CN116023691A - Preparation method of hydrophobic acrylate coating - Google Patents
Preparation method of hydrophobic acrylate coating Download PDFInfo
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- CN116023691A CN116023691A CN202210991113.7A CN202210991113A CN116023691A CN 116023691 A CN116023691 A CN 116023691A CN 202210991113 A CN202210991113 A CN 202210991113A CN 116023691 A CN116023691 A CN 116023691A
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- 238000000576 coating method Methods 0.000 title claims abstract description 89
- 239000011248 coating agent Substances 0.000 title claims abstract description 85
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 title claims abstract description 42
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000839 emulsion Substances 0.000 claims abstract description 62
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 56
- -1 acrylic ester Chemical class 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 40
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 35
- 229920002799 BoPET Polymers 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 31
- 230000008569 process Effects 0.000 claims abstract description 30
- 238000007761 roller coating Methods 0.000 claims abstract description 26
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 24
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 239000003522 acrylic cement Substances 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 4
- 239000000853 adhesive Substances 0.000 claims description 36
- 230000001070 adhesive effect Effects 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 20
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 17
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 14
- 239000012948 isocyanate Substances 0.000 claims description 11
- 150000002513 isocyanates Chemical group 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 10
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- 229940089951 perfluorooctyl triethoxysilane Drugs 0.000 claims description 9
- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 claims description 9
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 230000009477 glass transition Effects 0.000 claims description 2
- 125000005396 acrylic acid ester group Chemical group 0.000 claims 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 27
- 239000013043 chemical agent Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 15
- 239000002994 raw material Substances 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000010907 mechanical stirring Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000011253 protective coating Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000007720 emulsion polymerization reaction Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a hydrophobic acrylate coating, which comprises the following steps: step 1: preparing a mixture of an acrylic adhesive and a curing agent; step 2: adopting a roller coating process to bond and fix the acrylic ester adhesiveCoating the mixture of the chemical agents on a PET substrate, and drying; step 3: preparation of fluorine-silicon modified nano SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the Step 4: preparation of fluorine-silicon modified nano SiO 2 Acrylic emulsion; step 5: adopting roller coating technology to modify fluorine-silicon into nano SiO 2 Coating acrylic emulsion on a release PET film, and drying; step 6: the PET substrate coated with the acrylic adhesive obtained in the step 2 and the fluorosilicone modified nano SiO coated obtained in the step 5 are subjected to the following steps of 2 And (3) drying and curing the release PET film of the acrylic emulsion, pressing the two-sided coating by using a rubber roller, and uncovering the release PET film when in use to obtain the hydrophobic acrylate coating. The invention has simple process and lower cost, and effectively improves the hydrophobicity of the water-based acrylic ester coating.
Description
Technical Field
The invention relates to the field of hydrophobic coatings, in particular to a preparation method of a hydrophobic acrylate coating.
Background
The water-based acrylic ester has the advantages of wide raw material sources, simple preparation process, good drying film forming property, environmental friendliness and the like, so that the water-based acrylic ester is the earliest developed one in water-based paint products. Aqueous acrylic emulsions are often used as film formers for aqueous coatings because of their good film forming properties. However, the aqueous acrylic emulsion uses water as a dispersion medium, and the surfactant used in emulsion polymerization has amphiphilic properties, namely one end has lipophilicity and the other end has hydrophilicity, and the surfactant still remains in the emulsion after polymerization, remains in the coating after film formation, and reacts with water when meeting water, so that water molecules can permeate, diffuse and migrate in the coating, and the obtained coating has the problem of poor hydrophobicity and water resistance, so that the application of the aqueous acrylic ester as a protective coating is limited to a certain extent.
In order to solve the problem of poor hydrophobicity of the aqueous acrylic ester coating, fluorine-containing or silicon-containing monomers are generally introduced in the emulsion polymerization process, and the hydrophobicity of the coating is improved by reducing the surface energy of the coating, but the fluorine-containing monomers and the silicon-containing monomers are relatively expensive, and the high cost leads to difficulty in popularization of the coating in industrial application. In addition, the hydrophobicity of the coating can be improved by constructing a micro-nano structure on the surface of the coating, but in practice, the current preparation methods including a template method, an etching method, a chemical deposition method, a hydrothermal method, a sol-gel method and the like have high requirements on instruments and equipment, reagent raw materials, a sample matrix and production conditions, and are difficult to produce in a large scale, and the stability of the micro-nano structure on the surface of the coating often has the problem of losing functions due to scratch resistance in practical application, which is a difficulty in preventing the application of the coating in the field of protective coatings.
