CN114656610A - Carbon-fixed odorless water-based resin and preparation method and application thereof - Google Patents
Carbon-fixed odorless water-based resin and preparation method and application thereof Download PDFInfo
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- CN114656610A CN114656610A CN202111461464.9A CN202111461464A CN114656610A CN 114656610 A CN114656610 A CN 114656610A CN 202111461464 A CN202111461464 A CN 202111461464A CN 114656610 A CN114656610 A CN 114656610A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 230000009965 odorless effect Effects 0.000 title claims abstract description 48
- 229920005989 resin Polymers 0.000 title claims abstract description 47
- 239000011347 resin Substances 0.000 title claims abstract description 47
- 238000000576 coating method Methods 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 239000011248 coating agent Substances 0.000 claims abstract description 30
- 125000005442 diisocyanate group Chemical group 0.000 claims abstract description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004359 castor oil Substances 0.000 claims abstract description 11
- 235000019438 castor oil Nutrition 0.000 claims abstract description 11
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims abstract description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 10
- 229920005862 polyol Polymers 0.000 claims abstract description 9
- 150000003077 polyols Chemical class 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 53
- 239000000203 mixture Substances 0.000 claims description 22
- 239000004970 Chain extender Substances 0.000 claims description 19
- 239000003960 organic solvent Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000000839 emulsion Substances 0.000 claims description 10
- 230000003472 neutralizing effect Effects 0.000 claims description 8
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 claims description 5
- 230000001804 emulsifying effect Effects 0.000 claims description 5
- 238000005034 decoration Methods 0.000 claims description 4
- 150000003384 small molecules Chemical group 0.000 claims description 4
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 abstract description 8
- 239000000049 pigment Substances 0.000 abstract description 8
- 229920006313 waterborne resin Polymers 0.000 abstract description 8
- 239000013035 waterborne resin Substances 0.000 abstract description 8
- 238000005406 washing Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 description 45
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 38
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 32
- 238000003756 stirring Methods 0.000 description 26
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 19
- 229910000019 calcium carbonate Inorganic materials 0.000 description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 18
- 239000002518 antifoaming agent Substances 0.000 description 17
- 239000008367 deionised water Substances 0.000 description 17
- 229910021641 deionized water Inorganic materials 0.000 description 17
- 238000004321 preservation Methods 0.000 description 16
- 239000002562 thickening agent Substances 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000003973 paint Substances 0.000 description 12
- 239000002270 dispersing agent Substances 0.000 description 11
- 239000000080 wetting agent Substances 0.000 description 11
- 238000010992 reflux Methods 0.000 description 10
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000004408 titanium dioxide Substances 0.000 description 9
- 229920002635 polyurethane Polymers 0.000 description 8
- 239000004814 polyurethane Substances 0.000 description 8
- 230000000844 anti-bacterial effect Effects 0.000 description 7
- 239000003899 bactericide agent Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- 239000002243 precursor Substances 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 5
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- 229920005749 polyurethane resin Polymers 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 4
- 239000005058 Isophorone diisocyanate Substances 0.000 description 4
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 4
- 230000002528 anti-freeze Effects 0.000 description 4
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 4
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000013530 defoamer Substances 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- XXKOQQBKBHUATC-UHFFFAOYSA-N cyclohexylmethylcyclohexane Chemical compound C1CCCCC1CC1CCCCC1 XXKOQQBKBHUATC-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 description 2
- 150000002009 diols Chemical class 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 240000001829 Catharanthus roseus Species 0.000 description 1
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 1
- 229920002593 Polyethylene Glycol 800 Polymers 0.000 description 1
- -1 SILRES BS168 (watts) Chemical compound 0.000 description 1
- 241001478428 Syngnathus Species 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 229940085675 polyethylene glycol 800 Drugs 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000909 polytetrahydrofuran Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6625—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/34
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
-
- 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
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a carbon-fixed odorless waterborne resin and a preparation method and application thereof. The carbon-fixed odor-free water-based resin provided by the invention comprises the following raw materials: a first pre-mer and a second pre-mer; preparing raw materials of the first prepolymer, wherein the raw materials comprise poly (carbonate-ether) polyol and diisocyanate; the preparation raw materials of the second prepolymer comprise castor oil, diisocyanate and polyethylene glycol. The carbon-fixed odor-free water-based resin has good hand feeling and lower odor, can form a film by itself, shows excellent wrapping property on pigments and fillers, and promotes the interior wall coating to have the characteristics of low odor, excellent water resistance, washing resistance and smooth hand feeling.
Description
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to carbon-fixed odorless water-based resin as well as a preparation method and application thereof.
Background
The coating is a continuous film which is coated on the surface of an object to be protected or decorated and can form firm adhesion with the object to be coated, and is usually mainly composed of at least one of resin, oil and emulsion, and pigments, fillers and corresponding auxiliary agents can be added.
In current interior wall application systems, acrylic emulsions dominate. However, the acrylic emulsion generally has the performance defects of hot adhesion, cold brittleness, poor hand feeling, poor scratch resistance and the like, so that the overall quality of a paint film is influenced, and the increasingly improved consumer requirements are difficult to meet. The carbon dioxide is used as an initial reaction monomer to synthesize the water-based polyurethane resin and further prepare the water-based paint (namely the carbon-fixed paint), so that a new technical route is provided for carbon emission reduction in the paint field. However, the existing carbon-fixing paint usually needs to add a film-forming auxiliary agent to assist film formation, so that the paint has high VOC and large smell; in addition, the existing carbon-fixed paint is limited to a transparent paint system, and has the defects of poor coating property of pigments and fillers, poor film-forming property and the like during application, particularly poor scrubbing resistance, so that the existing carbon-fixed paint is difficult to apply to odorless powder paint.
