CN112920660A - Nano-material modified heat-insulation interior wall coating and preparation method thereof - Google Patents
Nano-material modified heat-insulation interior wall coating and preparation method thereof Download PDFInfo
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- 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
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/61—Additives non-macromolecular inorganic
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Abstract
The invention discloses a nano-material modified heat-insulation interior wall coating and a preparation method thereof, wherein the coating comprises the following raw materials in parts by weight: 30-50 parts of acrylic emulsion, 2-4 parts of titanium dioxide, 3-5 parts of reinforcing liquid, 0.3-0.5 part of defoaming agent, 0.5-2 parts of dispersing agent, 1-3 parts of film forming agent and 20-30 parts of water; the reinforcing liquid is prepared in the preparation process, and can also contain a large amount of long-chain alkyl, the long-chain alkyl has a good hydrophobic effect, after a coating is formed on the coating, the surface of the coating has a good hydrophobic effect, the coating is more convenient and fast to clean, and meanwhile, the reinforcing liquid contains a high molecular chain, has good corrosion resistance, low internal rotation barrier energy of the molecular chain and easy rotation of the molecular chain segment, so that the dried coating has higher toughness, the coating is not easy to scratch, and the attractiveness of the coating is ensured.
Description
Technical Field
The invention relates to the technical field of preparation of coatings, in particular to a nano-material modified heat-insulation interior wall coating and a preparation method thereof.
Background
The coating is a continuous film which is coated on the surface of a protected or decorated object and can form firm adhesion with the object to be coated, and is a viscous liquid which is prepared by taking resin, oil or emulsion as a main material, adding or not adding pigments and fillers, adding corresponding auxiliary agents and using organic solvent or water. The paint has various types and different performance characteristics, various paints and modified paints thereof appear on the market, and the interior wall paint is the latex paint for general decoration. The latex paint is an emulsion material and is divided into two categories, namely polyvinyl acetate emulsion and acrylic emulsion, according to different base materials. The emulsion paint uses water as diluent, is a material with convenient construction, safety, water washing resistance and good air permeability, and can be prepared into different colors according to different color matching schemes.
The existing heat-preservation interior wall coating has the advantages that in the using process, furniture can collide with a paint film due to the change of the position of the furniture, the paint film is damaged, meanwhile, the waterproof effect is poor, leakage is easy to occur, the paint film is corroded, and the service life of the paint film is short.
Disclosure of Invention
The invention aims to provide a nano material modified heat-insulation interior wall coating and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
the existing heat-preservation interior wall coating has the advantages that in the using process, furniture can collide with a paint film due to the change of the position of the furniture, the paint film is damaged, meanwhile, the waterproof effect is poor, leakage is easy to occur, the paint film is corroded, and the service life of the paint film is short.
The purpose of the invention can be realized by the following technical scheme:
a nano-material modified heat-insulation interior wall coating comprises the following raw materials in parts by weight: 30-50 parts of acrylic emulsion, 2-4 parts of titanium dioxide, 3-5 parts of reinforcing liquid, 0.3-0.5 part of defoaming agent, 0.5-2 parts of dispersing agent, 1-3 parts of film forming agent and 20-30 parts of water;
the heat-insulating interior wall coating is prepared by the following steps:
step S1: adding the defoaming agent, the dispersing agent and water into a stirring kettle, and stirring for 15-20min under the condition that the rotating speed is 300-;
step S2: adding the titanium dioxide and the first mixture into a grinder, grinding and mixing, and sieving by using a 25-30 micron sieve to obtain a second mixture;
step S3: and (4) adding the second mixture prepared in the step S2, the acrylic emulsion, the reinforcing liquid and the film forming agent into a stirring kettle, and stirring for 1-1.5 hours under the condition that the rotating speed is 1200-1500r/min to prepare the heat-insulating interior wall coating.
Further, the defoaming agent is one of GPES defoaming agent, GP defoaming agent and GPE defoaming agent, the dispersing agent is one or more of triethyl hexyl phosphoric acid, sodium dodecyl sulfate and methyl amyl alcohol which are mixed in any proportion, and the film forming agent is one or more of dodecyl glycol, propylene glycol and hexanediol which are mixed in any proportion.
