CN117965088A - Nanometer matt paint for wood floor and preparation method thereof - Google Patents
Nanometer matt paint for wood floor and preparation method thereof Download PDFInfo
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- 239000003973 paint Substances 0.000 title claims abstract description 55
- 239000002023 wood Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 8
- -1 hydroxypropyl Chemical group 0.000 claims abstract description 53
- 239000002562 thickening agent Substances 0.000 claims abstract description 40
- 229920005989 resin Polymers 0.000 claims abstract description 38
- 239000011347 resin Substances 0.000 claims abstract description 38
- 230000008033 biological extinction Effects 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 27
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- 239000002270 dispersing agent Substances 0.000 claims abstract description 21
- 239000000080 wetting agent Substances 0.000 claims abstract description 16
- 229920001661 Chitosan Polymers 0.000 claims abstract description 15
- 239000003822 epoxy resin Substances 0.000 claims abstract description 15
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 11
- 239000013530 defoamer Substances 0.000 claims abstract description 9
- 239000012141 concentrate Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 51
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 30
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 27
- 239000002202 Polyethylene glycol Substances 0.000 claims description 27
- 229920001223 polyethylene glycol Polymers 0.000 claims description 27
- 238000001816 cooling Methods 0.000 claims description 26
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 claims description 22
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 20
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 20
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 20
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- XFGANBYCJWQYBI-UHFFFAOYSA-N 11-bromoundecan-1-ol Chemical compound OCCCCCCCCCCCBr XFGANBYCJWQYBI-UHFFFAOYSA-N 0.000 claims description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 11
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 11
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 11
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 10
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 8
- 239000002518 antifoaming agent Substances 0.000 claims description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- 238000010008 shearing Methods 0.000 claims description 7
- 238000009775 high-speed stirring Methods 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 5
- 150000003863 ammonium salts Chemical class 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 229920002545 silicone oil Polymers 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000000543 intermediate Substances 0.000 claims 8
- 239000007806 chemical reaction intermediate Substances 0.000 claims 1
- 229920000058 polyacrylate Polymers 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 15
- 238000000576 coating method Methods 0.000 abstract description 15
- 239000004814 polyurethane Substances 0.000 abstract description 14
- 229920002635 polyurethane Polymers 0.000 abstract description 13
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical group C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 abstract description 6
- 238000007334 copolymerization reaction Methods 0.000 abstract description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 230000008719 thickening Effects 0.000 abstract description 3
- 238000003848 UV Light-Curing Methods 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000839 emulsion Substances 0.000 description 7
- 229920002125 Sokalan® Polymers 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000001804 emulsifying effect Effects 0.000 description 4
- 239000006224 matting agent Substances 0.000 description 4
- 239000004584 polyacrylic acid Substances 0.000 description 4
- 239000004970 Chain extender Substances 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 239000004005 microsphere Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000006356 dehydrogenation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000008366 benzophenones Chemical class 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009408 flooring Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Abstract
The invention discloses a nano matt paint for a wood floor and a preparation method thereof, wherein the nano matt paint comprises the following raw materials in parts by weight: 60-70 parts of extinction resin, 5-7 parts of thickener, 3-5 parts of handfeel wax powder, 3-5 parts of nano silicon dioxide dispersion liquid, 1-3 parts of aqueous color concentrate, 1-2 parts of wetting agent, 0.5-1 part of defoamer, 1-1.5 parts of dispersing agent and 20-30 parts of deionized water. The extinction resin obtained by using the waterborne polyurethane with the epoxy resin modified terminal hydroxypropyl polydimethylsiloxane to participate in copolymerization is used for enhancing the water resistance and extinction property of a matte paint film; the introduction of chitosan ensures that a paint film has good self-repairing performance; the introduction of the acrylate group enables the matt paint to have UV-curable properties. The molecular of the thickener has a benzophenone structure, so that the thickener plays a photoinitiation role while thickening in the matt paint, and after UV curing, the thickener is chemically connected with the extinction resin, so that migration and permeation of the thickener in a cured coating can be effectively reduced.
Description
Technical Field
The invention relates to the field of matt paint, in particular to a nano matt paint for a wood floor and a preparation method thereof.
