CN116694210A - Coating, preparation method and application thereof - Google Patents
Coating, preparation method and application thereof Download PDFInfo
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- CN116694210A CN116694210A CN202310625192.4A CN202310625192A CN116694210A CN 116694210 A CN116694210 A CN 116694210A CN 202310625192 A CN202310625192 A CN 202310625192A CN 116694210 A CN116694210 A CN 116694210A
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- China
- Prior art keywords
- coating
- parts
- microcapsule
- membrane body
- hollow part
- Prior art date
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- 239000011248 coating agent Substances 0.000 title claims abstract description 90
- 238000000576 coating method Methods 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003094 microcapsule Substances 0.000 claims abstract description 70
- 239000012528 membrane Substances 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 229920002635 polyurethane Polymers 0.000 claims abstract description 28
- 239000004814 polyurethane Substances 0.000 claims abstract description 28
- 229920006150 hyperbranched polyester Polymers 0.000 claims abstract description 24
- 239000003973 paint Substances 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 14
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 14
- 239000004480 active ingredient Substances 0.000 claims abstract description 10
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 10
- 239000011550 stock solution Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000013007 heat curing Methods 0.000 claims description 24
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 22
- 239000002270 dispersing agent Substances 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 17
- 229920000178 Acrylic resin Polymers 0.000 claims description 15
- 239000004925 Acrylic resin Substances 0.000 claims description 15
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 12
- 239000000194 fatty acid Substances 0.000 claims description 12
- 229930195729 fatty acid Natural products 0.000 claims description 12
- 150000004665 fatty acids Chemical group 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 229920006294 polydialkylsiloxane Polymers 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 5
- 229920000058 polyacrylate Polymers 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 27
- 238000002156 mixing Methods 0.000 description 21
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229920001187 thermosetting polymer Polymers 0.000 description 5
- 238000001723 curing Methods 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000000750 progressive effect Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000001029 thermal curing Methods 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 150000008054 sulfonate salts Chemical class 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 230000016776 visual perception Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a coating, a preparation method and application thereof; the paint comprises the following active ingredients in parts by weight: 25-50 parts of polyurethane; 10-25 parts of aliphatic dibasic acid; 10-30 parts of hyperbranched polyester; 20-40 parts of microcapsule; the microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 20-40% of the total volume in the membrane body; the preparation method of the coating comprises the following steps of: dispersing the inner liquid, adding the membrane stock solution, stirring or ultrasonic homogenizing, performing polymerization reaction, and introducing gas to obtain microcapsule; the coating has parts with different refractive indexes, so that the surface of the material has matte texture, and the light reflection of the material is improved.
Description
Technical Field
The invention relates to a coating, a preparation method and application thereof, and belongs to the technical field of functional reagents.
Background
The surfaces of different materials have different visual characteristics, such as metal, the surfaces are smooth and not easy to absorb light, most of the light can be reflected back, and therefore, the reflectivity of the metal is very high, so that the metal has high light reflection and luster. The metal surface can also greatly enhance the intensity of reflected light, and has the characteristic of complete reflection, which is much greater than the intensity of light reflected by a flat object. Therefore, the reflection effect of the metal surface is more obvious and more glaring. In some applications, the reflection of light from the surface of the object is too large and is easily visually noticeable and affected, for example, by strong glare, which greatly reduces the perceived comfort of the object. The conventional way to change the surface characteristics is to add a coating on the surface of a material, and the visual perception of the material is changed through the coating, so that the durability and the protection are improved, and a great room for improvement exists for the coating agent in the aspect.
Disclosure of Invention
In order to overcome the defects in the prior art, a first object of the invention is to provide a coating, which has parts with different refractive indexes, so that the surface of a material has a matt texture, and the light reflection of the material is improved.
A second object of the present invention is to provide a method for preparing the above coating to form a coating comprising a specific microcapsule structure.
The third object of the present invention is to provide an application of the above coating, which is a thermal curing method of the coating, and the progressive thermal curing method can enable the interior of the coating to form spaces with different refractive indexes, reduce the reflection on the surface of the material, and has good transparency and good diffuse reflection effect.
The first object of the invention can be achieved by adopting the following technical scheme: the paint comprises the following active ingredients in parts by weight:
the microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 20-40% of the total volume in the membrane body.
Further, the polyurethane is a sulfonate polyurethane.
Further, the hyperbranched polyester is a hyperbranched polyester modified with fatty acids.
