CN115521682B - High-fixation water-based paint and preparation method thereof - Google Patents
High-fixation water-based paint and preparation method thereof Download PDFInfo
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- CN115521682B CN115521682B CN202211251587.4A CN202211251587A CN115521682B CN 115521682 B CN115521682 B CN 115521682B CN 202211251587 A CN202211251587 A CN 202211251587A CN 115521682 B CN115521682 B CN 115521682B
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- 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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
- C09D7/65—Additives macromolecular
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Abstract
The invention relates to the technical field of high-fixation water-based paint, and discloses a high-fixation water-based paint and a preparation method thereof; according to the invention, through the 2-ethylhexyl acrylate, the N-acryloylmorpholine modified aqueous polyurethane/acrylic acid mixed solution and the modified cellulose, the hardness and wear resistance of the film are greatly enhanced while the good light transparency of the aqueous paint film is ensured, the friction-resistant color deflection is improved, and the water-based paint has excellent friction color fastness and washing fastness by the synergistic effect with the polyurethane prepared from the epoxy modified polyurethane.
Description
Technical Field
The invention relates to the technical field of high-fixation water-based paint, in particular to a high-fixation water-based paint and a preparation method thereof.
Background
In recent years, with the continuous progress of technology, environmental protection issues have come into the field of view of the public; the raw material selection and the product types in the production process of each enterprise are changed into environment-friendly type; the water-based paint is one of important environment-friendly products; because the attractive force between the pigment and the fabric or fiber is weak and can not interact with the fiber like fuel, the film needs to be formed on the surface of the fabric or fiber by means of an aqueous coating, and the fabric or fiber is coated, so that the pigment is fixed on the fabric or fiber, but the traditional aqueous coating has the problems of poor washing fastness and poor rubbing fastness, and the pigment is easy to fade.
Therefore, the invention of the high-fixation water-based paint has important significance.
Disclosure of Invention
The invention aims to provide a high-fixation water-based paint and a preparation method thereof, which are used for solving the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
the preparation method of the high-fixation water-based paint comprises the following steps:
s1: dissolving polyurethane in water, adding a defoaming agent, and uniformly stirring to obtain polyurethane emulsion; adding a coloring pigment under stirring; adding zirconium beads, and ball milling to obtain slurry;
s2: sequentially adding a water-based thickener, an emulsifier, a flexible curing agent, an enhancer and a defoamer into the emulsion under stirring to obtain a coating precursor;
s3: and adding the slurry and the coating precursor into a container, and uniformly stirring to obtain the high-fixation water-based coating.
Further, the polyurethane is prepared as follows:
adding polyethylene glycol and isophorone isocyanate into tetrahydrofuran, and heating for reaction; adding 2, 2-dimethylolpropionic acid and dibutyl tin dilaurate, performing secondary heating reaction, adding a tetrahydrofuran solution of trimethylolpropane, performing heat preservation reaction, adding 1- (3-aminopropyl) morpholine, performing cooling reaction, adding epoxypropanol for reaction, adding triethylamine, and performing neutralization reaction to obtain polyurethane.
Further, in the polyurethane, 60-80 parts of isophorone isocyanate, 20-40 parts of 2, 2-dimethylolpropionic acid, 5-10 parts of polyethylene glycol, 15 parts of trimethylolpropane, 12 parts of 1- (3-aminopropyl) morpholine and 5-6 parts of glycidol are calculated according to parts by weight.
Further, the emulsion is prepared as follows:
adding polypropylene glycol into propylene glycol adipate, heating, stirring and cooling; sequentially adding isophorone diisocyanate, dimethylol propionic acid and dibutyltin dilaurate under the nitrogen atmosphere, and heating for reaction; adding hydroxyethyl acrylate, and reacting at a constant temperature to obtain a reaction intermediate; adding a mixture of methyl methacrylate and butyl acrylate into a reaction intermediate, heating, adding triethylamine, and adding deionized water in a stirring state to obtain a polymer dispersion with a solid content of 35%; adding a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine into a polymer dispersion, heating and stirring, adding a potassium persulfate solution, and heating to react to obtain emulsion.
