CN110790858A - Environment-responsive coating and preparation method thereof - Google Patents
Environment-responsive coating and preparation method thereof Download PDFInfo
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- CN110790858A CN110790858A CN201910949003.2A CN201910949003A CN110790858A CN 110790858 A CN110790858 A CN 110790858A CN 201910949003 A CN201910949003 A CN 201910949003A CN 110790858 A CN110790858 A CN 110790858A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/22—Esters containing halogen
- C08F220/24—Esters containing halogen containing perhaloalkyl radicals
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
- C09D133/16—Homopolymers or copolymers of esters containing halogen atoms
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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
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
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Abstract
The invention discloses an environment-responsive coating, which comprises 50-80 parts by weight of poly (perfluoroalkyl acrylate-acrylic acid) emulsion; 15-20 parts of a solvent; 1-2 parts of a film-forming assistant; 0.1-1 part of hydrophobic modified acrylic emulsion thickening rheological agent; 0.1-0.5 part of a mixture defoamer of mineral oil and wax; 0.1-0.5 part of micromolecule modified polysiloxane wetting and leveling agent; 0.1-0.5 part of an antiseptic and mildew inhibitor; 0.1-0.3 part of thickening agent; 0.1-0.2 parts of ammonia water; the environment-responsive coating is prepared by replacing a comonomer with a hydrophilic monomer on the premise that the main chain structure of a perfluoroalkyl acrylate polymer is not changed, and a coating formed by the obtained polymer realizes a hydrophobic-hydrophilic conversion function when contacting different media.
Description
Technical Field
The invention relates to the field of polymer composite material manufacturing, in particular to an environment-responsive coating and a preparation method thereof.
Background
Fluorine-containing compounds are widely used for surface treatments such as hydrophobic and oleophobic surfaces due to their low surface free energy, good chemical and thermal stability. The polyacrylate emulsion has the characteristics of flexibility, weather resistance, good viscosity and the like, takes water as a medium, has low cost and less pollution, and plays an important role in the fields of emulsion polymerization research and production. Currently, perfluoroalkyl-containing (meth) acrylate polymers are composed of long chain perfluoroalkyl side chains, a polymer backbone, and other groups.
Generally these materials with low surface free energy do not readily adsorb dust or dirt particles in the environment. However, once liquid water-insoluble soils (primarily greases and fatty substances) are set on such materials, dust or soil particles can adhere to such materials by capillary action, resulting in staining of fluoropolymer materials having low surface energy. Moreover, the high hydrophobicity of fluoropolymers makes such materials difficult to clean with water after staining. This deficiency in fluoropolymers places some limitations on their practical use. The method for compensating this deficiency is focused on how to prepare an environmentally responsive coating from which the surface treated can be converted into oleophobic/hydrophobic-hydrophilic properties.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an environment response type coating and a preparation method thereof, the environment response type coating is prepared by replacing a comonomer with a hydrophilic monomer on the premise that the main chain structure of a perfluoroalkyl acrylate polymer is not changed, and a coating formed by the obtained polymer realizes the hydrophobic-hydrophilic conversion function when contacting different media, namely: the water-repellent oil-repellent surface has low surface energy in the air, has water-repellent and oil-repellent effects, can prevent dirt from being deposited on the surface of a material, and can gradually become hydrophilic after contacting with water, so that the polluted surface is easy to clean.
The invention is realized by the following steps:
one of the purposes of the invention is to provide a poly (perfluoroalkyl acrylate-acrylic acid) emulsion, which comprises the following components in parts by weight:
85-95 parts of deionized water, 0.8-1 part of emulsifier, 0.7-0.9 part of sodium dodecyl sulfate, 0.08-0.1 part of fluorocarbon nonionic surfactant, 20-25 parts of perfluoroalkyl acrylate monomer, 20-25 parts of acrylic acid monomer, 0.7-1 part of initiator and 40-60 parts of acetone solution; wherein the weight ratio of the perfluoroalkyl acrylate monomer to the acrylic acid monomer is 1: 1.