In conclusion, a method for improving the hydrophobicity of the aqueous acrylic ester coating is developed, and the method has important practical significance for application and popularization of the aqueous acrylic acid in the fields of aqueous paint and protective coating.
Disclosure of Invention
The invention aims at providing a preparation method of a hydrophobic acrylate coating with simple process and low cost to solve the problems, so as to improve the hydrophobicity of the water-based acrylate coating.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a preparation method of a hydrophobic acrylate coating is prepared by the following steps:
step 1: preparing a mixture of an acrylic adhesive and a curing agent;
step 2: coating a mixture of an acrylic adhesive and a curing agent on a PET substrate by adopting a roller coating process, and drying;
step 3: preparation of fluorine-silicon modified nano SiO 2 ；
Step 4: preparation of fluorine-silicon modified nano SiO 2 Acrylic emulsion;
step 5: adopting roller coating technology to modify fluorine-silicon into nano SiO 2 Coating acrylic emulsion on a release PET film, and drying;
step 6: PET coated with acrylate adhesive obtained in the step 2 and fluorosilicone coated obtained in the step 5 are mixedModified nano SiO 2 And (3) drying and curing the release PET film of the acrylic emulsion, pressing the two-sided coating by using a rubber roller, and uncovering the release PET film when in use to obtain the hydrophobic acrylate coating.
Further, in the step 1, the acrylate adhesive is a solvent type acrylate adhesive, the solvent is ethyl acetate, the solid content is 44+/-2%, and the viscosity is 3000-6000 cP.
Further, in step 1, the curing agent is an isocyanate curing agent.
Further, the step 1 is implemented as follows: mixing 90-110 parts of acrylate adhesive with 0.9-1.3 parts of isocyanate curing agent, and mechanically stirring for 30-50 min at the rotating speed of 600-800 r/min.
Further, in the step 2, the acrylic adhesive prepared in the step 1 is coated on the PET substrate by adopting a roller coating process, and the dry film thickness is 10-15 mu m.
Further, in step 3, the fluorosilicone modified nano SiO 2 The preparation method comprises the following steps:
2 to 4 parts of perfluoro octyl triethoxysilane and 1 to 3 parts of gamma-aminopropyl triethoxysilane are added into 20 to 35 parts of absolute ethyl alcohol, and after being mechanically stirred uniformly, 1 to 2 parts of nano-grade SiO is added 2 And 2-5 parts of polytetrafluoroethylene micro powder wax, and dispersing for 30-50 min by using ultrasonic after stirring for 2-3 h at high speed to obtain the fluorine-silicon modified nano SiO 2 . Still further, the nano-scale SiO 2 The grain diameter of the polytetrafluoroethylene micro powder wax is 200-300 nm, and the grain diameter of the polytetrafluoroethylene micro powder wax is 5.0-6.0 mu m.
Further, in step 4, the fluorosilicone modified nano SiO 2 The acrylic emulsion is prepared by the following process:
adding 100-120 parts of acrylic ester emulsion and 2-5 parts of sodium polyacrylate into the dispersion system in the step 3, fully stirring for 1.5-2 hours at the rotating speed of 800-1200 r/min to obtain the fluorosilicone modified nano SiO 2 Acrylic emulsion.
Further, in step 4, the aqueous acrylic emulsion has a solid content of 40 to 50%, a viscosity of 4000 to 8000cP.s, and a glass transition temperature of 50 to 65 ℃.
Further, in step 5, the fluorosilicone modified nano SiO prepared in step 4 is rolled by a roller coating process 2 The acrylic emulsion is coated on a release PET film, and the dry film thickness is 30-50 mu m.
Further, in step 6, PET coated with acrylate adhesive and nano SiO coated with fluorine-silicon modification are used 2 Drying and curing the release PET film of the acrylic emulsion in a temperature gradient of 60-90 ℃ for 5-10 min, and then mixing the acrylate adhesive surface with the fluorosilicone modified nano SiO through a rubber roller 2 And (3) pressing the acrylic emulsion surface, and uncovering the release PET film when in use to obtain the hydrophobic acrylic ester coating.