Further, in the emulsion, according to the mass parts, 35-40 parts of polypropylene glycol, 20-25 parts of propylene glycol adipate, 30-35 parts of isophorone diisocyanate, 8-9 parts of dimethylolpropionic acid, 16-20 parts of hydroxyethyl acrylate, 60-80 parts of a mixture of methyl methacrylate and butyl acrylate, 6 parts of triethylamine, and 15-20 parts of a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine; wherein, in the mixture of methyl methacrylate and butyl acrylate, methyl methacrylate: the mass ratio of the butyl acrylate is (1-1.5): (1.5-2) 2-ethylhexyl acrylate, N-acryloylmorpholine: the mass ratio of the N-acryloylmorpholine is (1-3): (1-3).
Further, the reinforcing agent is prepared by the following method:
dispersing gamma-aminopropyl triethoxy silane in deionized water, adding purified cellulose, and performing ultrasonic treatment to obtain the reinforcing agent.
Further, the gamma-aminopropyl triethoxysilane: the mass ratio of the purified cellulose is (0.6-4.2): (2-3).
Further, in the slurry, 5 to 8 parts of polyurethane, 0.3 to 0.8 part of defoamer, 20 to 25 parts of coloring pigment and 75 to 80 parts of water are calculated according to parts by weight; in the coating precursor, 3-5 parts of water-based thickener, 4-6 parts of emulsifier, 15-20 parts of flexible curing agent, 8-15 parts of reinforcing agent, 1-2 parts of defoamer and 75-80 parts of emulsion; in the Gao Guse aqueous coating, the slurry: the mass ratio of the coating precursor is (1-2): (2-3).
Further, the defoaming agent is one or more of an organic silicon defoaming agent and a polysiloxane defoaming agent; preferably, the defoamer is an organosilicon defoamer FT-58;
further, the coloring pigment is one or more of organic pigment and inorganic pigment; preferably, the organic pigment is phthalocyanine blue;
further, the aqueous thickener is one or more of the Liquiritigenin HIT and the Liquiritigenin GP; preferably, the aqueous thickener is a lidacin HIT;
further, the emulsifier is one or more of curculine CF and curculine LF; preferably, the emulsifier is a curbitone CF;
further, the flexible curing agent is one or more of the marine vertical diesel ET and the marine vertical diesel UDT; preferably, the flexible curing agent is maritima ET.
Compared with the prior art, the invention has the following beneficial effects: the invention introduces acrylic acid-2-ethylhexyl ester and N-acryloylmorpholine into the aqueous polyurethane/acrylic acid mixed emulsion; the soft chain of the 2-ethylhexyl acrylate and the N-acryloylmorpholine rigid ring form an intertwined and interpenetrating polymer network, so that the glossiness of the water-based paint after being cured is greatly improved; the 2-ethylhexyl acrylate enhances the elasticity of the film after the water-based paint is cured, and meanwhile, the long fatty chain of the film has water-based property, so that the problem of water resistance and elasticity reduction caused by adding N-acryloylmorpholine is solved, and the washing fastness is improved; the hydrogen bond formed by the-NH in the N-acryloylmorpholine enhances the physical crosslinking of the aqueous polyurethane/acrylic acid mixed emulsion, improves the toughness and rigidity of the polymer, solves the problem of film hardness reduction caused by adding the 2-ethylhexyl acrylate, and simultaneously improves the adhesive force and the friction-resistant color fastness of the polymer due to hydrophilic components.
According to the polyurethane prepared by epoxy modified polyurethane, 3-aminopropyl morpholine is used as an anchoring group, propylene oxide is used as a reaction group and introduced into the tail end of the polyurethane, the carboxyl groups in a dispersed concentration are dissolved in water to promote the ring opening of the epoxy groups, and the polymer-blocked isocyanate generates free-NCO to form hydroxyl groups with the epoxy groups and the hydroxyl groups of the silane coupling agent modified cellulose to carry out a crosslinking reaction in a high-temperature state, so that the coloring pigment is fixed on the fiber, and the washing fastness is greatly improved.
