CN117659771A - High-solid-content nano water-based color paste and preparation method thereof - Google Patents
High-solid-content nano water-based color paste and preparation method thereof Download PDFInfo
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- CN117659771A CN117659771A CN202311767817.7A CN202311767817A CN117659771A CN 117659771 A CN117659771 A CN 117659771A CN 202311767817 A CN202311767817 A CN 202311767817A CN 117659771 A CN117659771 A CN 117659771A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000587 hyperbranched polymer Polymers 0.000 claims abstract description 33
- 239000012860 organic pigment Substances 0.000 claims abstract description 28
- -1 amino acid compounds Chemical class 0.000 claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 10
- 125000003277 amino group Chemical group 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000013530 defoamer Substances 0.000 claims abstract description 5
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 19
- 229940024606 amino acid Drugs 0.000 claims description 17
- 235000001014 amino acid Nutrition 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000003960 organic solvent Substances 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- 150000003841 chloride salts Chemical class 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 239000002518 antifoaming agent Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000006221 furniture coating Substances 0.000 claims description 5
- 230000004224 protection Effects 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- KNWUVCLZVAITFP-UHFFFAOYSA-N 3,5-diamino-4-methylbenzoic acid Chemical compound CC1=C(N)C=C(C(O)=O)C=C1N KNWUVCLZVAITFP-UHFFFAOYSA-N 0.000 claims description 4
- UENRXLSRMCSUSN-UHFFFAOYSA-N 3,5-diaminobenzoic acid Chemical compound NC1=CC(N)=CC(C(O)=O)=C1 UENRXLSRMCSUSN-UHFFFAOYSA-N 0.000 claims description 4
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 claims description 4
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000004475 Arginine Substances 0.000 claims description 3
- DCXYFEDJOCDNAF-UHFFFAOYSA-N Asparagine Natural products OC(=O)C(N)CC(N)=O DCXYFEDJOCDNAF-UHFFFAOYSA-N 0.000 claims description 3
- DCXYFEDJOCDNAF-REOHCLBHSA-N L-asparagine Chemical compound OC(=O)[C@@H](N)CC(N)=O DCXYFEDJOCDNAF-REOHCLBHSA-N 0.000 claims description 3
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004472 Lysine Substances 0.000 claims description 3
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims description 3
- 229960001230 asparagine Drugs 0.000 claims description 3
- 235000009582 asparagine Nutrition 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229910001510 metal chloride Inorganic materials 0.000 claims description 3
- 239000004576 sand Substances 0.000 claims description 3
- BIKOQOQJOSLXSQ-UHFFFAOYSA-N 3,5-diamino-2,6-dimethylbenzoic acid Chemical compound CC1=C(N)C=C(N)C(C)=C1C(O)=O BIKOQOQJOSLXSQ-UHFFFAOYSA-N 0.000 claims description 2
- ZMWRKPGCMAXNRM-UHFFFAOYSA-N 3,5-diamino-4-(dimethylamino)benzoic acid Chemical compound CN(C)C1=C(N)C=C(C(O)=O)C=C1N ZMWRKPGCMAXNRM-UHFFFAOYSA-N 0.000 claims description 2
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 claims description 2
- ZDXPYRJPNDTMRX-VKHMYHEASA-N L-glutamine Chemical compound OC(=O)[C@@H](N)CCC(N)=O ZDXPYRJPNDTMRX-VKHMYHEASA-N 0.000 claims description 2
- HNDVDQJCIGZPNO-YFKPBYRVSA-N L-histidine Chemical compound OC(=O)[C@@H](N)CC1=CN=CN1 HNDVDQJCIGZPNO-YFKPBYRVSA-N 0.000 claims description 2
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 claims description 2
- ZFOMKMMPBOQKMC-KXUCPTDWSA-N L-pyrrolysine Chemical compound C[C@@H]1CC=N[C@H]1C(=O)NCCCC[C@H]([NH3+])C([O-])=O ZFOMKMMPBOQKMC-KXUCPTDWSA-N 0.000 claims description 2
- ZDXPYRJPNDTMRX-UHFFFAOYSA-N glutamine Natural products OC(=O)C(N)CCC(N)=O ZDXPYRJPNDTMRX-UHFFFAOYSA-N 0.000 claims description 2
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000012875 nonionic emulsifier Substances 0.000 claims description 2
- 239000002798 polar solvent Substances 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 3
- 238000004873 anchoring Methods 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 239000000049 pigment Substances 0.000 description 16
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000003973 paint Substances 0.000 description 6
- 229960001701 chloroform Drugs 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CZBYDJTWLGVCEV-UHFFFAOYSA-N 2,8-diaminononanedioic acid Chemical compound OC(=O)C(N)CCCCCC(N)C(O)=O CZBYDJTWLGVCEV-UHFFFAOYSA-N 0.000 description 2
- 240000005020 Acaciella glauca Species 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 239000001023 inorganic pigment Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 235000003499 redwood Nutrition 0.000 description 2
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001804 chlorine Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/003—Pigment pastes, e.g. for mixing in paints containing an organic pigment
