CN110922843A - Super-hydrophilic coating and preparation method thereof - Google Patents
Super-hydrophilic coating and preparation method thereof Download PDFInfo
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- CN110922843A CN110922843A CN201911306159.5A CN201911306159A CN110922843A CN 110922843 A CN110922843 A CN 110922843A CN 201911306159 A CN201911306159 A CN 201911306159A CN 110922843 A CN110922843 A CN 110922843A
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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
- C09D141/00—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 a bond to sulfur or by a heterocyclic ring containing sulfur; Coating compositions based on derivatives of such polymers
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- C08F216/12—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 an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
- C08F216/14—Monomers containing only one unsaturated aliphatic radical
- C08F216/1466—Monomers containing sulfur
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
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- C08F228/00—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 a bond to sulfur or by a heterocyclic ring containing sulfur
- C08F228/02—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 a bond to sulfur or by a heterocyclic ring containing sulfur by a bond to sulfur
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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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- 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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Abstract
The invention discloses a super-hydrophilic coating which comprises the following components in parts by mass: 10-15 parts of hydrophilic resin A; 10-15 parts of hydrophilic resin B; 1-2 parts of a hydrophilic auxiliary agent; 3-6 parts of a curing agent; 5-10 parts of a cosolvent; 0.1-0.2 part of alkali; 55-66 parts of deionized water; the hydrophilic resin A comprises the following components in parts by weight: 40-50 parts of reactive surface active monomer, 0.3-0.8 part of initiator, 0-0.5 part of alkali, 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 40-50 parts of deionized water; the reactive surface active monomer is a monomer containing sulfonic acid or sulfonate; the hydrophilic resin B comprises the following components in parts by weight: 2-4 parts of carboxyl-containing acrylic monomer, 8-10 parts of hydroxyl-containing acrylic monomer, 16-20 parts of acrylamide monomer, 0.2-0.6 part of alkali, 0.3-0.7 part of initiator, 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 40-50 parts of deionized water. The super-hydrophilic coating provided by the invention has good hydrophilic performance and heat resistance. The invention also discloses a preparation method of the super-hydrophilic coating.
Description
Technical Field
The invention relates to the technical field of water-based coatings, and particularly relates to a super-hydrophilic coating and a preparation method thereof.
Background
The polyester film (PET film) is a colorless, transparent and glossy film, has the characteristics of excellent mechanical property, high rigidity, hardness and toughness, puncture resistance, friction resistance, high temperature and low temperature resistance, chemical resistance, oil resistance, air tightness, aroma retention and the like, is one of common permeability-resistant composite film base materials, and is widely applied to detection test paper in medicine.
The PET film has small surface energy, low surface tension and poor hydrophilic ability due to high molecular chain rigidity and few polar groups, and is difficult to be firmly combined with a hydrophilic coating. With the continuous development of the technology, people continuously research the surface modification technology of the PET film, and find that the bonding of the PET film and the hydrophilic coating is facilitated by bonding a bottom coating liquid between the PET film and the hydrophilic coating.
In the prior art, after a primary coating material is roll-coated on a PET film, a hydrophilic surface coating is coated on the primary coating, so that the adhesive force and the hydrophilic performance are obviously improved. However, the hydrophilic angle of the hydrophilic coating is generally larger than 15 degrees, the difference of the hydrophilic angles of all points is large (the angle difference value is larger than 15 degrees), and the hydrophilic angle is obviously increased after heat aging resistance (65 ℃/70 days, the angle increase value is larger than 15 degrees).
In view of the above, the invention provides a super-hydrophilic coating with better hydrophilic performance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a super-hydrophilic coating, wherein the initial hydrophilic angle is less than or equal to 7 degrees, and the hydrophilic angle difference of each point is small (the angle difference value is less than or equal to 5 degrees), namely the super-hydrophilic coating has better hydrophilic uniformity; the hydrophilic angle after heat aging resistance is less than or equal to 10 degrees, and the hydrophilic performance is better compared with the prior art.
In order to solve the problems, the technical scheme of the invention is as follows:
the super-hydrophilic coating comprises the following components in parts by weight:
the hydrophilic resin A comprises the following components in parts by weight:
40-50 parts of reactive surface active monomer, 0.3-0.8 part of initiator, 0-0.5 part of alkali, 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 40-50 parts of deionized water; the reactive surface active monomer is a monomer containing sulfonic acid or sulfonate;
the hydrophilic resin B comprises the following components in parts by weight:
2-4 parts of carboxyl-containing acrylic monomer, 8-10 parts of hydroxyl-containing acrylic monomer, 16-20 parts of acrylamide monomer, 0.2-0.6 part of alkali, 0.3-0.7 part of initiator, 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 40-50 parts of deionized water.