Further, the reinforcing liquid is prepared by the following steps:
step A1: adding concentrated sulfuric acid, potassium persulfate and phosphorus pentoxide into a reaction kettle, stirring for 3-5min at the rotation speed of 200-90 ℃ and at the temperature of 80-90 ℃, adding graphite powder, cooling to the temperature of 30-35 ℃, reacting for 5-8h, filtering to remove filtrate, washing a filter cake to be neutral by using deionized water to obtain pre-oxidized graphite, adding the pre-oxidized graphite, sodium nitrate and concentrated sulfuric acid into the reaction kettle, stirring for 5-10min at the rotation speed of 150-200r/min and at the temperature of 3-5 ℃, adding potassium permanganate, stirring at the temperature of 10-15 ℃ for 20-30min, heating to 35-40 ℃, continuously stirring for 3-5h, adding deionized water and hydrogen peroxide, continuously stirring for 10-15min, dialyzing with deionized water to prepare graphene oxide;
step A2: adding tetraethoxysilane, ethanol and deionized water into a reaction kettle, stirring for 3-5h under the conditions that the rotating speed is 200-80 ℃ and the temperature is 70-80 ℃, adding octadecyltrimethoxysilane, reacting for 5-6h under the condition that the pH value of a reaction liquid is 5-6 to prepare modified nano-silicon, adding the modified nano-silicon, the graphene oxide prepared in the step A1 and the ethanol into the reaction kettle, and performing ultrasonic treatment for 2-3h under the condition that the frequency is 5-8MHz to prepare a first mixed glue solution;
step A3: uniformly mixing deionized water and span 80 to prepare pre-emulsion, uniformly mixing benzol olefine acid, lauryl methacrylate, acrylamide and deionized water to prepare monomer liquid, adding one third of the monomer liquid into one half of the pre-emulsion, stirring for 20-30min under the condition of the rotating speed of 500 plus 800r/min to prepare first mixed liquid, mixing one fourth of the pre-emulsion and potassium persulfate solution, adding the rest of the monomer liquid, stirring for 20-30min under the conditions of the rotating speed of 200 plus 300r/min and the temperature of 50-60 ℃ to prepare second mixed liquid, adding the first mixed liquid, the second mixed liquid, the rest of the pre-emulsion and ammonium persulfate solution into a reaction kettle, reacting for 1-1.5h under the conditions of the rotating speed of 150 plus 200r/min and the temperature of 80-85 ℃, preparing a composite emulsion;
step A4: adding diphenylmethane diisocyanate, 2-dimethylolpropionic acid and dichloromethane into a reaction kettle, stirring and adding triethylamine under the conditions of the rotation speed of 200-85 ℃ and the temperature of 80-85 ℃ to perform reflux reaction for 8-10h to obtain an intermediate 1, adding bisphenol A epoxy resin into the reaction kettle, melting at the temperature of 80-90 ℃, adding polyethylene glycol, deionized water and the intermediate 1, stirring at the rotation speed of 150-200r/min for 10-15min, performing reflux reaction at the temperature of 110-120 ℃ for 3-5h, cooling to 60-65 ℃, adding triethylamine, and continuing stirring for 20-30min to obtain a second mixed glue solution;
the reaction process is as follows:
step A5: and (2) adding the first mixed glue solution prepared in the step A2, the composite emulsion prepared in the step A3 and the second mixed glue solution prepared in the step A4 into a reaction kettle, stirring and adding 1-hydroxybenzotriazole under the conditions that the rotating speed is 150-200r/min and the temperature is 35-40 ℃, reacting for 3-5h, adding basalt fibers, and performing ultrasonic treatment for 2-3h under the condition that the frequency is 5-8MHz to prepare the reinforcing liquid.
Further, the amount ratio of concentrated sulfuric acid, potassium persulfate, phosphorus pentoxide and graphite powder used for preparing the pre-oxidized graphite in the step A1 is 4mL:1.5g:1g:3g, the mass fraction of the concentrated sulfuric acid is 95%, the amount ratio of the pre-oxidized graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, deionized water and hydrogen peroxide used for preparing the oxidized graphene is 1g:0.6g:25mL:3g:150mL:5mL, and the mass fraction of the hydrogen peroxide is 25%.
Further, the dosage ratio of the ethyl orthosilicate, the ethanol, the deionized water and the octadecyltrimethoxysilane in the step A2 is 5g to 3mL to 50mL to 2.5g, and the dosage ratio of the modified nano-silicon, the graphene oxide and the ethanol is 2g to 3g to 15 mL.
Further, the dosage ratio of the deionized water and the span 80 in the step A3 is 20mL:1g, the dosage ratio of the benzol olefine acid, the lauryl methacrylate, the acrylamide and the deionized water is 1g:1g:2g:5mL, the total dosage volume ratio of the pre-emulsion and the monomer liquid is 1:2, the dosage of the potassium persulfate is 1-2% of the total reactant dosage mass, and the dosage of the ammonium persulfate is 1-2% of the total reactant dosage mass.
Further, the molar ratio of the diphenylmethane diisocyanate to the 2, 2-dimethylolpropionic acid in the step A4 is 1:2, the amount of triethylamine is 15% of the mass of the diphenylmethane diisocyanate, the mass ratio of the bisphenol A type resin, the polyethylene glycol and the intermediate 1 is 5:3:3, and the amount of triethylamine is 15% of the mass of the bisphenol A type resin.
Further, the dosage ratio of the first mixed glue solution, the composite emulsion, the second mixed glue solution and the basalt fiber in the step A5 is 10mL:10mL:15mL:3g, and the dosage of the 1-hydroxybenzotriazole is 20% of the mass of the first mixed glue solution.
