CN118359778A - Environment-friendly waterproof agent and preparation method thereof - Google Patents
Environment-friendly waterproof agent and preparation method thereof Download PDFInfo
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- CN118359778A CN118359778A CN202410633797.2A CN202410633797A CN118359778A CN 118359778 A CN118359778 A CN 118359778A CN 202410633797 A CN202410633797 A CN 202410633797A CN 118359778 A CN118359778 A CN 118359778A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 63
- 238000001035 drying Methods 0.000 claims abstract description 61
- 238000000576 coating method Methods 0.000 claims abstract description 46
- 239000011248 coating agent Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 24
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229920000180 alkyd Polymers 0.000 claims abstract description 20
- 239000003973 paint Substances 0.000 claims abstract description 20
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- 239000000839 emulsion Substances 0.000 claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000002378 acidificating effect Effects 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 7
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 7
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 7
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 4
- 238000002604 ultrasonography Methods 0.000 claims abstract description 3
- 238000000265 homogenisation Methods 0.000 claims abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 17
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 16
- 229910017052 cobalt Inorganic materials 0.000 claims description 13
- 239000010941 cobalt Substances 0.000 claims description 13
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 13
- 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 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 150000002910 rare earth metals Chemical class 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052791 calcium Inorganic materials 0.000 claims description 11
- 239000011575 calcium Substances 0.000 claims description 11
- 235000010215 titanium dioxide Nutrition 0.000 claims description 11
- 239000011701 zinc Substances 0.000 claims description 11
- 229910052725 zinc Inorganic materials 0.000 claims description 11
- 239000002270 dispersing agent Substances 0.000 claims description 10
- -1 drier Substances 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 238000004078 waterproofing Methods 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 230000002940 repellent Effects 0.000 claims description 3
- 239000005871 repellent Substances 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000001038 titanium pigment Substances 0.000 claims 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 31
- 238000012360 testing method Methods 0.000 description 17
- 239000003921 oil Substances 0.000 description 7
- 235000019198 oils Nutrition 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 235000009161 Espostoa lanata Nutrition 0.000 description 4
- 240000001624 Espostoa lanata Species 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 230000001680 brushing effect Effects 0.000 description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000002596 correlated effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 125000005372 silanol group Chemical group 0.000 description 2
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000870659 Crassula perfoliata var. minor Species 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 229920001600 hydrophobic polymer Polymers 0.000 description 1
- WUQVMHPQRIQJMG-UHFFFAOYSA-L iron(2+);6-methylheptanoate Chemical compound [Fe+2].CC(C)CCCCC([O-])=O.CC(C)CCCCC([O-])=O WUQVMHPQRIQJMG-UHFFFAOYSA-L 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- ADJMNWKZSCQHPS-UHFFFAOYSA-L zinc;6-methylheptanoate Chemical compound [Zn+2].CC(C)CCCCC([O-])=O.CC(C)CCCCC([O-])=O ADJMNWKZSCQHPS-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention provides an environment-friendly waterproof agent and a preparation method thereof, belonging to the technical field of paint, wherein the preparation method comprises the following steps: s1, putting 45g of butyl acrylate, 24g of isooctyl acrylate, 20g of styrene, 1g of vinyl triethoxysilane, 5g of methacryloxyethyl trimethyl ammonium chloride, 60g of 4% polyvinyl alcohol aqueous solution and 10g of 8% acrylamide aqueous solution into a homogenizer for homogenization and ultrasound to obtain a pre-emulsion; s2, mixing 3mL of methacryloxypropyl trimethoxysilane, 15mL of deionized water and 8mL of ethanol, stirring and hydrolyzing for 1h at 40 ℃ under the condition of pH=3, and adding 30mL of acidic silica sol to obtain modified silica sol; s3, pouring the pre-emulsion and the modified silica sol into a three-mouth bottle, adding 1g of azo diiso Ding Mi hydrochloride and 276g of deionized water, and reacting for 6.5 hours at 65 ℃ under the protection of nitrogen to obtain the environment-friendly waterproof agent. The environment-friendly waterproof agent prepared by the invention is used together with the metal salt drier, so that the alkyd resin coating has excellent waterproof performance while quick surface drying and real drying are ensured.
