CN112358801A - High-quality water-based paint for wicker products and preparation method thereof - Google Patents
High-quality water-based paint for wicker products and preparation method thereof Download PDFInfo
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- C09D7/20—Diluents or solvents
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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
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a high-quality water-based paint for wicker products and a preparation method thereof, wherein the water-based paint comprises the following raw materials in parts by weight: 50-60 parts of water-based polycarbonate polyurethane, 10-15 parts of reinforcing filler, 20-30 parts of deionized water, 3-5 parts of film-forming assistant, 1-3 parts of defoaming agent and 2-6 parts of flatting agent; according to the reinforced filler, modified silicon dioxide and graphene oxide are mixed, amino groups of the modified silicon dioxide and carboxyl groups of the graphene oxide are subjected to dehydration condensation under the action of 1-ethyl-3 (3-dimethylpropylamine) carbodiimide, then organic silicone oil is added, and active hydroxyl groups on the side chains of the organic silicone oil and active hydroxyl groups on the surface of the modified silicon dioxide are connected under the action of hydrogen bonds to prepare the reinforced filler.
Description
Technical Field
The invention relates to the technical field of water-based paint preparation, and particularly relates to high-quality water-based paint for wicker products and a preparation method thereof.
Background
The wood lacquer is visible everywhere in daily life, not only has the decoration and beautification effect, but also has good protection effect on wood, and can be divided into two categories of water-based and oil-based. The water-based wood paint takes water as a solvent, has no volatilization of any harmful gas, and is the most safe and environment-friendly furniture paint at present. The research of the water-based wood lacquer in China has been developed for a long time, and along with the development of the technologies of resin, auxiliary agent, filler and the like related to water-based treatment, the water-based wood lacquer is applied in the fields of children furniture and the like with strict environmental protection requirements in large scale in recent years.
The existing high-quality water-based paint for the wicker products can protect the wicker products after being coated on the wicker products, but after being acted by external force, the surfaces of the wicker products are easy to scratch or crack, so that the paint film can not protect the wicker products.
Disclosure of Invention
The invention aims to provide a high-quality water-based paint for wicker products and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
the existing high-quality water-based paint for the wicker products can protect the wicker products after being coated on the wicker products, but after being acted by external force, the surfaces of the wicker products are easy to scratch or crack, so that the paint film can not protect the wicker products.
The purpose of the invention can be realized by the following technical scheme:
a high-quality water-based paint for wicker products comprises the following raw materials in parts by weight: 50-60 parts of water-based polycarbonate polyurethane, 10-15 parts of reinforcing filler, 20-30 parts of deionized water, 3-5 parts of film-forming assistant, 1-3 parts of defoaming agent and 2-6 parts of flatting agent;
the water paint is prepared by the following steps:
step S1: adding deionized water and a film-forming assistant into a stirring kettle, stirring for 20-30min under the condition that the rotating speed is 300-500r/min, adding water-based polycarbonate polyurethane, and continuously stirring for 1-1.5h to prepare a first mixture;
step S2: adding the first mixture prepared in the step S1, a defoaming agent and a leveling agent into a stirring kettle, and stirring for 1-1.5h at the rotation speed of 800-;
step S3: and (4) adding the second mixture prepared in the step (S2) and the reinforcing filler into a stirring kettle, and carrying out ultrasonic treatment for 30-50min under the condition that the frequency is 8-10MHz to prepare the water-based paint.
Further, the film-forming auxiliary agent is one or more of propylene glycol methyl ether, propylene glycol ethyl ether and propylene glycol butyl ether which are mixed in any proportion, the defoaming agent is one of defoaming agent GP, defoaming agent GPE and defoaming agent GPES, and the leveling agent is one or two of isophorone and diacetone alcohol which are mixed in any proportion.
Further, the aqueous polycarbonate polyurethane is prepared by the following steps:
step A1: adding polycarbonate diol into a reaction kettle, stirring and adding isophorone diisocyanate under the conditions that the rotating speed is 150-200r/min and the temperature is 60-70 ℃, stirring for 3-5min, heating to 80 ℃, reacting for 2-3h, cooling to 70-75 ℃, adding 2, 2-dimethylolpropionic acid and trimethylolpropane, continuing to react for 1-1.5h, cooling to 60 ℃, adding 1, 4-cyclohexanedimethanol and triethylamine, reacting for 2-3h, cooling to 20 ℃, adding isophorone diamine and deionized water, stirring for 20-30min under the condition of the rotation speed of 800-, distilling under reduced pressure for 1.5h at the temperature of 60 ℃ to obtain the water-based polycarbonate polyurethane.