A preparation method of a nano-material modified heat-insulation interior wall coating specifically comprises the following steps:
step S1: adding the defoaming agent, the dispersing agent and water into a stirring kettle, and stirring for 15-20min under the condition that the rotating speed is 300-;
step S2: adding the titanium dioxide and the first mixture into a grinder, grinding and mixing, and sieving by using a 25-30 micron sieve to obtain a second mixture;
step S3: and (4) adding the second mixture prepared in the step S2, the acrylic emulsion, the reinforcing liquid and the film forming agent into a stirring kettle, and stirring for 1-1.5 hours under the condition that the rotating speed is 1200-1500r/min to prepare the heat-insulating interior wall coating.
The invention has the beneficial effects that: the invention prepares a reinforcing liquid in the process of preparing a nano material modified heat-preservation interior wall coating, the reinforcing liquid takes graphite powder as a raw material, graphite is oxidized to convert active hydroxyl on the surface of the graphite into carboxyl to prepare graphene oxide, ethyl orthosilicate is hydrolyzed to prepare nano silicon dioxide, octadecyl trimethoxy silane is hydrolyzed to generate silanol and active hydroxyl on the surface of the nano silicon dioxide to form hydrogen bonds so as to graft a large amount of long-chain alkyl on the surface of the nano silicon dioxide, styrene acid, lauryl methacrylate and acrylamide are polymerized, the styrene acid, the lauryl methacrylate and the acrylamide all contain unsaturated double bonds, meanwhile, the formed polymer side chain contains the long-chain alkyl, diphenylmethane diisocyanate and 2, 2-dimethylolpropionic acid are reacted, preparing an intermediate 1, reacting an isocyanate group on the intermediate 1 with an epoxy group on bisphenol A epoxy resin, reacting another isocyanate based on a hydroxyl group at the end of polyethylene glycol to connect molecular chains of two polymers, reacting a polymer side chain in the first mixed glue solution, the composite emulsion and the second mixed glue solution under the action of 1-hydroxybenzotriazole to react with carboxyl on graphene oxide in the first mixed glue solution, reacting the residual amino of the polymer in the composite emulsion with the carboxyl on the second mixed glue solution to connect the molecular chains, and performing ultrasonic treatment on the molecular chains and basalt fibers to prepare a reinforcing liquid, wherein the reinforcing liquid can also contain a large amount of long-chain alkyl which has a good hydrophobic effect, and after a coating is formed on the coating, the surface of the coating has a good hydrophobic effect, meanwhile, the coating film is more convenient to clean, contains a high molecular chain, has good corrosion resistance, has low internal rotation barrier energy of the molecular chain, and is easy to rotate a molecular chain segment, so that the dried coating film has higher toughness, the coating film is not easy to scratch, and the coating film is ensured to be attractive.
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 nano-material modified heat-insulation interior wall coating comprises the following raw materials in parts by weight: 30 parts of acrylic emulsion, 2 parts of titanium dioxide, 3 parts of reinforcing liquid, 0.3 part of GP type defoaming agent, 0.5 part of triethyl hexyl phosphoric acid, 1 part of dodecyl glycol ester and 20 parts of water;
the heat-insulating interior wall coating is prepared by the following steps:
step S1: adding a GP type defoaming agent, triethylhexyl phosphoric acid and water into a stirring kettle, and stirring for 15min under the condition that the rotating speed is 300r/min to prepare a first mixture;
step S2: adding the titanium dioxide and the first mixture into a grinder, grinding and mixing, and sieving by using a 25-micron sieve to obtain a second mixture;
step S3: and (4) adding the second mixture prepared in the step (S2), acrylic emulsion, reinforcing liquid and lauryl ester into a stirring kettle, and stirring for 1h at the rotation speed of 1200r/min to prepare the heat-insulating interior wall coating.
The reinforcing liquid is prepared by the following steps:
step A1: adding concentrated sulfuric acid, potassium persulfate and phosphorus pentoxide into a reaction kettle, stirring for 3min at the rotation speed of 200r/min and the temperature of 80 ℃, adding graphite powder, cooling to the temperature of 30 ℃, reacting for 5h, filtering to remove filtrate, washing a filter cake to be neutral by using deionized water to obtain pre-oxidized graphite, adding the pre-oxidized graphite, sodium nitrate and concentrated sulfuric acid into the reaction kettle, stirring for 5min at the rotation speed of 150r/min and the temperature of 3 ℃, adding potassium permanganate, stirring for 20min at the temperature of 10 ℃, heating to 35 ℃, continuously stirring for 3h, adding deionized water and hydrogen peroxide, continuously stirring for 10min, and dialyzing by using deionized water to obtain graphene oxide;
step A2: adding tetraethoxysilane, ethanol and deionized water into a reaction kettle, stirring for 3 hours at the rotating speed of 200r/min and the temperature of 70 ℃, adding octadecyltrimethoxysilane, reacting for 5 hours under the condition that the pH value of a reaction liquid is 5 to prepare modified nano-silicon, adding the modified nano-silicon, the graphene oxide prepared in the step A1 and the ethanol into the reaction kettle, and performing ultrasonic treatment for 2 hours under the condition that the frequency is 5MHz to prepare a first mixed glue solution;
step A3: uniformly mixing deionized water and span 80 to prepare a pre-emulsion, uniformly mixing benzol olefine acid, lauryl methacrylate, acrylamide and deionized water to prepare a monomer liquid, adding one third of the monomer liquid into one half of the pre-emulsion, stirring for 20min at the rotation speed of 500r/min to prepare a first mixed liquid, mixing one fourth of the pre-emulsion and a potassium persulfate solution, adding the rest of the monomer liquid, stirring for 20min at the rotation speed of 200r/min and the temperature of 50 ℃ to prepare a second mixed liquid, adding the first mixed liquid, the second mixed liquid, the rest of the pre-emulsion and an ammonium persulfate solution into a reaction kettle, and reacting for 1h at the rotation speed of 150r/min and the temperature of 80 ℃ to prepare a composite emulsion;