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention provides a high-solid-content nano water-based color paste and a preparation method thereof, wherein the high-solid-content nano water-based color paste comprises the following components in percentage by mass: 1-5% of amino-terminated hyperbranched polymer, 0.5-3% of chloride, 3-5% of emulsifier, 0.8-1% of defoamer, 40-65% of organic pigment and the balance of deionized water, wherein the amino-terminated hyperbranched polymer is prepared by self-polycondensation of amino acid compounds containing at least two molecular weight amino groups. Amino groups of the amino-terminated hyperbranched polymer can be used as anchoring groups to form stronger hydrogen bonds with organic pigments in a system to combine, and meanwhile, a small amount of carboxyl groups and chloride ions in the system can form an electrostatic stable layer with the amino groups, so that stable dispersion of the organic pigments in the nano water-based color paste is finally realized. Due to the hydrophilicity of the amino-terminated hyperbranched polymer, the organic pigment particles are more easily wetted, and the reaggregation of the particles is prevented.
Description
Technical Field
The invention relates to the field of color paste coatings, in particular to a high-solid-content nano water-based color paste and a preparation method thereof.
Background
In recent years, with the enhancement of environmental awareness of people, the requirement of limiting the use of high-VOC-content coating is more established standard, the production, sales and use of organic solvents are completely forbidden in 2004, the development of the coating industry to low-toxicity and low-pollution type coating is promoted, and especially the health and safety problems of furniture coating become increasingly important. The development of the water-based paint can meet the time requirement and finally replace solvent-based paint.
In the field of furniture coating, the water-based paint is required to be various in variety, colorful in color, bright in appearance, relatively durable, safe and environment-friendly. The aqueous color paste-pigment dispersion is a coloring material necessary for aqueous paint, is a pigment preparation prepared by dispersing pigment particles in water by taking water as a dispersion medium, generally consists of water, powdery pigment, a surfactant, a cosolvent, a humectant and the like, and can be added with some assistants for improving the performance according to the use and storage requirements. Excellent aqueous color paste must have good compatibility with aqueous polymer emulsion, uniform texture, no cross-linking agent and alkylphenol polyglycol ether solvent, and high-quality pigment with excellent weather resistance, light aging resistance, chemical corrosion resistance and ultraviolet resistance should be selected on the materials. The finished product aqueous color paste has the excellent performances of strong tinting strength, good fluidity, no caking, no sedimentation, no coarsening after long-time storage, high solid content, stable product viscosity, low foam, no air drying, reuse after being dissolved in freezing, no mildew, low VOC and the like.
Currently, pigments can be classified into inorganic pigments and organic pigments according to their chemical composition. Inorganic pigments are generally complex mixtures with metal components, such as titanium dioxide, iron oxide, etc., having excellent thermal and light stability. The organic pigment has the characteristics of remarkable color, bright tone, high tinting strength and the like, but the organic pigment often has the problems of poor heat resistance and the like in the use process. With the continuous improvement of the pigment modification technology level, the problems are primarily improved, and the application field of the organic pigment is expanded to a certain extent, so that the organic pigment becomes an indispensable coloring material for producing various industrial products. However, the pigment still has some drawbacks in the use process, such as easy agglomeration in a dispersion medium, poor dispersion stability, and the like. Dispersing pigment in water by ultrasonic or ball milling, etc., the pigment dispersion liquid looks stable, and pigment particles are aggregated and deposited after standing for a period of time.
More importantly, due to the market development trend of high-end redwood furniture in recent years, the color paste used on the redwood furniture is required to have higher transparency and vividness. To achieve the retention of vividness, the amount of pigment used is correspondingly increased, with the result that: the viscosity of the color paste is increased, the system is unstable, and the like.