Description
Technical Field
The invention belongs to the technical field of paint, and particularly relates to an environment-friendly waterproof agent and a preparation method thereof.
Background
Alkyd resin paint is a synthetic resin paint with alkyd resin as a main film forming substance. Alkyd resins are resins made by reacting fatty acids (or their corresponding vegetable oils), dibasic acids, and polyols. The common polyalcohol used for producing alkyd resin is glycerol, pentaerythritol, trimethylolpropane, etc.; commonly used dibasic acids are phthalic anhydride (i.e., phthalic anhydride), isophthalic acid, and the like. The alkyd resin paint has the characteristics of weather resistance, good adhesive force, brightness, plumpness and the like, and is convenient to construct. Meanwhile, the coating film is softer and has poor waterproof property, so that a waterproof agent needs to be added.
On the other hand, because alkyd resins themselves dry at a slower rate, in order to increase the drying rate of the coating film, and reduce the construction time, it is also necessary to add a drier to the alkyd coating to accelerate the evaporation of the solvent in the coating film and/or to promote the curing process of the coating film.
However, in the alkyd coating construction process, the drying acceleration effect caused by the use of the drier may cause the performance of the waterproofing agent to be negatively affected. For example, zinc, cobalt, manganese and the like, which are metal salt drier, can accelerate the oxidative polymerization process of oil in the coating, thereby accelerating the drying of the coating, and meanwhile, the waterproof agent can be unevenly distributed in the coating and can not form a continuous and even waterproof layer, so that the overall waterproof performance of the coating can be reduced.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides an environment-friendly waterproof agent and a preparation method thereof, and when the prepared environment-friendly waterproof agent is used together with a metal salt drier, the prepared alkyd resin coating can be ensured to be quick in surface drying and real drying and has excellent waterproof performance.
In order to achieve the above object, the present invention provides the following technical solutions:
The preparation method of the environment-friendly waterproof agent comprises the following steps:
s1, putting 45g of butyl acrylate, 24g of isooctyl acrylate, 20g of styrene, 1g of vinyl triethoxysilane, 5g of methacryloxyethyl trimethyl ammonium chloride, 60g of 4% polyvinyl alcohol aqueous solution and 10g of 8% acrylamide aqueous solution into a homogenizer for homogenizing, and performing ultrasound to obtain a pre-emulsion;
S2, mixing 3mL of methacryloxypropyl trimethoxysilane, 15mL of deionized water and 8mL of ethanol, stirring and hydrolyzing for 1h at 40 ℃ under the condition of pH=3, adding 30mL of acidic silica sol, and reacting to obtain modified silica sol;
S3, pouring the pre-emulsion obtained in the step S1 and the modified silica sol obtained in the step S2 into a three-mouth bottle, and adding 1g of azo diiso Ding Mi hydrochloride and 276g of deionized water to react for 6.5 hours at 65 ℃ under the protection of nitrogen, thus obtaining the environment-friendly waterproof agent.
Further, in S1, homogenizing for 45-60min at normal temperature by using a homogenizer at 5000 r/min; 50Hz ultrasonic dispersion is carried out for 30min.
Further, in S2, 1M hydrochloric acid solution is used to adjust ph=3.
An environment-friendly waterproof agent is prepared by adopting the preparation method.
Further, the environment-friendly waterproof agent is used for preparing quick-drying waterproof paint; the quick-drying waterproof coating comprises the following raw material components in parts by weight: 45-55 parts of alkyd resin, 10-15 parts of titanium dioxide, 8-12 parts of talcum powder, 0.8-1 part of drier, 0.5-0.8 part of dispersing agent, 0.1-0.2 part of antiskinning agent, 0.2-0.3 part of environment-friendly waterproof agent and 4-7 parts of solvent.
Further, the drier comprises the following raw material components in parts by weight: 2-4 parts of 10% cobalt iso-octoate, 2-4 parts of 12% rare earth iso-octoate, 10-12 parts of 5% calcium iso-octoate, 12-14 parts of 6% iron iso-octoate and 13-15 parts of 9% zinc iso-octoate.