Background
The aqueous polyurethane (WPU) has the advantages of high film forming strength, good wear resistance, no toxicity, environmental protection and the like, and the low-gloss WPU is attracting attention along with the continuous improvement of aesthetic ideas of people. The traditional low-gloss WPU is prepared by adding a matting agent into Polyurethane (PU) dispersoid, wherein the matting agent floats on the surface of a glue film in the drying process of the glue film, and the microstructure of the surface of the glue film is uneven, so that the aim of matting is achieved, but the introduction of the matting agent is easy to reduce the performances of emulsion such as stability, scratch resistance and the like. The research has been carried out before to find that the novel single-component WPU with extinction performance is obtained without adding the extinction agent, but the water resistance, the thermal stability, the mechanical performance and the like are poor. In order to improve the comprehensive performance and expand the application range of the WPU matting resin, the WPU matting resin must be modified.
The water-based paint needs to be subjected to four processes of preparation, storage, brushing and leveling from preparation to final forming of a decorative paint film, and the paint system needs to have different viscosities at different stages. If in the production process, the coating is required to have certain viscosity, so that liquid splashing caused by high-speed stirring and shearing in the paint preparation process is prevented, and meanwhile, more sufficient dispersion of various auxiliary agents and fillers can be promoted; during the storage period, the coating is required to maintain higher viscosity in a low shear state, so that powder materials in the coating and the like are prevented from being deposited downwards due to the action of gravity to cause layering, and the stability of a coating system is improved; in the coating stage, the coating is required to have certain thixotropic property, and certain low viscosity of the coating is kept under the action of shearing force such as spraying, so that smooth coating is ensured, and good leveling of the coating film on the substrate is ensured; after the coating is leveled, the coating is required to be quickly restored to higher viscosity, so that the coating is prevented from sagging, and no liquid drops are splashed during rolling coating. With the increasing diversification of the current viscosity use requirements of the paint, the existing thickener can not meet the requirements far.
Disclosure of Invention
In order to solve the technical problems, the invention provides a nano matt paint for a wood floor and a preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
the nano matte paint for the wood floor comprises the following raw materials in parts by weight: 60-70 parts of extinction resin, 5-7 parts of thickener, 3-5 parts of handfeel wax powder, 3-5 parts of nano silicon dioxide dispersion liquid, 1-3 parts of aqueous color concentrate, 1-2 parts of wetting agent, 0.5-1 part of defoamer, 1-1.5 parts of dispersing agent and 20-30 parts of deionized water.
The hand feeling wax powder is polytetrafluoroethylene wax powder.
The wetting agent is polyether silicone oil.
The defoamer is polydimethylsiloxane.
The dispersing agent is a polyacrylic acid ammonium salt dispersing agent.
The extinction resin is prepared through the following steps:
Step A1: and drying the terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol for 1h at the temperature of 100 ℃ in vacuum for later use. Adding terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol into a flask provided with a thermometer, a stirrer and a condenser tube, heating to 90 ℃, adding toluene diisocyanate and catalyst dibutyl tin dilaurate under stirring, reacting at constant temperature for 4 hours, cooling to 50 ℃, adding 2, 2-dimethylolpropionic acid and tetrahydrofuran into the flask, reacting at constant temperature for 2 hours after heating to 70 ℃, cooling to room temperature to obtain an intermediate 1, wherein the dosage ratio of the terminal hydroxypropyl polydimethylsiloxane, the polyethylene glycol, the toluene diisocyanate and the dibutyl tin dilaurate is 0.3 mol:0.1-0.12 mol:0.0015 mol:0.002-0.003 mol:250-300 mL;
In the reaction process, hydroxyl groups of terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol react with isocyanate groups of toluene diisocyanate respectively, and 2, 2-dimethylolpropionic acid is used as a hydrophilic chain extender to react with the isocyanate groups to generate an intermediate 1, wherein the structure of the intermediate 1 is shown as follows:
Step A2: under the protection of nitrogen, bisphenol A type epoxy resin E-12 is added into toluene, stirring is started, intermediate 1 is slowly added into the mixture, the reaction is continued for 1 to 1.5 hours at the temperature of 70 to 80 ℃, the reaction liquid is obtained after the temperature of the system is reduced to room temperature, the reaction liquid is poured into an emulsifying barrel, triethylamine and deionized water are added, intermediate 2 is prepared under high-speed stirring and shearing, and the dosage ratio of bisphenol A type epoxy resin E-12, toluene, intermediate 1, triethylamine and deionized water is as follows: 0.1-0.13 g:70 mL:2-2.5 g:0.08 g:60 mL;
In the reaction process, epoxy groups and secondary hydroxyl groups in bisphenol A epoxy resin E-12 react with isocyanate groups in an intermediate 1 respectively to generate a cross-linking structure, and triethylamine neutralizes carboxyl groups introduced by a hydrophilic chain extender 2, 2-dimethylolpropionic acid to obtain an intermediate 2, wherein the structure of the intermediate 2 is shown as follows:
Step A3: adding chitosan and diethylamine into the intermediate 2, stirring at 600r/min and 60 ℃ for reaction for 5-6 hours, cooling to 40 ℃, adding pentaerythritol triacrylate, stirring for reaction for 3-4 hours to obtain extinction resin, wherein the dosage ratio of the intermediate 2 to the chitosan to the diethylamine to the pentaerythritol triacrylate is 2.6-3.0 g:0.2-0.3 g:0.5-0.6 g:0.33-0.40 g;
In the reaction process, hydroxyl and amino of chitosan respectively react with isocyanate groups of the intermediate 2, amino of diethylamine reacts with the isocyanate groups of the intermediate 2, and the rest unreacted terminal isocyanate groups react with pentaerythritol triacrylate to obtain the extinction resin. The hydroxypropyl-terminated polydimethylsiloxane contains a silicon-oxygen bond, so that the molecular chain is endowed with excellent flexibility, the silicon-oxygen bond energy is high, the heat resistance is good, the hydroxypropyl-terminated polydimethylsiloxane is introduced into a system in a copolymerization mode, the prepared emulsion is transferred to the surface after film formation, and a micro rough surface is generated, so that the diffuse reflection is enhanced to achieve the extinction effect; the epoxy group and the secondary hydroxyl in the introduced epoxy resin are copolymerized with the waterborne polyurethane to generate a cross-linking structure, a branching point is introduced into a polyurethane main chain, and the introduced benzene ring is of a rigid structure, so that the water resistance of the extinction resin is improved, a regular microsphere type stable emulsion is formed after water is added for emulsification, and after the emulsion is dried to form a film, microspheres with larger particle size are easily displayed on the surface of a film, so that the film is of a micro rough structure, and the extinction resin has excellent extinction property; the chitosan is introduced as a chain extender, so that the extinction resin is endowed with good self-repairing performance; the introduction of the acrylate group enables the extinction resin to have UV-curable performance.
The thickener is prepared through the following steps:
Step B1: adding 2-hydroxy-4-n-octoxybenzophenone, 11-bromo-undecanol, potassium carbonate and DMF into a three-neck flask, stirring and reacting for 12 hours at 80 ℃ under the protection of nitrogen, extracting with dichloromethane, drying, and steaming to obtain an intermediate a, wherein the dosage ratio of the 2-hydroxy-4-n-octoxybenzophenone, the 11-bromo-undecanol, the potassium carbonate and the DMF is 0.15 mol:0.18 mol:0.30 mol:50-60 mL;
In the reaction process, 2-hydroxy-4-n-octoxybenzophenone and 11-bromo-undecanol are subjected to etherification reaction to generate an intermediate a, wherein the structure of the intermediate a is shown as follows:
Step B2: adding polyethylene glycol and toluene into a flask, heating to 130 ℃ under the protection of nitrogen, distilling for 1.5-2h, cooling to 60-70 ℃, adding dibutyl tin dilaurate and isophorone diisocyanate into the flask, stirring at 80 ℃ for reaction for 3.5-4h, adding an intermediate a into the flask, stirring at 85 ℃ for reaction for 16h to obtain a mixed solution, cooling the mixed solution to room temperature, recrystallizing with diethyl ether, filtering, adding dichloromethane into a filter cake, and recrystallizing with diethyl ether to obtain a thickener, wherein the dosage ratio of the polyethylene glycol, the toluene, the dibutyl tin dilaurate, the isophorone diisocyanate and the intermediate a is 0.25 mmol/150 mL/0.01 g/2.5 mmol/5 mmol;
In the reaction process, firstly, after the terminal hydroxyl of polyethylene glycol reacts with the isocyanate group of isophorone diisocyanate, the rest terminal isocyanate group reacts with the hydroxyl of the intermediate a to obtain the thickener. The benzophenone structure is introduced into the molecules of the thickener through reaction, and the introduced benzophenone structure enables the thickener to play a role in photoinitiation while playing a role in thickening, and after UV curing, the thickener can be chemically connected with the extinction resin capable of being cured through hydrogen abstraction coupling reaction.