In conclusion, the carbon-fixed odor-free water-based resin based on the greenhouse gas carbon dioxide as the raw material is developed, and the water-based odor-free coating with excellent performance is prepared by combining the green formula, so that the use experience of consumers is improved, and the requirements of environmental protection and sustainable development can be met.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the carbon-fixed odor-free water-based resin provided by the invention adopts preparation raw materials including poly (carbonate-ether) polyol obtained by taking greenhouse gas carbon dioxide as a raw material, has excellent hand feeling, has the characteristics of self-filming and odor-free, and shows good wrapping property for pigments and fillers, so that the prepared coating product shows excellent washing and brushing resistance.
The invention also provides a preparation method of the carbon-fixed odorless water-based resin.
The invention also provides a coating, and the preparation raw material of the coating comprises the carbon-fixed odorless water-based resin.
The invention also provides an application of the coating in the field of decoration.
According to one aspect of the invention, a carbon-fixed odorless water-based resin is provided, and the preparation raw materials comprise: a first pre-mer and a second pre-mer;
the preparation raw materials of the first prepolymer comprise poly (carbonate-ether) polyol and diisocyanate A;
the raw materials for preparing the second prepolymer comprise castor oil, diisocyanate B and polyethylene glycol.
And combining hydrophilic monomers such as polyethylene glycol, internal emulsifying chain extender and the like with soft oligomer castor oil to react with soft diisocyanate to obtain a second prepolymer with enough hydrophilicity.
In some embodiments of the invention, the mass ratio of the first pre-polymer to the second pre-polymer is 1.1 to 3: 1.
the carbon-fixed odorless water-based resin obtained in the proportion has good hydrophobicity, hydrophilicity and hardness.
In some embodiments of the invention, the poly (carbonate-ether) polyol comprises a poly (carbonate-ether) diol.
In some embodiments of the invention, the poly (carbonate-ether) glycol in the first prepolymer has a molecular weight of 3000-5000 g/mol.
At this molecular weight, the order of the segments in the first prepolymer is ensured and sufficient water resistance is provided.
Poly (carbonate-ether) glycols were produced and provided by the institute of applied chemistry, catharanthus roseus, department of sciences.
In some embodiments of the present invention, the diisocyanate A used to prepare the first prepolymer comprises at least one of 4, 4-diisocyanate dicyclohexylmethane, toluene-2, 4-diisocyanate, and 4,4' -methylenebis (phenylisocyanate).
In some embodiments of the present invention, the raw materials for preparing the first prepolymer further comprise an organic solvent and a small molecule chain extender.
In some embodiments of the invention, the organic solvent in the first prepolymer comprises acetone.
In some embodiments of the invention, the small molecule chain extender in the first prepolymer comprises at least one of trimethylolpropane, butanediol, and ethylene glycol.
In some embodiments of the present invention, in the raw material for preparing the first prepolymer, the mass ratio of the poly (carbonate-ether) polyol to the diisocyanate a is 3 to 8: 1.
in some embodiments of the present invention, in the raw material for preparing the first prepolymer, the mass ratio of the poly (carbonate-ether) polyol, the diisocyanate a, and the small-molecule chain extender in the carbon-fixed prepolymer is 3 to 8: 1: 0.1 to 0.3.
In some embodiments of the invention, the method of preparing the first prepolymer comprises the steps of:
A1. reacting the poly (carbonate-ether) diol and diisocyanate in the organic solvent;
A2. and D, adding the small molecular chain extender into the mixture obtained in the step A1 to continue reacting to obtain the first prepolymer.
In some embodiments of the present invention, the temperature of the reaction in step A1 is 65-85 ℃.
In some embodiments of the invention, in step a1, the reaction time is 2 to 3 hours.
In some embodiments of the present invention, in the step A2, the reaction temperature is 65-85 ℃.
In some embodiments of the invention, in step a2, the reaction time is 2 to 3 hours.
In some embodiments of the present invention, the diisocyanate used to prepare the second prepolymer includes at least one of hexamethylene diisocyanate and isophorone diisocyanate.
In some embodiments of the present invention, the molecular weight of the polyethylene glycol in the raw material for preparing the second prepolymer is 400-800 g/mol.
In some embodiments of the present invention, in the preparation raw material of the second prepolymer, the mass ratio of the castor oil, the diisocyanate B and the polyethylene glycol is 1-3: 1: 0.9 to 1.
In some embodiments of the present invention, in the raw material for preparing the second prepolymer, the diisocyanate B includes at least one of hexamethylene diisocyanate and isophorone diisocyanate.
In some embodiments of the invention, in the second prepolymer, the preparation feedstock further comprises an internal emulsion chain extender.
In some embodiments of the invention, the second prepolymer, the internal emulsion chain extender, comprises at least one of dimethylolpropionic acid and dimethylolbutyric acid.
In some embodiments of the present invention, the preparation starting material in the second prepolymer further comprises an organic solvent.
In some embodiments of the invention, the organic solvent in the second prepolymer comprises at least one of acetone and butanone.
In some embodiments of the present invention, in the preparation raw materials of the second prepolymer, the mass ratio of the castor oil, the diisocyanate B, the polyethylene glycol, and the internal emulsifying chain extender is 1-3: 1: 0.9-1: 0.3 to 0.6.