Further, the particle size of the microcapsule is 10-40nm.
Further, the film body is prepared from at least one of tetraethoxysilane, tetramethoxysilane and polydialkylsiloxane.
Further, the internal liquid is at least one of polyacrylate, methyl methacrylate and ethyl methacrylate.
Further, the coating also includes an acrylic resin.
Further, the acrylic resin is a hydroxy acrylic resin.
The second object of the invention can be achieved by adopting the following technical scheme: a method for preparing a coating, the coating comprising microcapsules; the microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 20-40% of the total volume in the membrane body; the preparation method comprises the following steps of: dispersing the inner liquid, adding the membrane stock solution, stirring or ultrasonic homogenizing, performing polymerization reaction, and introducing gas to obtain microcapsule;
or adding the internal solution into a dispersing agent to disperse so as to obtain a dispersing solution; adding the polymerized film into the dispersion liquid to make the dispersion liquid absorbed into the film, and then removing the dispersing agent in the film to form hollow part to obtain the microcapsule.
Further, adding the internal solution into a dispersing agent for dispersing to obtain a dispersing solution; and adding the film stock solution into the dispersion liquid to perform polymerization reaction, and then removing the dispersing agent in the film to form hollow parts to obtain the microcapsule.
The third object of the invention can be achieved by adopting the following technical scheme: the application of the coating comprises the steps of performing primary heat curing at 55-80 ℃ for 2-8min after the coating is coated; then performing secondary heat curing at 90-150 ℃ for 30-60 min; the paint comprises the following active ingredients in parts by weight: 25-50 parts of polyurethane; 10-25 parts of aliphatic dibasic acid; 10-30 parts of hyperbranched polyester; 20-40 parts of microcapsule; the microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 20-40% of the total volume in the membrane body.
Further, after the coating is coated, performing primary heat curing under the conditions of 55-80 ℃ and 2-8 min; performing secondary heat curing at 90-150 ℃ for 30-60 min; and performing three times of heat curing at the temperature of 150-180 ℃ for 1-10 min.
Compared with the prior art, the invention has the beneficial effects that:
1. the coating provided by the invention has the matte texture on the surface of the material, improves the light reflection of the material, and is not easy to see even if scratches exist;
2. the coating can be used for various materials such as glass, wood, metal and the like;
3. the coating disclosed by the invention has the advantages of good flatness, smooth surface and good transparency, and the microcapsules are uniformly distributed in the formed coating;
4. the preparation method of the coating provides a mode of forming the coating containing a specific microcapsule structure;
5. the mode of film formation of the coating disclosed by the invention is progressive heat curing, so that spaces with different refractive indexes are formed in the coating, and the reflection of the surface of a material is reduced.
Drawings
FIG. 1 is a schematic illustration of example 1 prior to surface coating of a material;
FIG. 2 shows the material of example 1 after surface coating;
FIG. 3 is a schematic illustration of the material of example 2 prior to surface coating;
FIG. 4 shows the material of example 2 after surface coating.
Detailed Description
The invention will be further described with reference to the accompanying drawings and detailed description below:
the paint comprises the following active ingredients in parts by weight:
the sulfonate polyurethane can still have good stability under a wider pH environment, and has high bonding strength, water resistance and heat resistance.
Aliphatic dibasic acids are used to control the coating Tg.
The hyperbranched polyester is beneficial to the dispersion of the microcapsules and stabilizes the uniform distribution of the microcapsules in the coating, and simultaneously, the coating is easier to thermoset and form a film; the hyperbranched polyester has a highly branched structure, a large number of end functional groups are well connected with the sulfonate polyurethane and the film body, and the hyperbranched polyester and the sulfonate polyurethane form a combined structure and fix the microcapsule in the combined structure; when the coating is coated, the microcapsule is positioned in the coating and does not float on the surface, the smoothness of the surface of the cured and molded coating is not affected, and the smoothness of the surface of the coating is good.
The microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 20-40% of the total volume in the membrane body; the particle size of the microcapsule is 10-40nm; when the coating is thermally cured, the gas in the hollow part expands, and meanwhile, the initial curing of the sulfonate polyurethane and the expansion of the film body increase the density of the outer part of the microcapsule, the refractive indexes of the hollow part and the inner liquid are about 1 and 1.4 respectively, the refractive indexes of the sulfonate polyurethane and the hyperbranched polyester are about 1.5-1.7 respectively in the finally formed coating film, and the inner part and the outer part of the microcapsule form different refractive index parts to absorb and reflect light with different wavelengths respectively, so that the diffuse reflection of the coating is increased, and the reflection of the surface of the material is greatly weakened. In addition, the microcapsules also help to increase the light transmittance of the coating.