step A4: adding diphenylmethane diisocyanate, 2-dimethylolpropionic acid and dichloromethane into a reaction kettle, stirring and adding triethylamine under the conditions of the rotation speed of 200r/min and the temperature of 80 ℃, carrying out reflux reaction for 8 hours to obtain an intermediate 1, adding bisphenol A epoxy resin into the reaction kettle, melting at the temperature of 80 ℃, adding polyethylene glycol, deionized water and the intermediate 1, stirring for 10 minutes under the rotation speed of 150r/min, carrying out reflux reaction for 3 hours at the temperature of 110 ℃, cooling to the temperature of 60 ℃, adding triethylamine, and continuing stirring for 20 minutes to obtain a second mixed glue solution;
step A5: and (2) adding the first mixed glue solution prepared in the step A2, the composite emulsion prepared in the step A3 and the second mixed glue solution prepared in the step A4 into a reaction kettle, stirring and adding 1-hydroxy benzotriazole under the conditions that the rotating speed is 150r/min and the temperature is 35 ℃, reacting for 3 hours, adding basalt fibers, and carrying out ultrasonic treatment for 2 hours under the condition that the frequency is 5MHz to prepare the reinforcing liquid.
Example 2
A nano-material modified heat-insulation interior wall coating comprises the following raw materials in parts by weight: 35 parts of acrylic emulsion, 3 parts of titanium dioxide, 4 parts of reinforcing liquid, 0.4 part of GP type defoaming agent, 1 part of triethyl hexyl phosphate, 2 parts of dodecanol ester and 22 parts of water;
the heat-insulating interior wall coating is prepared by the following steps:
step S1: adding a GP type defoaming agent, triethylhexyl phosphoric acid and water into a stirring kettle, and stirring for 20min under the condition that the rotating speed is 300r/min to prepare a first mixture;
step S2: adding the titanium dioxide and the first mixture into a grinder, grinding and mixing, and sieving by using a 25-micron sieve to obtain a second mixture;
step S3: and (4) adding the second mixture prepared in the step (S2), acrylic emulsion, reinforcing liquid and lauryl ester into a stirring kettle, and stirring for 1h at the rotating speed of 1500r/min to prepare the heat-insulating interior wall coating.
The reinforcing liquid is prepared by the following steps:
step A1: adding concentrated sulfuric acid, potassium persulfate and phosphorus pentoxide into a reaction kettle, stirring for 5min at the rotation speed of 300r/min and the temperature of 80 ℃, adding graphite powder, cooling to the temperature of 30 ℃, reacting for 8h, filtering to remove filtrate, washing a filter cake to be neutral by using deionized water to obtain pre-oxidized graphite, adding the pre-oxidized graphite, sodium nitrate and concentrated sulfuric acid into the reaction kettle, stirring for 5min at the rotation speed of 150r/min and the temperature of 5 ℃, adding potassium permanganate, stirring for 20min at the temperature of 15 ℃, heating to 40 ℃, continuously stirring for 3h, adding deionized water and hydrogen peroxide, continuously stirring for 15min, and dialyzing by using deionized water to obtain graphene oxide;
step A2: adding tetraethoxysilane, ethanol and deionized water into a reaction kettle, stirring for 3 hours at the rotating speed of 200r/min and the temperature of 80 ℃, adding octadecyltrimethoxysilane, reacting for 5 hours under the condition that the pH value of a reaction liquid is 6 to prepare modified nano-silicon, adding the modified nano-silicon, the graphene oxide prepared in the step A1 and the ethanol into the reaction kettle, and performing ultrasonic treatment for 2 hours under the condition that the frequency is 8MHz to prepare a first mixed glue solution;
step A3: uniformly mixing deionized water and span 80 to prepare a pre-emulsion, uniformly mixing benzol olefine acid, lauryl methacrylate, acrylamide and deionized water to prepare a monomer liquid, adding one third of the monomer liquid into one half of the pre-emulsion, stirring for 20min at the rotation speed of 800r/min to prepare a first mixed liquid, mixing one fourth of the pre-emulsion and a potassium persulfate solution, adding the rest of the monomer liquid, stirring for 30min at the rotation speed of 300r/min and the temperature of 50 ℃ to prepare a second mixed liquid, adding the first mixed liquid, the second mixed liquid, the rest of the pre-emulsion and an ammonium persulfate solution into a reaction kettle, and reacting for 1h at the rotation speed of 150r/min and the temperature of 85 ℃ to prepare a composite emulsion;
step A4: adding diphenylmethane diisocyanate, 2-dimethylolpropionic acid and dichloromethane into a reaction kettle, stirring and adding triethylamine under the conditions of the rotating speed of 300r/min and the temperature of 80 ℃, carrying out reflux reaction for 10 hours to obtain an intermediate 1, adding bisphenol A epoxy resin into the reaction kettle, melting at the temperature of 80 ℃, adding polyethylene glycol, deionized water and the intermediate 1, stirring for 10 minutes at the rotating speed of 200r/min, carrying out reflux reaction for 3 hours at the temperature of 120 ℃, cooling to 65 ℃, adding triethylamine, and continuing stirring for 20 minutes to obtain a second mixed glue solution;
step A5: and (2) adding the first mixed glue solution prepared in the step A2, the composite emulsion prepared in the step A3 and the second mixed glue solution prepared in the step A4 into a reaction kettle, stirring and adding 1-hydroxy benzotriazole under the conditions that the rotating speed is 200r/min and the temperature is 35 ℃, reacting for 5 hours, adding basalt fibers, and carrying out ultrasonic treatment for 3 hours under the condition that the frequency is 5MHz to prepare the reinforcing liquid.