Further, in the hydrophilic resin A, the reactive surface active monomer is at least one of allyl sulfonic acid and sodium salt thereof, p-styrene sulfonic acid and sodium salt thereof, 2-allyl ether-3-hydroxy propane-1-sulfonic acid and sodium salt thereof, and 2-acrylamide-2-methyl propane sulfonic acid and sodium salt thereof.
Further, in the hydrophilic resin A, the initiator is at least one of potassium persulfate, sodium persulfate and ammonium persulfate; the alcohol solvent is at least one of n-butanol, isobutanol, isopropanol, ethanol and methanol; the alcohol ether solvent is at least one of propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether.
Preferably, the hydrophilic resin A comprises the following components in parts by weight:
40-45 parts of reactive surface active monomer, 0.5-0.8 part of initiator, 0.2-0.4 part of alkali, 5-8 parts of alcohol solvent, 5-8 parts of alcohol ether solvent and 45-50 parts of deionized water.
Further, in the hydrophilic resin B, the carboxyl-containing acrylic monomer is at least one of acrylic acid and methacrylic acid; the hydroxyl-containing acrylic monomer is at least one of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate; the initiator is at least one of potassium persulfate, sodium persulfate and ammonium persulfate; the alcohol solvent is at least one of n-butanol, isobutanol, isopropanol, ethanol and methanol; the alcohol ether solvent is at least one of propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether.
Further, the hydrophilic auxiliary agent is at least one of secondary alkyl sodium sulfonate, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium diisooctyl succinate sulfonate; the curing agent is at least one of methyl ethyl glycoluril, glyoxal and azapyridine cross-linked resin; the cosolvent is at least one of n-butanol, isobutanol, isopropanol, ethanol, methanol, propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether.
Further, the alkali is at least one of sodium hydroxide and potassium hydroxide.
The invention also provides a preparation method of the super-hydrophilic coating, which comprises the following steps:
and under the stirring state, sequentially adding deionized water, alkali, hydrophilic resin A, hydrophilic resin B, hydrophilic auxiliary agent, curing agent and cosolvent according to a proportion, and uniformly stirring to obtain the super-hydrophilic coating.
Further, the preparation method of the hydrophilic resin A comprises the following steps:
step S1, adding 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 20-25 parts of deionized water into a reaction kettle provided with a condensation reflux and dripping device; starting stirring, slowly adding 40-50 parts of reactive surface active monomer and 0-0.5 part of alkali in the formula, and heating to 80-90 ℃;
step S2, after fully mixing and dissolving 20-25 parts of deionized water and 0.2-0.7 part of initiator, uniformly dripping into a reaction kettle for 2-4 hours;
step S3, after the mixture is dripped in the step S2, the mixture is kept warm for 1 hour, 0.1 to 0.2 part of initiator and 3 to 5 parts of deionized water are fully mixed and dissolved, and then the mixture is dripped into a reaction kettle for 5 to 15 minutes;
step S4, preserving heat for 1h, fully mixing 0.1-0.2 part of initiator and 3-5 parts of deionized water, and then dripping into the reaction kettle for 5-15 min;
and step S5, preserving heat for 2-4h, cooling and filtering to obtain the hydrophilic resin A.
Further, the preparation method of the hydrophilic resin B comprises the following steps:
step S1, adding 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 20-25 parts of deionized water into a reaction kettle provided with a condensation reflux and dripping device, starting stirring, and heating to 80-90 ℃;
step S2, uniformly dripping 10-15 parts of deionized water, 2-4 parts of carboxyl-containing acrylic monomer, 8-10 parts of hydroxyl-containing acrylic monomer, 16-20 parts of acrylamide monomer and 0.2-0.6 part of alkali into a reaction kettle after fully mixing and dissolving, wherein the time for use is 2-4 hours;
step S3, simultaneously, uniformly dripping 10-15 parts of deionized water and 0.2-0.7 part of initiator into the reaction kettle after fully mixing and dissolving for 2-4 hours;
step S4, after the two mixtures are simultaneously dripped, preserving heat for 1h, dripping the mixture into a reaction kettle after 0.1-0.2 part of initiator and 3-5 parts of deionized water are fully mixed and dissolved, and taking 5-15 min;
and step S5, preserving heat for 1 hour, and after 0.1-0.2 part of initiator and 3-5 parts of deionized water are fully mixed and dissolved, dropwise adding the mixture into the reaction kettle for 5-15 min.
And step S6, preserving heat for 2-4h, cooling and filtering to obtain the hydrophilic resin B.