The invention has the beneficial effects that: the nano matt paint for the wood floor comprises raw materials of extinction resin, handfeel wax powder, nano silicon dioxide dispersion liquid, a thickening agent, aqueous color concentrates, a wetting agent, a defoaming agent, a dispersing agent and deionized water. The extinction resin is obtained by modifying waterborne polyurethane of epoxy resin opposite terminal hydroxypropyl polydimethylsiloxane participating in copolymerization. The hydroxypropyl-terminated polydimethylsiloxane contains a silicon-oxygen bond with high bond energy, has good heat resistance, is introduced into a system in a copolymerization mode, is prepared into emulsion, and after film formation, the organosilicon polymer migrates to the surface of a matte paint film to generate a micro rough surface, so that diffuse reflection is enhanced to achieve a extinction effect; the epoxy group and the secondary hydroxyl in the introduced epoxy resin are copolymerized with the waterborne polyurethane to generate a cross-linking structure, a branching point is introduced into a polyurethane main chain, and a benzene ring rigid structure is introduced together, so that the water resistance of the extinction resin is improved, a regular microspherical stable emulsion is formed after water is added for emulsification, and after the emulsion is dried to form a film, microspheres with larger particle size are easily displayed on the surface of a matt paint film, so that the micro coarse structure is formed, and the extinction resin has excellent extinction property; the introduced epoxy resin has the characteristics of high strength, high hardness and excellent corrosion resistance, and can improve the mechanical properties of the matte paint film; the introduction of chitosan endows the extinction resin with good self-repairing performance, so that scratches on the surface of the matt paint film can be recovered by itself, and the repairing characteristic is from the exchange reaction of hydroxyl groups of chitosan in the matt paint film and polyurethane groups at high temperature; the introduction of the acrylate group enables the matt paint to have UV-curable properties.
The thickener is a reactive polyurethane thickener, and a benzophenone derivative is synthesized to serve as a blocking agent of polyurethane, so that a benzophenone structure is introduced into the thickener structure, the thickener plays a role in photoinitiation while playing a role in thickening in the matt paint, and after UV (ultraviolet) curing, the thickener can be chemically connected with the UV-curable matt resin through hydrogen abstraction coupling reaction, so that migration and permeation of the thickener in a cured coating of the matt paint can be effectively reduced.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A matting resin prepared by the steps of:
Step A1: and drying the terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol for 1h at the temperature of 100 ℃ in vacuum for later use. Adding terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol into a flask provided with a thermometer, a stirrer and a condenser tube, heating to 90 ℃, adding toluene diisocyanate and catalyst dibutyl tin dilaurate under stirring, reacting at constant temperature for 4 hours, cooling to 50 ℃, adding 2, 2-dimethylolpropionic acid and tetrahydrofuran into the flask, reacting at constant temperature for 2 hours after heating to 70 ℃, cooling to room temperature to obtain an intermediate 1, wherein the dosage ratio of the terminal hydroxypropyl polydimethylsiloxane, the polyethylene glycol, the toluene diisocyanate and the dibutyl tin dilaurate is 0.3 mol:0.1 mol:0.0015 mol:0.002 mol:250 mL;
Step A2: under the protection of nitrogen, adding bisphenol A type epoxy resin E-12 into toluene, starting stirring, slowly adding an intermediate 1 into the mixture, continuing to react for 1h at 70 ℃, cooling the system to room temperature to obtain a reaction solution, pouring the reaction solution into an emulsifying barrel, adding triethylamine and deionized water, and preparing an intermediate 2 under high-speed stirring and shearing, wherein the dosage ratio of the bisphenol A type epoxy resin E-12 to the toluene to the intermediate 1 to the triethylamine to the deionized water is as follows: 0.1 g:70 mL:2 g:0.08 g:60 mL;
Step A3: adding chitosan and diethylamine into the intermediate 2, stirring at the rotating speed of 600r/min and the temperature of 60 ℃ for reaction for 5 hours, cooling to the temperature of 40 ℃, adding pentaerythritol triacrylate, stirring for reaction for 3 hours to obtain the extinction resin, wherein the dosage ratio of the intermediate 2, chitosan, diethylamine and pentaerythritol triacrylate is 2.6g to 0.2g to 0.5g to 0.33g.