Example 3
A nano-material modified heat-insulation interior wall coating comprises the following raw materials in parts by weight: 40 parts of acrylic emulsion, 3 parts of titanium dioxide, 4 parts of reinforcing liquid, 0.4 part of GP type defoaming agent, 1.5 parts of triethyl hexyl phosphate, 2 parts of dodecanol ester and 28 parts of water;
the heat-insulating interior wall coating is prepared by the following steps:
step S1: adding a GP type defoaming agent, triethylhexyl phosphoric acid and water into a stirring kettle, and stirring for 15min under the condition that the rotating speed is 500r/min to prepare a first mixture;
step S2: adding the titanium dioxide and the first mixture into a grinder, grinding and mixing, and sieving by a 30-micron sieve to obtain a second mixture;
step S3: and (4) adding the second mixture prepared in the step (S2), acrylic emulsion, reinforcing liquid and lauryl ester into a stirring kettle, and stirring for 1.5 hours at the rotating speed of 1200r/min to prepare the heat-insulating interior wall coating.
The reinforcing liquid is prepared by the following steps:
step A1: adding concentrated sulfuric acid, potassium persulfate and phosphorus pentoxide into a reaction kettle, stirring for 3min at the rotation speed of 200r/min and the temperature of 90 ℃, adding graphite powder, cooling to the temperature of 35 ℃, reacting for 5h, filtering to remove filtrate, washing a filter cake to be neutral by using deionized water to obtain pre-oxidized graphite, adding the pre-oxidized graphite, sodium nitrate and concentrated sulfuric acid into the reaction kettle, stirring for 10min at the rotation speed of 200r/min and the temperature of 3 ℃, adding potassium permanganate, stirring for 30min at the temperature of 10 ℃, heating to 35 ℃, continuously stirring for 5h, adding deionized water and hydrogen peroxide, continuously stirring for 10min, and dialyzing by using deionized water to prepare graphene oxide;
step A2: adding tetraethoxysilane, ethanol and deionized water into a reaction kettle, stirring for 5 hours at the rotating speed of 300r/min and the temperature of 70 ℃, adding octadecyltrimethoxysilane, reacting for 6 hours under the condition that the pH value of the reaction liquid is 5 to prepare modified nano-silicon, adding the modified nano-silicon, the graphene oxide prepared in the step A1 and the ethanol into the reaction kettle, and performing ultrasonic treatment for 3 hours under the condition that the frequency is 5MHz to prepare a first mixed glue solution;
step A3: uniformly mixing deionized water and span 80 to prepare a pre-emulsion, uniformly mixing benzol olefine acid, lauryl methacrylate, acrylamide and deionized water to prepare a monomer liquid, adding one third of the monomer liquid into one half of the pre-emulsion, stirring for 30min at the rotation speed of 500r/min to prepare a first mixed liquid, mixing one fourth of the pre-emulsion and a potassium persulfate solution, adding the rest of the monomer liquid, stirring for 20min at the rotation speed of 200r/min and the temperature of 60 ℃ to prepare a second mixed liquid, adding the first mixed liquid, the second mixed liquid, the rest of the pre-emulsion and an ammonium persulfate solution into a reaction kettle, and reacting for 1.5h at the rotation speed of 200r/min and the temperature of 80 ℃ to prepare a composite emulsion;
step A4: adding diphenylmethane diisocyanate, 2-dimethylolpropionic acid and dichloromethane into a reaction kettle, stirring and adding triethylamine under the conditions of the rotation speed of 200r/min and the temperature of 85 ℃, carrying out reflux reaction for 8 hours to obtain an intermediate 1, adding bisphenol A epoxy resin into the reaction kettle, melting at the temperature of 90 ℃, adding polyethylene glycol, deionized water and the intermediate 1, stirring for 15 minutes at the rotation speed of 150r/min, carrying out reflux reaction for 5 hours at the temperature of 110 ℃, cooling to the temperature of 60 ℃, adding triethylamine, and continuing stirring for 30 minutes to obtain a second mixed glue solution;
step A5: and (2) adding the first mixed glue solution prepared in the step A2, the composite emulsion prepared in the step A3 and the second mixed glue solution prepared in the step A4 into a reaction kettle, stirring and adding 1-hydroxy benzotriazole under the conditions that the rotating speed is 150r/min and the temperature is 40 ℃, reacting for 3 hours, adding basalt fibers, and carrying out ultrasonic treatment for 2 hours under the condition that the frequency is 8MHz to prepare the reinforcing liquid.