the invention also aims to provide a preparation method of the poly (perfluoroalkyl acrylate-acrylic acid) emulsion, which is characterized by comprising the following steps:
s1, under the protection of nitrogen, stirring 85-95 parts of deionized water, 0.8-1 part of emulsifier, 0.7-0.9 part of sodium dodecyl sulfate and 0.08-0.1 part of fluorocarbon nonionic surfactant uniformly in a reaction kettle according to the proportion to obtain a mixed solution;
s2, mixing 20-25 parts of perfluoroalkyl acrylate monomer and 20-25 parts of acrylic monomer according to the weight ratio of 1: 1 in proportion is dissolved in the acetone solution to obtain the acetone solution containing the perfluoroalkyl acrylate monomer and the acrylic acid monomer;
s3, adding a part of acetone solution containing perfluoroalkyl acrylate monomers and acrylic acid monomers obtained in the step 2 into the mixed solution obtained in the step 1, and heating to 45-55 ℃ for pre-emulsification for 1-1.5 h;
and S4, heating to 60-80 ℃, dropwise adding 0.7-1 part of the initiator to initiate copolymerization, dropwise adding the rest acetone solution containing the perfluoroalkyl acrylate monomer and the acrylic acid monomer, reacting for 2-4 h after dropwise adding, cooling to room temperature, and discharging to obtain the product.
The invention also aims to provide an environment-responsive coating, which comprises the following raw materials in parts by weight:
50-80 parts of poly (perfluoroalkyl acrylate-acrylic acid) emulsion;
15-20 parts of a solvent;
1-2 parts of a film-forming assistant;
0.1-1 part of hydrophobic modified acrylic emulsion thickening rheological agent;
0.1-0.5 part of a mixture defoamer of mineral oil and wax;
0.1-0.5 part of micromolecule modified polysiloxane wetting and leveling agent;
0.1-0.5 part of an antiseptic and mildew inhibitor;
0.1-0.3 part of thickening agent;
0.1-0.2 part of ammonia water.
The fourth purpose of the invention is to provide a preparation method of the environment-responsive coating, which comprises the following steps: and (3) uniformly dispersing and mixing the raw materials in the proportion by adopting a high-speed dispersion machine, grinding for 20-50 min by using a sand mill, and filtering to obtain the environment-responsive coating.
Compared with the prior art, the invention has the following advantages and effects:
according to the environment-responsive coating provided by the invention, Acrylic Acid (AA) is used as a hydrophilic monomer to modify a perfluoroalkyl acrylate monomer (PFAA), copolymerization reaction is carried out under the action of an initiator, and the obtained polymer has a hydrophobic chain segment with extremely low surface energy of perfluoroalkyl and hydrophilic chain segments of-OH and-COOH, so that the coating can be subjected to hydrophilic-hydrophobic conversion in a natural environment, and the problems of serious dust adsorption and difficult cleaning in the practical application of the outdoor stain-resistant coating are solved. Contact angle measurement experiments showed that the contact angle of a water drop onto the coating was initially relatively large, 110.1 °, indicating that the polymer coating initially exhibited hydrophobicity. However, the contact angle of water on the coating gradually decreases with time, and the contact angle sharply decreases from 110.1 degrees to 19.5 degrees within 10min, so that the coating is hydrophilic. And after the sample plate is completely dried, the static water contact angle can reach 110 degrees, and the sample plate has the hydrophobic characteristic.
Drawings
FIG. 1 is a graph showing contact angles of water drops dropped onto a coating layer formed of the environmentally responsive paint of the present invention at different times (0min, 2min, 5min, 8min, 10min) as provided in Experimental example 1;
FIG. 2 is an infrared spectrum of the poly (perfluoroalkyl acrylate-acrylic acid) emulsion prepared in example 1.