Further, the titanium dioxide comprises rutile titanium dioxide and/or anatase titanium dioxide.
Further, the particle size of the talcum powder is 1000-1500 meshes, and the oil absorption is 30-35 g/100g.
Further, the solvent comprises xylene and/or 200# solvent oil.
Further, the preparation method of the quick-drying waterproof paint comprises the following steps: adding alkyd resin into a dispersing machine, controlling the stirring speed at 800-1000rpm/min, then adding titanium white powder, talcum powder, drier, dispersing agent, antiskinning agent, waterproofing agent and solvent, continuously maintaining the stirring speed at 800-1000rpm/min, and stirring for 10-15min to obtain a mixture; and (3) putting the mixture into a grinder, and grinding until the fineness is not more than 25 mu m, thus obtaining the quick-drying waterproof coating.
The application has the following beneficial effects:
1. In the preparation of the environment-friendly waterproof agent, butyl acrylate, isooctyl acrylate and styrene are taken as main monomers to participate in copolymerization reaction to form a hydrophobic polymer chain; vinyl triethoxysilane and methacryloxyethyl trimethyl ammonium chloride as functional additives can provide additional crosslinking sites, thereby improving compactness and water resistance of the coating film in subsequent coating film formation; the aqueous solution of polyvinyl alcohol and the aqueous solution of acrylamide are used as dispersing agents and stabilizing agents to help form a stable pre-emulsion system; azo diiso Ding Mi hydrochloride is used as an initiator to initiate polymerization; the methacryloxypropyl trimethoxy silane can be hydrolyzed to generate silanol groups, and can be subjected to cross-linking reaction with polymer chains in a pre-emulsion system to form a more compact three-dimensional network structure; the participation of the acidic silica sol provides silicate species which can further react with polymer chains and silanol groups to subsequently enhance the crosslinking density and water resistance of the coating film.
2. In the preparation of the drier, 10% cobalt iso-octoate, 12% rare earth iso-octoate, 5% calcium iso-octoate, 6% iron iso-octoate and 9% zinc iso-octoate are reasonably proportioned, so that the quick-drying waterproof coating can be ensured to be quickly surface-dried and dried; experiments prove that the simple film drying speed is neither obviously positively correlated nor obviously inversely correlated with the waterproof performance playing effect of the environment-friendly waterproof agent; the time difference between the surface drying time and the actual drying time of the coating film has a positive correlation with the water resistance exerted by the environment-friendly waterproof agent; the drier is matched with the environment-friendly waterproof agent, so that the prepared quick-drying waterproof coating can be quickly surface-dried and dried, and has excellent waterproof performance.
Drawings
FIG. 1 is a graph showing the comparison trend of the surface dry time, the actual dry time and the time difference of the quick-drying waterproof paint brush plates prepared in the examples 1 to 7 of the invention and the comparative examples 1 to 4;
FIG. 2 is a graph showing the trend of comparative data of water contact angle test of coating films after the brush plates of quick-drying waterproof coating materials prepared in examples 1 to 7 of the present invention and comparative examples 1 to 4 are dried.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials of the examples and comparative examples of the present application are commercially available in general except for the specific descriptions.
Example 1: a preparation method of quick-drying waterproof paint comprises the following steps: according to the parts by weight, 50 parts of alkyd resin is put into a dispersing machine, the stirring speed is controlled at 900rpm/min, then 12 parts of titanium white powder, 10 parts of talcum powder, 0.9 part of drier, 0.7 part of dispersing agent, 0.15 part of antiskinning agent, 0.25 part of environment-friendly waterproof agent and 6 parts of solvent are added, and the stirring speed is continuously maintained at 900rpm/min, and the stirring is continued for 13min, so that the mixture is obtained. And then the mixture is put into a grinder, and ground to the fineness of not more than 25 mu m, thus obtaining the quick-drying waterproof coating.