Compared with the prior art, the super-hydrophilic coating and the preparation method thereof provided by the invention have the beneficial effects that:
the super-hydrophilic coating comprises a hydrophilic resin A and a hydrophilic resin B as main resin materials, wherein the hydrophilic resin A is a sulfonate system (a composition mainly comprising a copolymer containing sulfonic acid or sulfonate), the hydrophilic resin B is an acrylic acid system (a composition mainly comprising a copolymer containing carboxyl and hydroxyl and an acrylic acid amide), and the hydrophilic resin A and the hydrophilic resin B are subjected to microphase separation due to the water solubility difference with each other along with the volatilization of water and a solvent in the film forming process, so that a nano-scale fine concave-convex structure is generated, and the super-hydrophilic effect on the surface is better facilitated. The formed micro concave-convex structure is formed by combining chemical bonds, so that the structure is quite stable, the initial hydrophilicity is improved, and the continuous super hydrophilicity can be realized.
The super-hydrophilic coating has an initial hydrophilic angle of less than or equal to 7 degrees, small hydrophilic angle difference of each point (the angle difference value is less than or equal to 5 degrees), and good hydrophilic uniformity; the continuous hydrophilic angle is less than or equal to 9 degrees, and the continuous hydrophilic performance is good.
The components of the super-hydrophilic coating do not contain thermolabile groups such as benzene rings and the like, so the super-hydrophilic coating has the advantage of good heat resistance, and the hydrophilic angle is less than or equal to 9 degrees after heat aging resistance (65 ℃/70 days).
And thirdly, the super-hydrophilic coating comprises a basic component of sodium hydroxide, and carboxylic acid groups and sulfonic acid groups in the coating system react to form carboxylate and sulfonate. From the view point of hydrophilic/lipophilic value (HLB value), the system after salification has stronger hydrophilicity. And since the super hydrophilic coating of the present application is prepared by crosslinking the hydrophilic resin a containing sulfonic acid/sulfonate with the hydrophilic resin containing carboxylic acid groups, it is preferable to add an appropriate amount of basic components at the time of synthesizing the hydrophilic resin a and the hydrophilic resin B in order to completely react the carboxylic acid groups and the sulfonic acid groups in the system to form carboxylate and sulfonate.
Detailed Description
The following description of the present invention is provided to enable those skilled in the art to better understand the technical solutions in the embodiments of the present invention and to make the above objects, features and advantages of the present invention more comprehensible.
It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The super-hydrophilic coating comprises the following components in parts by weight:
wherein the hydrophilic resin A comprises the following components in percentage by weight:
40-50 parts of reactive surface active monomer, 0.3-0.8 part of initiator, 0-0.5 part of alkali, 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 40-50 parts of deionized water; the reactive surface active monomer is a monomer containing sulfonic acid or sulfonate;
the hydrophilic resin B comprises the following components in percentage by weight:
2-4 parts of carboxyl-containing acrylic monomer, 8-10 parts of hydroxyl-containing acrylic monomer, 16-20 parts of acrylamide monomer, 0.2-0.6 part of alkali, 0.3-0.7 part of initiator, 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 40-50 parts of deionized water.
Further, in the hydrophilic resin A, the reactive surface active monomer is at least one of allyl sulfonic acid and sodium salt thereof, p-styrene sulfonic acid and sodium salt thereof, 2-allyl ether-3-hydroxy propane-1-sulfonic acid and sodium salt thereof, and 2-acrylamide-2-methyl propane sulfonic acid and sodium salt thereof.
Further, in the hydrophilic resin A, the initiator is at least one of potassium persulfate, sodium persulfate and ammonium persulfate; the alcohol solvent is at least one of n-butanol, isobutanol, isopropanol, ethanol and methanol; the alcohol ether solvent is at least one of propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether.
Preferably, the hydrophilic resin a comprises the following components in percentage by weight:
40-45 parts of reactive surface active monomer, 0.5-0.8 part of initiator, 0.2-0.4 part of alkali, 5-8 parts of alcohol solvent, 5-8 parts of alcohol ether solvent and 45-50 parts of deionized water.
Further, in the hydrophilic resin B, the carboxyl-containing acrylic monomer is at least one of acrylic acid and methacrylic acid; the hydroxyl-containing acrylic monomer is at least one of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate; the initiator is at least one of potassium persulfate, sodium persulfate and ammonium persulfate; the alcohol solvent is at least one of n-butanol, isobutanol, isopropanol, ethanol and methanol; the alcohol ether solvent is at least one of propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether.
Further, the hydrophilic auxiliary agent is at least one of secondary alkyl sodium sulfonate, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium diisooctyl succinate sulfonate; the curing agent is at least one of methyl ethyl glycoluril, glyoxal and azapyridine cross-linked resin; the cosolvent is at least one of n-butanol, isobutanol, isopropanol, ethanol, methanol, propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether.