Further, the using amount mass ratio of the polycarbonate diol, the isophorone diisocyanate, the 2, 2-dimethylolpropionic acid, the trimethylolpropane, the 1, 4-cyclohexanedimethanol, the triethylamine, the isophorone diamine and the deionized water in the step A1 is 45:55:7.5:2.5:16:8:5.5: 300.
Further, the reinforcing filler is prepared by the following steps:
step B1: adding phthalic anhydride and deionized water into a reaction kettle, stirring for 5-10min under the conditions that the rotating speed is 200-300r/min and the temperature is 90-95 ℃, adding sodium hydroxide, stirring for 10-15min, adjusting the pH value of a reaction solution to be 4.5-5.5, cooling to 50 ℃, introducing chlorine gas at the introducing speed of 30-35mL/min, keeping the pH value of a reaction system to be 4.5-5.5, reacting for 3-5h, centrifuging at the rotating speed of 8000r/min to remove supernatant, and drying a substrate to obtain an intermediate 1;
the reaction process is as follows:
step B2: dissolving the intermediate 1 prepared in the step B1 in xylene, stirring and adding urea under the condition of the rotation speed of 150-135 ℃, reacting for 2-3h at the temperature of 130-135 ℃, cooling to the temperature of 5-10 ℃, filtering to remove filtrate, drying a filter cake to prepare an intermediate 2, dissolving the intermediate 2 in benzene to prepare an intermediate 2 solution, adding toluene and sodium powder into a reaction kettle, stirring for 10-15min at the rotation speed of 150-200r/min and the temperature of 110 ℃, slowly dripping the intermediate 2 solution, stirring for 30-40min, adding methyl orthosilicate, continuing to react for 1-1.5h, filtering to remove filtrate, and distilling the filtrate at the temperature of 120 ℃ to prepare an intermediate 3;
the reaction process is as follows:
step B3: adding phenyl trimethoxy silane and the intermediate 3 into a reaction kettle, stirring for 5-10min at the rotation speed of 200-300r/min and the temperature of 80-85 ℃, adding deionized water and boric acid, stirring for 3-5h, and distilling at the temperature of 110 ℃ to remove low-boiling-point substances to obtain organic silicon oil;
step B4: adding deionized water, ammonia water and absolute ethyl alcohol into a reaction kettle, stirring for 10-15min at the rotation speed of 150 plus materials at 200r/min and the temperature of 50 ℃, adding ethyl orthosilicate, continuously stirring for 5-8h, adding gamma-aminopropyltriethoxysilane, heating to 70-80 ℃, reacting for 3-5h, filtering to remove filtrate, and drying a filter cake to obtain modified silicon dioxide;
step B5: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite powder under the conditions that the rotation speed is 150-200r/min and the temperature is 1-3 ℃, stirring for 10-15min, adding potassium permanganate, heating to the temperature of 5-10 ℃, reacting for 30-50min, heating to the temperature of 15-20 ℃, continuing to react for 10-15min, heating to the temperature of 30-40 ℃, continuing to react for 1-1.5h, adding a hydrogen peroxide solution, reacting for 2-3h at the temperature of 80-85 ℃, filtering to remove filtrate, washing a filter cake for 2-3 times by using a hydrochloric acid solution, and washing by using deionized water until the pH value is 7 to obtain graphene oxide;
step B6: dispersing modified silicon dioxide in tetrahydrofuran, adding graphene, triethylamine and 1-ethyl-3 (3-dimethylpropylamine) carbodiimide prepared in the step B5, reacting for 3-5h at the temperature of 40-50 ℃, adding the organic silicone oil prepared in the step B3, carrying out ultrasonic treatment for 1-1.5h at the frequency of 5-8MHz, filtering to remove filtrate, and drying a filter cake to obtain the reinforcing filler.
Further, the molar ratio of the phthalic anhydride, the sodium hydroxide and the chlorine in the step B1 is 2:2:1, the molar ratio of the intermediate 1, the xylene and the urea in the step B2 is 1:5:2, the molar ratio of the intermediate 2, the sodium powder and the methyl orthosilicate in the step B2 is 1:1:1, the molar ratio of the phenyltrimethoxysilane to the intermediate 3 and the boric acid in the step B5 is 1.5:1:2, the molar ratio of the concentrated sulfuric acid, the graphite powder, the potassium permanganate and the hydrogen peroxide solution in the step B5 is 20mL to 0.5g to 3g to 5mL, the mass fraction of the hydrogen peroxide solution is 30%, the mass fraction of the hydrochloric acid solution is 20-25%, the molar ratio of the modified silica, the graphene and the organic silicon oil in the step B6 is 1:1: 1:2, the molar amount of the triethylamine is 10-15% of the modified silica, and the molar ratio of the 1-ethyl-3 (3-dimethyl-propylamine) in the modified silica is 30-35 percent.