Wherein the alkyd resin is industrial grade 389-9A alkyd resin, which is purchased from Hua New Material (Shandong) Inc. The titanium dioxide is rutile type titanium dioxide R-930, and is purchased from Hebei color pigment Limited. The talcum powder is GT-202 superfine talcum powder, the fineness is 1250 meshes, and the oil absorption detection data is 30-35g/100g. The dispersant was BYK-161. Anti-skinning agent KL-841 was purchased from Saint Anhua chemical Co., ltd. The solvent is No. 200 solvent oil.
The drier comprises the following raw material components in parts by weight: 3 parts of 10% cobalt iso-octoate, 3 parts of 12% rare earth iso-octoate, 11 parts of 5% calcium iso-octoate, 13 parts of 6% iron iso-octoate and 14 parts of 9% zinc iso-octoate. 10% cobalt iso-octoate, 12% rare earth iso-octoate, 5% calcium iso-octoate, 6% iron iso-octoate and 9% zinc iso-octoate were all purchased from paint auxiliary company, central Mountain in Zhengzhou, and the solvents were 200# solvent oil, as shown in table 1.
TABLE 1 Standard content of the drier components
| Name of the name | Appearance of | Metal content (%) | Solution stability |
| Cobalt iso-octoate | Purple liquid | 10±0.2 | Transparent and precipitate-free |
| Isooctanoic acid calcium salt | Pale yellow liquid | 5±0.2 | Transparent and precipitate-free |
| Zinc iso-octoate | Yellow liquid | 9±0.2 | Transparent and precipitate-free |
| Isooctanoic acid rare earth | Pale yellow liquid | 12±0.2 | Transparent and precipitate-free |
| Isooctanoic acid iron | Dark brown liquid | 6±0.3 | Transparent and precipitate-free |
The preparation method of the environment-friendly waterproof agent comprises the following steps:
S1, 45g of butyl acrylate, 24g of isooctyl acrylate, 20g of styrene, 1g of vinyl triethoxysilane, 5g of methacryloxyethyl trimethyl ammonium chloride, 60g of 4% polyvinyl alcohol aqueous solution and 10g of 8% acrylamide aqueous solution are put into a homogenizer, and the homogenizer is homogenized for 50min at 5000r/min at normal temperature, and then dispersed for 30min at 50Hz in an ultrasonic manner, so as to obtain the pre-emulsion.
S2, mixing 3mL of methacryloxypropyl trimethoxysilane, 15mL of deionized water and 8mL of ethanol, adjusting pH to be 3 by using 1M hydrochloric acid solution as an adjusting agent at 40 ℃, stirring and hydrolyzing for 1h, adding 30mL of commercial acidic silica sol, and reacting to obtain the modified silica sol.
When adjusting the pH, the initial pH of the solution is first measured using a pH meter to determine how much of the adjustor needs to be added. The hydrochloric acid solution was slowly added while stirring to ensure uniform mixing, taking care not to add too much at one time to avoid exceeding the target pH. In the process of dropwise adding the hydrochloric acid solution, the pH change of the solution is continuously monitored, the dropwise adding speed is slowed down when the pH value is close to a target value, and the dosage is finely controlled. Once the pH of the solution reached 3, the addition of hydrochloric acid solution was stopped and stirring continued for a period of time to ensure a stable pH. If the pH is inadvertently too low, the callback may be selected using NaOH solution to achieve the desired pH.
The commercial acidic silica sol is chemical nano-scale acidic silica sol with the content of 30 percent and is purchased from Guangzhou Changbright chemical industry Co.
S3, pouring the pre-emulsion obtained in the step S1 and the modified silica sol obtained in the step S2 into a three-mouth bottle, and adding 1g of azo diiso Ding Mi hydrochloride and 276g of deionized water to react for 6.5 hours at 65 ℃ under the protection of nitrogen, thus obtaining the environment-friendly waterproof agent.
Azo diiso Ding Mi hydrochloride is an azo initiator V50, and is purchased from Zhongshan until new materials are available.
Example 2: this embodiment differs from embodiment 1 in that: the quick-drying waterproof paint has different raw material component amounts.
