixing speed 85r/min, and maintenance system reaction temperature is
100 DEG C, reduced-pressure backflow reacts 3.5h under the conditions of -0.07MPa, product is evaporated under reduced pressure 1.5h, product warp through 110 DEG C, -0.07MPa
It is water washing 3 times, ethanol washing 3 times, dry, obtain waterproofing agent；
(3), it is different pungent that 1 part of styrene, 20 parts of butyl acrylates, 1.5 parts of methyl methacrylates, 15 parts of acrylic acid are weighed
Ester, 7 parts of glycidyl methacrylate, 15 parts of vinylacetates, 3.5 parts of SE-10 emulsifiers, 4 parts of nano-celluloses, 8 parts
Hydroxyethyl methacrylate and 0.05 part of azodiisobutyronitrile are added in reaction kettle, mixing speed 100r/min, maintain body
It is to react 0.7h under the conditions of reaction temperature is 57 DEG C, temperature of reaction kettle is warming up to 79 DEG C of reaction 30min to get acrylate is arrived
Resin；
(4), 46 parts of acrylates, 4 parts of adhesion promoters, 71 parts of water and 0.09 part of ammonium persulfate is weighed to be added to
In reaction kettle, mixing speed 95r/min reacts 40min under the conditions of 69 DEG C of maintenance system temperature, by 6 parts of waterproofing agents according to
The adding rate of 0.01 part/min is added in reaction kettle, after adding to waterproofing agent, maintains to continue under above-mentioned reaction condition
20min is reacted, temperature of reaction kettle is warming up to 82 DEG C of reaction 2h to get to ceramic tile water-repellent paint.
Embodiment 6
A kind of preparation method of ceramic tile water-repellent paint, comprising the following steps:
(1), 12 parts of 2- acrylamide-2-methyl propane sulfonics, 14 parts of acrylic acid, 17 parts of bisphenol A epoxy acrylates are weighed
It is added in reaction kettle, mixing speed 90r/min, maintains with 0.5 part of low viscosity tetrafunctional base polyester acrylate FS9601Y
System reaction temperature stirs 30min under the conditions of being 49 DEG C, by 8.7 parts of fumed silicas according to the adding rate of 0.2 part/min
It is added in reaction kettle, maintains to continue to stir 30min under above-mentioned reaction condition, obtain adhesion promoter；
(2), 23 parts of terminal hydroxy group fluorinated polysiloxanes, 19 parts of methacrylic acids, 6 parts of SE-10 emulsifiers, 4 parts of propylene are weighed
Nitrile, 68 parts of octanes and 0.5 part of alchlor are added in reaction kettle, mixing speed 85r/min, and maintenance system reaction temperature is
130 DEG C, reduced-pressure backflow reacts 5h under the conditions of -0.09MPa, product is evaporated under reduced pressure 2.5h through 110 DEG C, -0.08MPa, and product is through water
It is washing 3 times, ethanol washing 3 times, dry, obtain waterproofing agent；
(3), it is different pungent that 1 part of styrene, 20 parts of butyl acrylates, 1.8 parts of methyl methacrylates, 18.2 parts of acrylic acid are weighed
Ester, 8.3 parts of glycidyl methacrylate, 15.6 parts of vinylacetates, 4.3 parts of SE-10 emulsifiers, 5.2 parts of nanofibers
Element, 10 parts of hydroxyethyl methacrylates and 0.06 part of azodiisobutyronitrile are added in reaction kettle, mixing speed 100r/min,
Maintenance system reaction temperature reacts 0.8h under the conditions of being 62 DEG C, and temperature of reaction kettle is warming up to 82 DEG C of reaction 36min to get to third
Alkene acid ester resin；
(4), 46 parts of acrylates, 4.6 parts of adhesion promoters, 75 parts of water and 0.12 part of ammonium persulfate is weighed to be added
Into reaction kettle, mixing speed 95r/min reacts 40min under the conditions of 71 DEG C of maintenance system temperature, 7.3 parts of waterproofing agents is pressed
Be added in reaction kettle according to the adding rate of 0.01 part/min, to waterproofing agent addition after, maintain under above-mentioned reaction condition after
Temperature of reaction kettle is warming up to 82 DEG C of reaction 3.3h to get to ceramic tile water-repellent paint by continuous reaction 20min.
Reference examples 1
In this reference examples, adhesion promoter is not added, other components and preparation method are same as Example 1.
Reference examples 2
In this reference examples, waterproofing agent is not added, other components and preparation method are same as Example 1.
Reference examples 3
The acrylate in common pure acrylic acid butyl ester resin alternate embodiment 1 is selected in this reference examples, in formula,
Other components and preparation method are same as Example 1.
Reference examples 4
The adhesive force in common 2- acrylamide-2-methyl propane sulfonic alternate embodiment 1 is selected in this reference examples, in formula
Promotor, other components and preparation method are same as Example 1.
Reference examples 5
Select the waterproofing agent in common A-171 silane coupling agent alternate embodiment 1 in this reference examples, in formula, other groups
Divide same as Example 1 with preparation method.
To ceramic tile water-repellent paint made from Examples 1 to 6 and reference examples 1~5, waterproofness and adhesion strength are according to JC/
T547-2005 is tested, and test result sees below Tables 1 and 2.