Disclosure of Invention
The invention provides a high-solid-content nano water-based color paste and a preparation method thereof, aiming at solving the problem that the brightness and the viscosity or storage stability of a system of the existing common color paste cannot be compatible.
The high-solid-content nano water-based color paste comprises the following components in percentage by mass: 1-5% of amino-terminated hyperbranched polymer, 0.5-3% of chloride, 3-5% of emulsifier, 0.8-1% of defoamer, 40-65% of organic pigment and the balance of deionized water, wherein the amino-terminated hyperbranched polymer is obtained by polycondensation of amino acid compounds containing at least two molecular weight amino groups.
In some embodiments of the present invention, the amino-terminated hyperbranched polymer is prepared using an amino-acid compound comprising at least two molecular weight amino groups that is at least one of 3, 5-diaminobenzoic acid, 3, 5-diamino-4-methylbenzoic acid, 3, 5-diamino-4- (dimethylamino) -benzoic acid, 3, 5-diamino-2, 6-dimethylbenzoic acid, tryptophan, asparagine, glutamine, arginine, histidine, lysine, and pyrrolysine.
In preparing the amino-terminated hyperbranched polymer, the inventors studied the case when amino acid compounds of different structures are used as raw materials for self-polycondensation, and the results show that: when the aromatic amino acid compound is used, if the content of aromatic benzene ring is higher, the hardness of the obtained amino-terminated hyperbranched polymer is rapidly increased, the amino-terminated hyperbranched polymer is difficult to grind in a color paste system after being combined with an organic pigment, and the transparency of the paint formed by taking the color paste as a component on the surface of furniture is poor; when aliphatic amino acid compounds are used, if the carbon chain is too long, the reactivity is low and the reaction conditions required are severe when preparing amino-terminated hyperbranched polymers. Therefore, based on the ideal effect of the color paste application and the preparation cost, the amino-terminated hyperbranched polymer is prepared by selecting the amino acid compounds as raw materials.
In some embodiments of the invention, the method of preparing an amino-terminated hyperbranched polymer comprises the steps of:
s1: adding an amino acid compound into a reaction container, heating and stirring to dissolve the amino acid compound in a polar solvent, adjusting the temperature to 150-200 ℃, removing water for 1-2h under normal pressure, vacuumizing to negative pressure, keeping for 2-3h, and cooling to room temperature;
s2: under the protection of inert gas, adding the product obtained in the step S1 and an organic solvent into another reaction container, stirring and uniformly mixing, heating, condensing and refluxing for reaction for 8-12h, cooling, decompressing and distilling the organic solvent, cooling, pouring the organic solvent into an insoluble organic solvent for precipitation, and washing and drying to obtain the amino-terminated hyperbranched polymer.
In some embodiments of the present invention, when the amino-terminated hyperbranched polymer is prepared, the organic solvent in S2 is a mixed solution obtained by mixing N-methylpyrrolidone and a benzene solvent according to a volume ratio of 1:1-1.5.
In some embodiments of the invention, the temperature conditions of heating in S2 are 150-180 ℃ when preparing the amino-terminated hyperbranched polymer.
In some embodiments of the present invention, when preparing the amino-terminated hyperbranched polymer, the immiscible organic solvent in S2 is at least one of halogenated methane, and chloroform, dichloromethane, trichloromethane, etc. may be specifically selected.
In some embodiments of the present invention, the chloride salt is a monovalent metal chloride salt, and the specific choice may be sodium chloride, potassium chloride, etc.; the emulsifier is nonionic emulsifier, and specifically selected from nonylphenol polyoxyethylene ether NP-10 of Jinan YuanBaolai chemical technology Co., ltd, dodecylphenol polyoxyethylene ether OP-10 of Errelke chemical group Co., ltd, fatty alcohol polyoxypropylene ether PPG-20 of Jiangsu sea-An petrochemical plant, etc.
In the invention, monovalent metal chloride salt is selected to be added, because the inventor finds that the existence of chloride ions can form an electrostatic stable layer together with carboxyl groups in the amino-terminated hyperbranched polymer and amino groups, so that the organic pigment combined by the amino groups and the amino-terminated hyperbranched polymer can be stably dispersed in a color paste system, and the existence of the electrostatic stable layer can prevent the organic pigment from precipitating and separating out after standing for a period of time, so that the stability of the organic pigment is greatly improved; the free metal ions in the system are limited by the charge quantity carried by the free metal ions and the use amount of metal salt, so that the carboxyl groups in the system can not be fully occupied, the static stable layer is not seriously damaged, and even in some cases, the free metal ions can also participate in forming the static stable layer.