Example 2
A matting resin prepared by the steps of:
Step A1: and drying the terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol for 1h at the temperature of 100 ℃ in vacuum for later use. Adding terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol into a flask provided with a thermometer, a stirrer and a condenser, heating to 90 ℃, adding toluene diisocyanate and catalyst dibutyl tin dilaurate under stirring, reacting at constant temperature for 4 hours, cooling to 50 ℃, adding 2, 2-dimethylolpropionic acid and tetrahydrofuran into the flask, reacting at constant temperature for 2 hours after heating to 70 ℃, cooling to room temperature to obtain an intermediate 1, wherein the dosage ratio of the terminal hydroxypropyl polydimethylsiloxane, the polyethylene glycol, the toluene diisocyanate and the dibutyl tin dilaurate is 0.3 mol:0.1 mol:0.11 mol:0.0015 mol:0.0025 mol:280 mL;
Step A2: under the protection of nitrogen, bisphenol A type epoxy resin E-12 is added into toluene, stirring is started, an intermediate 1 is slowly added into the mixture, the reaction is continued for 1.2 hours at the temperature of 75 ℃, the reaction liquid is obtained after the temperature of the system is reduced to room temperature, triethylamine and deionized water are added into an emulsifying barrel, intermediate 2 is obtained after high-speed stirring and shearing, and the dosage ratio of bisphenol A type epoxy resin E-12, toluene, intermediate 1, triethylamine and deionized water is as follows: 0.12 g:70 mL:2.2 g:0.08 g:60 mL;
Step A3: adding chitosan and diethylamine into the intermediate 2, stirring at the rotating speed of 600r/min and the temperature of 60 ℃ for reaction for 5.5 hours, cooling to the temperature of 40 ℃, adding pentaerythritol triacrylate, stirring for reaction for 3.5 hours, and obtaining the extinction resin, wherein the dosage ratio of the intermediate 2 to the chitosan to the diethylamine to the pentaerythritol triacrylate is 2.8g to 0.25g to 0.55g to 0.37g.
Example 3
A matting resin prepared by the steps of:
Step A1: and drying the terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol for 1h at the temperature of 100 ℃ in vacuum for later use. Adding terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol into a flask provided with a thermometer, a stirrer and a condenser tube, heating to 90 ℃, adding toluene diisocyanate and catalyst dibutyl tin dilaurate under stirring, reacting at constant temperature for 4 hours, cooling to 50 ℃, adding 2, 2-dimethylolpropionic acid and tetrahydrofuran into the flask, reacting at constant temperature for 2 hours after heating to 70 ℃, cooling to room temperature to obtain an intermediate 1, wherein the dosage ratio of the terminal hydroxypropyl polydimethylsiloxane, the polyethylene glycol, the toluene diisocyanate and the dibutyl tin dilaurate is 0.3 mol:0.1 mol:0.12 mol:0.0015 mol:0.003 mol:300 mL;
step A2: under the protection of nitrogen, bisphenol A type epoxy resin E-12 is added into toluene, stirring is started, an intermediate 1 is slowly added into the mixture, the reaction is continued for 1.5 hours at the temperature of 80 ℃, the reaction liquid is obtained after the temperature of the system is reduced to room temperature, triethylamine and deionized water are added into an emulsifying barrel, intermediate 2 is obtained after high-speed stirring and shearing, and the dosage ratio of bisphenol A type epoxy resin E-12, toluene, intermediate 1, triethylamine and deionized water is as follows: 0.13 g:70 mL:2.5 g:0.08 g:60 mL;
step A3: adding chitosan and diethylamine into the intermediate 2, stirring at the rotating speed of 600r/min and the temperature of 60 ℃ for reaction for 6 hours, cooling to the temperature of 40 ℃, adding pentaerythritol triacrylate, stirring for reaction for 4 hours to obtain the extinction resin, wherein the dosage ratio of the intermediate 2, chitosan, diethylamine and pentaerythritol triacrylate is 3.0g to 0.3g to 0.6g to 0.40g.
Example 4
A thickener prepared by the steps of:
step B1: adding 2-hydroxy-4-n-octoxybenzophenone, 11-bromo-undecanol, potassium carbonate and DMF into a three-neck flask, stirring and reacting for 12 hours at 80 ℃ under the protection of nitrogen, extracting with dichloromethane, drying and steaming to obtain an intermediate a, wherein the dosage ratio of the 2-hydroxy-4-n-octoxybenzophenone, the 11-bromo-undecanol, the potassium carbonate and the DMF is 0.15 mol:0.18 mol:0.30 mol:50 mL;
Step B2: adding polyethylene glycol and toluene into a flask, heating to 130 ℃ under the protection of nitrogen, distilling for 1.5 hours, cooling to 60 ℃, adding dibutyl tin dilaurate and isophorone diisocyanate into the flask, stirring at 80 ℃ for reaction for 3.5 hours, adding an intermediate a into the flask, stirring at 85 ℃ for reaction for 16 hours to obtain a mixed solution, cooling the mixed solution to room temperature, recrystallizing with diethyl ether, filtering, adding methylene dichloride into a filter cake, and recrystallizing with diethyl ether to obtain the thickener, wherein the dosage ratio of the polyethylene glycol, the toluene, the dibutyl tin dilaurate, the isophorone diisocyanate and the intermediate a is 0.25 mmol/150 mL/0.01 g/2.5 mmol/5 mmol.