Furthermore, the pressure used for pressing ensures that the coating has no bubbles and no wrinkling, and is generally 4-10 kg/cm 2 。
According to the invention, a roller coating method is adopted for coating, and the surface of the obtained coating is smoother and smoother after the coating is dried and solidified and then transferred and attached, so that the hydrophobicity is improved to a degree.
Compared with the prior art, the invention has the beneficial effects that:
(1) Compared with a coating obtained by a single roller coating process, the coating obtained by the method has no roller marks and air holes on the surface, is smoother and smoother, has a larger static water contact angle after being modified by low surface energy resin, and is easier to slide down due to water drops, thereby having better self-cleaning capability.
(2) The bottom structure of the coating adopts solvent type acrylic resin, has strong adhesion to PET base material and quick drying speed, has better film forming property and water resistance, and avoids the phenomena of residual bubbles or shrinkage cavities and the like in the production of the coating.
(3) Introducing low amount of fluorine silicon resin to nano SiO 2 Modification is carried out, which is favorable for nano SiO 2 The dispersion in the system, while controlling low cost, allows the coating to have a lower surface energy.
(4) The polytetrafluoroethylene micro powder wax can make the coating have hydrophobicity, and the coating is matched with the polytetrafluoroethylene micro powder waxFluorine-silicon modified nano SiO 2 Can be uniformly distributed in the system, and the two have synergistic effect, so that the water-based acrylic ester coating has better hydrophobicity and produces lotus leaf-like effect.
Fig. 1 is a water contact angle of the coating prepared in example 1.
Fig. 2 is a water contact angle of the coating prepared in example 2.
Fig. 3 is a water contact angle of the coating prepared in comparative example 1.
Fig. 4 is a water contact angle of the coating prepared in comparative example 2.
Fig. 5 is a water contact angle of the coating prepared in comparative example 3.
Fig. 6 is a water contact angle of the coating prepared in comparative example 4.
Fig. 7 is a water contact angle of the coating prepared in comparative example 5.
Detailed Description
The invention is further illustrated below with reference to examples. These examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. The experimental procedures in the examples below, without specific details, are generally performed under conditions conventional in the art or recommended by the manufacturer; the raw materials, reagents and the like used, unless otherwise specified, are those commercially available from conventional markets and the like.
The sources of reagents used in the examples are as follows:
acrylic adhesive: an Zuo chemical Co., ltd
Aqueous acrylic emulsion: wanhua chemistry
Sodium polyacrylate: chinese medicine
Polytetrafluoroethylene micropowder wax: jiashan Shen Jia technology Co.Ltd
Perfluorooctyl triethoxysilane: nanjing full-Highway chemical Co., ltd
Gamma-aminopropyl triethoxysilane: hangzhou JieXika chemical Co., ltd
Absolute ethyl alcohol: chinese medicine
Nanoscale SiO 2 : zhiya Material technology Co., ltd
Isocyanate curing agent: shanghai Kaiyin chemical Co., ltd
Example 1
A hydrophobic acrylate coating prepared by the steps of:
step 1: 90 parts of acrylate adhesive and 1 part of isocyanate curing agent are mixed, and mechanically stirred for 30min at the rotating speed of 800r/min.
Step 2, coating the acrylic ester adhesive prepared in the step 1 on a PET substrate by adopting a roller coating process, and drying at 80 ℃ to obtain a dry film with the thickness of 10 mu m;
step 3: 2 parts of perfluorooctyl triethoxysilane and 1 part of gamma-aminopropyl triethoxysilane are added into 20 parts of absolute ethyl alcohol, and after mechanical stirring is uniform, 1 part of nano-grade SiO is added 2 And 2 parts of polytetrafluoroethylene micro powder wax, and dispersing for 30min by using ultrasonic after stirring for 2h at a high speed.
Step 4: adding 100 parts of acrylic ester emulsion and 2 parts of sodium polyacrylate into the dispersion system in the step 3, fully stirring for 1.5h at the rotating speed of 1000r/min to obtain the fluorosilicone modified nano SiO 2 Acrylic emulsion.
Step 5: adopting a roller coating process to prepare the fluorosilicone modified nano SiO prepared in the step 4 2 Acrylic emulsion is coated on a release PET film, and is dried at 80 ℃ with a dry film thickness of 35 mu m.