Further, the alkali is at least one of sodium hydroxide and potassium hydroxide.
The invention also provides a preparation method of the super-hydrophilic coating, which comprises the following steps:
and under the stirring state, sequentially adding deionized water, sodium hydroxide, hydrophilic resin A, hydrophilic resin B, hydrophilic auxiliary agent, curing agent and cosolvent according to a ratio, and uniformly stirring to obtain the super-hydrophilic coating.
Further, the preparation method of the hydrophilic resin A comprises the following steps:
step S1, adding 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 20-25 parts of deionized water into a reaction kettle provided with a condensation reflux and dripping device; starting stirring, slowly adding 40-50 parts of reactive surface active monomer and 0-0.5 part of alkali in the formula, and heating to 80-90 ℃;
step S2, after fully mixing and dissolving 20-25 parts of deionized water and 0.2-0.7 part of initiator, uniformly dripping into a reaction kettle for 2-4 hours;
step S3, after the mixture is dripped in the step S2, the mixture is kept warm for 1 hour, 0.1 to 0.2 part of initiator and 3 to 5 parts of deionized water are fully mixed and dissolved, and then the mixture is dripped into a reaction kettle for 5 to 15 minutes;
step S4, preserving heat for 1h, fully mixing 0.1-0.2 part of initiator and 3-5 parts of deionized water, and then dripping into the reaction kettle for 5-15 min;
and step S5, preserving heat for 2-4h, cooling and filtering to obtain the hydrophilic resin A.
Further, the preparation method of the hydrophilic resin B comprises the following steps:
step S1, adding 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 20-25 parts of deionized water into a reaction kettle provided with a condensation reflux and dripping device, starting stirring, and heating to 80-90 ℃;
step S2, uniformly dripping 10-15 parts of deionized water, 2-4 parts of carboxyl-containing acrylic monomer, 8-10 parts of hydroxyl-containing acrylic monomer, 16-20 parts of acrylamide monomer and 0.2-0.6 part of alkali into a reaction kettle after fully mixing and dissolving, wherein the time for use is 2-4 hours;
step S3, simultaneously, uniformly dripping 10-15 parts of deionized water and 0.2-0.7 part of initiator into the reaction kettle after fully mixing and dissolving for 2-4 hours;
step S4, after the two mixtures are simultaneously dripped, preserving heat for 1h, dripping the mixture into a reaction kettle after 0.1-0.2 part of initiator and 3-5 parts of deionized water are fully mixed and dissolved, and taking 5-15 min;
and step S5, preserving heat for 1 hour, and after 0.1-0.2 part of initiator and 3-5 parts of deionized water are fully mixed and dissolved, dropwise adding the mixture into the reaction kettle for 5-15 min.
And step S6, preserving heat for 2-4h, cooling and filtering to obtain the hydrophilic resin B.
The application method of the super-hydrophilic coating provided by the invention comprises the following steps: and rolling the super-hydrophilic coating on the surface of the bottom coat by a roller, wherein the thickness of the film is about 0.2-0.5 mu m, and baking and cooling to form a super-hydrophilic film. Of course, the super-hydrophilic coating provided by the invention can also be directly roll-coated on the surface of the aluminum foil.
The present invention is further illustrated by the following specific examples.
Example 1
The super-hydrophilic coating comprises the following components in parts by weight:
11.1 parts of hydrophilic resin A, 10 parts of hydrophilic resin B, 1.7 parts of hydrophilic auxiliary agent, 4.4 parts of curing agent, 6.6 parts of cosolvent, 0.1 part of sodium hydroxide and 66 parts of deionized water.
The hydrophilic resin A comprises the following components in parts by weight:
25 parts of sodium allylsulfonate, 20 parts of p-styrene sulfonic acid, 0.5 part of sodium persulfate, 5 parts of isopropanol, 5 parts of butyl cellosolve, 0.3 part of sodium hydroxide and 45 parts of deionized water.
The hydrophilic resin B comprises the following components in parts by weight:
3 parts of acrylic acid, 9 parts of hydroxypropyl acrylate, 18 parts of acrylamide, 0.5 part of sodium persulfate, 8 parts of isopropanol, 8 parts of butyl cellosolve, 0.3 part of sodium hydroxide and 45 parts of deionized water.
The hydrophilic auxiliary agent comprises the following components in percentage by weight: 5 parts of diisooctyl succinate sodium sulfonate and 10 parts of octyl phenol polyoxyethylene ether.
The curing agent comprises the following components in percentage by weight: 20 parts of glyoxal and 20 parts of azopyridine cross-linked resin.