According to the invention, through the 2-ethylhexyl acrylate, the N-acryloylmorpholine modified aqueous polyurethane/acrylic acid mixed solution and the modified cellulose, the hardness and wear resistance of the film are greatly enhanced while the good light transparency of the aqueous paint film is ensured, the friction-resistant color deflection is improved, and the water-based paint has excellent friction color fastness and washing fastness by the synergistic effect with the polyurethane prepared from the epoxy modified polyurethane.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the following examples, the molecular weight of polyethylene glycol is 400, the molecular weight of polypropylene glycol is 2000, and the molecular weight of polypropylene glycol diethyl ester is 2000; purified cellulose is prepared according to a method provided by literature 'preparation and modification research progress of cellulose nanofibrils'; methyl methacrylate: the mass ratio of the butyl acrylate is 1:2; 2-ethylhexyl acrylate: the mass ratio of the N-acryloylmorpholine is 1:1.
the reinforcing agent is prepared by the following steps:
3.6g of gamma-aminopropyl triethoxysilane is dispersed in 100mL of deionized water, 3g of purified cellulose is added, the mixture is stirred uniformly, and the mixture is subjected to ultrasonic treatment for 30min, so as to obtain the reinforcing agent.
Example 1
S1: preparing polyurethane:
5g of polyethylene glycol and 60g of isophorone isocyanate are added into tetrahydrofuran, and the mixture is heated to 70 ℃ for reaction for 2 hours; 20g of 2, 2-dimethylolpropionic acid and 1g of dibutyltin dilaurate are added, the mixture is heated to 80 ℃ to react for 2 hours, 15g of trimethylolpropane is dissolved in 100mL of tetrahydrofuran, the prepared tetrahydrofuran solution of trimethylolpropane is added, the reaction is continued for 4 hours at 80 ℃, 12g of 1- (3-aminopropyl) morpholine is added, the reaction is carried out for 2 hours at 60 ℃, 5g of epoxypropanol is added, the reaction is carried out for 2 hours at 60 ℃, 5g of triethylamine is added, and the reaction is carried out for 1 hour at 40 ℃ to obtain polyurethane.
S2: preparing slurry:
dissolving 5g of polyurethane in 75g of water, adding 0.3g of organosilicon defoamer FT-58, and uniformly stirring to obtain polyurethane emulsion; adding 20g of phthalocyanine blue under stirring; 150g of zirconium beads are added and ball-milled to obtain slurry.
S3: preparing emulsion:
35g of polypropylene glycol is added into 20g of propylene glycol adipate, heated to 110 ℃ and stirred for reaction for 2 hours, cooled to 65 ℃; under the nitrogen atmosphere, sequentially adding 30g of isophorone diisocyanate, 8g of dimethylolpropionic acid and 1g of dibutyltin dilaurate, and heating to 80 ℃ for reaction for 2 hours; adding 16g of hydroxyethyl acrylate, and reacting for 2 hours at 80 ℃ to obtain a reaction intermediate; 60g of a mixture of methyl methacrylate and butyl acrylate is added into the reaction intermediate, 6g of triethylamine is added at 50 ℃, deionized water is added under stirring, and a polymer dispersion with 35% of solid content is obtained; 15g of a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine was added to the polymer dispersion, heated to 75℃and stirred for 2 hours, 1wt% potassium persulfate solution was added, and heated to 80℃and reacted for 2 hours to obtain an emulsion.
S4: preparing a coating precursor:
3g of Lipuidambaris HIT, 4g of Lipustulan CF, 15g of Highway-Lichaise ET, 8g of reinforcing agent and 1g of organosilicon antifoaming agent are added into 75g of emulsion in sequence under stirring to obtain a coating precursor.