Wherein, tetraethoxysilane (TEOS), tetramethoxysilane (TMOS) or Polydialkylsiloxane (PDMS) are used as components of the film body; the internal liquid is at least one of polyacrylate, methyl methacrylate and ethyl methacrylate.
After solidification, the hardness of the film body is slightly higher than that of polyurethane and hyperbranched polyester, and the film body is used as a support in the formed coating film, so that the surface of the coating film attaching material is maintained, and the film body is not easy to deform and fall off.
The hydroxyl acrylic resin is used for diluting sulfonate polyurethane, the sulfonate polyurethane has higher viscosity, and the dilution before thermosetting is beneficial to improving the uniformity of components in the coating, particularly the uniformity of microcapsules, and enhancing the flexibility of the whole coating.
The preparation method of the coating comprises the following steps:
the preparation steps of the microcapsule comprise: the microcapsules are prepared by a process of one of the following:
1) Dispersing the inner liquid, adding the membrane stock solution, stirring or ultrasonic homogenizing, performing polymerization reaction, and introducing gas to obtain microcapsule;
2) Adding the internal solution into a dispersing agent for dispersing to obtain a dispersing solution; adding the polymerized film into the dispersion liquid, carrying out ultrasonic or high-speed stirring to enable the dispersion liquid to be absorbed into the film, removing the dispersing agent in the film and replacing the dispersing agent with gas to form a hollow part, thus obtaining the microcapsule;
3) Adding the internal solution into a dispersing agent for dispersing to obtain a dispersing solution; adding the film stock solution into the dispersion liquid for polymerization reaction, removing the dispersing agent in the film and replacing the dispersing agent with gas to form a hollow part, thus obtaining the microcapsule. Wherein the gas is air or carbon dioxide.
The dispersant is a reagent with a dissolution rate of less than or equal to 10% v/v with the internal liquid, and the dispersant in the specific embodiment can be water. The method for removing the dispersing agent in the membrane body can be a decompression drying method (the pressure is lower than 300Pa, the temperature is 20-40 ℃ and the time is 30min-1 h), a centrifugal separation method (the centrifugal separation is carried out in a centrifugal machine at 1500rpm for 2-3 min), an ultrafiltration method or an evaporation method, and the dispersing agent can be effectively removed to form a hollow part with the total volume of 20-40 percent.
Mixing: mixing sulfonate polyurethane, aliphatic dibasic acid and hydroxy acrylic resin, adding the microcapsule for mixing, and finally adding fatty acid modified hyperbranched polyester, and uniformly mixing to obtain the coating.
Diluting sulfonate polyurethane and aliphatic dibasic acid with hydroxy acrylic resin, mixing the microcapsules, and finally adding fatty acid modified hyperbranched polyester to connect the sulfonate polyurethane and the microcapsule membrane.
The application mode of the coating is that the coating is coated on the surface of a material to reduce strong reflection on the surface, the surface appearance is softer and the tolerance of the material is improved; the coating is covered on the surface of the material in a thermosetting way, and the thermosetting process is as follows: after the paint is coated on the surface of the material, performing primary heat curing under the conditions that the temperature is 55-80 ℃ and the time is 2-8 min; then performing secondary heat curing at 90-150 ℃ for 30-60 min; and performing three times of heat curing at the temperature of 150-180 ℃ for 1-10 min.
The heat curing adopts a three-time heating mode, the internal liquid and sulfonate polyurethane begin to cure at the first heat curing temperature, the gas in the hollow part of the microcapsule is heated and expanded to expand the film body, and an air bag is formed in the coating, and the expansion amplitude is 10-25% of the volume of the coating observed by a scanning electron microscope; the flexibility of tetraethoxysilane, tetramethoxysilane and polydialkylsiloxane film body can meet the volume expansion of 10-25% of the hollow part, and still can well wrap the inner liquid and the hollow part, and the complete structure is maintained in the formed coating film; because of the primary solidification of sulfonate polyurethane, a frame of a coating film is formed, deformation is not easy to occur, and the coating film can be attached to the surface of a material; the second curing is mainly the primary curing of sulfonate polyurethane and hyperbranched polyester; the third cure is the cure of the hyperbranched polyester. The progressive thermosetting mode can prevent the viscosity of the paint from growing too fast and cause more side reactions; more importantly, the coating can form spaces with different refractive indexes inside, so that the reflection on the surface of the material is reduced, and the coating has good transparency and good diffuse reflection effect.