The cosolvent comprises the following components in percentage by weight: 30 parts of propylene glycol methyl ether and 30 parts of ethanol.
The preparation method of the super-hydrophilic coating, the hydrophilic resin a and the hydrophilic resin B in the super-hydrophilic coating in this embodiment refers to the above process method, and is prepared according to the component proportion in this embodiment, which is not described herein again.
Example 2
The super-hydrophilic coating comprises the following components in parts by weight:
the coating comprises, by weight, 15 parts of hydrophilic resin A, 15 parts of hydrophilic resin B, 2 parts of hydrophilic auxiliary agent, 3 parts of curing agent, 10 parts of cosolvent and 55 parts of deionized water.
The hydrophilic resin A comprises the following components in parts by weight:
20 parts of 2-allyl ether-3-hydroxy propane-1-sodium sulfonate, 20 parts of 2-acrylamide-2-methyl sodium propane sulfonate, 0.3 part of potassium sulfate, 5 parts of n-butanol, 10 parts of propylene glycol monomethyl ether and 40 parts of deionized water. In this embodiment, all the reactive surface active monomers are sulfonate polymers, so that no sodium hydroxide component may be added to the hydrophilic resin a, and the hydrophilic property of the hydrophilic resin a can be ensured.
The hydrophilic resin B comprises the following components in parts by weight:
2 parts of methacrylic acid, 10 parts of hydroxyethyl acrylate, 16 parts of acrylamide, 0.3 part of sodium persulfate, 5 parts of ethanol, 10 parts of dipropylene glycol methyl ether, 0.2 part of potassium hydroxide and 40 parts of deionized water.
The hydrophilic auxiliary agent is secondary alkyl sodium sulfonate and sodium dodecyl benzene sulfate.
The curing agent is methyl ethyl glycoluril and azapyridine cross-linked resin.
The cosolvent is ethylene glycol butyl ether and isobutanol.
Example 3
The super-hydrophilic coating comprises the following components in parts by weight:
the coating comprises, by weight, 10 parts of hydrophilic resin A, 12 parts of hydrophilic resin B, 1 part of hydrophilic auxiliary agent, 5 parts of curing agent, 5 parts of cosolvent, 0.2 part of sodium hydroxide and 62 parts of deionized water.
The hydrophilic resin A comprises the following components in parts by weight:
22 parts of allyl sulfonic acid, 20 parts of 2-allyl ether-3-hydroxy propane-1-sulfonic acid, 0.4 part of sodium hydroxide, 0.8 part of ammonium persulfate, 8 parts of n-butanol, 8 parts of ethylene glycol monobutyl ether and 50 parts of deionized water.
The hydrophilic resin B comprises the following components in parts by weight:
4 parts of methacrylic acid, 8 parts of hydroxyethyl methacrylate, 20 parts of acrylamide, 0.7 part of sodium persulfate, 10 parts of isopropanol, 5 parts of dipropylene glycol methyl ether, 0.6 part of sodium hydroxide and 50 parts of deionized water.
The hydrophilic auxiliary agent is secondary alkyl sodium sulfonate and sodium dodecyl benzene sulfate.
The curing agent is methyl ethyl glycoluril and glyoxal.
The cosolvent is methanol and propylene glycol methyl ether.
Example 4
The super-hydrophilic coating comprises the following components in parts by weight:
the coating comprises, by weight, 14 parts of hydrophilic resin A, 13 parts of hydrophilic resin B, 1.5 parts of hydrophilic auxiliary agent, 6 parts of curing agent, 8 parts of cosolvent, 0.1 part of sodium hydroxide and 58 parts of deionized water.
The hydrophilic resin A comprises the following components in parts by weight:
20 parts of sodium allylsulfonate, 20 parts of p-styrene sulfonic acid, 0.8 part of ammonium persulfate, 6 parts of n-butanol, 6 parts of ethylene glycol monobutyl ether, 0.2 part of sodium hydroxide and 48 parts of deionized water.
The hydrophilic resin B comprises the following components in parts by weight:
3 parts of methacrylic acid, 8 parts of hydroxyethyl methacrylate, 18 parts of acrylamide, 0.6 part of sodium persulfate, 7 parts of isopropanol, 9 parts of dipropylene glycol methyl ether, 0.5 part of sodium hydroxide and 47 parts of deionized water.
The hydrophilic auxiliary agent is secondary alkyl sodium sulfonate and sodium dodecyl benzene sulfate.
The curing agent is methyl ethyl glycoluril and glyoxal.
The cosolvent is methanol and propylene glycol methyl ether.