According to the invention, hydrophilic monomers such as polyethylene glycol and internal emulsifying chain extender are combined with soft oligomer castor oil to react with soft diisocyanate to obtain a second precursor polymer with enough hydrophilicity, and meanwhile, due to the synergistic effect of the first precursor polymer and the second precursor polymer, the enough good film forming property of the carbon-fixed odorless waterborne resin is ensured without adding a film forming additive. The second precursor polymer which is hydrophilic enough and is combined with the soft monomer used in the synthesis process can ensure stronger storage stability and low-temperature self-film-forming property. The first prepolymer shows a harder chain structure, so that the sufficient hardness of the polyurethane is ensured, and the matching of hardness and softness is obviously different from the design thinking that the traditional polyurethane takes oligomer polyol as a soft segment and diisocyanate and a small molecular chain extender as a hard segment.
In some embodiments of the invention, the method for preparing the second prepolymer comprises the following steps:
B1. reacting the internal emulsifying chain extender with diisocyanate and an organic solvent,
B2. and C, adding the polyethylene glycol and the castor oil into the mixture obtained in the step B1 to continuously react to obtain the second prepolymer.
In some embodiments of the present invention, in the step B1, the temperature of the reaction is 75-85 ℃.
In some embodiments of the present invention, in the step B1, the reaction time is 1-3 h.
In some embodiments of the present invention, in the step B2, the temperature of the reaction is 75-85 ℃.
In some embodiments of the present invention, in the step B2, the reaction time is 2 to 4 hours.
In some embodiments of the present invention, the raw material for preparing the carbon-fixed odorless aqueous resin further comprises a chain extender and a neutralizing agent.
In some embodiments of the present invention, in the carbon-fixed odorless aqueous resin, the chain extender includes at least one of ethylene glycol, butanediol, and trimethylolpropane.
In some embodiments of the present invention, in the carbon-fixed odorless aqueous resin, the neutralizing agent is selected from at least one of sodium hydroxide, potassium hydroxide, SILRES BS168 (watts), and methyldiethanolamine.
In some embodiments of the present invention, the mass ratio of the first pre-polymer, the second pre-polymer, the chain extender and the neutralizing agent in the carbon-fixed odorless aqueous resin is 1.1 to 3: 1: 0.005-0.03: 0.02 to 0.09.
The second aspect of the invention provides a preparation method of carbon-fixed odorless water-based resin, which comprises the steps of mixing the first prepolymer and the second prepolymer, neutralizing and dispersing after the reaction is finished, and removing impurities to obtain the carbon-fixed odorless water-based resin.
The carbon-fixed odorless aqueous resin disclosed by the invention has at least the following beneficial effects:
1. according to the invention, the first precursor polymer with hydrophobicity and the second precursor polymer with hydrophilicity are independently synthesized and respectively added to react, so that the regularity and the display of hydrophilicity of the carbon-fixed odorless waterborne resin structure are facilitated, the structural regularity shows that an hydrophilic-hydrophobic structure exists in a polyurethane chain segment in a segmented manner, the stability of waterborne polyurethane can be promoted, the wrapping property of pigment and filler is improved, and the problem that the wrapping property of the final carbon-fixed odorless waterborne resin is poor due to the fact that the first precursor polymer is high in hardness is solved.
2. The carbon-fixed odorless aqueous resin provided by the invention improves the wrapping property of pigment and filler, has the characteristics of low odor and high film-forming property, and is applied to the preparation of interior wall coating.
In some preferred embodiments of the present invention, the method for preparing the carbon-fixed odorless aqueous resin comprises the steps of,
C1. adding the second prepolymer into the first prepolymer, and carrying out heat preservation reaction;
C2. and D, adding the neutralizing agent into the mixture obtained in the step C1, dispersing, and desolventizing to obtain the catalyst.
In some embodiments of the present invention, in the step C1, the temperature of the reaction is 70-80 ℃.
In some embodiments of the present invention, in the step C1, the reaction time is 2-4 h.
In some embodiments of the present invention, in the step C2, the temperature of the reaction is 20-40 ℃.
In some embodiments of the present invention, in the step C2, the reaction time is 0.5-1 h.
In some embodiments of the present invention, in the step C2, the desolventizing temperature is 50-60 ℃.
In some embodiments of the present invention, in the step C2, the vacuum degree of the desolventizing is-0.07 to-0.09 MPa.
In a third aspect of the invention, a coating is provided, and the raw materials for preparing the coating comprise the carbon-fixed odorless water-based resin.
In a fourth aspect of the invention, a coating is provided for use in the field of decoration.
In some embodiments of the present invention, the raw materials for preparing the coating further comprise a chain extender and a neutralizing agent;
in some embodiments of the invention, the preparation raw materials of the coating further comprise, by weight, 20-34 parts of a odorless water-based resin, 20-36 parts of deionized water, 0.4-0.6 part of a dispersing agent, 0.15-0.6 part of a defoaming agent, 0.1-0.2 part of a wetting agent, 0.20-0.65 part of a thickening agent, 9-15 parts of light calcium carbonate, 7-15 parts of heavy calcium carbonate, 10-25 parts of titanium dioxide, 3-5 parts of talcum powder, 0.05-0.1 part of a mildew-proof bactericide and 0.4-1 part of an antifreezing agent.
In some embodiments of the invention, the dispersant is at least one of a Goutah P30, TEGO Dispers 740W, or BYK-190.
In some embodiments of the invention, the wetting agent is at least one of DOW EH-9, TEGO 715W, or BYK-346.