Example 1:
a paint comprising the active ingredients in parts by weight as shown in table 1:
table 1 example 1 parts by weight of ingredients
| Composition of the components | Parts by weight of |
| Sulfonate polyurethanes | 30 parts of |
| Aliphatic dibasic acid | 15 parts of |
| Fatty acid modified hyperbranched polyesters | 25 parts of |
| Microcapsule | 35 parts of |
| Hydroxy acrylic resin | 10 parts of |
The preparation of the coating comprises the following steps:
the preparation steps of the microcapsule comprise: dispersing polyacrylate as internal liquid with water, adding polydialkylsiloxane, stirring or ultrasonic homogenizing, performing polymerization reaction, and introducing air to obtain microcapsule; the microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 33% of the total volume in the membrane body; the average particle diameter of the microcapsule is 25nm;
mixing: mixing sulfonate polyurethane, aliphatic dibasic acid and hydroxy acrylic resin, adding the microcapsule for mixing, and finally adding fatty acid modified hyperbranched polyester, and uniformly mixing to obtain the coating.
Coating the paint on the surface of a wood material, and performing primary heat curing under the conditions of 65 ℃ and 6 min; then performing secondary heat curing under the conditions of 95 ℃ and 34 min; performing three times of heat curing under the conditions of 160 ℃ and 2 min; the thickness of the film was 10. Mu.m, and the boundary of the microcapsule film was found, and the average particle diameter was 30nm. Fig. 1 and 2 are pictures before and after coating the surface of the material, respectively.
Example 2:
a coating comprising the active ingredients in parts by weight as shown in table 2:
table 2 example 2 weight parts of ingredients
| Composition of the components | Parts by weight of |
| Sulfonate polyurethanes | 30 parts of |
| Aliphatic dibasic acid | 15 parts of |
| Fatty acid modified hyperbranched polyesters | 25 parts of |
| Microcapsule | 35 parts of |
| Hydroxy acrylic resin | 10 parts of |
The preparation of the coating comprises the following steps:
the preparation steps of the microcapsule comprise: methyl methacrylate is used as an internal liquid, water is used for dispersing, polydialkylsiloxane is added, polymerization reaction is carried out after stirring or ultrasonic homogenization, and air is introduced at the same time, so that a microcapsule is obtained; the microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 35 percent of the total volume in the membrane body; the average particle diameter of the microcapsule is 32nm;
mixing: mixing sulfonate polyurethane, aliphatic dibasic acid and hydroxy acrylic resin, adding the microcapsule for mixing, and finally adding fatty acid modified hyperbranched polyester, and uniformly mixing to obtain the coating.
Coating the paint on the surface of an aluminum alloy material, and performing primary heat curing under the conditions of the temperature of 75 ℃ and the time of 6 min; then performing secondary heat curing under the conditions of 110 ℃ and 42 min; performing three times of heat curing under the conditions of 172 ℃ and 5 min; the thickness of the film was 12. Mu.m, and the boundary of the microcapsule film was found, and the average particle diameter was 38.5nm. Fig. 3 and 4 are pictures before and after coating the surface of the material, respectively.
Example 3:
a paint comprising the active ingredients in parts by weight as shown in table 3:
table 3 example 3 parts by weight of ingredients
| Composition of the components | Parts by weight of |
| Sulfonate polyurethanes | 45 parts of |
| Aliphatic dibasic acid | 20 parts of |
| Fatty acid modified hyperbranched polyesters | 15 parts of |
| Microcapsule | 25 parts of |
| Hydroxy acrylic resin | 8 parts of |
The preparation of the coating comprises the following steps:
the preparation steps of the microcapsule comprise: methyl methacrylate is used as an internal solution, and water is used for dispersing to obtain a dispersion liquid; adding polymerized polydialkylsiloxane film into the dispersion, ultrasonic or high-speed stirring to make the dispersion absorbed into the film, drying under reduced pressure (pressure below 300Pa, 30deg.C, 1 h) to remove dispersant in the film, and displacing with air to form hollow part to obtain microcapsule; the hollow part accounts for 25 percent of the total volume in the membrane body; the average particle diameter of the microcapsule is 18nm;
mixing: mixing sulfonate polyurethane, aliphatic dibasic acid and hydroxy acrylic resin, adding the microcapsule for mixing, and finally adding fatty acid modified hyperbranched polyester, and uniformly mixing to obtain the coating.