Example 5
The super-hydrophilic coating comprises the following components in parts by weight:
the coating comprises, by weight, 12 parts of hydrophilic resin A, 11 parts of hydrophilic resin B, 1.4 parts of hydrophilic auxiliary agent, 4 parts of curing agent, 7 parts of cosolvent, 0.2 part of sodium hydroxide and 60 parts of deionized water.
The hydrophilic resin A comprises the following components in parts by weight:
25 parts of sodium allylsulfonate, 25 parts of p-styrene sulfonic acid, 0.4 part of sodium persulfate, 10 parts of isopropanol, 10 parts of butyl cellosolve, 0.1 part of sodium hydroxide and 45 parts of deionized water.
The hydrophilic resin B comprises the following components in parts by weight:
3 parts of acrylic acid, 10 parts of hydroxypropyl acrylate, 17 parts of acrylamide, 0.6 part of sodium persulfate, 8 parts of isopropanol, 6 parts of butyl cellosolve, 0.4 part of sodium hydroxide and 50 parts of deionized water.
The hydrophilic auxiliary agent is diisooctyl succinate sodium sulfonate and octyl phenol polyoxyethylene ether.
The curing agent is glyoxal and azopyridine cross-linked resin.
The cosolvent is propylene glycol methyl ether and ethanol.
To further illustrate the advantages of the superhydrophilic coatings provided by the present invention, comparative examples are provided below with a combination of technical effects.
Comparative example 1
In addition to example 1, the amount of the hydrophilic resin A was increased by 10 parts by eliminating the component of the hydrophilic resin B, so that the hydrophilic coating component in this example is mainly composed of the hydrophilic resin A, and the content of the hydrophilic resin A is equivalent to the amount of the hydrophilic resin A + the hydrophilic resin B in example 1. Other components and contents are unchanged.
In the present example, the hydrophilic coating material is a sulfonate system (a composition mainly containing sulfonic acid or a sulfonate copolymer).
Comparative example 2
On the basis of example 1, the component of the hydrophilic resin a was eliminated, and the amount of the hydrophilic resin B was increased by 11.1 parts correspondingly, so that the hydrophilic coating component in this example was mainly composed of the hydrophilic resin B, and the content of the hydrophilic resin B was equivalent to the amount of the hydrophilic resin a + the hydrophilic resin B in example 1. Other components and contents are unchanged.
In this example, the hydrophilic coating material was an acrylic system (a composition mainly composed of an acrylic acid (ester) copolymer containing a carboxyl group and a hydroxyl group and an acrylic acid amide copolymer).
Comparative example 3
On the basis of example 1, a hydrophilic resin material was changed. In this embodiment, a sulfonate monomer and an acrylic monomer are polymerized to form a hydrophilic resin, and then the hydrophilic resin is prepared to obtain the hydrophilic coating. The difference from example 1 is that: example 1 is a coating material made of a main resin material obtained by crosslinking a sulfonate resin and an acrylic resin.
The preparation process of the hydrophilic resin of this example is as follows:
step S1, adding the following components into a reaction kettle provided with a condensation reflux and dropwise adding device: 13 parts of isopropanol, 13 parts of butyl cellosolve and 40 parts of deionized water, starting stirring, and heating to 80-90 ℃;
step S2, uniformly dripping 30 parts of deionized water, 25 parts of sodium allylsulfonate, 20 parts of p-styrene sulfonic acid, 3 parts of acrylic acid, 9 parts of hydroxypropyl acrylate, 18 parts of acrylamide and 0.6 part of sodium hydroxide into a reaction kettle after fully mixing and dissolving, wherein the time for use is 3 hours;
step S3, simultaneously, uniformly dripping 14 parts of deionized water and 0.8 part of initiator into the reaction kettle after fully mixing and dissolving, and taking 3 hours;
step S4, after the two mixtures are simultaneously dripped, preserving heat for 1h, and after 0.1 part of initiator and 3 parts of deionized water are fully mixed and dissolved, dripping the mixture into a reaction kettle for 10 min;
and step S5, preserving heat for 1 hour, and after 0.1 part of initiator and 3 parts of deionized water are fully mixed and dissolved, dropwise adding the mixture into the reaction kettle for 10 min.
And step S6, preserving heat for 3 hours, cooling and filtering to obtain the hydrophilic resin of the comparative example 3.
The hydrophilic coating of comparative example 3 comprises the following ingredients in parts by weight:
the hydrophilic resin comprises, by weight, 21.1 parts of hydrophilic resin, 1.7 parts of hydrophilic auxiliary agent, 4.4 parts of curing agent, 6.6 parts of cosolvent, 0.1 part of sodium hydroxide and 66 parts of deionized water. The other components and their contents were the same as those in example 1.