A preparation method of high-quality water-based paint for wicker products comprises the following steps:
step S1: adding deionized water and a film-forming assistant into a stirring kettle, stirring for 20-30min under the condition that the rotating speed is 300-500r/min, adding water-based polycarbonate polyurethane, and continuously stirring for 1-1.5h to prepare a first mixture;
step S2: adding the first mixture prepared in the step S1, a defoaming agent and a leveling agent into a stirring kettle, and stirring for 1-1.5h at the rotation speed of 800-;
step S3: and (4) adding the second mixture prepared in the step (S2) and the reinforcing filler into a stirring kettle, and carrying out ultrasonic treatment for 30-50min under the condition that the frequency is 8-10MHz to prepare the water-based paint.
The invention has the beneficial effects that: the invention prepares a water-based polycarbonate polyurethane in the process of preparing a high-quality water-based paint for wickerwork, the water-based polycarbonate polyurethane has better high temperature resistance, phthalic anhydride reacts with chlorine to prepare an intermediate 1, the intermediate 1 reacts with urea to prepare an intermediate 2, the intermediate 2 reacts with sodium powder and methyl orthosilicate in sequence to prepare an intermediate 3, the intermediate 3, phenyltrimethoxysilane and boric acid are polymerized to prepare the organic silicon oil, the side chain of the organic silicon oil contains a benzene ring and an imide group, so that the high temperature resistance of the water-based paint is improved, ethyl orthosilicate is used as a raw material to prepare nano silicon dioxide and is modified by gamma-aminopropyltriethoxysilane to prepare modified silicon dioxide, the surface of the modified silicon dioxide contains a large amount of amino groups, and graphite powder is oxidized by concentrated sulfuric acid, potassium permanganate and hydrogen peroxide solution, preparing graphene oxide, mixing modified silicon dioxide and graphene oxide, dehydrating and condensing amino groups of the modified silicon dioxide and carboxyl groups of the graphene oxide under the action of 1-ethyl-3 (3-dimethylpropylamine) carbodiimide, adding organic silicon oil, and connecting active hydroxyl groups of side chains of the organic silicon oil and active hydroxyl groups on the surface of the modified silicon dioxide under the action of hydrogen bonds to prepare the reinforcing filler.
Detailed Description
The technical solutions in the embodiments of the present invention will be 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
A high-quality water-based paint for wicker products comprises the following raw materials in parts by weight: 50 parts of water-based polycarbonate polyurethane, 10 parts of reinforcing filler, 20 parts of deionized water, 3 parts of propylene glycol methyl ether, 1 parts of defoaming agent GP and 2 parts of isophorone;
the water paint is prepared by the following steps:
step S1: adding deionized water and propylene glycol methyl ether into a stirring kettle, stirring for 20min under the condition that the rotating speed is 300r/min, adding aqueous polycarbonate polyurethane, and continuously stirring for 1h to prepare a first mixture;
step S2: adding the first mixture prepared in the step S1, a defoaming agent GP and isophorone into a stirring kettle, and stirring for 1h at the rotating speed of 800r/min to prepare a second mixture;
step S3: and (4) adding the second mixture prepared in the step (S2) and the reinforcing filler into a stirring kettle, and carrying out ultrasonic treatment for 30min under the condition that the frequency is 8MHz to prepare the water-based paint.
The aqueous polycarbonate polyurethane is prepared by the following steps:
step A1: adding polycarbonate diol into a reaction kettle, stirring and adding isophorone diisocyanate under the conditions of the rotation speed of 150r/min and the temperature of 60 ℃, stirring for 3min, heating to 80 ℃, reacting for 2h, cooling to 70 ℃, adding 2, 2-dimethylolpropionic acid and trimethylolpropane, continuing to react for 1h, cooling to 60 ℃, adding 1, 4-cyclohexanedimethanol and triethylamine, reacting for 2h, cooling to 20 ℃, adding isophorone diamine and deionized water, stirring for 20min under the condition of the rotation speed of 800r/min, and distilling under reduced pressure for 1.5h under the condition of the temperature of 60 ℃ to obtain the aqueous polycarbonate polyurethane.