The performance parameter of ceramic tile water-repellent paint made from 1 Examples 1 to 6 of table
The performance parameter of ceramic tile water-repellent paint made from 2 embodiment 1 of table and reference examples 1~5
Note: the waterproofing tests time starts to be immersed in the coating after forming a film to be dipped to coating surface in 25 DEG C of water and starts to send out
Until white.
By upper Tables 1 and 2 it is found that the waterproofness for the ceramic tile water-repellent paint that various embodiments of the present invention are prepared, immersion
Preceding tensile strength and immersion post-tensioning intensity are more excellent, this shows that the ceramic tile being prepared with raw material provided by the invention is applied with waterproof
Material has tensile strength and immersion post-tensioning intensity before preferable waterproofness, immersion；In contrast, the raw material preparation of each reference examples
Tensile strength and immersion post-tensioning intensity are poor before the waterproofness of obtained ceramic tile water-repellent paint, immersion.In addition, the present invention is each
The ceramic tile that embodiment is prepared is strong with tensile strength before preferable waterproofness, immersion and immersion post-tensioning with water-repellent paint
Degree.
The above is the preferred embodiment of the invention, it is noted that for those skilled in the art
For, under the premise of not departing from the inventive principle, several improvements and modifications can also be made, these improvements and modifications are also considered as
The protection scope of the invention.
Claims (6)
1. a kind of preparation method of ceramic tile water-repellent paint, it is characterised in that the following steps are included:
(1), 2- acrylamide-2-methyl propane sulfonic, acrylic acid, bisphenol A epoxy acrylate and low viscosity tetrafunctional base are gathered
Ester acrylate FS9601Y is that 12:8~15:6~20:0.01~0.6 is added in reaction kettle according to mass parts ratio, is stirred
Speed is 90r/min, and it is 3~9 by mass parts ratio that maintenance system reaction temperature, which stirs 30min under the conditions of being 30~50 DEG C,
Fumed silica is added in reaction kettle according to 0.2 mass parts/min adding rate, maintains to continue under above-mentioned reaction condition
30min is stirred, adhesion promoter is obtained；
(2), by terminal hydroxy group fluorinated polysiloxane, methacrylic acid, SE-10 emulsifier, acrylonitrile, octane and alchlor according to
Mass fraction ratio is that 23:12~20:2~7:1~5:53~70:0.1~0.6 is added in reaction kettle, mixing speed 85r/
Min, maintenance system reaction temperature is 87~140 DEG C, reduced-pressure backflow reacts 1.5~6h, product warp under the conditions of -0.05~0.1MPa
100~120 DEG C, -0.06~0.09MPa be evaporated under reduced pressure 1~3h, product is obtained through water washing 3 times, ethanol washing 3 times, dry
Waterproofing agent；
(3), by styrene, butyl acrylate, methyl methacrylate, Isooctyl acrylate monomer, glycidyl methacrylate,
Vinylacetate, SE-10 emulsifier, nano-cellulose, hydroxyethyl methacrylate and azodiisobutyronitrile are according to mass fraction
Than being added to reaction kettle for 1:18~21:1~2:11~19:6~9:13~17:2~5:3~6:5~11:0.03~0.07
In, mixing speed 100r/min, maintenance system reaction temperature reacts 0.5~1h under the conditions of being 50~63 DEG C, will react kettle temperature
Degree is warming up to 70~83 DEG C of 15~40min of reaction to get acrylate is arrived；
(4), by acrylate, adhesion promoter, water and ammonium persulfate according to mass fraction ratio be 46:3~6:65~
77:0.04~0.15 is added in reaction kettle, mixing speed 95r/min, is reacted under the conditions of 67~72 DEG C of maintenance system temperature
The waterproofing agent that mass parts ratio is 3~8 is added in reaction kettle by 40min according to 0.01 mass parts/min adding rate, to
After waterproofing agent adds, the 20min that maintains under above-mentioned reaction condition that the reaction was continued, by temperature of reaction kettle be warming up to 75~86 DEG C it is anti-
Answer 0.5~4h to get to ceramic tile water-repellent paint.
2. a kind of preparation method of ceramic tile water-repellent paint according to claim 1, which is characterized in that the methyl-prop
Contain hydroquinone polymerization inhibitor in acrylic monomer.
3. a kind of preparation method of ceramic tile water-repellent paint according to claim 1, which is characterized in that described in step 1
Bisphenol A epoxy acrylate number-average molecular weight be 1000.
4. a kind of preparation method of ceramic tile water-repellent paint according to claim 1, which is characterized in that described in step 2
Terminal hydroxy group fluorinated polysiloxane number-average molecular weight be 1000.
5. a kind of preparation method of ceramic tile water-repellent paint according to claim 1, which is characterized in that described in step 3
Nano-cellulose nanoparticle size is 50nm.
6. a kind of preparation method of ceramic tile water-repellent paint according to claim 1, which is characterized in that described in step 3
Acrylate be performed polymer.
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| CN111592675A (en) * | 2020-04-08 | 2020-08-28 | 苏州明冠新材料科技有限公司 | Multifunctional protective film material with wide applicability |
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