Detailed Description
Example 1
1. The poly (perfluoroalkyl acrylate-acrylic acid) emulsion comprises the following raw materials in parts by weight:
85 parts of deionized water, 1 part of emulsifier, 0.9 part of sodium dodecyl sulfate, 0.1 part of fluorocarbon nonionic surfactant, 20 parts of perfluoroalkyl acrylate monomer, 20 parts of acetone solution of acrylic monomer, 0.7 part of initiator and 40 parts of acetone solution;
the preparation method of the emulsion comprises the following steps:
under the protection of nitrogen, firstly uniformly stirring deionized water, an emulsifier, sodium dodecyl sulfate and a fluorocarbon nonionic surfactant in a reaction kettle, then adding an acetone solution of a perfluoroalkyl acrylate monomer and an acrylic acid monomer, heating to 50 ℃ for pre-emulsification for 1h, then heating to 60 ℃, dropwise adding an initiator to initiate copolymerization, heating to 70 ℃, dropwise adding an acetone solution of the perfluoroalkyl acrylate monomer and the acrylic acid monomer with equal quantity, stopping after the dropwise adding is finished, continuing to react, cooling to room temperature, and discharging to obtain the product.
2. The embodiment provides an environment-responsive coating, which comprises the following raw materials in parts by weight:
78 parts of poly (perfluoroalkyl acrylate-acrylic acid) emulsion;
19.2 parts of a solvent;
1 part of a film-forming assistant;
0.5 part of hydrophobic modified acrylic emulsion thickening rheological agent;
0.3 part of a mixture of mineral oil and wax as an antifoaming agent;
0.3 part of micromolecule modified polysiloxane wetting and leveling agent;
0.5 part of antiseptic and mildew-proof agent;
0.1 part of thickening agent;
0.1 part of ammonia water.
3. The preparation method of the environment-responsive coating comprises the following steps: and (3) uniformly dispersing and mixing the raw materials in the proportion by adopting a high-speed dispersion machine, grinding for 20-50 min by using a sand mill, and filtering to obtain the environment-responsive coating.
4. The paint film property test of the obtained environment-responsive paint is shown in table 1.
TABLE 1
Example 2
1. The poly (perfluoroalkyl acrylate-acrylic acid) emulsion comprises the following raw materials in parts by weight:
90 parts of deionized water, 0.9 part of emulsifier, 0.8 part of sodium dodecyl sulfate, 0.09 part of fluorocarbon nonionic surfactant, 22 parts of perfluoroalkyl acrylate monomer, 22 parts of acetone solution of acrylic monomer, 0.8 part of initiator and 50 parts of acetone solution;
the preparation method of the emulsion comprises the following steps:
under the protection of nitrogen, firstly uniformly stirring deionized water, an emulsifier, sodium dodecyl sulfate and a fluorocarbon nonionic surfactant in a reaction kettle, then adding an acetone solution of a perfluoroalkyl acrylate monomer and an acrylic acid monomer, heating to 45 ℃, pre-emulsifying for 1h, then heating to 70 ℃, dropwise adding an initiator to initiate copolymerization, heating to 85 ℃, dropwise adding an acetone solution of the perfluoroalkyl acrylate monomer and the acrylic acid monomer with equal quantity, stopping after the dropwise adding is finished, continuing to react, cooling to room temperature, and discharging to obtain the product.
2. The embodiment provides an environment-responsive coating, which comprises the following raw materials in parts by weight:
50 parts of poly (perfluoroalkyl acrylate-acrylic acid) emulsion;
15 parts of a solvent;
1.5 parts of a film-forming assistant;
0.1 part of hydrophobic modified acrylic emulsion thickening rheological agent;
0.1 part of a mixture defoamer of mineral oil and wax;
0.1 part of micromolecule modified polysiloxane wetting and leveling agent;
0.1 part of antiseptic and mildew inhibitor;
0.3 part of thickening agent;
0.2 part of ammonia water.
3. The preparation method of the environment-responsive coating comprises the following steps: and (3) uniformly dispersing and mixing the raw materials in the proportion by adopting a high-speed dispersion machine, grinding for 20-50 min by using a sand mill, and filtering to obtain the environment-responsive coating.