S5: preparing a high-fixation water-based paint:
10g of the slurry and 20g of the coating precursor were added to a vessel and stirred well to obtain a high-fixation aqueous coating.
And (3) testing: color fastness testing:
coating the high-fixation water-based paint on polyester fabric with the specification of 10cm multiplied by 10cm, drying and curing to obtain a sample; the samples were tested for rub and wash fastness according to AATCC8-2007 and AATCC 61-2006, respectively, as shown in table 1.
Example 2
S1: preparing polyurethane:
adding 8g of polyethylene glycol and 70g of isophorone isocyanate into tetrahydrofuran, heating to 70 ℃ and reacting for 2 hours; 30g of 2, 2-dimethylolpropionic acid and 2g of dibutyltin dilaurate were added, heated to 80℃for reaction for 2 hours, 15g of trimethylolpropane was dissolved in 100mL of tetrahydrofuran, the prepared tetrahydrofuran solution of trimethylolpropane was added, reaction was continued at 80℃for 4 hours, 12g of 1- (3-aminopropyl) morpholine was added, reaction was carried out at 60℃for 2 hours, 6g of epoxypropanol was added, reaction was carried out at 60℃for 2 hours, 5g of triethylamine was added, and reaction was carried out at 40℃for 1 hour to obtain polyurethane.
S2: preparing slurry:
dissolving 5g of polyurethane in 75g of water, adding 0.3g of organosilicon defoamer FT-58, and uniformly stirring to obtain polyurethane emulsion; adding 20g of phthalocyanine blue under stirring; 150g of zirconium beads are added and ball-milled to obtain slurry.
S3: preparing emulsion:
adding 40g of polypropylene glycol into 25g of propylene glycol adipate, heating to 110 ℃, stirring and reacting for 2 hours, and cooling to 65 ℃; under nitrogen atmosphere, sequentially adding 35g of isophorone diisocyanate, 9g of dimethylolpropionic acid and 1g of dibutyltin dilaurate, and heating to 80 ℃ for reaction for 2 hours; adding 20g of hydroxyethyl acrylate, and reacting for 2 hours at 80 ℃ to obtain a reaction intermediate; 70g of a mixture of methyl methacrylate and butyl acrylate is added into the reaction intermediate, 6g of triethylamine is added at 50 ℃, deionized water is added under stirring, and a polymer dispersion with 35% of solid content is obtained; 20g of a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine was added to the polymer dispersion, heated to 75℃and stirred for 2 hours, 1wt% potassium persulfate solution was added, and heated to 80℃and reacted for 2 hours to obtain an emulsion.
S4: preparing a coating precursor:
3g of Lipuidambaris HIT, 4g of Lipustulan CF, 15g of Highway-Lichaise ET, 8g of reinforcing agent and 1g of organosilicon antifoaming agent are added into 75g of emulsion in sequence under stirring to obtain a coating precursor.
S5: preparing a high-fixation water-based paint:
10g of the slurry and 20g of the coating precursor were added to a vessel and stirred well to obtain a high-fixation aqueous coating.
And (3) testing: color fastness testing:
coating the high-fixation water-based paint on polyester fabric with the specification of 10cm multiplied by 10cm, drying and curing to obtain a sample; the samples were tested for rub and wash fastness according to AATCC8-2007 and AATCC 61-2006, respectively, as shown in table 1.
Example 3
S1: preparing polyurethane:
adding 8g of polyethylene glycol and 70g of isophorone isocyanate into tetrahydrofuran, heating to 70 ℃ and reacting for 2 hours; 30g of 2, 2-dimethylolpropionic acid and 2g of dibutyltin dilaurate were added, heated to 80℃for reaction for 2 hours, 15g of trimethylolpropane was dissolved in 100mL of tetrahydrofuran, the prepared tetrahydrofuran solution of trimethylolpropane was added, reaction was continued at 80℃for 4 hours, 12g of 1- (3-aminopropyl) morpholine was added, reaction was carried out at 60℃for 2 hours, 6g of epoxypropanol was added, reaction was carried out at 60℃for 2 hours, 5g of triethylamine was added, and reaction was carried out at 40℃for 1 hour to obtain polyurethane.