In some embodiments of the present invention, the defoamer is an organosilicon defoamer, and specifically BYK028, BYK110, BYK530, BYK725, BYK1794, etc. of bikes, germany may be selected.
The preparation method of the high-solid-content nano water-based color paste comprises the following steps:
SS1: adding the organic pigment into a ball mill, adding the amino-terminated hyperbranched polymer according to the adding speed of 0.5-1kg/min, and grinding for 30-60min after the adding is finished;
SS2: sequentially adding chloride, an emulsifying agent, a defoaming agent and deionized water into a stirring kettle, stirring at a speed of 1000-1200r/min for 15-20min, adding the organic pigment treated in SS1, and stirring for 30-50min at a speed of 2000-2300 r/min;
SS3: after the system with the SS2 evenly mixed is transferred into a high-speed homogenizer for dispersion, adding an ultrafine nano sand mill for grinding for 3-5 times, so that the solid particle size in the color paste is not more than 150nm;
SS4: filtering the color paste ground in SS3 with a filter bag of 100-240nm for 2-3 times to obtain the high-solid-content nano water-based color paste.
In some embodiments of the present invention, the resulting high solids nano-aqueous color paste has a viscosity of less than 100CPS.
The high-solid-content nano water-based color paste is applied to the field of furniture coating.
The beneficial effects are that: compared with the prior art, the high-solid-content nano water-based color paste provided by the invention has the following advantages:
1. the amino-terminated hyperbranched polymer is added to promote the dispersibility of the organic pigment in the color paste, and the static stable layer formed between chloride ions and amino is utilized to realize the stable dispersion of the organic pigment, and the hyperbranched structure prevents the reaggregation of pigment particles; the hydrophilicity of the amino-terminated hyperbranched polymer ensures that a new interface generated in the grinding and crushing process of the organic pigment is easier to wet;
2. the pigment content is higher than that of the traditional color paste, but the viscosity is not increased obviously (the viscosity of the obtained aqueous color paste is less than 100 CPS); and the particle size of the pigment is nano-scale, so that the pigment can better permeate into the base material when in application, and the formed paint surface is more bright and transparent in color.
Detailed Description
The invention is described in further detail below with reference to examples. The following examples and comparative examples are illustrative of the present invention and are not intended to limit the present invention. Other combinations and various modifications within the spirit of the invention may be made without departing from the spirit or scope of the invention.
The preparation of the amino-terminated hyperbranched polymers used in the examples is illustrated below:
amino-terminated hyperbranched polymer-1
S1: adding 34.12g (0.2 mol) of 3, 5-diaminobenzoic acid into a reaction vessel, heating and stirring to dissolve the 3, 5-diaminobenzoic acid in 100ml of dimethyl sulfoxide, adjusting the temperature to 200 ℃, dehydrating for 1h under normal pressure, vacuumizing to 8000Pa, distilling for 2h, removing dimethyl sulfoxide, and cooling to room temperature;
s2: under the protection of nitrogen, adding 20g of the product obtained by S1, 50ml of N-methylpyrrolidone and 50ml of toluene into another reaction container, stirring and mixing uniformly, heating to 180 ℃ and condensing and refluxing for reaction for 12 hours, cooling, decompressing and distilling out an organic solvent, cooling, pouring into chloroform for precipitation, and washing and drying to obtain the amino-terminated hyperbranched polymer-1.
Amino-terminated hyperbranched polymer-2
S1: adding 33.24g (0.2 mol) of 3, 5-diamino-4-methylbenzoic acid into a reaction vessel, heating and stirring to dissolve the 3, 5-diamino-4-methylbenzoic acid in 100ml of dimethyl sulfoxide, adjusting the temperature to 180 ℃, dehydrating for 1.5h under normal pressure, vacuumizing to 7000Pa, maintaining for 3h, removing the dimethyl sulfoxide, and cooling to room temperature;
s2: under the protection of nitrogen, adding 20g of the product obtained by S1, 50ml of N-methylpyrrolidone and 65ml of toluene into another reaction vessel, stirring and mixing uniformly, heating to 160 ℃ and condensing and refluxing for reaction for 10 hours, cooling, decompressing and distilling out an organic solvent, cooling, pouring into chloroform for precipitation, and washing and drying to obtain the amino-terminated hyperbranched polymer-2.