Example 4
A nano-material modified heat-insulation interior wall coating comprises the following raw materials in parts by weight: 50 parts of acrylic emulsion, 4 parts of titanium dioxide, 5 parts of reinforcing liquid, 0.5 part of GP type defoaming agent, 2 parts of triethyl hexyl phosphate, 3 parts of dodecanol ester and 30 parts of water;
the heat-insulating interior wall coating is prepared by the following steps:
step S1: adding a GP type defoaming agent, triethylhexyl phosphoric acid and water into a stirring kettle, and stirring for 20min under the condition that the rotating speed is 500r/min to prepare a first mixture;
step S2: adding the titanium dioxide and the first mixture into a grinder, grinding and mixing, and sieving by a 30-micron sieve to obtain a second mixture;
step S3: and (4) adding the second mixture prepared in the step (S2), acrylic emulsion, reinforcing liquid and lauryl ester into a stirring kettle, and stirring for 1.5 hours at the rotating speed of 1500r/min to prepare the heat-insulating interior wall coating.
The reinforcing liquid is prepared by the following steps:
step A1: adding concentrated sulfuric acid, potassium persulfate and phosphorus pentoxide into a reaction kettle, stirring for 5min at the rotation speed of 300r/min and the temperature of 90 ℃, adding graphite powder, cooling to the temperature of 35 ℃, reacting for 8h, filtering to remove filtrate, washing a filter cake to be neutral by using deionized water to obtain pre-oxidized graphite, adding the pre-oxidized graphite, sodium nitrate and concentrated sulfuric acid into the reaction kettle, stirring for 10min at the rotation speed of 200r/min and the temperature of 5 ℃, adding potassium permanganate, stirring for 30min at the temperature of 15 ℃, heating to 40 ℃, continuously stirring for 5h, adding deionized water and hydrogen peroxide, continuously stirring for 15min, and dialyzing by using deionized water to obtain graphene oxide;
step A2: adding tetraethoxysilane, ethanol and deionized water into a reaction kettle, stirring for 5 hours at the rotating speed of 300r/min and the temperature of 80 ℃, adding octadecyltrimethoxysilane, reacting for 6 hours under the condition that the pH value of a reaction liquid is 6 to prepare modified nano-silicon, adding the modified nano-silicon, the graphene oxide prepared in the step A1 and the ethanol into the reaction kettle, and performing ultrasonic treatment for 3 hours under the condition that the frequency is 8MHz to prepare a first mixed glue solution;
step A3: uniformly mixing deionized water and span 80 to prepare a pre-emulsion, uniformly mixing benzol olefine acid, lauryl methacrylate, acrylamide and deionized water to prepare a monomer liquid, adding one third of the monomer liquid into one half of the pre-emulsion, stirring for 30min at the rotation speed of 800r/min to prepare a first mixed liquid, mixing one fourth of the pre-emulsion and a potassium persulfate solution, adding the rest of the monomer liquid, stirring for 30min at the rotation speed of 300r/min and the temperature of 60 ℃ to prepare a second mixed liquid, adding the first mixed liquid, the second mixed liquid, the rest of the pre-emulsion and an ammonium persulfate solution into a reaction kettle, and reacting for 1.5h at the rotation speed of 200r/min and the temperature of 85 ℃ to prepare a composite emulsion;
step A4: adding diphenylmethane diisocyanate, 2-dimethylolpropionic acid and dichloromethane into a reaction kettle, stirring and adding triethylamine under the conditions of the rotating speed of 300r/min and the temperature of 85 ℃, carrying out reflux reaction for 10 hours to obtain an intermediate 1, adding bisphenol A epoxy resin into the reaction kettle, melting at the temperature of 90 ℃, adding polyethylene glycol, deionized water and the intermediate 1, stirring for 15 minutes at the rotating speed of 200r/min, carrying out reflux reaction for 5 hours at the temperature of 120 ℃, cooling to the temperature of 65 ℃, adding triethylamine, and continuing stirring for 30 minutes to obtain a second mixed glue solution;
step A5: and (2) adding the first mixed glue solution prepared in the step A2, the composite emulsion prepared in the step A3 and the second mixed glue solution prepared in the step A4 into a reaction kettle, stirring and adding 1-hydroxy benzotriazole under the conditions that the rotating speed is 200r/min and the temperature is 40 ℃, reacting for 5 hours, adding basalt fibers, and carrying out ultrasonic treatment for 3 hours under the condition that the frequency is 8MHz to prepare the reinforcing liquid.