In some embodiments of the invention, the defoamer is at least one of BASF ST-2410, Tego airex-901w, and BYK-028.
In some embodiments of the invention, the thickener is at least one of Syngnathus 250HHBR, BYK OPTIFLO L100, and Natrosol Plus 330.
In some embodiments of the invention, the preparation method of the coating comprises the following steps of adding deionized water into a dispersion cylinder, starting a stirrer, sequentially adding a defoaming agent, a wetting agent, a dispersing agent and a thickening agent, stirring at medium speed for 15min, and dispersing until the mixture is uniform; increasing the rotation speed of the stirrer to a high speed, adding the powder, stirring for 20-30min, and dispersing uniformly; adding carbon fixed odorless water-based resin at medium speed, and supplementing a defoaming agent; and finally, adding the mildew-proof bactericide and the thickening agent, stirring at a low speed for 10min, and adjusting the viscosity to a proper value to obtain the interior wall coating.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Material preparation example 1
The preparation example of the material prepares a first prepolymer, and the preparation method comprises the following steps:
(1) adding 400 parts by weight of poly (carbonate-ether) glycol (3000g/mol) and 100 parts by weight of 4, 4-diisocyanate dicyclohexylmethane into a reaction kettle with a reflux condensing device, and reacting for 2 hours at 80 ℃;
(2) adding 10 parts by weight of trimethylolpropane into the reaction kettle in the step (1), adding 120 parts by weight of acetone according to the system viscosity to reduce the viscosity, and carrying out heat preservation reaction for 3 hours to obtain a first prepolymer-1.
Material preparation example 2
The preparation example of the material provides a first prepolymer, and the preparation method comprises the following steps:
(1) adding 500 parts by weight of poly (carbonate-ether) triol (5000g/mol) and 70 parts by weight of toluene-2, 4-diisocyanate into a reaction kettle with a reflux condensing device, and reacting for 1.5h at 70 ℃;
(2) adding 7 parts by weight of butanediol into the reaction kettle, adding 200 parts by weight of acetone according to the system viscosity to reduce the viscosity, and carrying out heat preservation reaction for 2 hours to obtain a first prepolymer-2.
Material preparation example 3
The preparation example of the material provides a first prepolymer, and the preparation method comprises the following steps:
(1) adding 300 parts by weight of poly (carbonate-ether) glycol (4000g/mol) and 80 parts by weight of 4,4' -methylene bis (phenyl isocyanate) into a reaction kettle with a reflux condensing device, and reacting for 1.5 hours at 70 ℃;
(2) adding 8 parts by weight of butanediol into the reaction kettle, adding 100 parts by weight of acetone according to the system viscosity to reduce the viscosity, and carrying out heat preservation reaction for 2 hours to obtain a first prepolymer-3.
Material preparation example 4
The preparation example of the material provides a second prepolymer, and the preparation method comprises the following steps:
(1) adding 210 parts by weight of dimethylolpropionic acid, 420 parts by weight of isophorone diisocyanate and 250 parts by weight of butanone into a reaction kettle with a reflux condensing device, and reacting for 2 hours at 85 ℃;
(2) adding 500 parts by weight of castor oil and 400 parts by weight of polyethylene glycol-800 into a reaction kettle, carrying out heat preservation reaction at 85 ℃ for 2 hours, and obtaining a second prepolymer-1 after the reaction is finished.
Material preparation example 5
The preparation example of the material provides a second prepolymer, and the preparation method comprises the following steps:
(1) adding 145 parts by weight of dimethylolbutyric acid, 340 parts by weight of hexamethylene diisocyanate and 250 parts by weight of butanone into a reaction kettle with a reflux condensing device, and reacting for 2 hours at 75 ℃;
(2) adding 820 parts by weight of castor oil and 320 parts by weight of polyethylene glycol-400 into a reaction kettle, carrying out heat preservation reaction at 75 ℃ for 2h, and obtaining a second prepolymer-2 after the reaction is finished.
Example 1
This example prepares a carbon-fixed odorless waterborne resin, and the preparation method includes the following steps:
(1) adding 630 parts by weight of first prepolymer-1 into a reaction kettle with a reflux condensing device, adding 90 parts by weight of second prepolymer-1 after the temperature is increased to 80 ℃, adding 90 parts by weight of second prepolymer-1 after 5 minutes, adding 95 parts by weight of second prepolymer-1 after 5 minutes, continuing to perform heat preservation reaction for 20 minutes, adding 2 parts by weight of ethylene glycol and 150 parts by weight of acetone, and continuing to perform heat preservation reaction for 3 hours;
(2) adding 150 parts by weight of acetone, reducing the reaction temperature to be within 40 ℃, adding a mixture of 24 parts by weight of methyldiethanolamine and 100g of water, stirring for 0.5h, and adding 1900 parts by weight of deionized water for dispersing.
(3) Separating the mixture obtained in the step C2 at 65 ℃ under reduced pressure to remove the organic solvent (acetone).
Example 2
The embodiment provides a carbon-fixed odorless waterborne resin, and a preparation method thereof comprises the following steps:
(1) adding 777 parts by weight of first prepolymer-2 into a reaction kettle with a reflux condensing device, adding 120 parts by weight of second prepolymer-1 after the temperature is raised to 75 ℃, adding 120 parts by weight of second prepolymer-1 after 5 minutes, adding 8 parts by weight of butanediol and 250 parts by weight of acetone mixture after continuing the heat preservation reaction for 20 minutes, and continuing the heat preservation reaction for 2 hours;
(2) adding 200 parts by weight of acetone, reducing the reaction temperature to be within 40 ℃, adding a mixture of 10 parts by weight of sodium hydroxide and 150g of water, stirring for 0.5h, and adding 1500 parts by weight of deionized water for dispersion.