Coating the paint on the surface of a metal material, and performing primary heat curing under the conditions of 65 ℃ and 3 min; then performing secondary heat curing under the conditions of 140 ℃ and 35 min; performing three times of heat curing under the conditions of 166 ℃ and 8 min; the thickness of the film was 16. Mu.m, and the boundary of the microcapsule film was found, and the average particle diameter was 20nm.
Example 4:
a paint comprising the active ingredients in parts by weight as shown in table 4:
table 4 example 4 parts by weight of ingredients
| Composition of the components | Parts by weight of |
| Sulfonate salt polymerizationAmmonia esters | 36 parts of |
| Aliphatic dibasic acid | 21 parts of |
| Fatty acid modified hyperbranched polyesters | 26 parts of |
| Microcapsule | 33 parts of |
| Hydroxy acrylic resin | 14 parts of |
The preparation of the coating comprises the following steps:
the preparation steps of the microcapsule comprise: dispersing polyacrylate serving as an internal solution by using water to obtain a dispersion; adding tetraethoxysilane into the dispersion liquid for polymerization reaction, and then removing the dispersing agent in the membrane body by a centrifugal separation method (centrifugal separation in a centrifugal machine of 1500rpm for 2.5 min) and replacing the dispersing agent with air to form a hollow part to obtain a microcapsule; the hollow part accounts for 28 percent of the total volume in the membrane body; the average particle diameter of the microcapsules is 33nm;
mixing: mixing sulfonate polyurethane, aliphatic dibasic acid and hydroxy acrylic resin, adding the microcapsule for mixing, and finally adding fatty acid modified hyperbranched polyester, and uniformly mixing to obtain the coating.
Coating the paint on the surface of a metal material, and performing primary heat curing under the conditions of the temperature of 70 ℃ and the time of 7 min; then performing secondary heat curing under the conditions of 100 ℃ and 55 min; performing three times of heat curing under the conditions of 160 ℃ and 9 min; the thickness of the film was 20. Mu.m, and the boundary of the microcapsule film was found, and the average particle diameter was 40nm.
Comparative example:
no microcapsules were added to the coating and the remaining parameters and features were the same as in example 2.
And (3) detection:
transmittance: coating borosilicate glass on two surfaces of the paint obtained in the examples 1-4, and detecting light transmittance after curing;
hardness: detecting according to GB/T6739-2006 standard;
abrasion resistance: detecting according to GB/T23988-2009 standard;
adhesion force: detection is carried out according to the GB/T9286-1998 standard;
impact-resistant: detecting according to GB/T1732-1993 standard;
flexibility: the detection is carried out according to the GB/T1731-1993 standard.
The results are shown in Table 5:
table 5 the results of the tests of examples 1-4 and comparative example
| Project | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| Transmittance (%) | 98.3 | 98.1 | 97.4 | 97.6 | 93.3 |
| Hardness of | 8H | 8H | 7H | 7H | 5H |
| Wear resistance (L/mum) | 1410 | 1382 | 1310 | 1350 | 1050 |
| Adhesion (grade) | 0 | 0 | 0 | 0 | 1 |
| Impact-resistant | Qualified product | Qualified product | Qualified product | Qualified product | Qualified product |
| Flexibility of the product | Qualified product | Qualified product | Qualified product | Qualified product | Qualified product |
| Diffuse reflectance(％) | 98 | 97.6 | 96.4 | 97.7 | 83.2 |
Various other corresponding changes and modifications will occur to those skilled in the art from the foregoing description and the accompanying drawings, and all such changes and modifications are intended to be included within the scope of the present invention as defined in the appended claims.
Claims (10)
1. The paint is characterized by comprising the following active ingredients in parts by weight:
the microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 20-40% of the total volume in the membrane body.
2. The coating of claim 1 wherein the polyurethane is a sulfonate polyurethane.
3. The coating of claim 1, wherein the hyperbranched polyester is a hyperbranched polyester modified with fatty acids.
4. The coating of claim 1, wherein the microcapsules have a particle size of 10 to 40nm.
5. The coating of claim 1, wherein the film body is prepared from at least one of tetraethoxysilane, tetramethoxysilane, and polydialkylsiloxane.