Step 6: PET coated with acrylate adhesive and nano SiO coated with fluorine-silicon modified nano SiO 2 The acrylic emulsion release PET film is placed in the temperature of 80 ℃ for 6min, and after drying and curing, the acrylic ester adhesive surface and the fluorosilicone modified nano SiO are carried out through a rubber roller 2 Acrylic emulsion level press-fit, roller pressure of 5kg/cm 2 When in use, the release PET film is uncovered to obtain the hydrophobic acrylic ester coating.
Example 2
A hydrophobic acrylate coating prepared by the steps of:
step 1: 100 parts of acrylate adhesive and 1.5 parts of isocyanate curing agent are mixed, and mechanically stirred for 40min at a rotating speed of 800r/min.
Step 2, coating the acrylic ester adhesive prepared in the step 1 on a PET substrate by adopting a roller coating process, and drying at 85 ℃ to obtain a dry film with a thickness of 15 mu m;
step 3: 2 parts of perfluorooctyl triethoxysilane and 3 parts of gamma-aminopropyl triethoxysilane are added into 35 parts of absolute ethyl alcohol, and after mechanical stirring is uniform, 2 parts of nano-grade SiO is added 2 And 5 parts of polytetrafluoroethylene micro powder wax, and dispersing for 50min by using ultrasonic after stirring for 3h at a high speed.
Step 4: adding 120 parts of acrylic ester emulsion and 4 parts of sodium polyacrylate into the dispersion system in the step 3, fully stirring for 1.5h at the rotating speed of 1000r/min to obtain the fluorosilicone modified nano SiO 2 Acrylic emulsion.
Step 5: adopting a roller coating process to prepare the fluorosilicone modified nano SiO prepared in the step 4 2 Acrylic emulsion is coated on a release PET film, and is dried at 85 ℃ with a dry film thickness of 45 mu m.
Step 6: PET coated with acrylate adhesive and nano SiO coated with fluorine-silicon modified nano SiO 2 The acrylic emulsion release PET film is placed in the temperature of 85 ℃ for 5min, and after drying and curing, the acrylic ester adhesive surface and the fluorosilicone modified nano SiO are carried out through a rubber roller 2 Acrylic emulsion level press-fit, roller pressure of 5kg/cm 2 When in use, the release PET film is uncovered to obtain the hydrophobic acrylic ester coating.
Comparative example 1
A hydrophobic acrylate coating prepared by the steps of:
step 1: 2 parts of perfluorooctyl triethoxysilane and 1 part of gamma-aminopropyl triethoxysilane are added into 20 parts of absolute ethyl alcohol, and after mechanical stirring is uniform, 1 part of nano-grade SiO is added 2 And 2 parts of polytetrafluoroethylene micro powder wax, and dispersing for 30min by using ultrasonic after stirring for 2h at a high speed.
Step 2: adding 100 parts of acrylic ester emulsion and 2 parts of sodium polyacrylate into the dispersion system in the step 1, fully stirring for 1.5h at the rotating speed of 1000r/min to obtain the fluorosilicone modified nano SiO 2 Acrylic emulsion.
Step 3: adopting a roller coating process to prepare the fluorosilicone modified nano SiO in the step 2 2 Acrylic emulsion is coated on a release PET film, and is dried at 85 ℃ and the dry film thickness is 35 mu m.
Step 4: coating fluorine-silicon modified nano SiO 2 And (3) placing the PET substrate of the acrylic emulsion at the temperature of 85 ℃ for 5min, and drying and curing to obtain the hydrophobic acrylate coating.
Comparative example 2: nano SiO modified without adding fluorine silicon 2 And polytetrafluoroethylene micropowder wax
A hydrophobic acrylate coating prepared by the steps of:
step 1: 90 parts of acrylate adhesive and 1 part of isocyanate curing agent are mixed, and mechanically stirred for 30min at the rotating speed of 800r/min.
Step 2, coating the acrylic ester adhesive prepared in the step 1 on a PET substrate by adopting a roller coating process, and drying at 85 ℃ to obtain a dry film with the thickness of 10 mu m;
step 3: mixing 100 parts of acrylic emulsion with 2 parts of sodium polyacrylate, and fully stirring for 1.5 hours at the rotating speed of 1000r/min to obtain acrylic emulsion;
step 4: and (3) coating the acrylic emulsion prepared in the step (3) on a release PET film by adopting a roller coating process, and drying at 85 ℃ to obtain a dry film with the thickness of 35 mu m.