(3) Separating the mixture obtained in the step (2) at 60 ℃ under reduced pressure to remove the organic solvent, thus obtaining the organic solvent.
Example 3
The embodiment provides a carbon-fixed odorless waterborne resin, and a preparation method thereof comprises the following steps:
(1) adding 534 parts by weight of first prepolymer-3 into a reaction kettle with a reflux condensing device, adding 100 parts by weight of second prepolymer-1 after the temperature is raised to 70 ℃, adding 100 parts by weight of second prepolymer-1 after 5 minutes, adding 110 parts by weight of second prepolymer-1 after 5 minutes, continuing to perform heat preservation reaction for 10 minutes, adding 6 parts by weight of trimethylolpropane and 200 parts by weight of acetone mixture, and continuing to perform heat preservation reaction for 2 hours;
(2) adding 200 parts by weight of acetone, reducing the reaction temperature to be within 40 ℃, adding a mixture of 10 parts by weight of sodium hydroxide and 150g of water, stirring for 0.5h, and adding 1700 parts by weight of deionized water for dispersion.
(3) Separating the mixture obtained in the step (2) at 60 ℃ under reduced pressure to remove the organic solvent.
Example 4
The embodiment provides a carbon-fixed odorless aqueous resin, and a preparation method thereof comprises the following steps:
(1) adding 534 parts by weight of first prepolymer-3 into a reaction kettle with a reflux condensing device, adding 150 parts by weight of second prepolymer-2 after the temperature is raised to 70 ℃, adding 100 parts by weight of second prepolymer-2 after 5 minutes, adding 120 parts by weight of second prepolymer-2 after 5 minutes, continuing to perform heat preservation reaction for 10 minutes, adding 3 parts by weight of trimethylolpropane and 200 parts by weight of acetone mixture, and continuing to perform heat preservation reaction for 2 hours;
(2) adding 150 parts by weight of acetone, reducing the reaction temperature to be within 40 ℃, adding a mixture of 10 parts by weight of sodium hydroxide and 150g of water, stirring for 0.5h, and adding 1700 parts by weight of deionized water for dispersion.
(3) Separating the mixture obtained in the step (2) at 60 ℃ under reduced pressure to remove the organic solvent.
Example 5
The embodiment provides a carbon-fixed odorless aqueous resin, and a preparation method thereof comprises the following steps:
(1) adding 630 parts by weight of first prepolymer-1 into a reaction kettle with a reflux condensing device, adding 100 parts by weight of second prepolymer-2 after the temperature is raised to 70 ℃, adding 100 parts by weight of second prepolymer-2 after 5 minutes, adding 120 parts by weight of second prepolymer-2 after 5 minutes, continuing to perform heat preservation reaction for 10 minutes, adding 2 parts by weight of glycol and 100 parts by weight of acetone mixture, and continuing to perform heat preservation reaction for 2 hours;
(2) adding 150 parts by weight of acetone, reducing the reaction temperature to be within 40 ℃, adding a mixture of 14 parts by weight of SILRES BS168 and 150g of water, stirring for 0.5h, and adding 1600 parts by weight of deionized water for dispersion.
(3) Separating the mixture obtained in the step (2) at 55 ℃ under reduced pressure to remove the organic solvent.
Example 6
The embodiment provides an interior wall coating, and the preparation method comprises the following steps:
(1) putting 24.5 parts by weight of deionized water into a dispersion kettle, starting a dispersion machine, putting 0.45 part by weight of dispersant P30, 0.15 part by weight of wetting agent DOW EH-9, 0.2 part by weight of defoaming agent BASF ST-2410, 0.5 part by weight of antifreeze, 0.2 part by weight of thickening agent 250HHBR and 0.05 part by weight of mildew-proof bactericide into the dispersion kettle in sequence, and stirring at low speed of 600r/min for 10min by using 300-;
(2) sequentially putting 20 parts by weight of titanium dioxide, 15 parts by weight of heavy calcium carbonate, 10 parts by weight of light calcium carbonate and 3.5 parts by weight of talcum powder into a dispersion kettle, and stirring at a high speed of 1400-1800r/min for 30 min.
(3) 25 parts by weight of the carbon-fixed odorless aqueous resin of example 1 and 0.25 part by weight of a defoaming agent Tego airex-901w are put into a dispersion kettle, stirred at a medium speed of 1200r/min for 10 minutes at 800-.
Example 7
The embodiment provides an interior wall coating, and the preparation method comprises the following steps:
(1) adding 35.8 parts by weight of deionized water into a dispersion kettle, starting a dispersion machine, sequentially adding 0.6 part by weight of a dispersant TEGO Dispers 740W, 0.15 part by weight of a wetting agent TEGO 715W, 0.15 part by weight of a defoaming agent Tego airex-901W, 0.25 part by weight of a thickening agent BYK OPTIFLO L100 and 0.4 part by weight of an antifreezing agent into the dispersion kettle, and stirring at a low speed of 600r/min for 10min by using 300 organic solvents;
(2) sequentially putting 10 parts by weight of titanium dioxide, 12 parts by weight of heavy calcium carbonate, 15 parts by weight of light calcium carbonate and 5 parts by weight of talcum powder into a dispersion kettle, and stirring at a high speed of 1400-1800r/min for 20 min;
(3) 20 parts by weight of the carbon-fixed odorless aqueous resin of example 2 and 0.2 part by weight of a defoaming agent BASF ST-2410 are put into a dispersion kettle, stirred at a medium speed of 1200r/min for 10min, added with 0.05 part by weight of a mildew-proof bactericide, and finally added with 0.4 part by weight of a thickening agent Natrosol Plus 330 to adjust the viscosity to 90-100KU, and then discharged.