Comparative example
The comparative example is a common thermal insulation coating in the market.
The performance tests of the heat-insulating coatings prepared in examples 1 to 4 and the comparative example are carried out, and the test results are shown in the following table 1;
water resistance: the assay was performed according to the method GB/T2733-2996.
Water impermeability: the heat-insulating coatings prepared in the examples 1-4 and the comparative example are coated on a glass plate, the thickness is 1.5mm, after standing for 7 days, the heat-insulating coatings are placed in an oven to be baked for 24 hours at 50 +/-2 ℃, the heat-insulating coatings are taken out to be prevented for 3 hours, and a water impermeability test is carried out, wherein the water impermeability is 0.3MPa, the condition that no permeation is qualified after 30min is maintained, the condition that no permeation is good after 45min is maintained, and the condition that no permeation is excellent after 60min is maintained.
Dry adhesion: the assay was performed according to GB/T9286-1998.
Wear resistance: coating the paint on a pan for wear resistance test, and testing the wear resistance at room temperature by a wear meter under the following test conditions: and (3) measuring the mass loss by using a grinding wheel CS-10 and a load force of 500g and circulating for 500 times.
TABLE 1
As can be seen from Table 1, the insulating coatings prepared in examples 1-4 have no abnormal water resistance, excellent water impermeability, grade 2 dry adhesion and 0.125-0.131g wear resistance, the insulating coatings prepared in comparative examples have abnormal water resistance, qualified water impermeability, grade 4 dry adhesion and 0.375g wear resistance, and the insulating coatings prepared in the invention have good water resistance, wear resistance and firm adhesion.
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 (9)
1. A nano-material modified heat-insulation interior wall coating is characterized in that: the feed comprises the following raw materials in parts by weight: 30-50 parts of acrylic emulsion, 2-4 parts of titanium dioxide, 3-5 parts of reinforcing liquid, 0.3-0.5 part of defoaming agent, 0.5-2 parts of dispersing agent, 1-3 parts of film forming agent and 20-30 parts of water;
the heat-insulating interior wall coating is prepared by the following steps:
step S1: adding the defoaming agent, the dispersing agent and water into a stirring kettle, and stirring for 15-20min under the condition that the rotating speed is 300-;
step S2: adding the titanium dioxide and the first mixture into a grinder, grinding and mixing, and sieving by using a 25-30 micron sieve to obtain a second mixture;
step S3: and (4) adding the second mixture prepared in the step S2, the acrylic emulsion, the reinforcing liquid and the film forming agent into a stirring kettle, and stirring for 1-1.5 hours under the condition that the rotating speed is 1200-1500r/min to prepare the heat-insulating interior wall coating.
2. The nano-material modified heat-insulating interior wall coating as claimed in claim 1, wherein: the defoaming agent is one of GPES defoaming agent, GP defoaming agent and GPE defoaming agent, the dispersing agent is one or more of triethyl hexyl phosphoric acid, sodium dodecyl sulfate and methyl amyl alcohol which are mixed in any proportion, and the film forming agent is one or more of dodecyl glycol, propylene glycol and hexanediol which are mixed in any proportion.
3. The nano-material modified heat-insulating interior wall coating as claimed in claim 1, wherein: the reinforcing liquid is prepared by the following steps:
step A1: adding concentrated sulfuric acid, potassium persulfate and phosphorus pentoxide into a reaction kettle, stirring for 3-5min at the rotation speed of 200-90 ℃ and at the temperature of 80-90 ℃, adding graphite powder, cooling to the temperature of 30-35 ℃, reacting for 5-8h, filtering to remove filtrate, washing a filter cake to be neutral by using deionized water to obtain pre-oxidized graphite, adding the pre-oxidized graphite, sodium nitrate and concentrated sulfuric acid into the reaction kettle, stirring for 5-10min at the rotation speed of 150-200r/min and at the temperature of 3-5 ℃, adding potassium permanganate, stirring at the temperature of 10-15 ℃ for 20-30min, heating to 35-40 ℃, continuously stirring for 3-5h, adding deionized water and hydrogen peroxide, continuously stirring for 10-15min, dialyzing with deionized water to prepare graphene oxide;
step A2: adding tetraethoxysilane, ethanol and deionized water into a reaction kettle, stirring for 3-5h under the conditions that the rotating speed is 200-80 ℃ and the temperature is 70-80 ℃, adding octadecyltrimethoxysilane, reacting for 5-6h under the condition that the pH value of a reaction liquid is 5-6 to prepare modified nano-silicon, adding the modified nano-silicon, the graphene oxide prepared in the step A1 and the ethanol into the reaction kettle, and performing ultrasonic treatment for 2-3h under the condition that the frequency is 5-8MHz to prepare a first mixed glue solution;