In particular to a preparation method of quick-drying waterproof paint, which comprises the following steps: according to the weight portions, 45 portions of alkyd resin are put into a dispersing machine, the stirring speed is controlled at 900rpm/min, then 10 portions of titanium white, 8 portions of talcum powder, 0.8 portion of drier, 0.5 portion of dispersing agent, 0.1 portion of antiskinning agent, 0.2 portion of environment-friendly waterproof agent and 4 portions of solvent are added, and the stirring speed is continuously maintained at 900rpm/min, and the stirring is continued for 13min, so that the mixture is obtained. And then the mixture is put into a grinder, and ground to the fineness of not more than 25 mu m, thus obtaining the quick-drying waterproof coating.
Example 3: this embodiment differs from embodiment 1 in that: the quick-drying waterproof paint has different raw material component amounts.
In particular to a preparation method of quick-drying waterproof paint, which comprises the following steps: according to the parts by weight, 55 parts of alkyd resin is put into a dispersing machine, the stirring speed is controlled at 900rpm/min, then 15 parts of titanium white, 12 parts of talcum powder, 1 part of drier, 0.8 part of dispersing agent, 0.2 part of antiskinning agent, 0.3 part of environment-friendly waterproof agent and 7 parts of solvent are added, and the stirring speed is continuously maintained at 900rpm/min, and the stirring is continued for 13min, so that the mixture is obtained. And then the mixture is put into a grinder, and ground to the fineness of not more than 25 mu m, thus obtaining the quick-drying waterproof coating.
Example 4: this embodiment differs from embodiment 1 in that: the quick-drying waterproof paint has different raw material component amounts.
In particular to a preparation method of quick-drying waterproof paint, which comprises the following steps: according to the weight portions, 55 portions of alkyd resin are put into a dispersing machine, the stirring speed is controlled at 900rpm/min, then 15 portions of titanium white, 12 portions of talcum powder, 0.8 portion of drier, 0.5 portion of dispersing agent, 0.1 portion of antiskinning agent, 0.2 portion of environment-friendly waterproof agent and 4 portions of solvent are added, and the stirring speed is continuously maintained at 900rpm/min, and the stirring is continued for 13min, so that the mixture is obtained. And then the mixture is put into a grinder, and ground to the fineness of not more than 25 mu m, thus obtaining the quick-drying waterproof coating.
Example 5: this embodiment differs from embodiment 1 in that: the drier has different raw material components.
Specifically, the drier comprises the following raw material components in parts by weight: 3 parts of 10% cobalt iso-octoate, 3 parts of 12% rare earth iso-octoate, 10 parts of 5% calcium iso-octoate, 14 parts of 6% iron iso-octoate and 13 parts of 9% zinc iso-octoate.
Example 6: this embodiment differs from embodiment 1 in that: the drier has different raw material components.
Specifically, the drier comprises the following raw material components in parts by weight: 2 parts of 10% cobalt iso-octoate, 2 parts of 12% rare earth iso-octoate, 10 parts of 5% calcium iso-octoate, 12 parts of 6% iron iso-octoate and 13 parts of 9% zinc iso-octoate.
Example 7: this embodiment differs from embodiment 1 in that: the drier has different raw material components.
Specifically, the drier comprises the following raw material components in parts by weight: 4 parts of 10% cobalt iso-octoate, 4 parts of 12% rare earth iso-octoate, 12 parts of 5% calcium iso-octoate, 14 parts of 6% iron iso-octoate and 15 parts of 9% zinc iso-octoate.
Comparative example 1: the difference between this comparative example and example 1 is that: in the preparation of the environment-friendly waterproof agent, the modified silica sol is replaced by the commercially available acidic silica sol.
Specifically, the preparation method of the environment-friendly waterproof agent comprises the following steps:
S1, 45g of butyl acrylate, 24g of isooctyl acrylate, 20g of styrene, 1g of vinyl triethoxysilane, 5g of methacryloxyethyl trimethyl ammonium chloride, 60g of 4% polyvinyl alcohol aqueous solution and 10g of 8% acrylamide aqueous solution are put into a homogenizer, and the homogenizer is homogenized for 50min at 5000r/min at normal temperature, and then dispersed for 30min at 50Hz in an ultrasonic manner, so as to obtain the pre-emulsion.