The reinforcing filler is prepared by the following steps:
step B1: adding phthalic anhydride and deionized water into a reaction kettle, stirring for 5min at the rotation speed of 200r/min and the temperature of 90 ℃, adding sodium hydroxide, stirring for 10min, adjusting the pH value of a reaction solution to 4.5, cooling to the temperature of 50 ℃, introducing chlorine at the speed of 30mL/min, keeping the pH value of the reaction system at 4.5, reacting for 3, centrifuging at the rotation speed of 8000r/min to remove a supernatant, and drying a substrate to obtain an intermediate 1;
step B2: dissolving the intermediate 1 prepared in the step B1 in xylene, stirring and adding urea under the condition of the rotation speed of 150r/min, reacting for 2 hours at the temperature of 130 ℃, cooling to the temperature of 5 ℃, filtering to remove filtrate, drying a filter cake to prepare an intermediate 2, dissolving the intermediate 2 in benzene to prepare an intermediate 2 solution, adding toluene and sodium powder into a reaction kettle, stirring for 10 minutes at the rotation speed of 150r/min and the temperature of 110 ℃, slowly dropwise adding the intermediate 2 solution, stirring for 30 minutes, adding methyl orthosilicate, continuing to react for 1 hour, filtering to remove filtrate, and distilling the filtrate at the temperature of 120 ℃ to prepare an intermediate 3;
step B3: adding phenyl trimethoxy silane and the intermediate 3 into a reaction kettle, stirring for 5min at the rotation speed of 200r/min and the temperature of 80 ℃, adding deionized water and boric acid, stirring for 3h, and distilling at the temperature of 110 ℃ to remove low-boiling-point substances to obtain organic silicone oil;
step B4: adding deionized water, ammonia water and absolute ethyl alcohol into a reaction kettle, stirring for 10min at the rotation speed of 150r/min and the temperature of 50 ℃, adding ethyl orthosilicate, continuously stirring for 5h, adding gamma-aminopropyltriethoxysilane, heating to the temperature of 70 ℃, reacting for 3h, filtering to remove filtrate, and drying a filter cake to obtain modified silicon dioxide;
step B5: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite powder under the conditions that the rotating speed is 150r/min and the temperature is 1 ℃, stirring for 10min, adding potassium permanganate, heating to the temperature of 5 ℃, reacting for 30min, heating to the temperature of 15 ℃, continuing to react for 10min, heating to the temperature of 30 ℃, continuing to react for 1h, adding a hydrogen peroxide solution, reacting for 2h under the temperature of 80 ℃, filtering to remove filtrate, washing a filter cake for 2 times by using a hydrochloric acid solution, and washing by using deionized water until the pH value is 7 to obtain graphene oxide;
step B6: dispersing modified silicon dioxide in tetrahydrofuran, adding graphene, triethylamine and 1-ethyl-3 (3-dimethylpropylamine) carbodiimide prepared in the step B5, reacting for 3 hours at the temperature of 40 ℃, adding organic silicon oil prepared in the step B3, carrying out ultrasonic treatment for 1 hour at the frequency of 5MHz, filtering to remove filtrate, and drying a filter cake to prepare the reinforcing filler.
Example 2
A high-quality water-based paint for wicker products comprises the following raw materials in parts by weight: 55 parts of water-based polycarbonate polyurethane, 13 parts of reinforcing filler, 25 parts of deionized water, 4 parts of propylene glycol methyl ether, 2 parts of defoaming agent GP and 4 parts of isophorone;
the water paint is prepared by the following steps:
step S1: adding deionized water and propylene glycol methyl ether into a stirring kettle, stirring for 30min at the rotating speed of 300r/min, adding aqueous polycarbonate polyurethane, and continuously stirring for 1h to prepare a first mixture;
step S2: adding the first mixture prepared in the step S1, a defoaming agent GP and isophorone into a stirring kettle, and stirring for 1h at the rotating speed of 1000r/min to prepare a second mixture;
step S3: and (4) adding the second mixture prepared in the step (S2) and the reinforcing filler into a stirring kettle, and carrying out ultrasonic treatment for 30min under the condition that the frequency is 10MHz to prepare the water-based paint.