Amino-terminated hyperbranched polymer-3
S1: adding 40.8g (0.2 mol) tryptophan into a reaction vessel, heating and stirring to dissolve the tryptophan in 100ml dimethyl sulfoxide, adjusting the temperature to 150 ℃, removing water for 2 hours under normal pressure, vacuumizing to 7000Pa, maintaining for 3 hours, removing the dimethyl sulfoxide, and cooling to room temperature;
s2: under the protection of nitrogen, adding 20g of the product obtained by S1, 50ml of N-methylpyrrolidone and 75ml of toluene into another reaction container, stirring and mixing uniformly, heating to 150 ℃ and condensing and refluxing for reaction for 8 hours, cooling, decompressing and distilling out an organic solvent, cooling, pouring into chloroform for precipitation, and washing and drying to obtain the amino-terminated hyperbranched polymer-3.
Amino-terminated hyperbranched polymer-4
The preparation process is the same as that of the amino-terminated hyperbranched polymer-3, except that the amino acid compound used is asparagine.
Amino-terminated hyperbranched polymer-5
The preparation process is the same as that of the amino-terminated hyperbranched polymer-3, except that the amino acid compound used is arginine.
Amino-terminated hyperbranched polymer-6
The preparation process is the same as that of the amino-terminated hyperbranched polymer-3, except that the amino acid compound used is lysine.
Amino-terminated hyperbranched polymer-7
The preparation process is the same as that of the amino-terminated hyperbranched polymer-3, except that the amino acid compound used is 1, 4-diamino-6, 7-dicarboxylic acid naphthalene (CAS: 859072-50-7).
Amino-terminated hyperbranched polymer-8
The preparation process is the same as that of the amino-terminated hyperbranched polymer-3, except that the amino acid compound used is 2, 8-diaminoazelaic acid (CAS: 98951-66-7).
The aqueous color pastes of examples 1-8 and comparative examples 1-4 were prepared according to the components and corresponding parts by weight given in tables 1-1, 1-2 and 1-3, the preparation steps being:
SS1: adding the organic pigment into a ball mill, adding the amino-terminated hyperbranched polymer according to the adding speed of 0.5-1kg/min, and grinding for 30-60min after the adding is finished;
SS2: sequentially adding chloride, an emulsifying agent, a defoaming agent and deionized water into a stirring kettle, stirring at a speed of 1000-1200r/min for 15-20min, adding the organic pigment treated in SS1, and stirring for 30-50min at a speed of 2000-2300 r/min;
SS3: after the system with the SS2 evenly mixed is transferred into a high-speed homogenizer for dispersion, adding an ultrafine nano sand mill for grinding for 3-5 times, so that the solid particle size in the color paste is not more than 150nm;
SS4: filtering the color paste ground in SS3 with a filter bag of 100-240nm for 2-3 times to obtain the high-solid-content nano water-based color paste.
The operating conditions of each of the examples and comparative examples were within the above-described ranges, and no additional special requirements were found.
The aqueous color paste obtained in the above examples and comparative examples was subjected to the following performance tests:
viscosity: testing at 25deg.C with NDJ-5S rotary digital viscometer;
dispersion stability: centrifuging at 3000 rpm for 30min, and checking whether precipitate is generated.
As can be seen from the data in Table 2, the nano water-based color paste provided by the invention has lower viscosity (less than 100 cps), even if the nano water-based color paste is subjected to the damp-heat environment treatment at 60 ℃ and 70% RH, the viscosity of the nano water-based color paste does not exceed 210cps, and precipitation delamination is not seen after the nano water-based color paste is subjected to high-speed centrifugation, so that the obtained nano water-based color paste has proper viscosity and excellent dispersion stability of the organic pigment in the color paste. This is mainly due to the addition of the amino-terminated hyperbranched polymer and chloride: because the amino-terminated hyperbranched polymer or the addition of the chlorine salt is removed respectively by the arrangement of comparative examples 1-2, the viscosity and dispersion stability of the obtained aqueous color paste are both deteriorated. The results of comparative examples 3-4 show that the addition of the amino-terminated hyperbranched polymer and the chloride salt should be proper in mass percent, otherwise the viscosity and dispersion stability of the aqueous color paste are also affected, which may be due to the fact that when the hyperbranched structure of the amino-terminated hyperbranched polymer exceeds a certain content in the system, intermolecular forces are formed, the viscosity of the aqueous color paste is increased together with the organic pigment, and the addition of the chloride salt is excessive, so that the thief breaks down the static stable layer, thereby the stability of the aqueous color paste is deteriorated.