4. The paint film property test of the obtained environment-responsive paint is shown in table 2.
TABLE 2
Example 3
1. The poly (perfluoroalkyl acrylate-acrylic acid) emulsion comprises the following raw materials in parts by weight:
95 parts of deionized water, 1 part of emulsifier, 0.9 part of sodium dodecyl sulfate, 0.08 part of fluorocarbon nonionic surfactant, 25 parts of perfluoroalkyl acrylate monomer, 25 parts of acetone solution of acrylic monomer, 1 part of initiator and 60 parts of acetone solution;
the preparation method of the emulsion comprises the following steps:
under the protection of nitrogen, firstly uniformly stirring deionized water, an emulsifier, sodium dodecyl sulfate and a fluorocarbon nonionic surfactant in a reaction kettle, then adding an acetone solution of a perfluoroalkyl acrylate monomer and an acrylic acid monomer, heating to 55 ℃ for pre-emulsification for 1h, then heating to 80 ℃, dropwise adding an initiator to initiate copolymerization, heating to 90 ℃, dropwise adding an acetone solution of the perfluoroalkyl acrylate monomer and the acrylic acid monomer with equal quantity, stopping after the dropwise adding is finished, continuing to react, cooling to room temperature, and discharging to obtain the product.
2. The embodiment provides an environment-responsive coating, which comprises the following raw materials in parts by weight:
80 parts of poly (perfluoroalkyl acrylate-acrylic acid) emulsion;
20 parts of a solvent;
2 parts of a film-forming additive;
1 part of hydrophobic modified acrylic emulsion thickening rheological agent;
0.5 part of a mixture defoamer of mineral oil and wax;
0.5 part of micromolecule modified polysiloxane wetting and leveling agent;
0.3 part of antiseptic and mildew-proof agent;
0.3 part of thickening agent;
0.2 part of ammonia water.
3. The preparation method of the environment-responsive coating comprises the following steps: and (3) uniformly dispersing and mixing the raw materials in the proportion by adopting a high-speed dispersion machine, grinding for 20-50 min by using a sand mill, and filtering to obtain the environment-responsive coating.
4. The paint film property test of the obtained environment-responsive paint is shown in Table 3.
TABLE 3
Experimental example 1
The structures of the monomers and polymers were characterized by infrared spectroscopy. FIG. 1 is an infrared spectrum of PFAA (perfluoroalkyl acrylate), AA (acrylic acid), P (PFAA-AA) (poly (perfluoroalkyl acrylate-acrylic acid)). From the infrared spectrum of P (PFAA-AA), it is clear that the wave number is 3448cm-1(iii) stretching vibration absorption peak at hydroxyl group O-H, 1743cm-1A characteristic absorption peak of CO of 2860-2965 cm-1Stretching vibration at aliphatic C-H, and 1205cm-1And 1242cm-1And C-F characteristic peak of stretching vibration. In addition, 1636cm-1The disappearance of the characteristic absorption peak at C-C confirms that the monomer has been completely converted to polymer.
Experimental example 2 contact Angle measurement experiment
The results of the contact angle detection experiment of the coating layer of the environmentally responsive paint prepared in example 1 are shown in fig. 1.
The contact angle of a water drop on the coating at the very beginning (t ═ 0min) is relatively large, 110.1 °, indicating that the polymer coating exhibits hydrophobicity at the very beginning. However, the contact angle of water on the coating gradually decreases with time, and the contact angle sharply decreases from 110.1 degrees to 19.5 degrees within 10min, so that the coating is hydrophilic. And after the sample plate is completely dried, the static water contact angle can reach 110 degrees, and the sample plate has the hydrophobic characteristic.
The invention is not to be considered as limited to the particular embodiments shown, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The poly (perfluoroalkyl acrylate-acrylic acid) emulsion is characterized by comprising the following components in parts by weight:
85-95 parts of deionized water, 0.8-1 part of emulsifier, 0.7-0.9 part of sodium dodecyl sulfate, 0.08-0.1 part of fluorocarbon nonionic surfactant, 20-25 parts of perfluoroalkyl acrylate monomer, 20-25 parts of acrylic acid monomer, 0.7-1 part of initiator and 40-60 parts of acetone solution; and the weight ratio of the perfluoroalkyl acrylate monomer to the acrylic acid monomer is 1: 1.
2. the poly (perfluoroalkylacrylate-acrylic acid) emulsion of claim 1, wherein the emulsifier comprises one of the non-ionic emulsifiers Sapogenat 110, Sapogenat 500, Sapogenat 180 of Crayne; the fluorocarbon nonionic surfactant comprises one of DuPont FS0-100, FSN-100 and FS-3100; the initiator comprises ammonium persulfate.