The aqueous polycarbonate polyurethane is prepared by the following steps:
step A1: adding polycarbonate diol into a reaction kettle, stirring and adding isophorone diisocyanate under the conditions of a rotation speed of 200r/min and a temperature of 60 ℃, stirring for 5min, heating to a temperature of 80 ℃, reacting for 2h, cooling to a temperature of 75 ℃, adding 2, 2-dimethylolpropionic acid and trimethylolpropane, continuing to react for 1h, cooling to a temperature of 60 ℃, adding 1, 4-cyclohexanedimethanol and triethylamine, reacting for 3h, cooling to a temperature of 20 ℃, adding isophorone diamine and deionized water, stirring for 20min under the condition of a rotation speed of 1000r/min, and distilling under reduced pressure for 1.5h under the condition of a temperature of 60 ℃ to obtain the aqueous polycarbonate polyurethane.
The reinforcing filler is prepared by the following steps:
step B1: adding phthalic anhydride and deionized water into a reaction kettle, stirring for 10min at the rotation speed of 300r/min and the temperature of 90 ℃, adding sodium hydroxide, stirring for 10min, adjusting the pH value of a reaction solution to 4.5-5.5, cooling to the temperature of 50 ℃, introducing chlorine at the speed of 35mL/min, keeping the pH value of a reaction system at 4.5, reacting for 5h, centrifuging at the rotation speed of 8000r/min to remove supernatant, and drying a substrate to obtain an intermediate 1;
step B2: dissolving the intermediate 1 prepared in the step B1 in xylene, stirring and adding urea under the condition of the rotation speed of 150r/min, reacting for 2 hours at the temperature of 135 ℃, cooling to the temperature of 10 ℃, filtering to remove filtrate, drying a filter cake to prepare an intermediate 2, dissolving the intermediate 2 in benzene to prepare an intermediate 2 solution, adding toluene and sodium powder into a reaction kettle, stirring for 15 minutes at the rotation speed of 150r/min and the temperature of 110 ℃, slowly dropwise adding the intermediate 2 solution, stirring for 30 minutes, adding methyl orthosilicate, continuing to react for 1.5 hours, filtering to remove filtrate, and distilling the filtrate at the temperature of 120 ℃ to prepare an intermediate 3;
step B3: adding phenyl trimethoxy silane and the intermediate 3 into a reaction kettle, stirring for 5min at the rotation speed of 200r/min and the temperature of 85 ℃, adding deionized water and boric acid, stirring for 5h, and distilling at the temperature of 110 ℃ to remove low-boiling-point substances to obtain organic silicone oil;
step B4: adding deionized water, ammonia water and absolute ethyl alcohol into a reaction kettle, stirring for 15min at the rotation speed of 150r/min and the temperature of 50 ℃, adding ethyl orthosilicate, continuously stirring for 5h, adding gamma-aminopropyltriethoxysilane, heating to 80 ℃, reacting for 3h, filtering to remove filtrate, and drying a filter cake to obtain modified silicon dioxide;
step B5: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite powder under the conditions that the rotating speed is 200r/min and the temperature is 1 ℃, stirring for 15min, adding potassium permanganate, heating to the temperature of 5 ℃, reacting for 50min, heating to the temperature of 15 ℃, continuing to react for 15min, heating to the temperature of 30 ℃, continuing to react for 1.5h, adding a hydrogen peroxide solution, reacting for 3h under the temperature of 80 ℃, filtering to remove filtrate, washing a filter cake for 2 times by using a hydrochloric acid solution, and washing by using deionized water until the pH value is 7 to obtain graphene oxide;
step B6: dispersing modified silicon dioxide in tetrahydrofuran, adding graphene, triethylamine and 1-ethyl-3 (3-dimethylpropylamine) carbodiimide prepared in the step B5, reacting for 3 hours at the temperature of 50 ℃, adding organic silicon oil prepared in the step B3, carrying out ultrasonic treatment for 1 hour at the frequency of 8MHz, filtering to remove filtrate, and drying a filter cake to prepare the reinforcing filler.
Example 3
A high-quality water-based paint for wicker products comprises the following raw materials in parts by weight: 60 parts of water-based polycarbonate polyurethane, 15 parts of reinforcing filler, 30 parts of deionized water, 5 parts of propylene glycol methyl ether, 3 parts of defoaming agent GP and 6 parts of isophorone;
the water paint is prepared by the following steps:
step S1: adding deionized water and propylene glycol methyl ether into a stirring kettle, stirring for 30min at the rotation speed of 500r/min, adding aqueous polycarbonate polyurethane, and continuously stirring for 1.5h to obtain a first mixture;
step S2: adding the first mixture prepared in the step S1, a defoaming agent GP and isophorone into a stirring kettle, and stirring for 1.5 hours at the rotating speed of 1000r/min to prepare a second mixture;
step S3: and (4) adding the second mixture prepared in the step (S2) and the reinforcing filler into a stirring kettle, and carrying out ultrasonic treatment for 50min under the condition that the frequency is 10MHz to prepare the water-based paint.