Example 5
A thickener prepared by the steps of:
step B1: adding 2-hydroxy-4-n-octoxybenzophenone, 11-bromo-undecanol, potassium carbonate and DMF into a three-neck flask, stirring and reacting for 12 hours at 80 ℃ under the protection of nitrogen, extracting with dichloromethane, drying and steaming to obtain an intermediate a, wherein the dosage ratio of the 2-hydroxy-4-n-octoxybenzophenone, the 11-bromo-undecanol, the potassium carbonate and the DMF is 0.15 mol:0.18 mol:0.30 mol:55 mL;
Step B2: adding polyethylene glycol and toluene into a flask, heating to 130 ℃ under the protection of nitrogen, distilling for 1.8 hours, cooling to 65 ℃, adding dibutyl tin dilaurate and isophorone diisocyanate into the flask, stirring at 80 ℃ for reaction for 3.7 hours, adding an intermediate a into the flask, stirring at 85 ℃ for reaction for 16 hours to obtain a mixed solution, cooling the mixed solution to room temperature, recrystallizing with diethyl ether, filtering, adding methylene dichloride into a filter cake, and recrystallizing with diethyl ether to obtain the thickener, wherein the dosage ratio of the polyethylene glycol, the toluene, the dibutyl tin dilaurate, the isophorone diisocyanate and the intermediate a is 0.25 mmol/150 mL/0.01 g/2.5 mmol/5 mmol.
Example 6
A thickener prepared by the steps of:
step B1: adding 2-hydroxy-4-n-octoxybenzophenone, 11-bromo-undecanol, potassium carbonate and DMF into a three-neck flask, stirring and reacting for 12 hours at 80 ℃ under the protection of nitrogen, extracting with dichloromethane, drying and steaming to obtain an intermediate a, wherein the dosage ratio of the 2-hydroxy-4-n-octoxybenzophenone, the 11-bromo-undecanol, the potassium carbonate and the DMF is 0.15 mol:0.18 mol:0.30 mol:60 mL;
Step B2: adding polyethylene glycol and toluene into a flask, heating to 130 ℃ under the protection of nitrogen, distilling for 2 hours, cooling to 70 ℃, adding dibutyl tin dilaurate and isophorone diisocyanate into the flask, stirring at 80 ℃ for reaction for 4 hours, adding an intermediate a into the flask, stirring at 85 ℃ for reaction for 16 hours to obtain a mixed solution, cooling the mixed solution to room temperature, recrystallizing with diethyl ether, filtering, adding methylene dichloride into a filter cake, and recrystallizing with diethyl ether to obtain the thickener, wherein the dosage ratio of the polyethylene glycol, the toluene, the dibutyl tin dilaurate, the isophorone diisocyanate to the intermediate a is 0.25 mmol/150 mL/0.01 g/2.5 mmol/5 mmol.
Example 7
The nano matte paint for the wood floor comprises the following raw materials in parts by weight: 60 parts of extinction resin, 5 parts of thickener, 3 parts of handfeel wax powder, 3 parts of nano silicon dioxide dispersion liquid, 1 part of aqueous color essence, 1 part of wetting agent, 0.5 part of defoamer, 1 part of dispersing agent and 20 parts of deionized water. The hand feeling wax powder is polytetrafluoroethylene wax powder, the wetting agent is polyether silicone oil, the defoaming agent is polydimethylsiloxane, and the dispersing agent is a polyacrylic acid ammonium salt dispersing agent.
The nano matt paint for the wood floor is prepared through the following steps:
Stirring the extinction resin obtained in the example 1 at a speed of 500r/min, adding a defoaming agent, a wetting agent, a dispersing agent and deionized water, stirring for 40min at a speed of 900r/min, then adding the hand feeling wax powder, the nano silicon dioxide dispersion liquid and the aqueous color concentrate, continuing stirring for 30min, finally adding the thickening agent obtained in the example 4, continuing stirring for 15min, and filtering to obtain the nano matte paint for the wood floor.