S2: preparing slurry:
8g of polyurethane is dissolved in 80g of water, 0.8g of organosilicon defoamer FT-58 is added, and the mixture is stirred uniformly to obtain polyurethane emulsion; while stirring, 25g of phthalocyanine blue was added; 200g of zirconium beads are added and ball milling is carried out to obtain slurry.
S3: preparing emulsion:
adding 40g of polypropylene glycol into 25g of propylene glycol adipate, heating to 110 ℃, stirring and reacting for 2 hours, and cooling to 65 ℃; under nitrogen atmosphere, sequentially adding 35g of isophorone diisocyanate, 9g of dimethylolpropionic acid and 1g of dibutyltin dilaurate, and heating to 80 ℃ for reaction for 2 hours; adding 20g of hydroxyethyl acrylate, and reacting for 2 hours at 80 ℃ to obtain a reaction intermediate; 70g of a mixture of methyl methacrylate and butyl acrylate is added into the reaction intermediate, 6g of triethylamine is added at 50 ℃, deionized water is added under stirring, and a polymer dispersion with 35% of solid content is obtained; 20g of a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine was added to the polymer dispersion, heated to 75℃and stirred for 2 hours, 1wt% potassium persulfate solution was added, and heated to 80℃and reacted for 2 hours to obtain an emulsion.
S4: preparing a coating precursor:
while stirring, 5g of Lipuidambaris HIT, 6g of Lipustulan CF, 20g of Highway Lichaise ET, 15g of reinforcing agent and 2g of organosilicon antifoaming agent are added into 80g of emulsion in sequence to obtain a coating precursor.
S5: preparing a high-fixation water-based paint:
10g of the slurry and 20g of the coating precursor were added to a vessel and stirred well to obtain a high-fixation aqueous coating.
And (3) testing: color fastness testing:
coating the high-fixation water-based paint on polyester fabric with the specification of 10cm multiplied by 10cm, drying and curing to obtain a sample; the samples were tested for rub and wash fastness according to AATCC8-2007 and AATCC 61-2006, respectively, as shown in table 1.
Comparative example 1 (2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane modified cellulose)
The reinforcing agent is prepared by the following steps:
adding 3.6g of 2- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane into 100mL of deionized water, adding 3g of purified cellulose, stirring uniformly, and performing ultrasonic treatment for 30min to obtain the reinforcing agent
S1: preparing polyurethane:
5g of polyethylene glycol and 60g of isophorone isocyanate are added into tetrahydrofuran, and the mixture is heated to 70 ℃ for reaction for 2 hours; 20g of 2, 2-dimethylolpropionic acid and 1g of dibutyltin dilaurate are added, the mixture is heated to 80 ℃ to react for 2 hours, 15g of trimethylolpropane is dissolved in 100mL of tetrahydrofuran, the prepared tetrahydrofuran solution of trimethylolpropane is added, the reaction is continued for 4 hours at 80 ℃, 12g of 1- (3-aminopropyl) morpholine is added, the reaction is carried out for 2 hours at 60 ℃, 5g of epoxypropanol is added, the reaction is carried out for 2 hours at 60 ℃, 5g of triethylamine is added, and the reaction is carried out for 1 hour at 40 ℃ to obtain polyurethane.
S2: preparing slurry:
dissolving 5g of polyurethane in 75g of water, adding 0.3g of organosilicon defoamer FT-58, and uniformly stirring to obtain polyurethane emulsion; adding 20g of phthalocyanine blue under stirring; 150g of zirconium beads are added and ball-milled to obtain slurry.