The aqueous polycarbonate polyurethane is prepared by the following steps:
step A1: adding polycarbonate diol into a reaction kettle, stirring and adding isophorone diisocyanate under the conditions of a rotation speed of 200r/min and a temperature of 70 ℃, stirring for 5min, heating to a temperature of 80 ℃, reacting for 3h, cooling to a temperature of 75 ℃, adding 2, 2-dimethylolpropionic acid and trimethylolpropane, continuing to react for 1.5h, cooling to a temperature of 60 ℃, adding 1, 4-cyclohexanedimethanol and triethylamine, reacting for 3h, cooling to a temperature of 20 ℃, adding isophorone diamine and deionized water, stirring for 30min under the condition of a rotation speed of 1000r/min, and distilling under reduced pressure for 1.5h under the condition of a temperature of 60 ℃ to obtain the aqueous polycarbonate polyurethane.
The reinforcing filler is prepared by the following steps:
step B1: adding phthalic anhydride and deionized water into a reaction kettle, stirring for 10min at the rotation speed of 300r/min and the temperature of 95 ℃, adding sodium hydroxide, stirring for 15min, adjusting the pH value of a reaction solution to 5.5, cooling to the temperature of 50 ℃, introducing chlorine at the speed of 35mL/min, keeping the pH value of a reaction system at 5.5, reacting for 5h, centrifuging at the rotation speed of 8000r/min to remove a supernatant, and drying a substrate to obtain an intermediate 1;
step B2: dissolving the intermediate 1 prepared in the step B1 in xylene, stirring and adding urea under the condition of the rotating speed of 200r/min, reacting for 3 hours at the temperature of 135 ℃, cooling to the temperature of 10 ℃, filtering to remove filtrate, drying a filter cake to prepare an intermediate 2, dissolving the intermediate 2 in benzene to prepare an intermediate 2 solution, adding toluene and sodium powder into a reaction kettle, stirring for 15 minutes at the rotating speed of 200r/min and the temperature of 110 ℃, slowly dropwise adding the intermediate 2 solution, stirring for 40 minutes, adding methyl orthosilicate, continuing to react for 1.5 hours, filtering to remove filtrate, and distilling the filtrate at the temperature of 120 ℃ to prepare an intermediate 3;
step B3: adding phenyl trimethoxy silane and the intermediate 3 into a reaction kettle, stirring for 10min at the rotation speed of 300r/min and the temperature of 85 ℃, adding deionized water and boric acid, stirring for 5h, and distilling at the temperature of 110 ℃ to remove low-boiling-point substances to obtain organic silicone oil;
step B4: adding deionized water, ammonia water and absolute ethyl alcohol into a reaction kettle, stirring for 15min at the rotation speed of 200r/min and the temperature of 50 ℃, adding ethyl orthosilicate, continuously stirring for 8h, adding gamma-aminopropyltriethoxysilane, heating to 80 ℃, reacting for 5h, filtering to remove filtrate, and drying a filter cake to obtain modified silicon dioxide;
step B5: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite powder under the conditions that the rotating speed is 200r/min and the temperature is 3 ℃, stirring for 15min, adding potassium permanganate, heating to the temperature of 10 ℃, reacting for 50min, heating to the temperature of 20 ℃, continuing to react for 15min, heating to the temperature of 40 ℃, continuing to react for 1.5h, adding a hydrogen peroxide solution, reacting for 3h under the temperature of 85 ℃, filtering to remove filtrate, washing a filter cake for 3 times by using a hydrochloric acid solution, and washing by using deionized water until the pH value is 7 to obtain graphene oxide;
step B6: dispersing modified silicon dioxide in tetrahydrofuran, adding graphene, triethylamine and 1-ethyl-3 (3-dimethylpropylamine) carbodiimide prepared in the step B5, reacting for 5 hours at the temperature of 50 ℃, adding organic silicon oil prepared in the step B3, carrying out ultrasonic treatment for 1.5 hours at the frequency of 8MHz, filtering to remove filtrate, and drying a filter cake to obtain the reinforcing filler.
Comparative example
The comparative example is a common water-based paint on the market.