Example 8
The embodiment provides an interior wall coating, and the preparation method comprises the following steps:
(1) adding 20 parts by weight of deionized water into a dispersion kettle, starting a dispersion machine, sequentially adding 0.6 part by weight of dispersant BYK-190, 0.2 part by weight of wetting agent BYK-346, 0.15 part by weight of defoaming agent Tego airex-901w, 0.2 part by weight of thickening agent BYK OPTIFLO L100 and 0.4 part by weight of antifreezing agent into the dispersion kettle, and stirring at low speed of 600r/min for 10min by using 300-;
(2) sequentially putting 25 parts by weight of titanium dioxide, 7 parts by weight of heavy calcium carbonate, 9 parts by weight of light calcium carbonate and 3 parts by weight of talcum powder into a dispersion kettle, and stirring at a high speed of 1400-1800r/min for 25 min;
(3) 34 parts by weight of the carbon-fixed odorless aqueous resin of example 3 and 0.2 part by weight of a defoaming agent BYK-028 are put into a dispersion kettle, stirred at a medium speed of 1200r/min for 10min at 800-.
Example 9
The embodiment provides an interior wall coating, and a preparation method thereof comprises the following steps:
(1) adding 28 parts by weight of deionized water into a dispersion kettle, starting a dispersion machine, sequentially adding 0.5 part by weight of a dispersing agent P30, 0.17 part by weight of a wetting agent TEGO 715W, 0.2 part by weight of a defoaming agent BASF ST-2410, 0.25 part by weight of a thickening agent Natrosol Plus 330 and 0.6 part by weight of an antifreezing agent into the dispersion kettle, and stirring at a low speed of 600r/min for 10 min;
(2) sequentially putting 15 parts by weight of titanium dioxide, 10 parts by weight of heavy calcium carbonate, 12 parts by weight of light calcium carbonate and 4 parts by weight of talcum powder into a dispersion kettle, and stirring at a high speed of 1400-1800r/min for 25 min;
(3) 23 parts by weight of the carbon-fixed odorless aqueous resin obtained in example 4 and 0.25 part by weight of defoaming agent BYK-028 are put into a dispersion kettle, stirred at a medium speed of 1200r/min for 10 minutes at 800-.
Example 10
The embodiment provides an interior wall coating, and the preparation method comprises the following steps:
(1) adding 28 parts by weight of deionized water into a dispersion kettle, starting a dispersion machine, sequentially adding 0.5 part by weight of a dispersing agent P30, 0.17 part by weight of a wetting agent TEGO 715W, 0.2 part by weight of a defoaming agent BASF ST-2410, 0.25 part by weight of a thickening agent Natrosol Plus 330 and 0.6 part by weight of an antifreezing agent into the dispersion kettle, and stirring at a low speed of 600r/min for 10 minutes by using 300-;
(2) sequentially putting 15 parts by weight of titanium dioxide, 10 parts by weight of heavy calcium carbonate, 12 parts by weight of light calcium carbonate and 4 parts by weight of talcum powder into a dispersion kettle, and stirring at a high speed of 1400-1800r/min for 25 minutes;
(3) 23 parts by weight of the carbon-fixed odorless aqueous resin obtained in example 5 and 0.25 part by weight of defoaming agent BYK-028 are put into a dispersion kettle, stirred at a medium speed of 1200r/min for 10 minutes at 800-.
Comparative example 1
The present comparative example provides an aqueous polyurethane resin based on CN201510660415.6, and the preparation method thereof comprises the following steps:
(1) under the protection of nitrogen, 680g of poly (carbonate-ether) dihydric alcohol (the number average molecular weight is 3400 daltons) and 600g of polytetrahydrofuran dihydric alcohol (the number average molecular weight is 3000 daltons) are added into a reaction kettle, the temperature is raised to 100 ℃, after reduced pressure distillation for 3 hours, the temperature is lowered to 80 ℃, 160g of dicyclohexylmethane diisocyanate is dissolved in 160g of butanone, the solution is dripped into the reaction kettle at the speed of 10ml/min, and after polymerization for 2.5 hours, a first prepolymer with NCO at the end is obtained;
(2) dissolving 90g of 2, 2-dimethylolbutyric acid and 0.5g of dibutyltin dilaurate in 280g of butanone, adding the mixture into a reaction kettle, and continuously reacting for 4 hours to obtain an OH-terminated second prepolymer;
(3) dissolving 110g of dicyclohexylmethane diisocyanate in 320g of butanone, dripping the mixture into the reaction kettle at the speed of 14ml/min, and continuing to polymerize for 3 hours to obtain a third prepolymer with NCO at the tail end;
(4) dissolving 32g of triethylene glycol in 480g of butanone, slowly adding the mixture into the reaction kettle, and continuously reacting for 3 hours to obtain a macromolecular polyurethane system;
(5) adding 30g of ammonia water (28%) and 2500g of deionized water into the macromolecular polyurethane system, stirring at 1100rpm for 2h, and extracting butanone by rotary evaporation to obtain the polyurethane.