S3: preparing emulsion:
35g of polypropylene glycol is added into 20g of propylene glycol adipate, heated to 110 ℃ and stirred for reaction for 2 hours, cooled to 65 ℃; under the nitrogen atmosphere, sequentially adding 30g of isophorone diisocyanate, 8g of dimethylolpropionic acid and 1g of dibutyltin dilaurate, and heating to 80 ℃ for reaction for 2 hours; adding 16g of hydroxyethyl acrylate, and reacting for 2 hours at 80 ℃ to obtain a reaction intermediate; 60g of a mixture of methyl methacrylate and butyl acrylate is added into the reaction intermediate, 6g of triethylamine is added at 50 ℃, deionized water is added under stirring, and a polymer dispersion with 35% of solid content is obtained; 15g of a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine was added to the polymer dispersion, heated to 75℃and stirred for 2 hours, 1wt% potassium persulfate solution was added, and heated to 80℃and reacted for 2 hours to obtain an emulsion.
S4: preparing a coating precursor:
3g of Lipuidambaris HIT, 4g of Lipustulan CF, 15g of Highway-Lichaise ET, 8g of reinforcing agent and 1g of organosilicon antifoaming agent are added into 75g of emulsion in sequence under stirring to obtain a coating precursor.
S5: preparing a high-fixation water-based paint:
10g of the slurry and 20g of the coating precursor were added to a vessel and stirred well to obtain a high-fixation aqueous coating.
And (3) testing: color fastness testing:
coating the high-fixation water-based paint on polyester fabric with the specification of 10cm multiplied by 10cm, drying and curing to obtain a sample; the samples were tested for rub and wash fastness according to AATCC8-2007 and AATCC 61-2006, respectively, as shown in table 1.
Comparative example 2 (mixture without 2-ethylhexyl acrylate, N-acryloylmorpholine in emulsion)
S1: preparing polyurethane:
5g of polyethylene glycol and 60g of isophorone isocyanate are added into tetrahydrofuran, and the mixture is heated to 70 ℃ for reaction for 2 hours; 20g of 2, 2-dimethylolpropionic acid and 1g of dibutyltin dilaurate are added, the mixture is heated to 80 ℃ to react for 2 hours, 15g of trimethylolpropane is dissolved in 100mL of tetrahydrofuran, the prepared tetrahydrofuran solution of trimethylolpropane is added, the reaction is continued for 4 hours at 80 ℃, 12g of 1- (3-aminopropyl) morpholine is added, the reaction is carried out for 2 hours at 60 ℃, 5g of epoxypropanol is added, the reaction is carried out for 2 hours at 60 ℃, 5g of triethylamine is added, and the reaction is carried out for 1 hour at 40 ℃ to obtain polyurethane.
S2: preparing slurry:
dissolving 5g of polyurethane in 75g of water, adding 0.3g of organosilicon defoamer FT-58, and uniformly stirring to obtain polyurethane emulsion; adding 20g of phthalocyanine blue under stirring; 150g of zirconium beads are added and ball-milled to obtain slurry.
S3: preparing emulsion:
35g of polypropylene glycol is added into 20g of propylene glycol adipate, heated to 110 ℃ and stirred for reaction for 2 hours, cooled to 65 ℃; under the nitrogen atmosphere, sequentially adding 30g of isophorone diisocyanate, 8g of dimethylolpropionic acid and 1g of dibutyltin dilaurate, and heating to 80 ℃ for reaction for 2 hours; adding 16g of hydroxyethyl acrylate, and reacting for 2 hours at 80 ℃ to obtain a reaction intermediate; 60g of a mixture of methyl methacrylate and butyl acrylate was added to the reaction intermediate, 6g of triethylamine was added at 50℃and deionized water was added with stirring to obtain an emulsion.
S4: preparing a coating precursor:
3g of Lipuidambaris HIT, 4g of Lipustulan CF, 15g of Highway-Lichaise ET, 8g of reinforcing agent and 1g of organosilicon antifoaming agent are added into 75g of emulsion in sequence under stirring to obtain a coating precursor.