The aqueous paints obtained in examples 1 to 3 and comparative example were subjected to performance tests, the test results of which are shown in table 1 below;
TABLE 1
| Example 1 | Example 2 | Example 3 | Comparative example | Test method | |
| Hardness of | 3H | 3H | 3H | H | CB/T1768-2006 |
| Wear-resistant | 0.028 | 0.026 | 0.025 | 0.038 | GB/T6739-2006 |
| Scratch | No scratch | No scratch | No scratch | Obvious scratch | 1kg weight |
As is apparent from Table 1 above, the hardness of the paint films of the aqueous paints obtained in examples 1 to 3 was 3H and the film resistance was 0.025 to 0.028, and no scratch was caused by the use of a 1kg weight, while the hardness of the paint film of the aqueous paint obtained in comparative example was H and the film resistance was 0.038, and marked scratch was caused by the use of a 1kg weight, indicating that the present invention has a very good scratch resistance.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (7)
1. A high-quality water-based paint for wicker products is characterized in that: the feed comprises the following raw materials in parts by weight: 50-60 parts of water-based polycarbonate polyurethane, 10-15 parts of reinforcing filler, 20-30 parts of deionized water, 3-5 parts of film-forming assistant, 1-3 parts of defoaming agent and 2-6 parts of flatting agent;
the water paint is prepared by the following steps:
step S1: adding deionized water and a film-forming assistant into a stirring kettle, stirring for 20-30min under the condition that the rotating speed is 300-500r/min, adding water-based polycarbonate polyurethane, and continuously stirring for 1-1.5h to prepare a first mixture;
step S2: adding the first mixture prepared in the step S1, a defoaming agent and a leveling agent into a stirring kettle, and stirring for 1-1.5h at the rotation speed of 800-;
step S3: and (4) adding the second mixture prepared in the step (S2) and the reinforcing filler into a stirring kettle, and carrying out ultrasonic treatment for 30-50min under the condition that the frequency is 8-10MHz to prepare the water-based paint.
2. The high-quality water-based paint for wicker products according to claim 1, which is characterized in that: the film-forming auxiliary agent is one or a mixture of more of propylene glycol methyl ether, propylene glycol ethyl ether and propylene glycol butyl ether in any proportion, the defoaming agent is one of defoaming agent GP, defoaming agent GPE and defoaming agent GPES, and the leveling agent is one or a mixture of two of isophorone and diacetone alcohol in any proportion.
3. The high-quality water-based paint for wicker products according to claim 1, which is characterized in that: the aqueous polycarbonate polyurethane is prepared by the following steps:
step A1: adding polycarbonate diol into a reaction kettle, stirring and adding isophorone diisocyanate under the conditions that the rotating speed is 150-200r/min and the temperature is 60-70 ℃, stirring for 3-5min, heating to 80 ℃, reacting for 2-3h, cooling to 70-75 ℃, adding 2, 2-dimethylolpropionic acid and trimethylolpropane, continuing to react for 1-1.5h, cooling to 60 ℃, adding 1, 4-cyclohexanedimethanol and triethylamine, reacting for 2-3h, cooling to 20 ℃, adding isophorone diamine and deionized water, stirring for 20-30min under the condition of the rotation speed of 800-, distilling under reduced pressure for 1.5h at the temperature of 60 ℃ to obtain the water-based polycarbonate polyurethane.
4. The high-quality water-based paint for wicker products according to claim 3, wherein: the using amount mass ratio of the polycarbonate diol, the isophorone diisocyanate, the 2, 2-dimethylolpropionic acid, the trimethylolpropane, the 1, 4-cyclohexanedimethanol, the triethylamine, the isophorone diamine and the deionized water in the step A1 is 45:55:7.5:2.5:16:8:5.5: 300.