Comparative example 2
This comparative example provides an aqueous polyurethane resin according to CN201310011715.2, the preparation method of which comprises the following steps:
(1) under the protection of nitrogen, 5400g of poly (carbonate-ether) glycol (with the number average molecular weight of 5400 dalton) is added into a three-mouth bottle, the temperature is raised to 110 ℃, the reduced pressure distillation is carried out for 1.5 hours, the temperature is lowered to 85 ℃, 350g of butanone is added, 620g of isophorone diisocyanate is added dropwise at the dropping speed of 12ml/min, and after the dropwise addition is finished, the reaction is carried out for 4 hours, so as to obtain a first intermediate;
(2) adding 150g of butanone into the first intermediate, cooling to 75 ℃, adding 0.002g of dibutyltin dilaurate, dividing into three batches, adding 143g of dimethylolbutyric acid, and reacting for 1.5 hours after the addition is finished to obtain a second intermediate;
(3) adding 260g of butanone and 270g of diethylene glycol into the second intermediate, heating to 90 ℃, reacting for 2 hours, then adding 4800g of deionized water, then adding 87g of triethylamine dropwise at the speed of 22ml/min, stirring at the speed of 1300rpm for 2 hours, and then distilling under reduced pressure to remove the butanone to obtain the poly (carbonate-ether) waterborne polyurethane which is marked as comparative resin-2.
Comparative example 3
This comparative example is a Bardfish RS-5608 emulsion for interior walls.
Comparative example 4
The present comparative example provides an interior wall coating, the method of preparation comprising the steps of:
(1) putting 24.5 parts by weight of deionized water into a dispersion kettle, starting a dispersion machine, putting 0.45 part by weight of dispersant P30, 0.15 part by weight of wetting agent DOW EH-9, 0.2 part by weight of defoaming agent BASF ST-2410, 0.5 part by weight of antifreeze, 0.2 part by weight of thickening agent 250HHBR and 0.05 part by weight of mildew-proof bactericide into the dispersion kettle in sequence, and stirring at low speed of 600r/min for 10 minutes by using 300-;
(2) sequentially putting 20 parts by weight of titanium dioxide, 15 parts by weight of heavy calcium carbonate, 10 parts by weight of light calcium carbonate and 3.5 parts by weight of talcum powder into a dispersion kettle, and stirring at a high speed of 1400-1800r/min for 30 minutes;
(3) 25 parts by weight of the waterborne polyurethane resin of the comparative example 1 and 0.25 part by weight of the defoaming agent Tego airex-901w are put into a dispersion kettle, stirred at the medium speed of 1200r/min for 10 minutes at 800-.
Comparative example 5
The present comparative example provides an interior wall coating, the method of preparation comprising the steps of:
(1) putting 24.5 parts by weight of deionized water into a dispersion kettle, starting a dispersion machine, putting 0.45 part by weight of dispersant P30, 0.15 part by weight of wetting agent DOW EH-9, 0.2 part by weight of defoaming agent BASF ST-2410, 0.5 part by weight of antifreeze, 0.2 part by weight of thickening agent 250HHBR and 0.05 part by weight of mildew-proof bactericide into the dispersion kettle in sequence, and stirring at low speed of 600r/min for 10 minutes by using 300-;
(2) sequentially putting 20 parts by weight of titanium dioxide, 15 parts by weight of heavy calcium carbonate, 10 parts by weight of light calcium carbonate and 3.5 parts by weight of talcum powder into a dispersion kettle, and stirring at a high speed of 1400-1800r/min for 30 minutes;
(3) 25 parts by weight of the aqueous polyurethane resin of the comparative example 2 and 0.25 part by weight of the defoamer Tegoairex-901w are put into a dispersion kettle, stirred at a medium speed of 1200r/min for 10 minutes at 800-.
Comparative example 6
The present comparative example provides an interior wall coating, the method of preparation comprising the steps of:
(1) putting 24.5 parts by weight of deionized water into a dispersion kettle, starting a dispersion machine, putting 0.45 part by weight of dispersant P30, 0.15 part by weight of wetting agent DOW EH-9, 0.2 part by weight of defoaming agent BASF ST-2410, 0.5 part by weight of antifreeze, 0.2 part by weight of thickening agent 250HHBR and 0.05 part by weight of mildew-proof bactericide into the dispersion kettle in sequence, and stirring at low speed of 600r/min for 10 minutes by using 300-;
(2) sequentially putting 20 parts by weight of titanium dioxide, 15 parts by weight of heavy calcium carbonate, 10 parts by weight of light calcium carbonate and 3.5 parts by weight of talcum powder into a dispersion kettle, and stirring at a high speed of 1400-1800r/min for 30 minutes;
(3) 25 parts by weight of Badfu RS-5608 emulsion for inner walls and 0.25 part by weight of defoamer Tego airex-901w are put into a dispersion kettle, stirred at a medium speed of 1200r/min for 10 minutes at 800-.
Test examples
The first aspect of this test example tested the performance of the odorless aqueous resins of examples 1-5 and comparative examples 1-3, and the data results are shown in Table 1. Compared with comparative examples 1-2, the odorless water-based resin obtained in examples 1-5 has excellent open-can odor, low-temperature film-forming property, water resistance and pigment and filler wrapping property; compared with comparative resin-3, the resin composition has excellent open odor, low-temperature film forming property, tensile strength and elongation at break. From the evaluation of the various properties of the resin, the odorless waterborne resin is suitable for use in interior wall coating systems.