S2, pouring 30mL of the pre-emulsion obtained in the step S1 and commercial acidic silica sol into a three-mouth bottle, and adding 1g of azo diiso Ding Mi hydrochloride and 276g of deionized water to react for 6.5h at 65 ℃ under the protection of nitrogen, thus obtaining the environment-friendly waterproof agent.
Comparative example 2: the difference between this comparative example and example 1 is that: in the preparation of the environment-friendly waterproof agent, modified silica sol is deleted.
Specifically, the preparation method of the environment-friendly waterproof agent comprises the following steps:
S1, 45g of butyl acrylate, 24g of isooctyl acrylate, 20g of styrene, 1g of vinyl triethoxysilane, 5g of methacryloxyethyl trimethyl ammonium chloride, 60g of 4% polyvinyl alcohol aqueous solution and 10g of 8% acrylamide aqueous solution are put into a homogenizer, and the homogenizer is homogenized for 50min at 5000r/min at normal temperature, and then dispersed for 30min at 50Hz in an ultrasonic manner, so as to obtain the pre-emulsion.
S2, pouring 30mL of the pre-emulsion obtained in the step S1 and deionized water into a three-port bottle, adding 1g of azo diiso Ding Mi hydrochloride and 276g of deionized water, and reacting at 65 ℃ for 6.5h under the protection of nitrogen, thus obtaining the environment-friendly waterproof agent.
Comparative example 3: the difference between this comparative example and example 1 is that: in the preparation of the drier, 5% of calcium iso-octoate is replaced by 5% of rare earth iso-octoate; diluting the rare earth isooctanoate with 200# solvent oil to obtain the rare earth isooctanoate with 5% by weight.
Specifically, the drier comprises the following raw material components in parts by weight: 3 parts of 10% cobalt iso-octoate, 3 parts of 12% rare earth iso-octoate, 11 parts of 5% rare earth iso-octoate, 13 parts of 6% iron iso-octoate and 14 parts of 9% zinc iso-octoate.
Comparative example 4: the difference between this comparative example and example 1 is that: in the preparation of the drier, 10% cobalt iso-octoate is deleted.
Specifically, the drier comprises the following raw material components in parts by weight: 3 parts of 12% rare earth isooctanoate, 11 parts of 5% calcium isooctanoate, 13 parts of 6% iron isooctanoate and 14 parts of 9% zinc isooctanoate.
Test example 1: test items: surface drying and real drying.
Test object: examples 1-7 and comparative examples 1-4 were prepared as quick-drying waterproof coatings.
The testing method comprises the following steps: brushing the board, wherein the surface drying is tested by adopting a cotton ball blowing method, namely, lightly placing a cotton ball on the surface of the paint film, and lightly blowing the cotton ball by using a nozzle, if the cotton ball can be blown away, and cotton filaments are not remained on the surface of the paint film, namely, the surface drying is considered; the actual drying is tested by adopting a filter paper pressing method, wherein the filter paper pressing method is to put a piece of filter paper on the surface of a coating film, press a drying tester (200 g weight) for 30s, remove the weight, turn over a test board, and enable the filter paper to fall freely, thus the actual drying is considered; time difference = real dry time period-surface dry time period. Drying environment after brushing the plates: the process is carried out in a constant temperature and humidity box, the constant temperature is 45 ℃, and the constant humidity is 55%.
Test results: see table 2.
Test example 2: test items: water repellency-water contact angle.
Test object: examples 1-7 and comparative examples 1-4 quick-drying waterproof coatings were prepared in test example 1, and the brush plate was tested for a coating after drying.
The test basis is as follows: DB 44/T1232-2013.
Test results: see table 2.
TABLE 2 test results data for test example 1 and test example 2
Conclusion of the test: as can be seen from analysis of examples 1-7 and combination of the data in table 2 and fig. 1-2, the quick-drying waterproof paint prepared by the invention is as low as 4.47 hours when the brush board is used for surface drying in a constant-temperature 45 ℃ and constant-humidity 55% environment, and as low as 6.23 hours when the brush board is used for real drying; the water contact angle of the film after the film is dried is up to 159 degrees, and the waterproof performance is excellent.