Step 5: placing PET coated with acrylate adhesive and release PET film coated with acrylic emulsion at 85deg.C for 5min, drying and solidifying, pressing acrylate adhesive surface with acrylic emulsion liquid surface by rubber roller with pressure of 5kg/cm 2 When in use, the release PET film is uncovered to obtain the hydrophobic acrylic ester coating.
Comparative example 3: no polytetrafluoroethylene micro powder wax is added
A hydrophobic acrylate coating prepared by the steps of:
step 1: 90 parts of acrylate adhesive and 1 part of isocyanate curing agent are mixed, and mechanically stirred for 30min at the rotating speed of 800r/min.
Step 2, coating the acrylic ester adhesive prepared in the step 1 on a PET substrate by adopting a roller coating process, and drying at 80 ℃ to obtain a dry film with the thickness of 10 mu m;
step 3: 2 parts of perfluorooctyl triethoxysilane and gamma-aminopropyl triethyleneAdding 1 part of oxysilane into 20 parts of absolute ethyl alcohol, mechanically stirring uniformly, and adding 1 part of nano-grade SiO 2 After stirring at high speed for 2h, ultrasonic dispersion was used for 30min.
Step 4: adding 100 parts of acrylic ester emulsion and 2 parts of sodium polyacrylate into the dispersion system in the step 3, fully stirring for 1.5h at the rotating speed of 1000r/min to obtain the fluorosilicone modified nano SiO 2 Acrylic emulsion.
Step 5: adopting a roller coating process to prepare the fluorosilicone modified nano SiO prepared in the step 4 2 Acrylic emulsion is coated on a release PET film, and is dried at 80 ℃ with a dry film thickness of 35 mu m.
Step 6: PET coated with acrylate adhesive and nano SiO coated with fluorine-silicon modified nano SiO 2 The acrylic emulsion release PET film is placed in the temperature of 80 ℃ for 6min, and after drying and curing, the acrylic ester adhesive surface and the fluorosilicone modified nano SiO are carried out through a rubber roller 2 Acrylic emulsion level press-fit, roller pressure of 5kg/cm 2 When in use, the release PET film is uncovered to obtain the hydrophobic acrylic ester coating.
Comparative example 4: without addition of silane
A hydrophobic acrylate coating prepared by the steps of:
step 1: 90 parts of acrylate adhesive and 1 part of isocyanate curing agent are mixed, and mechanically stirred for 30min at the rotating speed of 800r/min.
Step 2, coating the acrylic ester adhesive prepared in the step 1 on a PET substrate by adopting a roller coating process, and drying at 80 ℃ to obtain a dry film with the thickness of 10 mu m;
step 3: 1 part of nano-SiO is added into 20 parts of absolute ethyl alcohol 2 And 2 parts of polytetrafluoroethylene micro powder wax, and dispersing for 30min by using ultrasonic after stirring for 2h at a high speed.
Step 4: adding 100 parts of acrylic ester emulsion and 2 parts of sodium polyacrylate into the dispersion system in the step 3, fully stirring for 1.5h at the rotating speed of 1000r/min to obtain nano SiO 2 Acrylic emulsion.
Step 5: adopting a roller coating process to prepare the nano SiO prepared in the step 4 2 Acrylic emulsion is coated on a release PET film,drying at 80 deg.c to obtain dry film thickness of 35 microns.
Step 6: PET coated with acrylate adhesive and SiO coated with nanometer 2 The release PET film of the acrylic emulsion is placed in the temperature of 80 ℃ for 6min, and after drying and solidification, the acrylic ester adhesive surface and the nano SiO are carried out through a rubber roller 2 Acrylic emulsion level press-fit, roller pressure of 5kg/cm 2 When in use, the release PET film is uncovered to obtain the hydrophobic acrylic ester coating.
Comparative example 5:
a hydrophobic acrylate coating prepared by the steps of:
step 1: 90 parts of acrylate adhesive and 1 part of isocyanate curing agent are mixed, and mechanically stirred for 30min at the rotating speed of 800r/min.