The interior wall coatings of examples 6-10 and comparative examples 4-6 were compared in performance and the data results are shown in table 2. Wherein, compared with the comparative examples 1-2, the paint has obvious advantages in the aspects of heat storage, smell, washing resistance and the like; compared with comparative example 3, the coating has advantages in the aspects of smell, hand feeling, scratch resistance and the like.
Table 1: carbon fixed odor-free water-based resin performance comparison table
Note: for the test convenience, the film forming assistant which is additionally added for necessary test items is the common dipropylene glycol butyl ether, and the adding amount is 5 percentaThe content of the non-volatile matter is measured according to GB/T11175-2002 synthetic resin emulsion test method;bthe grade of the pot opening smell is determined according to the grade when the pot opening smell is smelled by a nose after 48 small trials of pot sealing and storage at room temperature, wherein 1 is the smell maximum, and 10 is the smell free;cthe low-temperature film-forming property is measured at 4 ℃ according to the method in GB/T11175-2002 synthetic resin emulsion test method;dglass transition temperature was measured by differential scanning calorimetry; e tensile strength and elongation at break were determined according to GB/T13022-1991 method for testing tensile Properties of Plastic films; f, measuring the water resistance according to a method of GB/T23999-2009 waterborne wood coating for indoor decoration;gthe pigment and filler wrapping performance grading experiment is 1: resin of 9: the powder dropping condition is observed after the heavy calcium carbonate is used as a simple coating formula, wherein 1 is the most serious, and 10 is the most optimal.
The second aspect of this test example tested the performance of the coatings obtained in examples 11 to 15 and comparative examples 4 to 6, and the test results are shown in Table 2.
Table 2: paint performance comparison table
Note: in the scoring items, 1 is the worst, 10 is the best, and each testing item is carried out by a testing method defined by the national standard GBT 9756-.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the embodiments, and various changes can be made without departing from the gist of the present invention within the knowledge of those skilled in the art. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. The carbon-fixed odorless aqueous resin is characterized by being prepared from the following raw materials: a first pre-mer and a second pre-mer;
the raw materials for preparing the first prepolymer comprise poly (carbonate-ether) polyol and diisocyanate A;
the raw materials for preparing the second prepolymer comprise castor oil, diisocyanate B and polyethylene glycol.
2. The carbon-fixed odorless aqueous resin according to claim 1, wherein the mass ratio of the first prepolymer to the second prepolymer is 1.1 to 3: 1.
3. the carbon-fixed odorless aqueous resin of claim 1 wherein the raw materials for preparing the first prepolymer further comprise an organic solvent and a small molecule chain extender.
4. The carbon-fixed odorless aqueous resin according to claim 1, wherein the mass ratio of the poly (carbonate-ether) polyol to the diisocyanate A in the raw materials for preparing the first prepolymer is 3-8: 1.
5. the carbon-fixed odorless water resin as claimed in claim 1, wherein in the preparation raw material of the second prepolymer, the mass ratio of the castor oil, the diisocyanate B and the polyethylene glycol is 1-3: 1: 0.9 to 1.
6. The carbon-fixed odorless aqueous resin of claim 1 wherein in the second prepolymer, the preparation raw material further comprises an internal emulsifying chain extender;
preferably, the internal emulsion chain extender comprises at least one of dimethylolpropionic acid and dimethylolbutyric acid.
7. The carbon-fixed odorless aqueous resin of claim 1 wherein the raw materials for preparing the odorless aqueous resin further comprise a chain extender and a neutralizing agent.
8. The method for preparing a carbon-fixed odorless aqueous resin according to claim 1 or 2, which comprises mixing the first prepolymer and the second prepolymer, neutralizing and dispersing the mixture after the reaction is completed, and removing impurities to obtain the carbon-fixed odorless aqueous resin.
9. A coating material, characterized in that the raw material for preparing the coating material comprises the carbon-fixed odorless water-based resin as defined in any one of claims 1 to 7.
10. Use of the coating according to claim 9 in the field of decoration.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5859122A (en) * | 1996-10-21 | 1999-01-12 | Nicca Chemical Co., Ltd. | Polycarbonate polyurethane resin composition |
| CN111393596A (en) * | 2020-04-02 | 2020-07-10 | 上海应用技术大学 | Castor oil modified waterborne polyurethane nano-emulsion and preparation method thereof |
| CN111925497A (en) * | 2020-07-02 | 2020-11-13 | 嘉宝莉化工集团股份有限公司 | Self-thickening waterborne polyurethane resin, coating, and preparation method and application thereof |
| CN111925496A (en) * | 2020-07-02 | 2020-11-13 | 嘉宝莉化工集团股份有限公司 | Bio-based self-thickening resin and preparation method and application thereof |
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2021
- 2021-12-02 CN CN202111461464.9A patent/CN114656610B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5859122A (en) * | 1996-10-21 | 1999-01-12 | Nicca Chemical Co., Ltd. | Polycarbonate polyurethane resin composition |
| CN111393596A (en) * | 2020-04-02 | 2020-07-10 | 上海应用技术大学 | Castor oil modified waterborne polyurethane nano-emulsion and preparation method thereof |
| CN111925497A (en) * | 2020-07-02 | 2020-11-13 | 嘉宝莉化工集团股份有限公司 | Self-thickening waterborne polyurethane resin, coating, and preparation method and application thereof |
| CN111925496A (en) * | 2020-07-02 | 2020-11-13 | 嘉宝莉化工集团股份有限公司 | Bio-based self-thickening resin and preparation method and application thereof |
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