Example 8
The nano matte paint for the wood floor comprises the following raw materials in parts by weight: 65 parts of extinction resin, 6 parts of thickener, 4 parts of handfeel wax powder, 4 parts of nano silicon dioxide dispersion liquid, 2 parts of aqueous color essence, 1.5 parts of wetting agent, 0.7 part of defoamer, 1.2 parts of dispersing agent and 25 parts of deionized water. The hand feeling wax powder is polytetrafluoroethylene wax powder, the wetting agent is polyether silicone oil, the defoaming agent is polydimethylsiloxane, and the dispersing agent is a polyacrylic acid ammonium salt dispersing agent.
The nano matt paint for the wood floor is prepared through the following steps:
Stirring the extinction resin obtained in the example 2 at the speed of 550r/min, adding a defoaming agent, a wetting agent, a dispersing agent and deionized water, stirring for 45min at the speed of 950r/min, then adding the hand feeling wax powder, the nano silicon dioxide dispersion liquid and the water-based color concentrate, continuing stirring for 35min, finally adding the thickening agent obtained in the example 5, continuing stirring for 25min, and filtering to obtain the nano matte paint for the wood floor.
Example 9
The nano matte paint for the wood floor comprises the following raw materials in parts by weight: 70 parts of extinction resin, 7 parts of thickener, 5 parts of handfeel wax powder, 5 parts of nano silicon dioxide dispersion liquid, 3 parts of aqueous color essence, 2 parts of wetting agent, 1 part of defoamer, 1.5 parts of dispersing agent and 30 parts of deionized water. The hand feeling wax powder is polytetrafluoroethylene wax powder, the wetting agent is polyether silicone oil, the defoaming agent is polydimethylsiloxane, and the dispersing agent is a polyacrylic acid ammonium salt dispersing agent.
The nano matt paint for the wood floor is prepared through the following steps:
Stirring the extinction resin obtained in the example 3 at the speed of 600r/min, adding the defoamer, the wetting agent, the dispersing agent and the deionized water, stirring for 50min at the speed of 1000r/min, then adding the hand feeling wax powder, the nano silicon dioxide dispersion liquid and the water-based color concentrate, continuing stirring for 40min, finally adding the thickener obtained in the example 6, continuing stirring for 30min, and filtering to obtain the nano matte paint for the wood floor.
Comparative example 1
The comparative example is a commercially available nano matt paint for wood floors.
Comparative example 2
Compared with example 9, the matting resin was changed to a general aqueous polyurethane and 4 parts of nano silica was added as a matting agent, and the other was completely the same as in example 9, to prepare a nano matt paint for a wood floor.
Comparative example 3
In comparison with example 9, the intermediate a for preparing a thickener was replaced by 11-bromo-undecanol, and otherwise, the nano-gloss paint for wood floors was prepared exactly as in example 9.
The nano matt paint for the wood floor prepared by the invention is further tested for effect, and the test results are as follows.
To test the nano matt paint for wood flooring prepared according to the present invention, performance was measured according to the relevant standards, and the results are shown in table 1.
Table 1:
From the data in table 1, it is clear that the nano-gloss paint for wood floor prepared by the invention has excellent toughness, adhesive force, pencil hardness and water resistance compared with the nano-gloss paint for wood floor sold in the market as compared with comparative example 1 in example 7, example 8 and example 9; as can be seen from comparison of example 9 with comparative example 2, the toughness, water resistance and adhesion of the matt paint are reduced by using only the general aqueous polyurethane and adding the matt powder to prepare the matt paint, compared with the matt resin obtained by using the aqueous polyurethane with the epoxy resin modified terminal hydroxypropyl polydimethylsiloxane involved in copolymerization; as is clear from comparison between example 9 and comparative example 3, the use of a thickener having no benzophenone structure has a possibility of migration of the thickener, which reduces the toughness of the matt paint, compared with the use of a thickener having a benzophenone structure.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (9)
1. The nanometer matt paint for the wood floor is characterized in that: the material comprises the following raw materials in parts by weight: 60-70 parts of extinction resin, 5-7 parts of thickener, 3-5 parts of handfeel wax powder, 3-5 parts of nano silicon dioxide dispersion liquid, 1-3 parts of aqueous color concentrate, 1-2 parts of wetting agent, 0.5-1 part of defoamer, 1-1.5 parts of dispersing agent and 20-30 parts of deionized water;
the extinction resin is prepared through the following steps:
Step A1: and drying the terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol for 1h at the temperature of 100 ℃ in vacuum for later use. Adding terminal hydroxypropyl polydimethylsiloxane and polyethylene glycol into a flask provided with a thermometer, a stirrer and a condenser, heating to 90 ℃, adding toluene diisocyanate and dibutyl tin dilaurate under stirring, reacting for 4 hours at constant temperature, cooling to 50 ℃, adding 2, 2-dimethylolpropionic acid and tetrahydrofuran into the flask, reacting for 2 hours at constant temperature after heating to 70 ℃, and cooling to room temperature to obtain an intermediate 1;
Step A2: under the protection of nitrogen, bisphenol A type epoxy resin E-12 is added into toluene, stirring is started, intermediate 1 is slowly added into the mixture, the reaction is continued for 1 to 1.5 hours at the temperature of 70 to 80 ℃, the temperature of the system is reduced to room temperature, reaction liquid is obtained, the reaction liquid is poured into an emulsification barrel, triethylamine and deionized water are added into the reaction liquid, and intermediate 2 is prepared under high-speed stirring and shearing;
Step A3: adding chitosan and diethylamine into the intermediate 2, stirring at 600r/min and 60 ℃ for reaction for 5-6h, cooling to 40 ℃, adding pentaerythritol triacrylate, and stirring for reaction for 3-4h to obtain the extinction resin.