Step 2, coating the acrylic ester adhesive prepared in the step 1 on a PET substrate by adopting a roller coating process, and drying at 80 ℃ to obtain a dry film with the thickness of 10 mu m;
step 3: 2 parts of polytetrafluoroethylene micro powder wax is added into 20 parts of absolute ethyl alcohol, and after stirring for 2 hours at a high speed, ultrasonic dispersion is used for 30 minutes.
Step 4: and (3) adding 100 parts of acrylic emulsion and 2 parts of sodium polyacrylate into the dispersion system in the step (3), and fully stirring for 1.5h at the rotating speed of 1000r/min to obtain the acrylic emulsion.
Step 5: and (3) coating the acrylic emulsion prepared in the step (4) on a release PET film by adopting a roller coating process, and drying at 80 ℃ to obtain a dry film with the thickness of 35 mu m.
Step 6: placing PET coated with acrylate adhesive and release PET film coated with acrylic emulsion at 80deg.C for 6min, drying, solidifying, and pressing acrylate adhesive surface with acrylic emulsion liquid surface by rubber roller with pressure of 5kg/cm 2 When in use, the release PET film is uncovered to obtain the hydrophobic acrylic ester coating.
The coatings prepared by using the example 1 and the example 2 as raw materials and adopting the same roller coating process for coating and transfer printing and laminating after drying and curing are tested to have corresponding water contact angles of 111.5 degrees and 109.6 degrees respectively, as shown in fig. 1 and 2. Comparative example1 is a coating prepared by the same raw material adding proportion as in example 1, but using different preparation processes, and the corresponding water contact angles are respectively 95.5 degrees, as shown in fig. 3. Comparative example 2 was a coating using an acrylic emulsion, which was coated using the same roll coating process as in example 1, and was transferred and attached to the prepared coating after drying and curing, and the corresponding water contact angles were measured to be 92.9 °, respectively, as shown in fig. 4. Comparative example 3 is a coating prepared by the same process as example 1 without the addition of polytetrafluoroethylene micropowder, and has a corresponding water contact angle of 105.5 ° as shown in fig. 5. Comparative example 4 is a coating prepared using the same process as example 1, without the addition of perfluorooctyltriethoxysilane and gamma-aminopropyltriethoxysilane, and tested for a water contact angle of 102.3 °, see figure 6. Comparative example 5 Using the same procedure as in example 1, without the addition of perfluorooctyl triethoxysilane, gamma-aminopropyl triethoxysilane and nano SiO 2 The corresponding water contact angle was measured to be 97.9 deg. for the coating prepared under the conditions of (a) and see figure 7.
The results show that the method for improving the hydrophobicity of the aqueous acrylic ester provided by the invention is simple in process, and the obtained coating has a flat and smooth surface, lower surface energy and better hydrophobicity than the traditional aqueous acrylic acid coating.
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention.
Claims (10)
1. A preparation method of a hydrophobic acrylate coating is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1: preparing a mixture of an acrylic adhesive and a curing agent;
step 2: coating a mixture of an acrylic adhesive and a curing agent on a PET substrate by adopting a roller coating process, and drying;
step 3: preparation of fluorine-silicon modified nano SiO 2 ；
Step 4: preparation of fluorine-silicon modified nano SiO 2 Acrylic emulsion;
step 5: adopting roller coating technology to modify fluorine-silicon into nano SiO 2 Coating acrylic emulsion on a release PET film, and drying;
step 6: the PET substrate coated with the acrylic adhesive obtained in the step 2 and the fluorosilicone modified nano SiO coated obtained in the step 5 are subjected to the following steps of 2 And (3) drying and curing the release PET film of the acrylic emulsion, pressing the two-sided coating by using a rubber roller, and uncovering the release PET film when in use to obtain the hydrophobic acrylate coating.
2. The method of manufacturing according to claim 1, wherein: in the step 1, the acrylic acid ester adhesive is solvent acrylic acid ester adhesive, the solvent is ethyl acetate, the solid content is 44+/-2%, and the viscosity is 3000-6000 cP.s.
3. The method of manufacturing according to claim 1, wherein: in step 1, the curing agent is an isocyanate curing agent.
4. A method of preparation as claimed in claim 3, wherein: the step 1 is implemented as follows: mixing 90-110 parts of acrylate adhesive with 0.9-1.3 parts of isocyanate curing agent, and mechanically stirring for 30-50 min at the rotating speed of 600-800 r/min.