3. A method of preparing a poly (perfluoroalkyl acrylate-acrylic acid) emulsion as claimed in any of claims 1-2, comprising:
s1, under the protection of nitrogen, stirring 85-95 parts of deionized water, 0.8-1 part of emulsifier, 0.7-0.9 part of sodium dodecyl sulfate and 0.08-0.1 part of fluorocarbon nonionic surfactant uniformly in a reaction kettle according to the proportion to obtain a mixed solution;
s2, mixing 20-25 parts of perfluoroalkyl acrylate monomer and 20-25 parts of acrylic monomer according to the weight ratio of 1: 1 in proportion is dissolved in the acetone solution to obtain the acetone solution containing the perfluoroalkyl acrylate monomer and the acrylic acid monomer;
s3, adding a part of acetone solution containing perfluoroalkyl acrylate monomers and acrylic acid monomers obtained in the step 2 into the mixed solution obtained in the step 1, and heating to 45-55 ℃ for pre-emulsification for 1-1.5 h;
and S4, heating to 60-80 ℃, dropwise adding 0.7-1 part of the initiator to initiate copolymerization, heating to 10-15 ℃ on the basis of the temperature, dropwise adding the rest of acetone solution containing the perfluoroalkyl acrylate monomer and the acrylic acid monomer, reacting for 2-4 h after dropwise adding, cooling to room temperature, and discharging to obtain the product.
4. The method of claim 3, wherein the pre-emulsification temperature in S3 is 50 ℃.
5. The method according to claim 3, wherein the copolymerization temperature in S4 is 70 ℃.
6. The environment-responsive coating is characterized by comprising the following raw materials in parts by weight:
50-80 parts of poly (perfluoroalkyl acrylate-acrylic acid) emulsion as defined in claim 1-2;
15-20 parts of a solvent;
1-2 parts of a film-forming assistant;
0.1-1 part of hydrophobic modified acrylic emulsion thickening rheological agent;
0.1-0.5 part of a mixture defoamer of mineral oil and wax;
0.1-0.5 part of micromolecule modified polysiloxane wetting and leveling agent;
0.1-0.5 part of an antiseptic and mildew inhibitor;
0.1-0.3 part of thickening agent;
0.1-0.2 part of ammonia water.
7. The environment-responsive paint of claim 6, wherein the environment-responsive paint comprises the following raw materials in parts by weight:
78 parts of poly (perfluoroalkyl acrylate-acrylic acid) emulsion;
19.2 parts of a solvent;
1 part of a film-forming assistant;
0.5 part of hydrophobic modified acrylic emulsion thickening rheological agent;
0.3 part of a mixture of mineral oil and wax as an antifoaming agent;
0.3 part of micromolecule modified polysiloxane wetting and leveling agent;
0.5 part of antiseptic and mildew-proof agent;
0.1 part of thickening agent;
0.1 part of ammonia water.
8. The environmentally responsive coating of claim 6 wherein said solvent is deionized water; the filler comprises oligomeric silsesquioxane; the film-forming additive is decaglycol ester; the hydrophobically modified acrylic emulsion thickening rheological agent comprises a humble RHEOLATE 150 and a rhoolate 175; the antifoaming agent is a mixture of mineral oil and wax, and comprises moded DAPRO AP 7010.
9. The environmentally responsive coating of claim 6 wherein the small molecule modified polysiloxane wetting and leveling agent comprises one of modestly levell w-469, Levaslip w-461; the antiseptic and mildew preventive comprises a Dow skana M-8; the thickener comprises hydroxyethyl cellulose.
10. A method of preparing the environmentally responsive coating of any one of claims 1 to 9, wherein the method of preparation comprises: and (3) uniformly dispersing and mixing the raw materials in the proportion by adopting a high-speed dispersion machine, grinding for 20-50 min by using a sand mill, and filtering to obtain the environment-responsive coating.
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| CN115671640A (en) * | 2022-08-30 | 2023-02-03 | 北京理工大学 | High-cooling-performance water-based fire extinguishing agent for lithium ion battery and preparation method thereof |
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| CN115671640B (en) * | 2022-08-30 | 2023-11-24 | 北京理工大学 | High-cooling water-based fire extinguishing agent for lithium ion battery and preparation method thereof |
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