Testing the performance of the super-hydrophilic coating:
the hydrophilic coatings of the embodiments 1-5 and the comparative examples 1-3 are applied to a PET film, specifically, the PET film is used as a substrate, a base coat is roll-coated on the surface of the substrate (the base coat is selected from ZTC-03D acrylic acid base coat of Hunan Zhi coating environmental protection technology Co., Ltd.), then the super-hydrophilic coating of the invention is roll-coated on the surface of a base coat material to form a hydrophilic surface layer, the thickness of the surface layer is about 0.2-0.5 mu m, and then the hydrophilic surface layer is baked at the temperature of 120-160 ℃ for 15-20S (the plate temperature is controlled at the temperature of 110-150 ℃). The formed super hydrophilic film was then subjected to performance tests, the test results are shown in table 1:
table 1: performance test result of super-hydrophilic coating applied to PET (polyethylene terephthalate) substrate
The hydrophilic coatings of the examples 1-5 and the comparative examples 1-3 are applied to an aluminum foil, specifically, the aluminum foil is used as a substrate, a bottom coating is roll-coated on the surface of the substrate, then the super-hydrophilic coating of the invention is roll-coated on the surface of the bottom coating material to form a hydrophilic surface layer, the thickness of the surface layer is about 0.2-0.5 μm, and then the hydrophilic surface layer is baked at 200-280 ℃ for 15-20S (the plate temperature is controlled at 196-268 ℃). The formed super hydrophilic film was then subjected to performance tests, the test results are shown in table 2:
table 2: performance test result of super-hydrophilic coating applied to aluminum foil substrate
In the performance test, the test method of each performance is as follows:
film thickness: a film thickness meter;
initial hydrophilicity: testing by a contact angle tester, 25 ℃;
continuous hydrophilicity: dry-wet cycle, 300 cycles (wet water 2min, air drying 6min for 1 cycle), and testing hydrophilic angle after natural air drying;
uniformity of hydrophilicity: testing by a contact angle tester, 25 ℃;
moisture corrosion resistance: measuring the corrosion degree according to JIS K56007-;
moisture-resistant hydrophilic property: measuring the hydrophilic angle according to JIS K56007-;
heat resistance: the angle of hydrophilicity was tested at 65 deg.C/70 days.
According to the analysis of the performance test result, the super-hydrophilic coating disclosed by the invention has the advantages that the sulfonate system hydrophilic resin A and the acrylic acid system hydrophilic resin are crosslinked, and the hydrophilic resin A and the hydrophilic resin B are subjected to microphase separation due to the water solubility difference along with the volatilization of water and a solvent in the film forming process, so that a nano-scale fine concave-convex structure is generated, and the super-hydrophilic effect on the surface is better facilitated. The specific expression is that the initial hydrophilic angle is less than or equal to 7 degrees, the difference of the hydrophilic angles of each point is small (the angle difference value is less than or equal to 5 degrees), and the hydrophilic uniformity is better; the continuous hydrophilic angle is less than or equal to 9 degrees, and the hydrophilic angle is less than or equal to 10 degrees after heat aging resistance (65 ℃/70 days); meanwhile, the coating has better moisture-proof hydrophilicity, the hydrophilic angle of the moisture-proof hydrophilicity is less than or equal to 12 degrees, and the effect is far better than that of the hydrophilic coating in the prior art.
The hydrophilic properties of comparative examples 1 to 3 are inferior to those of examples 1 to 5 because the hydrophilic coating materials of comparative examples 1 to 3 do not undergo microphase separation during film formation to form a fine textured structure.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. Various changes, modifications, substitutions and alterations to these embodiments will occur to those skilled in the art without departing from the spirit and scope of the present invention.
Claims (10)
1. The super-hydrophilic coating is characterized by comprising the following components in parts by weight:
the hydrophilic resin A comprises the following components in parts by weight:
40-50 parts of reactive surface active monomer, 0.3-0.8 part of initiator, 0-0.5 part of alkali, 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 40-50 parts of deionized water; the reactive surface active monomer is a monomer containing sulfonic acid or sulfonate;
the hydrophilic resin B comprises the following components in parts by weight:
2-4 parts of carboxyl-containing acrylic monomer, 8-10 parts of hydroxyl-containing acrylic monomer, 16-20 parts of acrylamide monomer, 0.2-0.6 part of alkali, 0.3-0.7 part of initiator, 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 40-50 parts of deionized water.
2. The super-hydrophilic coating according to claim 1, wherein the reactive surface active monomer in the hydrophilic resin A is at least one of allyl sulfonic acid and sodium salt thereof, p-styrene sulfonic acid and sodium salt thereof, 2-allyl ether-3-hydroxypropane-1-sulfonic acid and sodium salt thereof, and 2-acrylamido-2-methylpropane sulfonic acid and sodium salt thereof.