As can be seen from analysis of example 1 and comparative examples 1-2 in combination with the data of table 2 and fig. 1-2, the film surface drying and the dry time length of comparative examples 1 and comparative examples 2 remain substantially the same as example 1, indicating that the change in the environment-friendly water repellent does not directly affect the drying speed of the film; the water contact angle of the coating film after the comparative example 1 is dried is 144 degrees, which is obviously lower than that of the coating film of the example 1, the water contact angle of the coating film after the comparative example 2 is dried is 131 degrees, the water contact angle is further reduced, and in the preparation of the environment-friendly waterproof agent, the addition of the acidic silica sol can improve the waterproof performance of the environment-friendly waterproof agent, and the modification of the acidic silica sol can further improve the waterproof performance of the environment-friendly waterproof agent.
As can be seen from analyzing example 1 and comparative example 3 in combination with the data of table 2 and fig. 1-2, the surface dry time length of the coating film of comparative example 3 is substantially consistent with that of example 1, and the time difference between the surface dry time length and the actual dry time length is significantly lower than that of example 1, which means that in the preparation of the drier, 5% calcium iso-octoate is replaced by 5% rare earth iso-octoate, and the surface dry speed is almost not affected, but the actual dry speed can be accelerated, so that the time difference between the surface dry time length and the actual dry time length is shortened; under the condition that the used environment-friendly waterproof agent is unchanged, the water contact angle of the coating film after the comparative example 3 is dried is 136 degrees, which is obviously lower than that of the example 1.
As can be seen from analyzing example 1 and comparative example 4 in combination with the data of table 2 and fig. 1-2, compared with example 1, the surface drying time and the real drying time of the coating film of comparative example 4 are both significantly higher than those of example 1, and the time difference between the surface drying time and the real drying time is significantly lower than that of example 1, which means that in the preparation of the drier, the removal of 10% cobalt iso-octoate results in a decrease in both the surface drying speed and the real drying speed, but the decrease in the surface drying speed is greater, so that the time difference between the surface drying time and the real drying time is shortened; under the condition that the used environment-friendly waterproof agent is unchanged, the water contact angle of a coating film after the comparative example 4 is dried is 130 degrees, which is obviously lower than that of the example 2.
In summary, in the case of using the same type of the environment-friendly waterproofing agent of the present invention, the measured data of the water contact angle of the dried coating film were reduced, regardless of whether the drying speed of the coating film was increased (comparative example 3) or decreased (comparative example 4), indicating that neither a clear positive nor a clear negative correlation was observed between the drying speed of the coating film and the waterproofing performance of the environment-friendly waterproofing agent of the present invention. However, the time difference between the surface dry time and the real dry time of the coating films of comparative example 3 and comparative example 4 was shortened as compared with example 1, and as a result, the measured data of the water contact angles of the real dry coating films of comparative example 3 and comparative example 4 were reduced in the case of using the same type of the environment-friendly waterproof agent of the present invention, indicating that there was a positive correlation between the time difference between the surface dry time and the real dry time of the coating film and the waterproof performance of the environment-friendly waterproof agent of the present invention.
The drier and the environment-friendly waterproof agent are matched for use, so that the prepared quick-drying waterproof coating can be quickly surface-dried and real-dried, and has excellent waterproof performance.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (10)
1. The preparation method of the environment-friendly waterproof agent is characterized by comprising the following steps of:
s1, putting 45g of butyl acrylate, 24g of isooctyl acrylate, 20g of styrene, 1g of vinyl triethoxysilane, 5g of methacryloxyethyl trimethyl ammonium chloride, 60g of 4% polyvinyl alcohol aqueous solution and 10g of 8% acrylamide aqueous solution into a homogenizer for homogenizing, and performing ultrasound to obtain a pre-emulsion;
S2, mixing 3mL of methacryloxypropyl trimethoxysilane, 15mL of deionized water and 8mL of ethanol, stirring and hydrolyzing for 1h at 40 ℃ under the condition of pH=3, adding 30mL of acidic silica sol, and reacting to obtain modified silica sol;
S3, pouring the pre-emulsion obtained in the step S1 and the modified silica sol obtained in the step S2 into a three-mouth bottle, and adding 1g of azo diiso Ding Mi hydrochloride and 276g of deionized water to react for 6.5 hours at 65 ℃ under the protection of nitrogen, thus obtaining the environment-friendly waterproof agent.