6. The coating of claim 1, wherein the internal fluid is at least one of polyacrylate, methyl methacrylate, and ethyl methacrylate.
7. The coating of claim 1, wherein the coating further comprises an acrylic resin.
8. A method of preparing a coating, wherein the coating comprises microcapsules; the microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 20-40% of the total volume in the membrane body; the preparation method comprises the following steps of: dispersing the inner liquid, adding the membrane stock solution, stirring or ultrasonic homogenizing, performing polymerization reaction, and introducing gas to obtain microcapsule;
or adding the internal solution into a dispersing agent to disperse so as to obtain a dispersing solution; adding the polymerized film into the dispersion liquid to make the dispersion liquid absorbed into the film, and then removing the dispersing agent in the film to form hollow part to obtain the microcapsule.
9. The method for preparing the coating according to claim 8, wherein the internal liquid is added into a dispersing agent for dispersion to obtain a dispersion; and adding the film stock solution into the dispersion liquid to perform polymerization reaction, and then removing the dispersing agent in the film to form hollow parts to obtain the microcapsule.
10. The application of the coating is characterized in that after the coating is coated, the coating is thermally cured for one time under the conditions that the temperature is 55-80 ℃ and the time is 2-8 min; then performing secondary heat curing at 90-150 ℃ for 30-60 min; the paint comprises the following active ingredients in parts by weight: 25-50 parts of polyurethane; 10-25 parts of aliphatic dibasic acid; 10-30 parts of hyperbranched polyester; 20-40 parts of microcapsule; the microcapsule comprises a membrane body, and inner liquid and a hollow part which are coated in the membrane body; the hollow part accounts for 20-40% of the total volume in the membrane body.
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| JP2002296410A (en) * | 2001-03-29 | 2002-10-09 | Kazunari Jinguji | Retroreflective microcapsule and retroreflective composition mixed with the same |
| CN101037563A (en) * | 2007-03-30 | 2007-09-19 | 德谦（上海）化学有限公司 | Resin for super branched polyester modified coating |
| US20070251422A1 (en) * | 2004-04-05 | 2007-11-01 | Hiroshi Maenaka | Hollow Resin Fine Particles, Organic/Inorganic Hybrid Fine Particles, and Method for Producing Hollow Resin Fine Particles |
| US20160025905A1 (en) * | 2014-06-13 | 2016-01-28 | Whiteoptics Llc | Low Refractive Index Coating With Fluroelastomer Encapsulated Glass Bubbles |
| TW201734056A (en) * | 2016-03-22 | 2017-10-01 | 積水化成品工業股份有限公司 | Hollow particle and use thereof |
| CN109776837A (en) * | 2018-12-18 | 2019-05-21 | 合肥乐凯科技产业有限公司 | A kind of anti-blue light protective film |
| WO2022012181A1 (en) * | 2020-07-14 | 2022-01-20 | 华南师范大学 | Color-changeable reflective paint, preparation method therefor, and application thereof |
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2023
- 2023-05-30 CN CN202310625192.4A patent/CN116694210A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002296410A (en) * | 2001-03-29 | 2002-10-09 | Kazunari Jinguji | Retroreflective microcapsule and retroreflective composition mixed with the same |
| US20070251422A1 (en) * | 2004-04-05 | 2007-11-01 | Hiroshi Maenaka | Hollow Resin Fine Particles, Organic/Inorganic Hybrid Fine Particles, and Method for Producing Hollow Resin Fine Particles |
| CN101037563A (en) * | 2007-03-30 | 2007-09-19 | 德谦（上海）化学有限公司 | Resin for super branched polyester modified coating |
| US20160025905A1 (en) * | 2014-06-13 | 2016-01-28 | Whiteoptics Llc | Low Refractive Index Coating With Fluroelastomer Encapsulated Glass Bubbles |
| TW201734056A (en) * | 2016-03-22 | 2017-10-01 | 積水化成品工業股份有限公司 | Hollow particle and use thereof |
| CN109776837A (en) * | 2018-12-18 | 2019-05-21 | 合肥乐凯科技产业有限公司 | A kind of anti-blue light protective film |
| WO2022012181A1 (en) * | 2020-07-14 | 2022-01-20 | 华南师范大学 | Color-changeable reflective paint, preparation method therefor, and application thereof |
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