S5: preparing a high-fixation water-based paint:
10g of the slurry and 20g of the coating precursor were added to a vessel and stirred well to obtain a high-fixation aqueous coating.
And (3) testing: color fastness testing:
coating the high-fixation water-based paint on polyester fabric with the specification of 10cm multiplied by 10cm, drying and curing to obtain a sample; the samples were tested for rub and wash fastness according to AATCC8-2007 and AATCC 61-2006, respectively, as shown in table 1.
Comparative example 3 (branched polyurethane)
S1: preparing polyurethane:
heating 0.02mol of isophorone diisocyanate to 70 ℃, and adding 0.01mol of 1,4 butanediol to react for 4 hours to obtain a reaction intermediate; adding 0.005mol of polyethylene glycol monomethyl ether 2000 into tetrahydrofuran solution of a reaction intermediate, reacting for 2 hours at 70 ℃, adding 0.07mol of 4-hydroxyethyl imidazole, and keeping the temperature at 70 ℃ for continuous reaction for 2 hours to obtain polyurethane.
S2: preparing slurry:
dissolving 5g of polyurethane in 75g of water, adding 0.3g of organosilicon defoamer FT-58, and uniformly stirring to obtain polyurethane emulsion; adding 20g of phthalocyanine blue under stirring; 150g of zirconium beads are added and ball-milled to obtain slurry.
S3: preparing emulsion:
35g of polypropylene glycol is added into 20g of propylene glycol adipate, heated to 110 ℃ and stirred for reaction for 2 hours, cooled to 65 ℃; under the nitrogen atmosphere, sequentially adding 30g of isophorone diisocyanate, 8g of dimethylolpropionic acid and 1g of dibutyltin dilaurate, and heating to 80 ℃ for reaction for 2 hours; adding 16g of hydroxyethyl acrylate, and reacting for 2 hours at 80 ℃ to obtain a reaction intermediate; 60g of a mixture of methyl methacrylate and butyl acrylate is added into the reaction intermediate, 6g of triethylamine is added at 50 ℃, deionized water is added under stirring, and a polymer dispersion with 35% of solid content is obtained; 15g of a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine was added to the polymer dispersion, heated to 75℃and stirred for 2 hours, 1wt% potassium persulfate solution was added, and heated to 80℃and reacted for 2 hours to obtain an emulsion.
S4: preparing a coating precursor:
3g of Lipuidambaris HIT, 4g of Lipustulan CF, 15g of Highway-Lichaise ET, 8g of reinforcing agent and 1g of organosilicon antifoaming agent are added into 75g of emulsion in sequence under stirring to obtain a coating precursor.
S5: preparing a high-fixation water-based paint:
10g of the slurry and 20g of the coating precursor were added to a vessel and stirred well to obtain a high-fixation aqueous coating.
And (3) testing: color fastness testing:
coating the high-fixation water-based paint on polyester fabric with the specification of 10cm multiplied by 10cm, drying and curing to obtain a sample; the samples were tested for rub and wash fastness according to AATCC8-2007 and AATCC 61-2006, respectively, as shown in table 1.