In conclusion, the high-solid-content nano water-based color paste prepared according to the technical scheme provided by the invention can still keep lower viscosity while containing higher-concentration organic pigment, and the high-concentration organic pigment can also keep excellent dispersion stability in a system, so that the high-solid-content nano water-based color paste has good application prospect in the field of furniture coating.
Claims (10)
1. The high-solid-content nano water-based color paste is characterized by comprising the following components in percentage by mass: 1-5% of amino-terminated hyperbranched polymer, 0.5-3% of chloride, 3-5% of emulsifier, 0.8-1% of defoamer, 40-65% of organic pigment and the balance of deionized water, wherein the amino-terminated hyperbranched polymer is obtained by polycondensation of amino acid compounds containing at least two molecular weight amino groups.
2. The high-solid-content nano-aqueous color paste according to claim 1, wherein the amino acid compound containing at least two molecular weight amino groups is at least one of 3, 5-diaminobenzoic acid, 3, 5-diamino-4-methylbenzoic acid, 3, 5-diamino-4- (dimethylamino) -benzoic acid, 3, 5-diamino-2, 6-dimethylbenzoic acid, tryptophan, asparagine, glutamine, arginine, histidine, lysine and pyrrolysine.
3. The high-solid-content nano-aqueous color paste according to claim 1, wherein the preparation method of the amino-terminated hyperbranched polymer comprises the following steps:
s1: adding an amino acid compound into a reaction container, heating and stirring to dissolve the amino acid compound in a polar solvent, adjusting the temperature to 150-200 ℃, removing water for 1-2h under normal pressure, vacuumizing to negative pressure, keeping for 2-3h, and cooling to room temperature;
s2: under the protection of inert gas, adding the product obtained in the step S1 and an organic solvent into another reaction container, stirring and uniformly mixing, heating, condensing and refluxing for reaction for 8-12h, cooling, decompressing and distilling the organic solvent, cooling, pouring the organic solvent into an insoluble organic solvent for precipitation, and washing and drying to obtain the amino-terminated hyperbranched polymer.
4. The high-solid-content nano water-based color paste according to claim 3, wherein the organic solvent in S2 is a mixed solution obtained by mixing N-methyl pyrrolidone and benzene solvent according to a volume ratio of 1:1-1.5.
5. The high-solid-content nano-aqueous color paste according to claim 3, wherein the heating temperature in S2 is 150-180 ℃.
6. The high-solid-content nano-aqueous color paste according to claim 3, wherein the immiscible organic solvent in S2 is at least one of halomethanes.
7. The high-solid-content nano-aqueous color paste according to claim 1, wherein the chloride salt is monovalent metal chloride salt; the emulsifier is a nonionic emulsifier; the defoaming agent is an organosilicon defoaming agent.
8. The method for preparing the high-solid-content nano-aqueous color paste according to claims 1 to 7, which is characterized by comprising the following steps:
SS1: adding the organic pigment into a ball mill, adding the amino-terminated hyperbranched polymer according to the adding speed of 0.5-1kg/min, and grinding for 30-60min after the adding is finished;
SS2: sequentially adding chloride, an emulsifying agent, a defoaming agent and deionized water into a stirring kettle, stirring at a speed of 1000-1200r/min for 15-20min, adding the organic pigment treated in SS1, and stirring for 30-50min at a speed of 2000-2300 r/min;
SS3: after the system with the SS2 evenly mixed is transferred into a high-speed homogenizer for dispersion, adding an ultrafine nano sand mill for grinding for 3-5 times, so that the solid particle size in the color paste is not more than 150nm;
SS4: filtering the color paste ground in SS3 with a filter bag of 100-240nm for 2-3 times to obtain the high-solid-content nano water-based color paste.
9. The method for preparing the high-solid-content nano-aqueous color paste according to claim 8, wherein the viscosity of the obtained high-solid-content nano-aqueous color paste is less than 100CPS.
10. Use of the high-solid-content nano-aqueous color paste according to claims 1-7 in the field of furniture coating.
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