5. The high-quality water-based paint for wicker products according to claim 1, which is characterized in that: the reinforcing filler is prepared by the following steps:
step B1: adding phthalic anhydride and deionized water into a reaction kettle, stirring for 5-10min under the conditions that the rotating speed is 200-300r/min and the temperature is 90-95 ℃, adding sodium hydroxide, stirring for 10-15min, adjusting the pH value of a reaction solution to be 4.5-5.5, cooling to 50 ℃, introducing chlorine gas at the introducing speed of 30-35mL/min, keeping the pH value of a reaction system to be 4.5-5.5, reacting for 3-5h, centrifuging at the rotating speed of 8000r/min to remove supernatant, and drying a substrate to obtain an intermediate 1;
step B2: dissolving the intermediate 1 prepared in the step B1 in xylene, stirring and adding urea under the condition of the rotation speed of 150-135 ℃, reacting for 2-3h at the temperature of 130-135 ℃, cooling to the temperature of 5-10 ℃, filtering to remove filtrate, drying a filter cake to prepare an intermediate 2, dissolving the intermediate 2 in benzene to prepare an intermediate 2 solution, adding toluene and sodium powder into a reaction kettle, stirring for 10-15min at the rotation speed of 150-200r/min and the temperature of 110 ℃, slowly dripping the intermediate 2 solution, stirring for 30-40min, adding methyl orthosilicate, continuing to react for 1-1.5h, filtering to remove filtrate, and distilling the filtrate at the temperature of 120 ℃ to prepare an intermediate 3;
step B3: adding phenyl trimethoxy silane and the intermediate 3 into a reaction kettle, stirring for 5-10min at the rotation speed of 200-300r/min and the temperature of 80-85 ℃, adding deionized water and boric acid, stirring for 3-5h, and distilling at the temperature of 110 ℃ to remove low-boiling-point substances to obtain organic silicon oil;
step B4: adding deionized water, ammonia water and absolute ethyl alcohol into a reaction kettle, stirring for 10-15min at the rotation speed of 150 plus materials at 200r/min and the temperature of 50 ℃, adding ethyl orthosilicate, continuously stirring for 5-8h, adding gamma-aminopropyltriethoxysilane, heating to 70-80 ℃, reacting for 3-5h, filtering to remove filtrate, and drying a filter cake to obtain modified silicon dioxide;
step B5: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite powder under the conditions that the rotation speed is 150-200r/min and the temperature is 1-3 ℃, stirring for 10-15min, adding potassium permanganate, heating to the temperature of 5-10 ℃, reacting for 30-50min, heating to the temperature of 15-20 ℃, continuing to react for 10-15min, heating to the temperature of 30-40 ℃, continuing to react for 1-1.5h, adding a hydrogen peroxide solution, reacting for 2-3h at the temperature of 80-85 ℃, filtering to remove filtrate, washing a filter cake for 2-3 times by using a hydrochloric acid solution, and washing by using deionized water until the pH value is 7 to obtain graphene oxide;
step B6: dispersing modified silicon dioxide in tetrahydrofuran, adding graphene, triethylamine and 1-ethyl-3 (3-dimethylpropylamine) carbodiimide prepared in the step B5, reacting for 3-5h at the temperature of 40-50 ℃, adding the organic silicone oil prepared in the step B3, carrying out ultrasonic treatment for 1-1.5h at the frequency of 5-8MHz, filtering to remove filtrate, and drying a filter cake to obtain the reinforcing filler.
6. The high-quality water-based paint for wicker products according to claim 5, wherein: the molar ratio of the use amounts of the phthalic anhydride, the sodium hydroxide and the chlorine in the step B1 is 2:2:1, the molar ratio of the use amounts of the intermediate 1, the xylene and the urea in the step B2 is 1:5:2, the molar ratio of the use amounts of the intermediate 2, the sodium powder and the methyl orthosilicate is 1:1:1, the molar ratio of the use amounts of the phenyltrimethoxysilane, the intermediate 3 and the boric acid is 1.5:1:2, and the molar ratio of the use amounts of the concentrated sulfuric acid, the graphite powder, the potassium permanganate and the hydrogen peroxide solution in the step B5 is 20mL:0.5g:3g:5mL, the mass fraction of the hydrogen peroxide solution is 30%, the mass fraction of the hydrochloric acid solution is 20-25%, the mass ratio of the modified silicon dioxide, the graphene and the organic silicon oil in the step B6 is 1:1:2, the amount of triethylamine is 10-15% of the mass of the modified silicon dioxide, and the amount of 1-ethyl-3 (3-dimethylpropylamine) carbodiimide is 30-35% of the mass of the modified silicon dioxide.
7. The method for preparing the high-quality water-based paint for the wicker products according to claim 1, which is characterized in that: the method specifically comprises the following steps:
step S1: adding deionized water and a film-forming assistant into a stirring kettle, stirring for 20-30min under the condition that the rotating speed is 300-500r/min, adding water-based polycarbonate polyurethane, and continuously stirring for 1-1.5h to prepare a first mixture;
step S2: adding the first mixture prepared in the step S1, a defoaming agent and a leveling agent into a stirring kettle, and stirring for 1-1.5h at the rotation speed of 800-;
step S3: and (4) adding the second mixture prepared in the step (S2) and the reinforcing filler into a stirring kettle, and carrying out ultrasonic treatment for 30-50min under the condition that the frequency is 8-10MHz to prepare the water-based paint.
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