5. The method of manufacturing according to claim 1, wherein: in step 3, the fluorosilicone modified nano SiO 2 The preparation method comprises the following steps:
2 to 4 parts of perfluoro octyl triethoxysilane and 1 to 3 parts of gamma-aminopropyl triethoxysilane are added into 20 to 35 parts of absolute ethyl alcohol, and after being mechanically stirred uniformly, 1 to 2 parts of nano-grade SiO is added 2 And 2-5 parts of polytetrafluoroethylene micro powder wax, and dispersing for 30-50 min by using ultrasonic after stirring for 2-3 h at high speed to obtain the fluorine-silicon modified nano SiO 2 。
6. The method of manufacturing according to claim 5, wherein: the nano-scale SiO 2 The grain diameter of the polytetrafluoroethylene micro powder wax is 200-300 nm, and the grain diameter of the polytetrafluoroethylene micro powder wax is 5.0-6.0 mu m.
7. The method of manufacturing according to claim 1, wherein: in step 4, the fluorosilicone modified nano SiO 2 The acrylic emulsion is prepared by the following process:
adding 100-120 parts of acrylic ester emulsion and 2-5 parts of sodium polyacrylate into the dispersion system in the step 3, fully stirring for 1.5-2 hours at the rotating speed of 800-1200 r/min to obtain the fluorosilicone modified nano SiO 2 Acrylic emulsion.
8. The method of manufacturing according to claim 1, wherein: in the step 4, the solid content of the aqueous acrylic emulsion is 40-50%, the viscosity is 4000-8000 cP.s, and the glass transition temperature is 50-65 ℃.
9. The method of manufacturing according to claim 1, wherein: in the step 2, a roller coating process is adopted, the acrylic ester adhesive prepared in the step 1 is coated on the PET substrate, and the dry film thickness is 10-15 mu m; in the step 5, the fluorosilicone modified nano SiO prepared in the step 4 is prepared by adopting a roller coating process 2 The acrylic emulsion is coated on a release PET film, and the dry film thickness is 30-50 mu m.
10. The method of manufacturing according to claim 1, wherein: in step 6, PET coated with acrylate adhesive and nano SiO coated with fluorine-silicon modification are processed 2 Drying and curing the release PET film of the acrylic emulsion at the temperature of between 60 and 90 ℃ for 5 to 10 minutes, and then mixing the acrylate adhesive surface with the fluorosilicone modified nano SiO through a rubber roller 2 And (3) pressing the acrylic emulsion surface, and uncovering the release PET film when in use to obtain the hydrophobic acrylic ester coating.
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| US20070248810A1 (en) * | 2006-04-25 | 2007-10-25 | Mcgee Dennis E | Coated polymeric film |
| CN103626911A (en) * | 2013-10-14 | 2014-03-12 | 杭州师范大学 | Hydrophobic organic and inorganic acrylate polymer emulsion with high silicon content and preparation method and application thereof |
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| CN111944087A (en) * | 2020-07-22 | 2020-11-17 | 广州工程技术职业学院 | Fluorosilicone hybrid water-based acrylate emulsion and preparation method and application thereof |
| CN114133817A (en) * | 2021-12-15 | 2022-03-04 | 重庆大学 | Firm and transparent super-hydrophobic coating and preparation method thereof |
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| US20070248810A1 (en) * | 2006-04-25 | 2007-10-25 | Mcgee Dennis E | Coated polymeric film |
| CN103626911A (en) * | 2013-10-14 | 2014-03-12 | 杭州师范大学 | Hydrophobic organic and inorganic acrylate polymer emulsion with high silicon content and preparation method and application thereof |
| CN106024994A (en) * | 2016-07-29 | 2016-10-12 | 无锡中洁能源技术有限公司 | Production technology of solar backboard easy to clean |
| CN111944087A (en) * | 2020-07-22 | 2020-11-17 | 广州工程技术职业学院 | Fluorosilicone hybrid water-based acrylate emulsion and preparation method and application thereof |
| CN114133817A (en) * | 2021-12-15 | 2022-03-04 | 重庆大学 | Firm and transparent super-hydrophobic coating and preparation method thereof |
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