3. The super-hydrophilic coating according to claim 2, wherein in the hydrophilic resin a, the initiator is at least one of potassium persulfate, sodium persulfate and ammonium persulfate;
the alcohol solvent is at least one of n-butanol, isobutanol, isopropanol, ethanol and methanol;
the alcohol ether solvent is at least one of propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether.
4. The superhydrophilic coating according to any one of claims 1-3, wherein the hydrophilic resin A comprises the following components in parts by weight:
40-45 parts of reactive surface active monomer, 0.5-0.8 part of initiator, 0.2-0.4 part of alkali, 5-8 parts of alcohol solvent, 5-8 parts of alcohol ether solvent and 45-50 parts of deionized water.
5. The super-hydrophilic coating according to claim 1, wherein in the hydrophilic resin B, the carboxyl group-containing acrylic monomer is at least one of acrylic acid and methacrylic acid;
the hydroxyl-containing acrylic monomer is at least one of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate;
the initiator is at least one of potassium persulfate, sodium persulfate and ammonium persulfate;
the alcohol solvent is at least one of n-butanol, isobutanol, isopropanol, ethanol and methanol;
the alcohol ether solvent is at least one of propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether.
6. The super-hydrophilic coating as claimed in claim 1, wherein the hydrophilic auxiliary agent is at least one of secondary alkyl sodium sulfonate, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, and sodium diisooctyl succinate sulfonate;
the curing agent is at least one of methyl ethyl glycoluril, glyoxal and azapyridine cross-linked resin;
the cosolvent is at least one of n-butanol, isobutanol, isopropanol, ethanol, methanol, propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether.
7. The superhydrophilic coating of claim 1, wherein the base is at least one of sodium hydroxide and potassium hydroxide.
8. A method for preparing the superhydrophilic coating of claim 1, comprising the steps of:
and under the stirring state, sequentially adding deionized water, alkali, hydrophilic resin A, hydrophilic resin B, hydrophilic auxiliary agent, curing agent and cosolvent according to a proportion, and uniformly stirring to obtain the super-hydrophilic coating.
9. The method for preparing the superhydrophilic coating of claim 8, wherein the method for preparing the hydrophilic resin a comprises the steps of:
step S1, adding 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 20-25 parts of deionized water into a reaction kettle provided with a condensation reflux and dripping device; starting stirring, slowly adding 40-50 parts of reactive surface active monomer and 0-0.5 part of alkali in the formula, and heating to 80-90 ℃;
step S2, after fully mixing and dissolving 20-25 parts of deionized water and 0.2-0.7 part of initiator, uniformly dripping into a reaction kettle for 2-4 hours;
step S3, after the mixture is dripped in the step S2, the mixture is kept warm for 1 hour, 0.1 to 0.2 part of initiator and 3 to 5 parts of deionized water are fully mixed and dissolved, and then the mixture is dripped into a reaction kettle for 5 to 15 minutes;
step S4, preserving heat for 1h, fully mixing 0.1-0.2 part of initiator and 3-5 parts of deionized water, and then dripping into the reaction kettle for 5-15 min;
and step S5, preserving heat for 2-4h, cooling and filtering to obtain the hydrophilic resin A.
10. The method for preparing the superhydrophilic coating of claim 8, wherein the method for preparing the hydrophilic resin B comprises the steps of:
step S1, adding 5-10 parts of alcohol solvent, 5-10 parts of alcohol ether solvent and 20-25 parts of deionized water into a reaction kettle provided with a condensation reflux and dripping device, starting stirring, and heating to 80-90 ℃;
step S2, uniformly dripping 10-15 parts of deionized water, 2-4 parts of carboxyl-containing acrylic monomer, 8-10 parts of hydroxyl-containing acrylic monomer, 16-20 parts of acrylamide monomer and 0.2-0.6 part of alkali into a reaction kettle after fully mixing and dissolving, wherein the time for use is 2-4 hours;
step S3, simultaneously, uniformly dripping 10-15 parts of deionized water and 0.2-0.7 part of initiator into the reaction kettle after fully mixing and dissolving for 2-4 hours;
step S4, after the two mixtures are simultaneously dripped, preserving heat for 1h, dripping the mixture into a reaction kettle after 0.1-0.2 part of initiator and 3-5 parts of deionized water are fully mixed and dissolved, and taking 5-15 min;
and step S5, preserving heat for 1 hour, and after 0.1-0.2 part of initiator and 3-5 parts of deionized water are fully mixed and dissolved, dropwise adding the mixture into the reaction kettle for 5-15 min.
And step S6, preserving heat for 2-4h, cooling and filtering to obtain the hydrophilic resin B.
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