2. The nano matt paint for wood floors according to claim 1, wherein: the thickener is prepared through the following steps:
Step B1: adding 2-hydroxy-4-n-octoxybenzophenone, 11-bromo-undecanol, potassium carbonate and DMF into a three-neck flask, stirring and reacting for 12 hours at 80 ℃ under the protection of nitrogen, extracting with dichloromethane, drying and rotary steaming to obtain an intermediate a;
Step B2: adding polyethylene glycol and toluene into a flask, heating to 130 ℃ under the protection of nitrogen, distilling for 1.5-2 hours, cooling to 60-70 ℃, adding dibutyl tin dilaurate and isophorone diisocyanate into the flask, stirring at 80 ℃ for reaction for 3.5-4 hours, adding an intermediate a into the flask, stirring at 85 ℃ for reaction for 16 hours to obtain a mixed solution, cooling the mixed solution to room temperature, recrystallizing with diethyl ether, filtering, adding dichloromethane into a filter cake, and recrystallizing with diethyl ether to obtain the thickener.
3. The nano matt paint for wood floors according to claim 1, wherein: the hand feeling wax powder is polytetrafluoroethylene wax powder, the wetting agent is polyether silicone oil, the defoaming agent is polydimethylsiloxane, and the dispersing agent is a polyacrylate ammonium salt dispersing agent.
4. The nano matt paint for wood floors according to claim 1, wherein: in the step A1, the dosage ratio of the terminal hydroxypropyl polydimethylsiloxane, the polyethylene glycol, the toluene diisocyanate and the dibutyl tin dilaurate to the 2, 2-dimethylolpropionic acid to the tetrahydrofuran is 0.3mol:0.1mol:0.1 to 0.12mol:0.0015mol:0.002-0.003mol:250-300mL.
5. The nano matt paint for wood floors according to claim 1, wherein: in the step A2, the dosage ratio of bisphenol A epoxy resin E-12, toluene, intermediate 1, triethylamine and deionized water is as follows: 0.1-0.13g:70mL:2-2.5g:0.08g:60mL.
6. The nano matt paint for wood floors according to claim 1, wherein: in the step A3, the dosage ratio of the intermediate 2 to the chitosan to the diethylamine to the pentaerythritol triacrylate is 2.6-3.0g:0.2-0.3g:0.5-0.6g:0.33-0.40g.
7. The nano matt paint for wood floors according to claim 2, characterized in that: in the step B1, the dosage ratio of 2-hydroxy-4-n-octoxybenzophenone, 11-bromo-undecanol, potassium carbonate and DMF was 0.15mol:0.18mol:0.30mol:50-60mL.
8. The nano matt paint for wood floors according to claim 2, characterized in that: in step B2, the dosage ratio of polyethylene glycol, toluene, dibutyltin dilaurate, isophorone diisocyanate and intermediate a was 0.25mmol:150mL:0.01g:2.5mmol:5mmol.
9. The method for preparing the nano matt paint for the wood floor according to claim 1, which is characterized in that: the method comprises the following steps:
Stirring the extinction resin at the speed of 500-600r/min, adding the defoamer, the wetting agent, the dispersing agent and the deionized water, stirring at the speed of 900-1000r/min for 40-50min, then adding the hand feeling wax powder, the nano silicon dioxide dispersion liquid and the water-based color concentrate, continuously stirring for 30-40min, finally adding the thickener, continuously stirring for 15-30min, and filtering to obtain the nano matte paint for the wood floor.
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