2. The method for producing an environmentally friendly water repellent according to claim 1, wherein in S1, a homogenizer performs homogenization at 5000r/min for 45 to 60min at room temperature; 50Hz ultrasonic dispersion is carried out for 30min.
3. The method for producing an environment-friendly waterproof agent according to claim 1, wherein in S2, 1M hydrochloric acid solution is used to adjust ph=3.
4. An environment-friendly waterproof agent, which is prepared by the preparation method according to any one of claims 1 to 3.
5. The environment-friendly waterproof agent according to claim 4, which is used for preparing quick-drying waterproof paint; the quick-drying waterproof coating comprises the following raw material components in parts by weight: 45-55 parts of alkyd resin, 10-15 parts of titanium dioxide, 8-12 parts of talcum powder, 0.8-1 part of drier, 0.5-0.8 part of dispersing agent, 0.1-0.2 part of antiskinning agent, 0.2-0.3 part of environment-friendly waterproof agent and 4-7 parts of solvent.
6. The environment-friendly waterproof agent according to claim 5, wherein the drier comprises the following raw material components in parts by weight: 2-4 parts of 10% cobalt iso-octoate, 2-4 parts of 12% rare earth iso-octoate, 10-12 parts of 5% calcium iso-octoate, 12-14 parts of 6% iron iso-octoate and 13-15 parts of 9% zinc iso-octoate.
7. The environmentally friendly water repellent according to claim 5, wherein the titanium pigment comprises rutile titanium pigment and/or anatase titanium pigment.
8. The environment-friendly waterproof agent according to claim 5, wherein the particle size of the talcum powder is 1000-1500 meshes, and the oil absorption is 30-35 g/100g.
9. The environment-friendly waterproof agent according to claim 5, wherein the solvent comprises xylene and/or 200# solvent oil.
10. The environment-friendly waterproof agent according to claim 5, wherein the preparation method of the quick-drying waterproof paint comprises the following steps: adding alkyd resin into a dispersing machine, controlling the stirring speed at 800-1000rpm/min, then adding titanium white powder, talcum powder, drier, dispersing agent, antiskinning agent, waterproofing agent and solvent, continuously maintaining the stirring speed at 800-1000rpm/min, and stirring for 10-15min to obtain a mixture; and (3) putting the mixture into a grinder, and grinding until the fineness is not more than 25 mu m, thus obtaining the quick-drying waterproof coating.
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| CN102604006A (en) * | 2012-03-09 | 2012-07-25 | 太原理工大学 | Preparation method for acidic silica sol in-situ modified acrylate emulsion |
| CN103554343A (en) * | 2013-09-24 | 2014-02-05 | 江苏荣昌新材料科技有限公司 | Nano SiO2 hybridized acrylic acid ester soap-free emulsion and manufacturing method |
| CN108587424A (en) * | 2018-05-29 | 2018-09-28 | 芜湖市元奎新材料科技有限公司 | Water-proof heat-insulating paint |
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- 2024-05-21 CN CN202410633797.2A patent/CN118359778A/en active Pending
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| CN102604006A (en) * | 2012-03-09 | 2012-07-25 | 太原理工大学 | Preparation method for acidic silica sol in-situ modified acrylate emulsion |
| CN103554343A (en) * | 2013-09-24 | 2014-02-05 | 江苏荣昌新材料科技有限公司 | Nano SiO2 hybridized acrylic acid ester soap-free emulsion and manufacturing method |
| CN108587424A (en) * | 2018-05-29 | 2018-09-28 | 芜湖市元奎新材料科技有限公司 | Water-proof heat-insulating paint |
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