step A3: uniformly mixing deionized water and span 80 to prepare pre-emulsion, uniformly mixing benzol olefine acid, lauryl methacrylate, acrylamide and deionized water to prepare monomer liquid, adding one third of the monomer liquid into one half of the pre-emulsion, stirring for 20-30min under the condition of the rotating speed of 500 plus 800r/min to prepare first mixed liquid, mixing one fourth of the pre-emulsion and potassium persulfate solution, adding the rest of the monomer liquid, stirring for 20-30min under the conditions of the rotating speed of 200 plus 300r/min and the temperature of 50-60 ℃ to prepare second mixed liquid, adding the first mixed liquid, the second mixed liquid, the rest of the pre-emulsion and ammonium persulfate solution into a reaction kettle, reacting for 1-1.5h under the conditions of the rotating speed of 150 plus 200r/min and the temperature of 80-85 ℃, preparing a composite emulsion;
step A4: adding diphenylmethane diisocyanate, 2-dimethylolpropionic acid and dichloromethane into a reaction kettle, stirring and adding triethylamine under the conditions of the rotation speed of 200-85 ℃ and the temperature of 80-85 ℃ to perform reflux reaction for 8-10h to obtain an intermediate 1, adding bisphenol A epoxy resin into the reaction kettle, melting at the temperature of 80-90 ℃, adding polyethylene glycol, deionized water and the intermediate 1, stirring at the rotation speed of 150-200r/min for 10-15min, performing reflux reaction at the temperature of 110-120 ℃ for 3-5h, cooling to 60-65 ℃, adding triethylamine, and continuing stirring for 20-30min to obtain a second mixed glue solution;
step A5: and (2) adding the first mixed glue solution prepared in the step A2, the composite emulsion prepared in the step A3 and the second mixed glue solution prepared in the step A4 into a reaction kettle, stirring and adding 1-hydroxybenzotriazole under the conditions that the rotating speed is 150-200r/min and the temperature is 35-40 ℃, reacting for 3-5h, adding basalt fibers, and performing ultrasonic treatment for 2-3h under the condition that the frequency is 5-8MHz to prepare the reinforcing liquid.
4. The nano-material modified heat-insulating interior wall coating as claimed in claim 3, wherein: the using amount ratio of the concentrated sulfuric acid, the potassium persulfate, the phosphorus pentoxide and the graphite powder used in the pre-oxidized graphite preparation in the step A1 is 4mL:1.5g:1g:3g, the mass fraction of the concentrated sulfuric acid is 95%, the using amount ratio of the pre-oxidized graphite, the sodium nitrate, the concentrated sulfuric acid, the potassium permanganate, the deionized water and the hydrogen peroxide used in the oxidized graphene preparation is 1g:0.6g:25mL:3g:150mL:5mL, and the mass fraction of the hydrogen peroxide is 25%.
5. The nano-material modified heat-insulating interior wall coating as claimed in claim 3, wherein: the dosage ratio of the ethyl orthosilicate, the ethanol, the deionized water and the octadecyl trimethoxy silane in the step A2 is 5g to 3mL to 50mL to 2.5g, and the dosage ratio of the modified nano silicon, the graphene oxide and the ethanol is 2g to 3g to 15 mL.
6. The nano-material modified heat-insulating interior wall coating as claimed in claim 3, wherein: the dosage ratio of the deionized water and the span 80 in the step A3 is 20mL:1g, the dosage ratio of the benzonic acid, the lauryl methacrylate, the acrylamide and the deionized water is 1g:1g:2g:5mL, the total dosage volume ratio of the pre-emulsion and the monomer liquid is 1:2, the dosage of the potassium persulfate is 1-2% of the total reactant dosage mass, and the dosage of the ammonium persulfate is 1-2% of the total reactant dosage mass.
7. The nano-material modified heat-insulating interior wall coating as claimed in claim 3, wherein: the molar ratio of the diphenylmethane diisocyanate to the 2, 2-dimethylolpropionic acid in the step A4 is 1:2, the amount of triethylamine is 15% of the mass of the diphenylmethane diisocyanate, the mass ratio of the bisphenol A type resin, the polyethylene glycol and the intermediate 1 is 5:3:3, and the amount of triethylamine is 15% of the mass of the bisphenol A type resin.
8. The nano-material modified heat-insulating interior wall coating as claimed in claim 3, wherein: the dosage ratio of the first mixed glue solution, the composite emulsion, the second mixed glue solution and the basalt fiber in the step A5 is 10mL:10mL:15mL:3g, and the dosage of the 1-hydroxy benzotriazole is 20% of the mass of the first mixed glue solution.
9. The preparation method of the nano-material modified heat-insulation interior wall coating according to claim 1, characterized by comprising the following steps: the method specifically comprises the following steps:
step S1: adding the defoaming agent, the dispersing agent and water into a stirring kettle, and stirring for 15-20min under the condition that the rotating speed is 300-;
step S2: adding the titanium dioxide and the first mixture into a grinder, grinding and mixing, and sieving by using a 25-30 micron sieve to obtain a second mixture;
step S3: and (4) adding the second mixture prepared in the step S2, the acrylic emulsion, the reinforcing liquid and the film forming agent into a stirring kettle, and stirring for 1-1.5 hours under the condition that the rotating speed is 1200-1500r/min to prepare the heat-insulating interior wall coating.
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