TABLE 1
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of a high-fixation water-based paint is characterized by comprising the following steps: the method comprises the following steps:
s1: dissolving polyurethane in water, adding a defoaming agent, and uniformly stirring to obtain polyurethane emulsion; adding a coloring pigment under stirring; adding zirconium beads, and ball milling to obtain slurry;
s2: sequentially adding a water-based thickener, an emulsifier, a flexible curing agent, an enhancer and a defoamer into the emulsion under stirring to obtain a coating precursor;
s3: adding the sizing agent and the coating precursor into a container, and uniformly stirring to obtain a high-fixation water-based coating;
the polyurethane is prepared according to the following method: adding polyethylene glycol and isophorone isocyanate into tetrahydrofuran, and heating for reaction; adding 2, 2-dimethylolpropionic acid and dibutyl tin dilaurate, performing a secondary heating reaction, adding a tetrahydrofuran solution of trimethylolpropane, performing a heat preservation reaction, adding 1- (3-aminopropyl) morpholine, performing a cooling reaction, adding epoxypropanol for a reaction, adding triethylamine, and performing a neutralization reaction to obtain polyurethane;
the emulsion is prepared according to the following method: adding polypropylene glycol into propylene glycol adipate, heating, stirring and cooling; sequentially adding isophorone diisocyanate, dimethylol propionic acid and dibutyltin dilaurate under the nitrogen atmosphere, and heating for reaction; adding hydroxyethyl acrylate, and reacting at a constant temperature to obtain a reaction intermediate; adding a mixture of methyl methacrylate and butyl acrylate into a reaction intermediate, heating, adding triethylamine, and adding deionized water in a stirring state to obtain a polymer dispersion with a solid content of 35%; adding a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine into a polymer dispersion, heating and stirring, adding a potassium persulfate solution, and heating to react to obtain emulsion;
the reinforcing agent is prepared by the following steps: dispersing gamma-aminopropyl triethoxy silane in deionized water, adding purified cellulose, and performing ultrasonic treatment to obtain the reinforcing agent.
2. The method for preparing the high-fixation water-based paint according to claim 1, which is characterized in that: in the polyurethane, 60-80 parts of isophorone isocyanate, 20-40 parts of 2, 2-dimethylolpropionic acid, 5-10 parts of polyethylene glycol, 15 parts of trimethylolpropane, 12 parts of 1- (3-aminopropyl) morpholine and 5-6 parts of epoxypropanol are calculated according to parts by weight.
3. The method for preparing the high-fixation water-based paint according to claim 1, which is characterized in that: in the emulsion, according to parts by weight, 35-40 parts of polypropylene glycol, 20-25 parts of propylene glycol adipate, 30-35 parts of isophorone diisocyanate, 8-9 parts of dimethylolpropionic acid, 16-20 parts of hydroxyethyl acrylate, 60-80 parts of a mixture of methyl methacrylate and butyl acrylate, 6 parts of triethylamine, and 15-20 parts of a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine; wherein, in the mixture of methyl methacrylate and butyl acrylate, methyl methacrylate: the mass ratio of the butyl acrylate is (1-1.5): (1.5-2) in a mixture of 2-ethylhexyl acrylate and N-acryloylmorpholine, 2-ethylhexyl acrylate: the mass ratio of the N-acryloylmorpholine is (1-3): (1-3).
4. The method for preparing the high-fixation water-based paint according to claim 1, which is characterized in that: gamma-aminopropyl triethoxysilane: the mass ratio of the purified cellulose is (0.6-4.2): (2-3).
5. The method for preparing the high-fixation water-based paint according to claim 1, which is characterized in that: in the slurry, 5-8 parts of polyurethane, 0.3-0.8 part of defoamer, 20-25 parts of coloring pigment and 75-80 parts of water are calculated according to parts by weight; in the coating precursor, 3-5 parts of an aqueous thickener, 4-6 parts of an emulsifier, 15-20 parts of a flexible curing agent, 8-15 parts of an enhancer, 1-2 parts of a defoaming agent and 75-80 parts of emulsion; in the Gao Guse aqueous coating, the slurry: the mass ratio of the coating precursor is (1-2): (2-3).
6. The method for preparing the high-fixation water-based paint according to claim 1, which is characterized in that: the defoaming agent is an organic silicon defoaming agent, the coloring pigment is one or more of organic pigment and inorganic pigment, the water-based thickening agent is one or more of Lipuidamba HIT and Lipuidamba GP, the emulsifying agent is one or more of Lipuidamba CF and Lipuidamba LF, and the flexible curing agent is one or more of Lipuidambalin ET and Lipuidambalin UDT.
7. The method for preparing the high-color-fixation water-based paint according to any one of claims 1-6, wherein the water-based paint is prepared.
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